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

Date: 9/1/2011

Subject: FGS Data Review Narrative for Total & Dissolved Mercury – Episode 6564

Frontier Global Sciences (FGS) generated analytical data for total and dissolved mercury. 

The samples were analyzed according to EPA Method 1631E for total mercury by Cold 

Vapor Atomic Fluorescence Spectrometry (CVA-FS) analysis.

Table 1 summarizes the 27 samples (excluding laboratory filter blanks) FGS extracted

and analyzed for total and dissolved mercury. 

Table 1. EPA Episode 6564 Total & Dissolved Mercury – Sample Identification

EPA 

Sample #

Lab Sample 

ID #

Sample 

Matrix Sample Description

Sampling 

Date

Analysis 

Date

71941 1012060-03 Aqueous FGD Influent, Day 1 12/6/2010 1/6/2011

71941 1012060-08 Aqueous Dissolved FGD Influent, Day 1 12/6/2010 12/22/2010

71941 1012060-10 Solid FGD Influent, Day 1 (Solids) 12/6/2010 1/7/2011

71942 1012070-03 Aqueous FGD Influent, Day 2 12/7/2010 1/6/2011

71942 1012070-04 Aqueous Dissolved FGD Influent, Day 2 12/7/2010 1/6/2011

71942 1012070-13 Solid FGD Influent, Day 2 (Solids) 12/7/2010 1/7/2011

71943 1012100-03 Aqueous FGD Influent, Day 3 12/8/2010 1/6/2011

71943 1012100-04 Aqueous Dissolved FGD Influent, Day 3 12/8/2010 12/23/2010

71943 1012100-13 Solid FGD Influent, Day 3 (Solids) 12/8/2010 1/7/2011

71944 1012110-04 Aqueous FGD Influent, Day 4 12/9/2010 1/6/2011

71944 1012110-05 Aqueous Dissolved FGD Influent, Day 4 12/9/2010 12/28/2010

71944 1012110-12 Solid FGD Influent, Day 4 (Solids) 12/9/2010 1/7/2011

71945 1012070-05 Aqueous FGD Effluent, Day 1 12/7/2010 12/22/2010

71945 1012070-06 Aqueous Dissolved FGD Effluent, Day 1 12/6/2010 12/22/2010

71946 1012100-05 Aqueous FGD Effluent, Day 2 12/7/2010 12/23/2010

71946 1012100-06 Aqueous Dissolved FGD Effluent, Day 2 12/7/2010 12/23/2010

71947 1012110-06 Aqueous FGD Effluent, Day 3 12/8/2010 12/28/2010

71947 1012110-07 Aqueous Dissolved FGD Effluent, Day 3 12/8/2010 12/28/2010

71948 1012120-06 Aqueous FGD Effluent, Day 4 12/9/2010 12/28/2010

71948 1012120-07 Aqueous Dissolved FGD Effluent, Day 4 12/9/2010 12/28/2010
2

Table 1. EPA Episode 6564 Total & Dissolved Mercury – Sample Identification

EPA 

Sample #

Lab Sample 

ID #

Sample 

Matrix Sample Description

Sampling 

Date

Analysis 

Date

71949 1012100-07 Aqueous FGD Effluent Duplicate, Day 2 12/7/2010 12/23/2010

71949 1012100-08 Aqueous Dissolved FGD Effluent Duplicate, Day 2 12/7/2010 12/23/2010

71950 1012060-04 Aqueous FGD Influent Field Blank, Day 1 12/6/2010 12/22/2010

71951 1012060-06 Aqueous FGD Effluent Field Blank, Day 1 12/6/2010 12/22/2010

71952 1012070-07 Aqueous FGD Effluent Field Blank, Day 2 12/7/2010 12/22/2010

71953 1012100-11 Aqueous FGD Effluent Field Blank, Day 3 12/8/2010 12/23/2010

71954 1012110-08 Aqueous FGD Effluent Field Blank, Day 4 12/9/2010 12/28/2010

SUMMARY

The samples were prepared according to EPA Method 1631E to be analyzed by CVAFS.

Due to TSS values greater than 1%, samples 71941, 71942, 71943, and 71944 were phase 

separated. 

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 instrument and preparation blanks met method specified criteria. Preparation Blanks 

F012184-BLK1, F012184-BLK5, F012215-BLK5, F012215–BLK6, F012243–BLK6, 

F101058–BLK1, F101058–BLK4, and F101058-BLK5 had mercury levels of 0.13, 0.19, 

0.08, 0.09, 0.15, 0.15, 0.08, and 0.20 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.
3

DUPLICATES

A field duplicate, Sample 71949 was collected on the Sample 71946. The total mercury 

relative percent difference (RPD) was 42% and the dissolved mercury RPD was 9.4%.

