Appendix B

DATA REVIEW NARRATIVES
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD

Deb Bartram, ERG

TJ Finseth, ERG

From: Randy Mercurio, ERG

Donna Tedder, ERG

Date: 9/1/2011

Subject: FGS Data Review Narrative for Total and Dissolved Mercury – Episode 6560

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 27 samples (excluding laboratory filter blanks) FGS extracted 

and analyzed for total and dissolved mercury.

Table 1. EPA Episode 6560 Total & Dissolved Mercury – Sample Identification

EPA 

Sample #

Lab Sample 

ID #

Sample 

Matrix Sample Description

Sampling 

Date

71741 1007078-01 Aqueous FGD Influent Day 1 7/12/2010

71741 1007078-08 Solid FGD Influent, Day 1 (Solids) 7/12/2010

71741 1007078-06 Aqueous Dissolved FGD Influent, Day 1 7/12/2010

71742 1007095-01 Aqueous FGD Influent, Day 2 7/13/2010

71742 1007095-11 Solid FGD Influent, Day 2 (Solids) 7/13/2010

71742 1007095-02 Aqueous Dissolved FGD Influent, Day 2 7/13/2010

71743 1007105-04 Aqueous FGD Influent, Day 3 7/14/2010

71743 1007105-11 Solid FGD Influent, Day 3 (Solids) 7/14/2010

71743 1007105-05 Aqueous Dissolved FGD Influent, Day 3 7/14/2010

71744 1007121-01 Aqueous FGD Influent, Day 4 7/15/2010

71744 1007121-09 Solid FGD Influent, Day 4 (Solids) 7/15/2010

71744 1007121-02 Aqueous Dissolved FGD Influent, Day 4 7/15/2010

71745 1007095-03 Aqueous FGD Effluent, Day 1 7/13/2010

71745 1007095-04 Aqueous Dissolved FGD Effluent, Day 1 7/13/2010

71746 1007105-06 Aqueous FGD Effluent, Day 2 7/14/2010

71746 1007105-07 Aqueous Dissolved FGD Effluent, Day 2 7/14/2010

71747 1007121-03 Aqueous FGD Effluent, Day 3 7/15/2010

71747 1007121-04 Aqueous Dissolved FGD Effluent, Day 3 7/15/2010

71748 1007131-02 Aqueous FGD Effluent, Day 4 7/16/2010
2

Table 1. EPA Episode 6560 Total & Dissolved Mercury – Sample Identification

EPA 

Sample #

Lab Sample 

ID #

Sample 

Matrix Sample Description

Sampling 

Date

71748 1007131-03 Aqueous Dissolved FGD Effluent, Day 4 7/16/2010

71749 1007105-08 Aqueous FGD Effluent Duplicate, Day 2 7/14/2010

71749 1007105-09 Aqueous Dissolved FGD Effluent Duplicate, Day 2 7/14/2010

71750 1007078-02 Aqueous FGD Influent Field Blank, Day 1 7/12/2010

71751 1007078-04 Aqueous FGD Effluent Field Blank Day 1 7/12/2010

71752 1007095-05 Aqueous FGD Effluent Field Blank, Day 2 7/13/2010

71753 1007105-03 Aqueous FGD Effluent Field Blank, Day 3 7/14/2010

71754 1007121-05 Aqueous FGD Effluent Field Blank, Day 4 7/15/2010

SUMMARY

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

There were no issues requiring qualifiers with the mercury data in this episode. ERG 

noted the following during the data review:

• An ongoing precision and recovery (OPR) sample was not analyzed at the 

beginning and end of the solid fraction sample analysis.

• A matrix spike (MS) and matrix spike duplicate (MSD) were not performed on a

solid sample fraction from this episode.

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

blanks (CCBs) met method-specified criteria. 
3

DUPLICATES

Field duplicates, sample 71749, were collected on sample 71746. The 71746/71749 total 

mercury relative percent difference (RPD) was 9.72% and the dissolved mercury RPD

was 5.20%. The method-suggested RPD criterion between field duplicates is 20%.

Laboratory duplicates were performed on samples 71742, 71747, and 71748. All RPDs 

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

method does not require the analysis of laboratory duplicates).

A laboratory duplicate was not performed on the solid sample fraction from this episode; 

however, FGS analyzed another client’s sample as the duplicate for this batch, which 

passed the method-specified criteria.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

MS and MSDs were performed on samples 71742, 71743, 71747, and 71748 for the total 

mercury analyses. MS and MSDs were performed on samples 71742 and 71747 for the 

dissolved mercury analyses. All aqueous MS/MSD recoveries were within method 

specifications of 71-125%. All RPDs met method-specified criteria.

