Appendix B

DATA REVIEW NARRATIVES1 

### 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 /201 1 Subject: FGS Data R eview Narrat ive for Total and Dissolved Mercury

– Episode 65 60

Frontier Global Sciences (FGS) generated analytical data for total and dissolved mercury. FGS analyzed t he samples according to EPA Method 1631E for mercury by Cold Vapor Atomic Fluorescence Spectrometry (CVAFS) analysis.

Table 1 summarizes the 27 s amples ( exc luding laboratory filter blanks) FG S extracted and analyzed for total and dissolved mercury

.

Table 1. EPA Episode 6560 Total & Dissolved Mercury

– Sample Identification

EPA Sample # Lab Sample

I D # 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 Aqu eous 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 Infl uent, 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 7/16/20102 Table 1. EPA Episode 6560 Total & Dissolved Mercury

– Sample Identification

EPA Sample # Lab Sample

I D # Sample

Matrix Sample Description Sampling

Date

71748 1007131

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

7 1749 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 Bla nk 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 prepa red 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 o ngoing p recision and r ecovery (OPR) sample was not analyzed at the beginning and end of the solid fraction sample analysis.

**•** A m atrix s pike (MS) and m atrix s pike d uplicate (MSD) were not performed on a solid sample fraction f rom this episode.

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES

There were no s ample receipt issues in this data package

.

I NITIAL CAL IBRATION

FGS performed the initial calibrations on each analysis day. The i nitial 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 C ONTINUING C ALIBRATION V ERIFICATION S

All initial and c ontinuing c alib ration v erifications ( ICVs, CCVs ) met method

- specified

criteria

.

BLANK S

All preparation blanks or laboratory reagent blanks (LRBs) and the continuing calibration blanks (CCBs) met method

- specified criteria.3 DUPLICATES

Field duplicates

, s ample 71749, were collected on s ample 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%.

L aboratory 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

- specif ied criteria.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

MS and MSD s were performed on samples 71742, 7174 3

, 71747, and 71748 for the total mercury analyses

. MS and MSDs were performed on samples 71742 and 71747 for t he dissolved mercury analys e s. All aqueous MS/MSD recoveries were within method specifications of 71

- 125%. All RPDs met method

- specified criteria.

A n M S / MSD w as not performed on a solid sample fraction f rom this episode. FGS performed an MS/MSD on another client’s sample that was not part of this episode,

which met method

- specified criteria.

D ETECTION 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 R eview Narrative for Total and Dissolved Metals by 200.8

– Episode 65 60

TestAmerica generated analytical data for total and dissolved metals ( a ntimony, a rsenic,

c admium, c hromium, c opper, l ead, n ickel, s elenium, s ilver, t hallium, v anadium and z inc )

. T he 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 7/13/20102 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

T he sample s 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 a re summarized below. Specific results that required additional qualifiers appear in Table 2.

**•** The dissolved s elenium 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

s ame 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 an timony result failed the 70

- 130% control limits with poor recoveries.

INTERNAL STANDARDIZA TION

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

.

I NITIAL AND CONTINUING CALIBRATION VERIFICATION

The i nitial c alibration v erifications ( ICV ) and c ontinuing c alibration v erifications (CCV) performed by TestAmerica all had recoveries within the method criteria.3 METHOD/INSTRUMENT BLANK S

All the m ethod b lanks were less than the r eporting l imit (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 m ethod b lanks.

All i nstrument b lanks ( 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 )

A ll CRI samples passed TestAmer ica’s SOP control limits of 50

– 150%.

LABORATORY CONTROL SAMPLE S (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 contaminant s are present in the stock solution used to make the

ICS

.

All interference check sample B ( ICSAB ) synthetic s pikes 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 s e lenium at 1 4 %. 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 a rsenic, 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 DUPLICAT ES

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 concentration s in the parent sample s were greater than four times the spike amount s

. All MS/MSDs for total and dissolved s ilver failed the 70

– 130% control limits. The poor recoveries for s ilver are probably due to high sulfates in the samples that could form insoluble s ilver s ulfide and/or s ilver s ulfate. 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 s ilver.