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

Laboratory duplicates were performed on samples 71941, 71941 (solid), 71942, and 

71947. All RPDs were less than 20% (the method-suggested RPD criterion between field 

duplicates; the method does not require the analysis of laboratory duplicates), except for 

sample 71947, which had an RPD of 79.7%. Because the method does not require the 

analysis of laboratory duplicates, this result was not qualified.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

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

71941, 71941 (solid), 71942, and 71947 for the total mercury analyses. MS and MSDs 

were performed on sample 71947 for the dissolved mercury analyses. All aqueous 

MS/MSD recoveries were within method specifications of 70-125%. All RPDs met 

method-specified criteria.

Two sets of MS/MSD were performed on the solid sample 71941 from this episode.

MS/MSD1 did not meet method-specified criteria for recovery or RPD. The laboratory 

does state that the sample concentration was more than two times the spike amount. 

MS/MSD2 did meet method-specified criteria for recovery and RPD. 
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 6564

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

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

Sample Episode 6564. 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

71941 FGD Influent, Day 1 280-10453-1 Aqueous 12/06/2010 12/07/2010

71941 FGD Influent, Day 1 – Solid 280-10453-3 Solid 12/06/2010 12/07/2010

71941 FGD Influent, Day 1 – Filtrate 280-10453-4 Aqueous 12/06/2010 12/07/2010

71942 FGD Influent, Day 2 280-10513-1 Aqueous 12/07/2010 12/08/2010

71942 FGD Influent, Day 2 – Solid 280-10513-4 Solid 12/07/2010 12/08/2010

71942 FGD Influent, Day 2 – Filtrate 280-10513-5 Aqueous 12/07/2010 12/08/2010

71943 FGD Influent, Day 3 280-10583-1 Aqueous 12/08/2010 12/09/2010

71943 FGD Influent, Day 3 – Solid 280-10583-3 Solid 12/08/2010 12/09/2010

71943 FGD Influent, Day 3 – Filtrate 280-10583-4 Aqueous 12/08/2010 12/09/2010

71944 FGD Influent, Day 4 280-10656-1 Aqueous 12/09/2010 12/10/2010

71944 FGD Influent, Day 4 - Solid 280-10656-4 Solid 12/09/2010 12/10/2010

71944 FGD Influent, Day 4 - Filtrate 280-10656-5 Aqueous 12/09/2010 12/10/2010

71945 FGD Effluent, Day 1 280-10513-2 Aqueous 12/07/2010 12/08/2010

71946 FGD Effluent, Day 2 280-10583-2 Aqueous 12/08/2010 12/09/2010

71947 FGD Effluent, Day 3 280-10656-2 Aqueous 12/09/2010 12/10/2010

71948 FGD Effluent, Day 4 280-10724-1 Aqueous 12/10/2010 12/11/2010

71950 FGD Influent Field Blank, Day 1 280-10453-2 Aqueous 12/06/2010 12/07/2010
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

71951 FGD Effluent Filed Blank, Day 1 280-10513-3 Aqueous 12/07/2010 12/08/2010

71955 FGD Effluent – Duplicate 280-10656-3 Aqueous 12/09/2010 12/10/2010

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 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 matrix spike (MS) and matrix spike duplicate (MSD) recoveries that failed 

the EPA Method 200.8 control limits of 70–130% are as follows: total and 

dissolved silver (71945 MS/MSD); and total and dissolved silver (71948

MS/MSD).

• The MS/MSD relative percent difference (RPD) for dissolved silver for samples 

71945 and 71948 failed TestAmerica’s SOP control limits of ±20%.

• The MS/MSD RPD for total silver for sample 71945 failed TestAmerica’s SOP 

control limits of ±20%.

• The post digestion spikes (PDS) for total and dissolved silver for sample 71945 

failed the method criteria of 85–115%.

• The PDS for silver in the filtrate phase for sample 71944 failed the method 

criteria of 85–115%.

• The PDS for silver in the solid phase for sample 71944 failed the method criteria 

of 85–115%.

• The PDS for total cadmium and total nickel in the aqueous sample for sample 

71944 failed the method criteria of 85–115%.

INTERNAL STANDARDIZATION

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

INITIAL CALIBRATION

TestAmerica performed the initial calibrations on each analysis 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 TestAmerica’s SOP control limits of 50–150%.