An MS/MSD was not performed on a solid sample fraction from this episode. FGS 

performed an MS/MSD on another client’s sample that was not part of this episode, 

which 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 6560

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

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

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 6560 Total and Dissolved Metals – Sample Identification

EPA 

Sample #

EPA Sample Description Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71741 FGD Influent, Day 1 280-5257-1 Aqueous 7/12/2010 7/13/2010

71741 FGD Influent, Day 1 - Filtrate 280-5257-3 Aqueous 7/12/2010 7/13/2010

71741 FGD Influent, Day 1 - Solids 280-5257-4 Solid 7/12/2010 7/13/2010

71742 FGD Influent, Day 2 280-5302-1 Aqueous 7/13/2010 7/14/2010

71742 FGD Influent, Day 2 - Filtrate 280-5302-4 Aqueous 7/13/2010 7/14/2010

71742 FGD Influent, Day 2 - Solids 280-5302-5 Solid 7/13/2010 7/14/2010

71743 FGD Influent, Day 3 280-5343-1 Aqueous 7/14/2010 7/15/2010

71743 FGD Influent, Day 3 - Filtrate 280-5343-4 Aqueous 7/14/2010 7/15/2010

71743 FGD Influent, Day 3 - Solids 280-5343-5 Solid 7/14/2010 7/15/2010

71744 FGD Influent, Day 4 280-5398-1 Aqueous 7/15/2010 7/16/2010

71744 FGD Influent, Day 4 - Filtrate 280-5398-3 Aqueous 7/15/2010 7/16/2010

71744 FGD Influent, Day 4 - Solids 280-5398-4 Solid 7/15/2010 7/16/2010

71745 FGD Effluent, Day 2 280-5302-2 Aqueous 7/13/2010 7/14/2010

71746 FGD Effluent, Day 2 280-5343-2 Aqueous 7/14/2010 7/15/2010

71747 FGD Effluent, Day 3 280-5398-2 Aqueous 7/15/2010 7/16/2010

71748 FGD Effluent, Day 4 280-5438-1 Aqueous 7/16/2010 7/17/2010

71749 FGD Effluent Duplicate 280-5343-3 Aqueous 7/14/2010 7/15/2010

71750 FGD Influent Field Blank, 

Day 1

280-5257-2 Aqueous 7/12/2010 7/13/2010
2

Table 1. EPA Episode 6560 Total and Dissolved Metals – Sample Identification

EPA 

Sample #

EPA Sample Description Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71751 FGD Effluent Field Blank, 

Day 1

280-5302-3 Aqueous 7/13/2010 7/14/2010

SUMMARY

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

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

Trace Elements Analysis in Flue Gas Desulfurization Wastewaters,” dated October 6, 

2010, based on EPA Method 200.8, by ICP/MS analysis.

Any significant findings are summarized below. Specific results that required additional 

qualifiers appear in Table 2.

• The dissolved selenium result of 530 μg/L for sample 71748 FGD Effluent Day 4 

(280-5438-1) is greater than the total Selenium value of 480 μg/L reported for the 

same sample.

• The serial dilution analysis for total selenium for sample 71741 did not meet 

TestAmerica’s requirement of ±10%.

• The matrix spike (MS) and matrix spike duplicate (MSD) analyses performed for 

this sampling episode had several silver and one antimony result failed the 70-

130% control limits with poor recoveries.

INTERNAL STANDARDIZATION

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

INITIAL CALIBRATION

TestAmerica performed the initial calibrations on each analysis day or before each 

analysis if more than one analysis was performed in one day. The initial calibration for 

the ICP-MS analysis consisted of a blank and four calibration standards. 

INITIAL AND CONTINUING CALIBRATION VERIFICATION

The initial calibration verifications (ICV) and continuing calibration verifications (CCV) 

performed by TestAmerica all had recoveries within the method criteria.
3

METHOD/INSTRUMENT BLANKS

All the method blanks were less than the reporting limit (RL); however, some elements 

were found above the method detection limit (MDL) and were flagged with the “J” 

qualifier indicating the concentrations were an estimated value. No additional data 

qualifiers were required for method blanks.

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

(CCB)) were less than the RL; however, some elements were above the MDL and were 

flagged with the “J” qualifier.

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 control limits of 85–115%.

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION

Based on TestAmerica’s SOP, all interference check sample A (ICSA) results had 

analytes of interest with concentrations less than the RL or less than five times the RL

when known inherent contaminants are present in the stock solution used to make the 

ICS.

All interference check sample B (ICSAB) synthetic spikes recovered within 

TestAmerica’s SOP criteria of 70–130% of the true value.