**•** The MS/MSD performed on solid sample 7174 3 FGD Influent, Day 3 ( 280

- 5343

- 5 ) failed the 7 0

– 130% control limits for a ntimony and s ilver.

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

- 5343

- 2)

failed the 70

– 130% control limits for total and dissolved s ilver. The RPD for the

total s ilver 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 s ilver. Additionally, t he

RPD between the to tal and dissolved s ilver 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 SPIKE S

The p ost d igestion s pike (PDS) performed on sample 71747 FGD Effluent, Day 3 (280

- 5398

- 2) failed TestAmerica’s control limits of 85

– 115% recovery for total s elenium and

total s ilver , with recoveries of 69% and 80%

, respectively

. The s elenium result was flagged by the laboratory ; however, the s ilver result was not flagged by the laboratory and therefore, has been included in Table 2 below.

D ETECTION 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 Se lenium ( filtrate,

total ) Matrix

Interference SR D Failed ± 10%

Difference 320 μg/L

71741 Silver (total) Minimum value MS/MSD Failed

70

– 130% recovery ND

717 43 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 ND1 

### 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 ( a luminum, b oron, b arium, b eryllium, c alcium, c obalt, i ron, m agnesium, m anganese, m olybdenum, s odium,

t in and t itanium ) for S a mple Episode 6560

. T he samples were analyzed according to EPA

Method 200. 7

.

Table 1 summarizes the s ample s 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 7/15/20102 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 sample s 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 creati ng 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

.

**•** T he MS and MSD recoveries for t itanium in the solid phase of sample 71743

failed the 70

- 130% control limits

.

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES

There were no s ample receipt issues in this data package

.

INTERNAL STANDARDIZA TION

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.

I NITIAL CAL IBRATION

TestAmerica performed the initial calibrations on each analysis day. The initial

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

I NITIAL AND CONTINUING CALIBRATION VERIFICATION S

All i nitial c alibration v erifications ( ICV ) and c ontinuing v alibration v erifications (CCV)

had recoveries within the method criteria.

METHOD/INSTRUMENT BLANK S3 All the Method B lanks were less than the r eporting l imit (RL) ; however, some elements

had levels above the method detect ion limit ( MDL ) and were flagged with the “J” qualifier.

All i nstrument b lanks ( 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)

A ll 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 SOLUTION S

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 met h od require d ±10% difference for cobalt (11%), whi ch was flagged “V” as failing the QC criteria. Otherwise, all serial dilution percent differences were less

than 10%.

FIELD DUPLICATES

T he RPD of the field duplicates 71746/71749 were less than 20% for all values equal to or greater than the RL, except f or 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 DUPLICATE S

M S and MSD were performed on sample s 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 t itanium 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 t he 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 16 3 %.

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 t otal a luminum and total t itanium . 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/kg1 

### 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 /201 1

Su bject: FGS Data R eview Narrative for Dissolved Hex avalent Chromium

– Episode

65 60

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

chromium for Sample Episode 6560

. FGS analyzed t he samples according to a m odified

EPA Method 2 18. 6 for dissolved hexavalent chromium by Liq uid Chromatography

– Inductively Coupled Plasma Mass Spectrometry (LC

- ICP

- MS)

.

Table 1 summarizes the s amples 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

71 74 1 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 F ield B lank Day 1 7/12/10 8/9/10

71751 Aqueous FGD Effluent F ield B lank Day 1 7/14/10 8/9/10

SUMMARY

The samples were prepared for dissolved hexavalent chromium analysis according to

FGS

- 129.01 Standard Operatin g Procedure ( SOP ) , a modified EPA Method 218. 6

.2 Several s amples ( 71741, 71742, 71743, and 71744 ) were diluted prior to analysis due to the presence of high levels of non

- target chloride interferences

.

SAMPLE REC E IPT, 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.

I NITIAL P RECISION AND ACCURACY/ R ECOVERY

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

method criteria.

O N

- GOING P RECISION AND ACCURACY/ R EC OVERY

The analytical method did not require the analysis of an on

- going precision and recovery ( OPR )

.

I NITIAL CAL IBRATION

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

the LC

- ICP

- MS analysis consisted of a bl ank 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

.