LABORATORY CONTROL SAMPLES (LCS)

All LCS samples passed the method QC 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 71945 FGD Effluent, 

Day 1 (280-10513-2) met Test America’s requirement of ±10% difference.
4

FIELD DUPLICATES

The RPD of the field duplicates 71947/71955 for total and dissolved results 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 samples 71945 FGD Effluent, Day 1 and 71948 FGD 

Effluent, Day 4 for total and dissolved analytes. The total and dissolved selenium results 

in the MS and MSD samples for samples 71945 and 71948 failed the 70–130% method 

control limits and were flagged with a “4” qualifier indicating concentrations in the 

parent samples were greater than four times the spike amounts. Otherwise, the MS/MSD 

spike recoveries were always within the control limits of 70-130% with the exception of 

total and dissolved silver for the MS and MSD samples for both 71945 and 71948, which 

were flagged with an “F” qualifier. The RPD for all MS/MSD samples passed the 

method-specified criteria of ±20%, except for dissolved silver for samples 71945 and 

71948 and total silver for 71945. 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.

POST DIGESITON SPIKES

PDSs were performed on sample 71945 FGD Effluent, Day 1 (280-10513-2 PDS) and the 

solid and aqueous sample of 71944 FGD Influent, Day 4 (280-10656-4 PDS; 280-10656-

5 PDS respectively). Total and dissolved silver failed TestAmerica’s aqueous control 

limits of 85–115% for sample 71945, total silver failed the filtrate of sample 71944, and 

total silver failed the solid control limits of 75–115% for sample 71944. All failures were

all 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. The 

aqueous sample 71944 also failed TestAmerica’s 85-115% control limits for total 

cadmium and total nickel, which were flagged “W”.

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 6564

TestAmerica 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 TestAmerica extracted and analyzed for total and 

dissolved metals by EPA Method 200.7.

Table 1. EPA Episode 6564 Total & Dissolved Metals – Sample Identification

EPA 

Sample 

# EPA Sample Description

Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71941 FGD Influent, Day 1 280-10453-1 Aqueous 12/06/2010 12/07/2010

71941 FGD Influent, Day 1 – Solid 280-10453-3 Solid 12/06/2010 12/07/2010

71941 FGD Influent, Day 1 - Filtrate 280-10453-4 Aqueous 12/06/2010 12/07/2010

71942 FGD Influent, Day 2 280-10513-1 Aqueous 12/07/2010 12/08/2010

71942 FGD Influent, Day 2 – Solid 280-10513-4 Solid 12/07/2010 12/08/2010

71942 FGD Influent, Day 2 – Filtrate 280-10513-5 Aqueous 12/07/2010 12/08/2010

71943 FGD Influent, Day 3 280-10583-1 Aqueous 12/08/2010 12/09/2010

71943 FGD Influent, Day 3 – Solid 280-10583-3 Solid 12/08/2010 12/09/2010

71943 FGD Influent, Day 3 – Filtrate 280-10583-4 Aqueous 12/08/2010 12/09/2010

71944 FGD Influent, Day 4 280-10656-1 Aqueous 12/09/2010 12/10/2010

71944 FGD Influent, Day 4 – Solid 280-10656-4 Solid 12/09/2010 12/10/2010

71944 FGD Influent, Day 4 - Filtrate 280-10656-5 Aqueous 12/09/2010 12/10/2010

71945 FGD Effluent, Day 1 280-10513-2 Aqueous 12/07/2010 12/08/2010

71946 FGD Effluent, Day 2 280-10583-2 Aqueous 12/08/2010 12/09/2010

71947 FGD Effluent, Day 3 280-10656-2 Aqueous 12/09/2010 12/10/2010

71948 FGD Effluent, Day 4 280-10724-1 Aqueous 12/10/2010 12/11/2010

71950 FGD Influent Field Blank, Day 1 280-10453-2 Aqueous 12/06/2010 12/07/2010
2

Table 1. EPA Episode 6564 Total & Dissolved Metals – Sample Identification

EPA 

Sample 

# EPA Sample Description

Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71951 FGD Effluent Filed Blank, Day 1 280-10513-3 Aqueous 12/07/2010 12/08/2010

71955 FGD Effluent – Duplicate 280-10656-3 Aqueous 12/09/2010 12/10/2010

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. Any significant 

findings are summarized below. No additional data qualifiers were required.

• The serial dilution analysis for dissolved manganese, dissolved molybdenum, and 

dissolved sodium for sample 71945 did not meet TestAmerica’s requirement of 

±10% difference.

• The serial dilution analysis for barium, cobalt, magnesium, manganese, titanium, 

and zinc in the solid phase of sample 71944 did not meet TestAmerica’s 

requirement of ±10% difference.

• The matrix spike (MS) and matrix spike duplicate (MSD) recoveries that failed 

the EPA Method 200.7 control limits of 70–130% are as follows: dissolved 

barium (71945 MS/MSD); dissolved barium (71948 MS/MSD); and total iron 

(71945 MSD).