SERIAL DILUTION

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

dilution on sample 71741 (280-5257-3) passed TestAmerica’s requirement of ±10% for

all analytes except total selenium at 14%. The total selenium result is flagged with a “V” 

qualifier.

FIELD DUPLICATES

The RPD of the field duplicates 71746/71749 were less than 20% for all values above the 

reporting limit, with the exception of total arsenic, which had an RPD of 30.9%. Even 

though the RPD was greater than 20%, the total arsenic result was not qualified because 

there are no specific control limits for field duplicates specified in EPA Method 200.8.
4

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

MS and MSDs were performed on samples 71741, 71743, 71746, and 71747. Many 

spike recoveries were outside the method contrl limits of 70–130% when sample 

concentrations exceeded the spike concentration by a factor of four or more, which have 

been flagged “4,” indicating concentrations in the parent samples were greater than four

times the spike amounts. All MS/MSDs for total and dissolved silver failed the 70–130% 

control limits. The poor recoveries for silver are probably due to high sulfates in the

samples that could form insoluble silver sulfide and/or silver sulfate. Otherwise, the

MS/MSD spike recoveries were within the control limits of 70-130%, with the exception 

of the following:

• The MS/MSD performed on sample 71741 FGD Influent, Day 1 (280-5257-3) 

failed the 70–130% control limits for total silver.

• The MS/MSD performed on solid sample 71743 FGD Influent, Day 3 (280-5343-

5) failed the 70–130% control limits for antimony and silver.

• The MS/MSD performed on sample 71746 FGD Effluent, Day 2 (280-5343-2) 

failed the 70–130% control limits for total and dissolved silver. The RPD for the 

total silver MS/MSD also failed at 58%.

• The MS/MSD performed on sample 71747 FGD Effluent, Day 3 (280-5398-2) 

failed the 70–130% control limits for total and dissolved silver. Additionally, the 

RPD between the total and dissolved silver MS/MSD for this sample failed the 

method control limits.

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

POST DIGESITON SPIKES

The post digestion spike (PDS) performed on sample 71747 FGD Effluent, Day 3 (280-

5398-2) failed TestAmerica’s control limits of 85–115% recovery for total selenium and 

total silver, with recoveries of 69% and 80%, respectively. The selenium result was 

flagged by the laboratory; however, the silver result was not flagged by the laboratory 

and therefore, has been included in Table 2 below.

DETECTION LIMITS

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

of reagent water.
5

Table 2. Data Review Summary

Sample Analyte Qualifier/Action Reason Level Detected

71741 Selenium

(filtrate, 

total)

Matrix 

Interference

SRD Failed ±10% 

Difference

320 μg/L

71741 Silver (total) Minimum value MS/MSD Failed 

70–130% recovery

ND

71743 Antimony

(solid)

Minimum value MS/MSD Failed 

70–130% recovery

160 μg/kg

71743 Silver

(solid)

Minimum value MS/MSD Failed 

70–130% recovery

140 μg/kg

71746 Silver (total) Minimum value MS/MSD Failed 

70–130% recovery

ND

71746 Silver 

(dissolved)

Minimum value MS/MSD Failed 

70–130% recovery

ND

71747 Silver (total) Minimum value MS/MSD Failed 

70–130% recovery

ND

71747 Silver 

(dissolved)

Minimum value MS/MSD Failed 

70–130% recovery

ND

71747 Silver (total) Minimum value PDS Failed 85–

115% recovery

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 200.7 –

Episode 6560

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

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

tin and titanium) for Sample Episode 6560. 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 6560 Total and Dissolved Metals – Sample Identification

EPA 

Sample # EPA Sample Description

Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71741 FGD Influent, Day 1 280-5257-1 Aqueous 7/12/2010 7/13/2010