C ONTINUING C ALIBRATION V ERIFICAT ION

All CCVs met method

- specified criteria

, ± 10% of true value with recoveries ranging

from 98.5 to 109%.

BLANK

All of the prep aration blanks /laboratory reagent blanks (LRBs) and the continuing calibration blanks (CCBs) met method

- specified requirement s

.

OTHER CHECKS

The l aboratory c ontrol s ample /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 quali ty 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.

D ETECTION LIMITS

The laboratory method detection li mit (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 w as collected and analyzed. Sample 71 749, with a result of 7.35 μg/L, was a duplicate of sample 71 74 6 , which had 7.32 μg/L hexavalent chromium

. These duplicate s ample s had an RPD of 0.41%, which meets the method

- suggested

criteria

.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

The M S and matrix spike duplicate ( MSD ) w as performed using a secondary source spike on sample 71 74 7

. The MS and MSD r ecoveries were 101% and 99.5%, respectively, with an RPD of 1.07 %

. A second set of MS and MSD s 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

71 751 Chromium (VI) Estimated value pH outside of

method

- specified

range. ND

ND

- Not d etected

.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 / 20 11 Subject: TestAmerica Data Review Narrative for Clas sicals Analyses

– Episode 65 60

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry analyses for Sample Episode 65 60

. All samples were tested for the following analytes:

**•** Ammonia by EPA method 350.1,

**•** Biochemical Oxygen Dem and

– 5 day (BOD 5 ) by SM 5210B,

**•** Chloride and S ulfate 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 D issolved S olids (TDS) by SM 2540C,

**•** Total K jeldakl N itrogen (TKN) by EPA method 351 .2

, and

**•** Total S uspended S olids (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

a nalyzed both portion s 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

techni que
, but they mistakenly only analyze d the solids fraction and not the filtrate

fraction. Th erefore

, TestAmerica instead analyzed and reported the results for the raw sample without phase separation for chloride and sulfate.

Table 1 summarizes the nine fi eld sampl es 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 BOD 5 , COD, Chloride, Sulfate, TDS, and TSS

Water Filtrate Ammonia, Cyanide

, Nitrate/Nitrite, Phosphorus, and TKN

Solids Solids Ammonia, Chloride, Cyanide, Nitrate/Nitrite, Phosphor us, Sulfate, and

TKN

71742 FGD Influent, Day 2 7/13/10 Water Entire

Fraction BOD 5 , COD, Chloride, Sulfate, TDS, and TSS

Water Filtrate Ammonia, Cyanide, Nitrate/Nitrite, Phosphorus, and TKN

Solids Solids Ammonia, Chloride, Cyanide, Nitrate/Nit rite, Phosphorus, Sulfate, and

TKN

71743 FGD Influent, Day 3 7/14/10 Water Entire

Fraction BOD 5 , COD, Chloride, Sulfate, TDS, and TSS

Water Filtrate Ammonia, Cyanide, Nitrate/Nitrite, Phosphorus, and TKN

Solids Solids Ammonia, Chloride, Cyanide, N itrate/Nitrite, Phosphorus, Sulfate, and

TKN

71744 FGD Influent, Day 4 7/15/10 Water Entire

Fraction BOD 5 , 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 analytes3 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 o therwise noted below

.

TestAmerica could not perform the phase separation of the preserved Group II influent samples; t herefore, t he laboratory use d 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. Th e r elative

p ercent d ifference (RPD) between the sample and its duplicate was less than 20% unless

otherwise noted below.

If applicab le, 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 t he lowest and highest standards

unless noted below. Additionally, all c alibration 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 spec ified 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 (M S) analysis was run on sample 71 747 (FGD

effluent ) for each analyte to check for matrix interferences

. F or some analytes,

TestAmerica s piked more sample s 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 sample s 71741

- 71744 w ere 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 value s

.

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 day s 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.

T he results for the MS/MSD samples for 71 74 7 were above the highest calibration

standard. The laboratory did not dilute and re analyze these samples becau se the MS/MSD percent recoveries were within the control limits specified by EPA method 350.1. Therefore, if the MS/MSD results for sample 71 74 7 are reported

, they will be qualified as

estimated value s

. The result for sample 71 74 7 was within the calibratio n range, so this sample does not need to be qualified. The LFB associated with sample 71747 met the

method criteria.