• The MS/MSD relative percent difference (RPD) for dissolved barium for samples 

71945 and 71948 failed TestAmerica’s SOP control limits of ±20%.

• The post digestion spikes (PDS) for total barium for sample 71945 failed the 

method criteria of 85–115%.

• The PDS for magnesium and tin in the solid phase for sample 71944 failed the 

method criteria of 85–115%.

• The PDS for titanium and zinc in the filtrate phase for sample 71944 failed the 

method criteria of 85–115%.

SAMPLE RECEIPT, HANDLING, AND STORAGE

There were no issues associated with receipt, handling and storage.
3

INTERNAL STANDARDIZATION

While the internal standard (ISTD) Yttrium was used for these analyses, no checks on the 

ISTD recoveries in 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.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

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

LABORATORY CONTROL SAMPLES (LCS)

All LCS 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 (SRD)

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

dilution results for dissolved manganese, dissolved molybdenum and dissolved sodium 

for sample 71945 FGD Effluent, Day 1 (280-10513-2) had percent differences of 25%, 

22% and 20% respectively, which were appropriately flagged. The serial dilution results 

for total barium, total cobalt, total magnesium, total manganese, total titanium and total 

zinc of the solid fraction for sample 71944 FGD Influent, Day 4 (280-10656-4) had 
4

percent differences of 41%, 53%, 51%, 50%, 44% and 43% respectively, which were also 

appropriately flagged. No additional qualifiers were required.

FIELD DUPLICATES

The total and dissolved RPDs of the field duplicate (71955) to parent sample (71947) 

were less than 20% for values greater than the reporting limit.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

MS and MSD were performed on the total and dissolved samples of 71945 FGD Effluent, 

Day1 (280-10513-2) and 71948 FGD Effluent, Day 4 (280-10724-1). 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. Otherwise, the MS/MSD spike recoveries were always within the control 

limits of 70-130% with the exception of dissolved barium for both the MS and MSD for 

samples 71945 and 71948 and the total iron MSD for sample 71945. All relative percent 

differences (RPDs) were within ± 20% with the exception of dissolved barium for both 

samples 71945 and 71948. No additional data qualifiers were needed.

POST DIGESTION SPIKE

The PDS of sample 71945 FGD Effluent, Day 1 (280-10513-2 PDS) failed the method 

criteria of 85–115% for total barium, which was flagged. The solid fraction PDS of 

sample 71944 FGD Influent, Day 4 (280-10656-4 PDS) failed for magnesium and tin, 

which were flagged. The filtrate fraction PDS of sample 71944 FGD Influent, Day 5 

(280-10656-5 PDS) failed for titanium and zinc, which were flagged. No additional 

qualifiers were required.

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 

6564

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

chromium for Sample Episode 6564. The samples were analyzed 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 prepared and analyzed for dissolved hexavalent 

chromium.

Table 1. EPA Episode 6564 Dissolved Hexavalent Chromium – Sample 

Identification

EPA 

Sample #

Sample 

Matrix Sample Description

Sampling 

Date

Analysis 

Date

71941 Aqueous FGD Influent Day 1 12/6/10 12/29/10

71943 Aqueous FGD Influent Day 3 12/8/10 12/29/10

71944 Aqueous FGD Influent Day 4 12/9/10 12/29/10

71945 Aqueous FGD Effluent Day 1 12/7/10 12/29/10

71946 Aqueous FGD Effluent Day 2 12/8/10 12/29/10

71947 Aqueous FGD Effluent Day 3 12/9/10 12/29/10

71950 Aqueous FGD Influent Field Blank Day 1 12/6/10 12/29/10

71951 Aqueous FGD Effluent Field Blank Day 1 12/7/10 12/29/10

71955 Aqueous FGD Effluent Dup Day 3 12/9/10 12/29/10

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.

Samples 71941, 71943, and 71944 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.
2

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES

The collection date and time were not recorded on the chain of custody for samples 

71945 and 71951.

INITIAL PRECISION AND ACCURACY/RECOVERY

The initial precision and recovery (IPR) performed by FGS had recoveries within the 

method criteria.