71741 FGD Influent, Day 1 - Filtrate 280-5257-3 Aqueous 7/12/2010 7/13/2010

71741 FGD Influent, Day 1 - Solids 280-5257-4 Solid 7/12/2010 7/13/2010

71742 FGD Influent, Day 2 280-5302-1 Aqueous 7/13/2010 7/14/2010

71742 FGD Influent, Day 2 - Filtrate 280-5302-4 Aqueous 7/13/2010 7/14/2010

71742 FGD Influent, Day 2 - Solids 280-5302-5 Solid 7/13/2010 7/14/2010

71743 FGD Influent, Day 3 280-5343-1 Aqueous 7/14/2010 7/15/2010

71743 FGD Influent, Day 3 - Filtrate 280-5343-4 Aqueous 7/14/2010 7/15/2010

71743 FGD Influent, Day 3 - Solids 280-5343-5 Solid 7/14/2010 7/15/2010

71744 FGD Influent, Day 4 280-5398-1 Aqueous 7/15/2010 7/16/2010

71744 FGD Influent, Day 4 - Filtrate 280-5398-3 Aqueous 7/15/2010 7/16/2010

71744 FGD Influent, Day 4 - Solids 280-5398-4 Solid 7/15/2010 7/16/2010

71745 FGD Effluent, Day 2 280-5302-2 Aqueous 7/13/2010 7/14/2010

71746 FGD Effluent, Day 2 280-5343-2 Aqueous 7/14/2010 7/15/2010

71747 FGD Effluent, Day 3 280-5398-2 Aqueous 7/15/2010 7/16/2010

71748 FGD Effluent, Day 4 280-5438-1 Aqueous 7/16/2010 7/17/2010

71749 FGD Effluent Duplicate 280-5343-3 Aqueous 7/14/2010 7/15/2010
2

Table 1. EPA Episode 6560 Total and Dissolved Metals – Sample Identification

EPA 

Sample # EPA Sample Description

Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71750 FGD Influent Field Blank, Day 1 280-5257-2 Aqueous 7/12/2010 7/13/2010

71751 FGD Effluent Field Blank, Day 1 280-5302-3 Aqueous 7/13/2010 7/14/2010

SUMMARY

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

TestAmerica’s SOP for ICP Analysis of Trace Metals by Method 200.7. Due to the total 

suspended solids being in excess of 1% in the influent samples a phase separation was 

performed creating four solid samples. Any significant findings are summarized below. 

Specific sample or QC results that required additional data qualifiers appear in Table 2.

• The relative percent difference (RPD) for total aluminum for the field duplicate 

samples 71746 and 71749 161%; however, the duplicate sample was less than the 

reporting limit; therefore, the RPD could not be accurately calculated. 

• The serial dilution analysis for cobalt for sample 71741 did not meet 

TestAmerica’s requirement of ±10% difference.

• The MS and MSD recoveries for titanium in the solid phase of sample 71743 

failed the 70-130% control limits.

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 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

All initial calibration verifications (ICV) and continuing valibration verifications (CCV)

had recoveries within the method criteria.

METHOD/INSTRUMENT BLANKS
3

All the Method Blanks were less than the reporting limit (RL); however, some elements

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

qualifier.

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

were above the MDL and were flagged with the “J” qualifier.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

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

LABORATORY CONTROL SAMPLES (LCS)

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

SYNTHETIC FGD INTERFERENCE CHECK SOLUTIONS

Interference checks were performed using the synthetic matrix as the check solution. All 

recoveries met the method-specified criteria.

SERIAL DILUTION

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

71741 failed the method required ±10% difference for cobalt (11%), which was flagged 

“V” as failing the QC criteria. Otherwise, all serial dilution percent differences were less 

than 10%.

FIELD DUPLICATES

The RPD of the field duplicates 71746/71749 were less than 20% for all values equal to 

or greater than the RL, except for total aluminum, which had an RPD of 161%. The 

parent sample value (260 ug/L) was greater than the RL, but the duplicate value (28 ug/L) 

was less than the RL; therefore, the RPD could not be accurately calculated. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

MS and MSD were performed on samples 71741 (total), 71743 (total solid), 71746 (total 

and dissolved) and 71747 (total and dissolved). Many elements with high concentrations 

frequently failed the spike recovery but were flagged with a “4” qualifier indicating that 

the concentration in the parent sample was greater than four times the spike and could not 

be reliably calculated. Otherwise, the MS/MSD spike recoveries were within the control 

limits of 70–130% with the exception of the following:

• The MS and MSD recoveries for titanium in the solid phase of sample 71743 

were 131% and 137%, respectively.
4

The RPDs between the MS and MSD samples were always within ± 20% except for the 

following:

• The RPD between the MS and MSD for boron for sample 71746 was 165% for 

both total and dissolved analyses.

• The RPD between the MS and MSD for magnesium for sample 71746 was 165% 

for both total and dissolved analyses.

• The RPD between the MS and MSD for total boron and total magnesium for 

sample 71747 was 162%.

• The RPD between the MS and MSD for dissolved boron and dissolved 

magnesium for sample 71747 was 163%.

POST DIGESTION SPIKE

The post digestion spike (PDS) performed on sample 71741 FGD Influent, Day 1 passed

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

except for total aluminum and total titanium. The post digestion spike performed on 

sample 71746 FGD Effluent, Day 2 passed TestAmerica’s control limits of 85-115% 

recovery for all total and dissolved analytes except for total aluminum, total titanium, and 

dissolved titanium. 

DETECTION LIMITS

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

of reagent water.