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 analytical 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 96% and 95%. 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.
3

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 71955, was a duplicate of 

effluent sample 71947, with an RPD of 8%. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

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

spike on sample 71948. Two set of MS/MSD were performed at two different 

concentration levels. The MS/MSD1 (spiked at 50 ug/L) recoveries were within criteria, 

92.5% and 91.0%, with an RPD of 1.59%. The MS/MSD2 (spiked at 250 ug/L) 

recoveries were within criteria, 96.2% and 96.8%, with an RPD of 0.56%.
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 6564

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for Sample Episode 6564. 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 (total) by SM 4500 CN- E, 

• Nitrate/Nitrite by EPA method 353.2

• Phosphorus (total) by EPA method 365.1, 

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

• Total Kjeldakl 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 6564 Classical Analytes – Sample Identification

EPA

Sample #

Sample 

Description

Sampling

Date

Sample

Matrix

Portion of 

Sample

Analytes 

71941 FGD Influent, 

Day 1 12/06/10

Water Entire 

Fraction

BOD5, COD, TDS, and 

TSS

Water Filtrate

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

71942 FGD Influent, 

Day 2 12/07/10

Water Entire 

Fraction

BOD5, COD, TDS, and 

TSS

Water Filtrate

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

71943 FGD Influent, 

Day 3 12/08/10

Water Entire 

Fraction

BOD5, COD, TDS, and 

TSS

Water Filtrate

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

71944 FGD Influent, 

Day 4 12/09/10

Water Entire 

Fraction

BOD5, COD, TDS, and 

TSS

Water Filtrate

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite,

Phosphorus, Sulfate, and 

TKN

71945 FGD Effluent, 

Day 1 12/07/10 Water Entire Fraction All analytes
3

EPA

Sample #

Sample 

Description

Sampling

Date

Sample

Matrix

Portion of 

Sample

Analytes 

71946 FGD Effluent, 

Day 2 12/08/10 Water Entire Fraction All analytes

71947 FGD Effluent, 

Day 3 12/09/10 Water Entire Fraction All analytes

71948 FGD Effluent, 

Day 4 12/10/10 Water Entire Fraction All analytes

71955 FGD Effluent -

Duplicate 12/09/10 Water Entire Fraction All analytes

SUMMARY

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

unless otherwise noted below.

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 specified 

below.

If required by the method, a matrix spike (MS) analysis was run on sample 71948 (FGD 

effluent) for each analyte to check for matrix interferences. For some analytes, 

TestAmerica spiked more than one sample. All MS samples analyzed met the criteria 

specified in the method unless described below. 
4

DATA NOTES/ISSUES

Ammonia

As stated above, filtrate and solid aliquots of samples 71941 - 71944 were not preserved 

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

phase separation. The filtrate volume of samples 71941 - 71944 were already qualified by 

TestAmerica 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 these samples. The solid aliquot 

of samples 71941 - 71944 were qualified as estimated values because the samples were 

not preserved immediately following sample collection.

The filtrate and solid aliquots of samples 71941, 71942, 71943, and 71944 were analyzed 

9, 8, 7, and 6 days, respectively, after the 28-day hold time. These samples were already 

qualified as estimated values either because their result was less than the RL or because 

they were not preserved immediately following sample collection, so no further action 

was necessary.

Ammonia was detected at 0.0610 mg/L in the LRB associated with samples 71945 and 

71946. The blank result was above the MDL (0.055 mg/L), but below the RL (1.0 mg/L), 

so these samples were not qualified based on this LRB result.

BOD5

TestAmerica analyzed five dilutions, but no dilutions had a dissolved oxygen (DO) 

depletion greater than 2.0 mg/L for sample 71945. Therefore, BOD5 was reported as not 

detected for this sample. The rest of the samples had at least one dilution with a DO 

depletion greater than 2.0 mg/L. As required in the method, the final result was calculated 

by taking the average of the results for all dilutions with a DO depletion greater than 2.0 

mg/L and a final DO greater than 1.0 mg/L. 

BOD was not detected above the RL in any method blanks. However, for batch 44128, 

the results for the three water/unseeded blanks were 0.23 mg/L, 0.21 mg/L, and 0.19 

mg/L. Two of these water blanks were above the method control criteria of 0.20 mg/L.

Because of these blank results, sample 71941 was qualified with a “B” meaning the 

analyte was detected in the sample and the blank. 

The glucose-glutamic acid (GGA) standards associated with sample 71948 had percent 

recoveries of 84% and 86%. The percent recovery of the first GGA standard was below

the method and laboratory criteria of 85-115%. TestAmerica flagged sample 71948 with 

a “*” meaning the laboratory control sample was not within laboratory control limits. 

Sample 71948 was additionally qualified as a minimum value.
5

Chloride and Sulfate

Solid aliquots of samples 71941, 71942, 71943, and 71944 were analyzed 9, 8, 7, and 6 

days, respectively, after the 28-day hold time. Additionally, filtrate aliquots of samples 

71941, 71942, 71943, and 71944 were analyzed 8, 7, 6, and 5 days, respectively, outside 

of the 28-day hold time. These samples were qualified as estimated values.

The laboratory diluted the MS and MSD samples for 71941 and 71948 by 200, but the 

diluted results for sulfate and chloride were still above the highest calibration standard. 

The laboratory did not reanalyze these samples with a higher dilution factor, because the 

MS and MSD percent recoveries were within the control limits specified by EPA method 

300.0. Therefore, if the MS and MSD results for sample 71941 for chloride and sulfate 

are reported, they will be qualified as estimated values. The results for samples 71941 

and 71948 were within the calibration range, so there was no need to qualify these 

samples. The LFB associated with sample 71941 and 71948 met the method criteria.

COD

Samples 71941, 71943, and 71944 were preserved to pH less than 2 S.U. after sample 

collection. However, when the laboratory received the samples, the pH was neutral. The 

samples were preserved again by the laboratory. These samples were qualified as 

estimated values.

The percent recoveries for the MS and MSD samples associated with 71948 were 93% 

and 79%, respectively. Only the MS sample was within the control limits of 90 - 110%

specified in the method. However, since the method does not require an MSD analysis,

sample 71948 was not qualified because of the low MSD percent recovery. Also, the MS

and MSD results associated with sample 71948 were above 150 mg/L. COD is calculated 

using a reverse curve meaning that the 200 mg/L calibration point represents the zero in 

the curve and the 0 mg/L calibration point represents the highest absorbance. 

TestAmerica has noticed that results in the 150-200 mg/L range yield inconsistent results, 

so typically the lab dilutes these samples and reanalyzes. The MS and MSD samples 

associated with 71948 were not diluted further and reanalyzed, so TestAmerica flagged 

them with an “E” meaning that the results exceeded the calibration range. If reported, the 

MS and MSD results for sample 71948 will be qualified as estimated values. 

The percent recoveries for the MS and MSD samples associated with 71941 were 68% 

and 71%, respectively. Both the MS and MSD sample results for this sample were not 

within the control limits specified in the method. Sample 71941 was already qualified as 

an estimated value because the sample was not preserved appropriately, so there was no 

need to further qualify the sample as a minimum value. The LFB associated with sample 

71941 and 71948 met the method criteria. 
6

Cyanide 

As stated above, filtrate and solid aliquots of samples 71941-71944 were not preserved 

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

phase separation. Filtrate aliquots of samples 71941 and 71944 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 there was no need to further qualify these samples. Because the 

filtrate aliquots of samples 71942 and 71943 and the solid aliquots of samples 71941 -

71944 were not preserved immediately following sample collection as required by the 

method, these samples were qualified as estimated values.

Solid and filtrate aliquots of samples 71941, 71942, 71943, and 71944 were analyzed 25, 

24, 23, and 22 days, respectively, outside of the 14-day holding time. These samples were 

already qualified as estimated values because they were not preserved immediately

following sample collection as required by the method, so no further qualification was 

necessary.

All aqueous 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 diluted results for

the filtrate aliquot of samples 71941 and 71944 were less than 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 

there was no need to further qualify these samples.

The percent recoveries for the MS and MSD samples associated with sample 71948 were 

79% and 78%, respectively. These percent recoveries were not within the laboratory 

control criteria of 90-110%. Additionally, the percent recoveries for the MS and MSD 

samples associated with sample 71955 were 67% and 69%, respectively. These percent 

recoveries were also not within the laboratory control criteria. Since there are no MS or 

MSD criteria specified in SM 4500 CN- E, samples 71948 and 71955 were not qualified 

based on the low MS and MSD percent recoveries. The LFBs associated with samples 

71948 and 71955 met the method criteria.

The RPD between sample 71947 and its field duplicate 71955 for cyanide was 46.2%. 

Even though the RPD was greater than 20%, the sample was not qualified because there 

are no control limits for field duplicates specified in SM 4500 CN- E. 

Nitrate/Nitrite

As stated above, filtrate and solid aliquots of samples 71941 - 71944 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 as required by the method, these samples were qualified as estimated 

values.
7

The filtrate and solid aliquots of samples 71941, 71942, 71943, and 71944 were analyzed 

11, 10, 9, and 8 days, respectively, outside of the 28-day hold time. These samples were 

already qualified as estimated values because they were not preserved immediately 

following sample collection, so no further action was necessary.

TestAmerica diluted the MS and MSD samples for 71948 by 20 fold, but the analyzed 

result was still above the highest calibration standard. The samples were not diluted and 

reanalyzed because the percent recoveries were within the control limits specified in the 

method. If the MS and MSD results are reported, they will be qualified as estimated 

values. The result for sample 71948 was within the calibration range, so there was no 

need to qualify this sample. The LFB associated with sample 71948 met the method 

criteria. 

Phosphorus 

As stated above, filtrate and solid aliquots of samples 71941 - 71944 were not preserved 

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

phase separation. The solid aliquot of sample 71944 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 this sample. Phosphorus was not 

detected in the solid aliquot for sample 71941, so there was no need to further qualify this 

sample. Solid samples 71942 and 71943 and filtrate samples 71941 - 71944 were 

qualified as estimated values because they were not preserved immediately following 

sample collection as required by the method.