Table 2. Data Review Summary

Sample Analyte Qualifier/Action Reason Level Detected

71743 Titanium 

(solid) Maximum value MS/MSD recovery > 130% 140 mg/kg
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 

6560

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

chromium for Sample Episode 6560. 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 6560 Dissolved Hexavalent Chromium – Sample Identification

EPA 

Sample 

#

Sample 

Matrix Sample Description

Sampling 

Date Analysis Date

71741 Aqueous FGD Influent Day 1 7/12/10 8/9/10

71742 Aqueous FGD Influent Day 2 7/14/10 8/9/10

71743 Aqueous FGD Influent Day 3 7/14/10 8/9/10

71744 Aqueous FGD Influent Day 4 7/15/10 8/9/10

71745 Aqueous FGD Effluent Day 1 7/14/10 8/9/10

71746 Aqueous FGD Effluent Day 2 7/14/10 8/9/10

71747 Aqueous FGD Effluent Day 3 7/15/10 8/9/10

71748 Aqueous FGD Effluent Day 4 7/16/10 8/9/10

71749 Aqueous FGD Effluent Day 2 Duplicate 7/14/10 8/9/10

71750 Aqueous FGD Influent Field Blank Day 1 7/12/10 8/9/10

71751 Aqueous FGD Effluent Field Blank Day 1 7/14/10 8/9/10

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 (71741, 71742, 71743, and 71744) were diluted prior to analysis due to 

the presence of high levels of non-target chloride interferences.

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES

The pH for sample 71751 (FGD Effluent Field Blank) was 9.98 S.U. upon receipt at the 

laboratory, which is outside the appropriate range of 9.0-9.5 S.U.; therefore, the 

laboratory adjusted the pH. The final sample pH was 9.68 S.U. Because this sample was 

not at the method-specified pH, this sample was qualified as an estimated value. 

INITIAL PRECISION AND ACCURACY/RECOVERY

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

method criteria.

ON-GOING PRECISION AND ACCURACY/RECOVERY

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

(OPR).

INITIAL CALIBRATION

FGS performed the initial calibrations on each analysis day. The initial calibration for 

the LC-ICP-MS analysis consisted of a blank and eight calibration standards with a 

correlation factor ≥0.995 as required by the method.

A secondary source initial calibration verification (ICV) was analyzed and passed ± 10% 

of true value required by the method.

CONTINUING CALIBRATION VERIFICATION

All CCVs met method-specified criteria, ± 10% of true value with recoveries ranging 

from 98.5 to 109%.

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 102% and 102%. The laboratory SOP indicated that a second source 

quality control sample (QCS) must be analyzed by the laboratory at least once a quarter. 
3

The data for the QCS was not included in the data package for review. However, the 

ICV was a second source standard.

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 71749, with a result of 7.35 

μg/L, was a duplicate of sample 71746, which had 7.32 μg/L hexavalent chromium. 

These duplicate samples had an RPD of 0.41%, which meets the method-suggested 

criteria.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

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

spike on sample 71747. The MS and MSD recoveries were 101% and 99.5%,

respectively, with an RPD of 1.07%. A second set of MS and MSDs were prepared on 

the diluted sample and had recoveries of 95.3% and 96.0%, respectively, with an RPD of 

0.64%.

Table 2. Data Review Summary Table

Sample Analyte Qualifier Reason Level Detected

71751 Chromium (VI) Estimated value

pH outside of 

method-specified 

range.

ND

ND - Not detected.
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 6560

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for Sample Episode 6560. 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, 

• Cyanide, 

• Nitrate/Nitrite, 

• Phosphorus, and

• TKN. 

TestAmerica was also required to analyze chloride and sulfate using this phase separation

technique, but they mistakenly only analyzed the solids fraction and not the filtrate 

fraction. Therefore, TestAmerica instead analyzed and reported the results for the raw 

sample without phase separation for chloride and sulfate.

Table 1 summarizes the nine field samples analyzed by TestAmerica, including how the

laboratory split and analyzed the influent samples.
2

Table 1. EPA Episode 6560 Classical Analytes – Sample Identification

EPA

Sample #

Sample 

Description

Sampling

Date

Sample

Matrix

Portion of 

Sample

Analytes 

71741 FGD Influent, 

Day 1 7/12/10

Water Entire 

Fraction

BOD5, COD, Chloride, 

Sulfate, TDS, and TSS

Water Filtrate

Ammonia, Cyanide, 

Nitrate/Nitrite, 

Phosphorus, and TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

71742 FGD Influent, 

Day 2 7/13/10

Water Entire 

Fraction

BOD5, COD, Chloride, 

Sulfate, TDS, and TSS

Water Filtrate

Ammonia, Cyanide, 

Nitrate/Nitrite, 

Phosphorus, and TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

71743 FGD Influent, 

Day 3 7/14/10

Water Entire 

Fraction

BOD5, COD, Chloride, 

Sulfate, TDS, and TSS

Water Filtrate

Ammonia, Cyanide, 

Nitrate/Nitrite, 

Phosphorus, and TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

71744 FGD Influent, 

Day 4 7/15/10

Water Entire 

Fraction

BOD5, COD, Chloride, 

Sulfate, TDS, and TSS

Water Filtrate

Ammonia, Cyanide, 

Nitrate/Nitrite, 

Phosphorus, and TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

71745 FGD Effluent, 

Day 1 7/13/10 Water Entire Fraction All analytes

71746 FGD Effluent, 

Day 2 7/14/10 Water Entire Fraction All analytes

71747 FGD Effluent, 

Day 3 7/15/10 Water Entire Fraction All analytes
3

Table 1. EPA Episode 6560 Classical Analytes – Sample Identification

EPA

Sample #

Sample 

Description

Sampling

Date

Sample

Matrix

Portion of 

Sample

Analytes 

71748 FGD Effluent, 

Day 4 7/16/10 Water Entire Fraction All analytes

71749 FGD Effluent 

- Duplicate 7/14/10 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 perform the phase separation of the preserved Group II influent 

samples; therefore, the laboratory used some of the extra volume from the unpreserved 

metals sample volume for the analyses. After phase separation, TestAmerica preserved 

the samples accordingly. Because of this process, the ammonia, nitrate/nitrite, TKN, 

phosphorus, and cyanide influent samples used for the analyses 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.

If required by the method, a matrix spike (MS) analysis was run on sample 71747 (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. 
4

DATA NOTES/ISSUES

Ammonia

As stated above, filtrate and solid aliquots of samples 71741 - 71744 were not preserved 

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

phase separation. Because these samples were not preserved immediately as required by 

the method, these samples were qualified as estimated values.

The filtrate of sample 71741 and the solids portion of 71742 were analyzed one day after 

the 28-day hold time. The solids portion of sample 71741 was analyzed two days after 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.

The results for the MS/MSD samples for 71747 were above the highest calibration 

standard. The laboratory did not dilute and reanalyze these samples because the MS/MSD 

percent recoveries were within the control limits specified by EPA method 350.1. 

Therefore, if the MS/MSD results for sample 71747 are reported, they will be qualified as

estimated values. The result for sample 71747 was within the calibration range, so this 

sample does not need to be qualified. The LFB associated with sample 71747 met the 

method criteria.

BOD5

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

depletion greater than 2.0 mg/L for sample 71744. 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. 

The glucose-glutamic acid (GGA) standards associated with samples 71744 and 71747 

had percent recoveries of 80% and 78%. The GGA standards associated with sample

71748 had percent recoveries of 79% and 81%. These percent recoveries were below the

method and laboratory criteria of 85-115%. TestAmerica flagged these samples with a 

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

was not detected in sample 71744, so no further qualification was necessary for this 

sample. Samples 71747 and 71748 were additionally qualified as minimum values.

The seed correction factor associated with sample 71748 was 0.5328 mg/L, which is less 

than the method and laboratory control limits of 0.6-1.0 mg/L. The result for this sample 

could be biased low. This sample was qualified by TestAmerica with an “s” meaning the 

seed control blank (SCB) recovery was low. Since this sample was already qualified as a 

minimum value because the GGA percent recovery was low, no further action was taken. 
5

All laboratory duplicates and water blanks were analyzed appropriately and met method 

criteria.

Chloride and Sulfate

The laboratory diluted the MSD sample for 71747 by 500 fold, but the diluted result for 

sulfate was still above the highest calibration standard. The laboratory did not reanalyze 

this sample with a higher dilution factor, because the MSD percent recovery was within 

the control limits specified by EPA method 300.0. Therefore, if the MSD result for 

sample 71747 for sulfate is reported, it will be qualified as an estimated value. 

COD

The RPD between sample 71746 and its field duplicate 71749 for COD was 33.3%. Even 

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

control limits for field duplicates specified in EPA Method 410.4.

The percent recoveries for the MS and MSD samples associated with 71747 were 87% 

and 93% respectively. The MS percent recovery did not meet the method control limits 

of 90-110%. Because the percent recovery for the MS sample was below the method

control limits, sample 71747 was flagged as a minimum value.

Cyanide 

As stated above, filtrate and solid aliquots of samples 71741 - 71744 were not preserved 

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

phase separation. Solid aliquots of samples 71741 - 71744 were all 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 71741 - 71744 were not preserved immediately as required by 

the method, these samples were qualified as estimated values.