Filtrate and solid aliquots of samples 71941, 71942, 71943, and 71944 were analyzed 10, 

9, 8, and 7 days, respectively, past the 28-day hold time. These samples were not 

detected, already qualified with a “J”, or qualified as estimated values because they were 

not preserved immediately following sample collection, so no further action was 

necessary.

Phosphorus was detected at 0.0114 mg/L in the LRB associated with the filtrate aliquot

of samples 71941 - 71944. Phosphorus was also detected at 0.0103 mg/L in the LRB

associated with sample 71948. Additionally, phosphorus was detected at 0.0103 mg/L in 

the LRB associated with samples 71945, 71946, 71947, and 71955. Since all of these 

blank results were less than the RL (0.050 mg/L), no samples were qualified based on 

these LRB results.

The percent recoveries for the MS and MSD analyses for sample 71948 were not within 

the method control limits of 90-110% or within the laboratory control limits of 71-128%. 

The percent recoveries for the MS and MSD samples were 28% and 24%, respectively.

Sample 71948 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 this sample as a minimum value. The LFB associated with sample 71948 

met the method criteria.
8

TDS

One laboratory duplicate was analyzed on sample 71948. The RPD between this sample 

and its laboratory duplicate was 14%. This RPD was not less than 10% as required by the 

method, so sample 71948 was qualified as an estimated value.

Samples 71941, 71942, 71943, 71945, 71946, 71947, 71948, and 71955 did not achieve a 

constant weight after three drying cycles. The weight increased from the first weighing to 

the second weighing for sample 71948. 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 may be the cause for the inconsistent weight calculations. These 

samples were not qualified, but results may be biased high.

The RPD between sample 71947 and its field duplicate 71955 for TDS was 24%. Even 

though the RPD was greater than 20%, the sample was not qualified because there are no 

control limits for field duplicates specified in SM 2540C. 

TKN

As stated above, filtrate and solid aliquots of samples 71941 - 71944 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 as required by the method, these samples were qualified as estimated 

values.

Filtrate and solid aliquots of samples 71941, 71942, 71943, and 71944 were analyzed 10, 

9, 8, and 7 days, respectively, past the 28-day hold time. These samples were already 

qualified as estimated values because they were not preserved immediately following 

sample collection, so no further action was necessary. 

TKN was detected at 0.264 mg/L in the laboratory reagent blank associated with the 

filtrate aliquot of samples 71941 - 71944. Because this blank result was less than the RL

(1.0 mg/L), no samples were qualified based on this LRB result.

TestAmerica preformed MS and MSD analysis on sample 71948. The percent recoveries

for the MS and MSD samples were 77% and 76%. The samples did not meet the method 

control limits of 90-110%, but did meet the laboratory control limits of 54-131%. 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 71948 was not qualified because it is not possible to 

determine if the MS and MSD failures were a result of matrix interferences or the low 

spiking level. The LFB associated with sample 71948 met the method criteria.
9

TSS 

Two laboratory duplicates were analyzed for TSS. The RPD for sample 71941 and its 

duplicate was less than 10% as required by the method; however, the RPD for sample 

71948 and its duplicate was 50%. The result for 71948 was at the RL (4.0 mg/L) and the 

result for the laboratory duplicate was 2.40 mg/L, which was less than the RL. The low 

concentration of TSS was likely the cause for the high RPD value. Sample 71948 was 

qualified as an estimated value.
10

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71941 (solid) Ammonia H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 9 

days past holding 

time.

15 mg/Kg

71942 (solid) Ammonia H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 8 

days past holding 

time.

12 mg/Kg

71943 (solid) Ammonia H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 7 

days past holding 

time.

11 mg/Kg

71944 (solid) Ammonia H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 6 

days past holding 

time.

15 mg/Kg

71941 BOD B Unseeded water blank 

> method-specified 

criteria

3.0 mg/L

71948 BOD Minimum Value GGA % recovery 

below methodspecified criteria

2.6 mg/L

71941 (solid) Chloride H, Estimated

Value

Analyzed 9 days past 

holding time.

1,500 

mg/Kg

71942 (solid) Chloride H, Estimated

Value

Analyzed 8 days past 

holding time.

3,000 

mg/Kg

71943 (solid) Chloride H, Estimated

Value

Analyzed 7 days past 

holding time.

1,900 

mg/Kg

71944 (solid) Chloride H, Estimated

Value

Analyzed 6 days past 

holding time.

2,200 

mg/Kg

71941 (filtrate) Chloride H, Estimated

Value

Analyzed 8 days past 

holding time.

6,100 mg/L

71942 (filtrate) Chloride H, Estimated

Value

Analyzed 7 days past 

holding time.

9,400 mg/L

71943 (filtrate) Chloride H, Estimated

Value

Analyzed 6 days past 

holding time.

8,700 mg/L
11

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71944 (filtrate) Chloride H, Estimated

Value

Analyzed 5 days past 

holding time.

6,800 mg/L

71941 (solid) Sulfate H, Estimated

Value

Analyzed 9 days past 

holding time.

27,000 

mg/Kg

71942 (solid) Sulfate H, Estimated

Value

Analyzed 8 days past 

holding time.

29,000 

mg/Kg

71943 (solid) Sulfate H, Estimated

Value

Analyzed 7 days past 

holding time.

24,000 

mg/Kg

71944 (solid) Sulfate H, Estimated

Value

Analyzed 6 days past 

holding time.

27,000 

mg/Kg

71941 (filtrate) Sulfate H, Estimated

Value

Analyzed 8 days past 

holding time.

9,700 mg/L

71942 (filtrate) Sulfate H, Estimated

Value

Analyzed 7 days past 

holding time.

11,000 

mg/L

71943 (filtrate) Sulfate H, Estimated

Value

Analyzed 6 days past 

holding time.

9,300 mg/L

71944 (filtrate) Sulfate H, Estimated

Value

Analyzed 5 days past 

holding time.

9,800 mg/L

71941 COD Estimated Value pH upon receipt > 2

S.U., MS % recovery 

below methodspecified criteria 

250 mg/L

71943 COD Estimated Value pH upon receipt > 2

S.U.

350 mg/L

71944 COD Estimated Value pH upon receipt > 2

S.U.

280 mg/L

71942 (filtrate) Cyanide H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 

24 days past holding 

time.

0.19 mg/L

71943 (filtrate) Cyanide H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 

23 days past holding 

time.

0.16 mg/L

71941 (solid) Cyanide H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 

25 days past holding 

time.

0.54 

mg/Kg
12

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71942 (solid) Cyanide H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 

24 days past holding 

time.

0.69 

mg/Kg

71943 (solid) Cyanide H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 

23 days past holding 

time.

0.73 

mg/Kg

71944 (solid) Cyanide H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 

22 days past holding 

time.

0.96 

mg/Kg

71941 (solid) Nitrate/Nitrite H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 

11 days past holding 

time.

34 mg/Kg

71942 (solid) Nitrate/Nitrite H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 

10 days past holding 

time.

69 mg/Kg

71943 (solid) Nitrate/Nitrite H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 9

days past holding 

time.

39 mg/Kg

71944 (solid) Nitrate/Nitrite H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 8

days past holding 

time.

49 mg/Kg

71941 (filtrate) Nitrate/Nitrite H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 

11 days past holding 

time.

140 mg/L
13

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71942 (filtrate) Nitrate/Nitrite H, Estimated 

Value

Sample not preserved

immediately following 

collection. Analyzed 

10 days past holding 

time.

230 mg/L

71943 (filtrate) Nitrate/Nitrite H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 9

days past holding 

time.

170 mg/L

71944 (filtrate) Nitrate/Nitrite H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 8

days past holding 

time.

140 mg/L

71942 (solid) Phosphorus H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 9

days past holding

time.

250 mg/Kg

71943 (solid) Phosphorus H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 8

days past holding 

time.

190 mg/Kg

71941 (filtrate) Phosphorus H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 

10 days past holding 

time.

0.12 mg/L

71942 (filtrate) Phosphorus H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 9

days past holding 

time.

0.14 mg/L

71943 (filtrate) Phosphorus H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 8

days past holding 

time.

0.13 mg/L
14

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71944 (filtrate) Phosphorus H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 7

days past holding 

time.

0.11 mg/L

71948 TDS Estimated Value Laboratory duplicate 

RPD > methodspecified criteria

15,000 

mg/L

71941 (solid) TKN H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 

10 days past holding 

time.

560 mg/Kg

71942 (solid) TKN H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 9

days past holding 

time.

500 mg/Kg

71943 (solid) TKN H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 8

days past holding 

time.

83 mg/Kg

71944 (solid) TKN H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 7

days past holding 

time.

620 mg/Kg

71941 (filtrate) TKN H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 

10 days past holding 

time.

14 mg/L

71942 (filtrate) TKN H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 9

days past holding 

time.

25 mg/L
15

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71943 (filtrate) TKN H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 8

days past holding 

time.

36 mg/L

71944 (filtrate) TKN H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 7

days past holding 

time.

14 mg/L

71948 TSS Estimated Value Laboratory duplicate 

RPD > methodspecified criteria

4.0 mg/L