Sample 71747 was preserved to pH 10 with NaOH immediately after sample collection, 

but the pH was neutral when the sample was received by the laboratory. The laboratory 

added more NaOH to correct the pH upon receipt. This sample was flagged as an 

estimated value.

Both the filtrate and solids fraction of samples 71741, 71742, 71743, and 71744 were 

analyzed 16, 15, 14, and 13 days respectively past the 14-day hold time. Since all of these 

samples were already qualified as estimated values because the sample was not preserved 

appropriately or because the sample result was greater than the MDL but less than the RL 

(i.e., a J-value), no further action was necessary. 

Cyanide was detected at 0.00240 mg/L in the LRB associated with the filtrate fraction of 

samples 71741 - 71744. Additionally, cyanide was detected at 0.141 mg/kg in the LRB

associated with the solids fraction of samples 71741 - 71744. Cyanide was also detected 
6

at 0.00499 mg/L in the LRB associated with the samples 71745 - 71749. Because all of 

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

results. 

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

The diluted result for sample 71749 was less than the lowest calibration standard. The 

solid fraction results for samples 71741 - 71744 were also all below the lowest calibration 

standard. These sample results 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 RPD between sample 71746 and its field duplicate 71749 for cyanide was 193%. 

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 71741 - 71744 were not preserved 

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

phase separation. Because these samples were not preserved immediately as required by 

the method, these samples were qualified as estimated values.

The 28-day hold time was exceeded by one day for the filtrate fraction of sample 71741 

and for the solids fraction of sample 71742. The solids fraction of sample 71741 was 

analyzed two days past the holding time. These samples were already qualified as 

estimated values because they were not preserved immediately following sample 

collection, so no further action was necessary.

Phosphorus 

As stated above, filtrate and solid aliquots of samples 71741 - 71744 were not preserved 

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

phase separation. Filtrate samples 71741 - 71744 and solid sample 71743 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. 

Solid samples 71741, 71742, and 71744 were qualified as estimated values because they 

were not preserved immediately following sample collection, as required by the method.

The filtrate and solids fractions from sample 71741 were analyzed two days after the 28-

day hold time and the filtrate and solids fractions from sample 71742 were analyzed one

day outside of the hold time. TestAmerica did not flag these results; therefore, ERG 

qualified these samples with an “H”. These samples were already qualified as estimated 

values because they were not preserved immediately following sample collection.

Phosphorus was detected at 0.00837 mg/L in the laboratory reagent blank associated with 

samples 71745 - 71749. Phosphorus was also detected at 0.00977 mg/L in the laboratory 
7

reagent blank associated with the filtrate of samples 71741 - 71744. Because all of these 

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

results.

The filtrate results for samples 71741 - 71744 were all below the lowest calibration 

standard. 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 RPD between sample 71746 and its field duplicate 71749 for phosphorus was 93.9%. 

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

are no control limits for field duplicates specified in the method.

The percent recoveries for the MS and MSD analyses for sample 71747, 55% and 57%, 

respectively, were not within the method control limits of 90-110% or within the 

laboratory control limits of 71-128%. Results for samples with a similar matrix (i.e., FGD 

effluent) could be biased low because of matrix interferences. Sample 71747 was

qualified as a minimum value because the MS percent recovery was less than the control 

limits specified in the method.

TDS

Two laboratory duplicates were analyzed. The RPDs for these laboratory duplicates were

less than 10%, which is required by the method. 

Samples 71743, 71746, 71748, and 71749 did not achieve a constant weight after three 

drying cycles. 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.

TKN

As stated above, filtrate and solid aliquots of samples 71741 - 71744 were not preserved 

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

phase separation. Because these samples were not preserved immediately as required by 

the method, these samples were qualified as estimated values.

The solids and filtrate fraction of samples 71741 and 71742 were analyzed two days and 

one day after the 28-day hold time, respectively. These samples were already qualified as 

estimated values because they were not preserved immediately following sample 

collection, so no further action was necessary. 
8

TKN was detected at 0.234 mg/L in the laboratory reagent blank associated with samples 

71745 - 71749. Because this blank result was less than the RL, no samples were qualified 

based on the LRB result.

TestAmerica performed MS and MSD analyses on sample 71747. The percent recoveries

for the MS and MSD samples were 88% and 116% and the results were 23.2 and 24.0 

mg/L. 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. Considering that the MS percent 

recovery was below the control limits and the MSD percent recovery was above the 

limits, this was likely the case. Sample 71747 was not qualified because it is not possible 

to determine if the MS/MSD failure was a result of matrix interferences or caused by the 

low spiking level.

TSS 

Four laboratory duplicates were analyzed. The RPDs for these laboratory duplicates were 

less than or equal to 10% as required by the method. 

TSS was detected at 1.60 mg/L in the method blank (MB) associated with sample 71747. 

Because this blank result was less than the RL, no samples were qualified based on the 

MB result

The RPD between sample 71746 and its field duplicate 71749 for TSS was 27.3%. 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 the SM 2540D.

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71741 

(filtrate)

Ammonia Estimated value Sample not preserved 

immediately following 

collection. Analyzed one 

day past holding time

5.1 mg/L

71741 

(solid)

Ammonia Estimated value Sample not preserved 

immediately following 

collection. Analyzed two 

days past holding time

24 mg/kg

71742 

(filtrate)

Ammonia Estimated value Sample not preserved 

immediately following 

collection

5.3 mg/L
9

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71742 

(solid)

Ammonia Estimated value Sample not preserved 

immediately following 

collection. Analyzed one 

day past holding time

28 mg/kg

71743 

(filtrate)

Ammonia Estimated value Sample not preserved 

immediately following 

collection

7.7 mg/L

71743 

(solid)

Ammonia Estimated value Sample not preserved 

immediately following 

collection

26 mg/kg

71744 

(filtrate)

Ammonia Estimated value Sample not preserved 

immediately following 

collection

6.2 mg/L

71744 

(solid)

Ammonia Estimated value Sample not preserved 

immediately following 

collection

23 mg/kg

71747 BOD5 Minimum value GGA % recovery below 

method-specified criteria

6.9 mg/L

71748 BOD5 Minimum value GGA % recovery and 

SCB recovery below 

method-specified criteria

4.6 mg/L

71747 COD Minimum value MS % recovery below 

method-specified criteria

560 mg/L

71741 

(filtrate)

Total Cyanide H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed 16 

days past holding time

0.27 mg/L

71742 

(filtrate)

Total Cyanide H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed 15 

days past holding time

0.62 mg/L

71743 

(filtrate)

Total Cyanide H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed 14 

days past holding time

2.2 mg/L

71744 

(filtrate)

Total Cyanide H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed 13 

days past holding time

0.21 mg/L

71747 Total Cyanide Estimated value pH upon receipt < 10 0.60 mg/L
10

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71741 

(filtrate)

Nitrate/nitrite H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed 1 

day past holding time

77 mg/L

71741 

(solids)

Nitrate/nitrite H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed two

days past holding time

49 mg/kg

71742 

(filtrate)

Nitrate/nitrite Estimated value Sample not preserved 

immediately following 

collection.

83 mg/L

71742 

(solids)

Nitrate/nitrite H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed one

day past holding time

64 mg/kg

71743 

(filtrate)

Nitrate/nitrite Estimated value Sample not preserved 

immediately following 

collection.

79 mg/L

71743 

(solids)

Nitrate/nitrite Estimated value Sample not preserved 

immediately following 

collection.

56 mg/kg

71744 

(filtrate)

Nitrate/nitrite Estimated value Sample not preserved 

immediately following 

collection.

90 mg/L

71744 

(solids)

Nitrate/nitrite Estimated value Sample not preserved 

immediately following 

collection.

65 mg/kg

71741 

(filtrate)

Total 

Phosphorus

H Analyzed two days past 

holding time

0.0096 

mg/L

71741 

(solids)

Total 

Phosphorus

H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed two

days past holding time

21 mg/kg

71742 

(filtrate)

Total

Phosphorus

H Analyzed one day past 

holding time

0.0081 

mg/L

71742 

(solids)

Total 

Phosphorus

H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed one

day past holding time

310 mg/kg

71744 

(solids)

Total 

Phosphorus

Estimated value Sample not preserved 

immediately following 

collection.

340 mg/kg
11

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71747 Total 

Phosphorus

Minimum value MS % recovery below 

method-specified criteria

0.18 mg/L

71741 

(filtrate)

TKN H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed two

days past holding time

24 mg/L

71741 

(solids)

TKN H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed two

days past holding time

830 mg/kg

71742 

(filtrate)

TKN H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed one

day past holding time

31 mg/L

71742 

(solids)

TKN H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed one

day past holding time

840 mg/kg

71743 

(filtrate)

TKN Estimated value Sample not preserved 

immediately following 

collection.

29 mg/L

71743 

(solids)

TKN Estimated value Sample not preserved 

immediately following 

collection.

700 mg/kg

71744 

(filtrate)

TKN Estimated value Sample not preserved 

immediately following 

collection.

26 mg/L

71744 

(solids)

TKN Estimated value Sample not preserved 

immediately following 

collection.

900 mg/kg