BOD 5

TestAmerica analyzed five dilutions, but no dilutions had a dissolved oxygen (DO) depletion greater than 2.0 mg/L for sample 71744. Therefore, BOD 5 was reported as not

detect ed for th is 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 sample s 71744 and 71747

h ad percent recover ies of 80% and 78% . The GGA standards associated with sampl e 71748 had percent recoveries of 79% and 81%. These percent recoveries were below the

meth od and laboratory criteria of 85

- 115%. TestAmerica flagged these samples with a “*” meaning the laboratory control sample was not within laboratory control limits. B OD

was not detected in sample 71744, so no further qualification was necessary for this sample. Sample s 71747 and 71748 were additionally qualified as minimum value s

.

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

t han 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 t his sample was already qualifie d as a

minimum value because th e 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 71 747 by 500 fold, but the diluted result for

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

this sample with a higher dilution factor, because the MSD percent recover y w as within the control limits specified by EPA method 300.0. Therefore, if the MSD result for sample 71 74 7 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 2 0%, the sample was not qualified because there are no control limits for field duplicates specified in EPA Method 410.4

.

T he percent recoveries for the MS and MSD samples associated with 71 74 7 were 87%

and 93 % respectively. The MS percent recovery did n ot meet the method control limits

of 90

- 110%

. Because t he percent recovery for the MS sample w as below the method

control limits

, sample 71747 was flagged as a minimum value.

Cyanide

As stated above, filtrate and solid aliquots of sample s 71741

- 71744 were not preserved immediately after sample collection. Instead

, TestAmerica preserved the sample after phase separation. Solid aliquots of sample s 71741

- 71744 were all qualified by the laboratory with a “J” meaning the sample result was an estimated val ue because it was

less than the RL, so there was no need to further qualify these samples. Because the filtrate aliquots of sample s 71741

- 71744 were not preserved immediately as required by the method, these samples were qualified as estimated values.

S ample 71747 w as preserved to pH 10 with NaOH immediately after sample collection, but the pH was neutral when the sample w as received by the laboratory. The laboratory added more NaOH to correct the pH upon receipt. Th is sample w as flagged as an estimated value.

Both the filtrate and solids fraction of sample s 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 value s because the sample w as 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 sample s 71741

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

associated with the solids fraction of sample s 71741

- 71744

. Cyanide was also detected6 at 0.00499 mg/L in the LRB associated with the sample s 71745

- 71749. Because all of

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

results.

All samples w ere diluted prior to distillation by a factor of 10 due to matrix interferences

. T he diluted result for sample 71749 was less than the lowe st calibrat ion standard. The

solid fraction results for sample s 71741

- 71744 were also all below the lowest calibration

standard. T hese 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 sample s 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 fracti on 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 sample s 71741

- 71744 were not preserved immediately after sample collection. Instead

, TestAmerica preserved the sample after phase separation. Filtrate sample s 71741

- 71744 and soli d 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 sample s 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 fraction s from sample 71741 were analyzed two days after the 28

- day hold time and the filtrate and solids frac tion s from sample 71742 w ere 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 imm ediately following sample collection.

Phosphorus was detected at 0.00837 mg/L in the laboratory reagent blank associated with sample s 71745

- 71749. Phosphorus was also detected at 0.00977 mg/L in the laboratory7 reagent blank associated with the filtrate of sample s 71741

- 71744. Because all of these blank results were less than the RL, no samples were qualified based on these LRB

results.

The filt rate results for sample s 71741

- 71744 were all below the lowest calibration

standard. These samples were alr eady 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 anal ys e s for sample 71 74 7 , 55% and 57%, respecti vely, were not within the method control limits of 90

- 110% or within the laboratory control limits of 71

- 128%

. R esults 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 l aboratory duplicates were analyzed

. The RPDs for these l aboratory duplicates were less than 10 % , which is required by the method.

Sample s 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. F GD 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 s ample s 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 e stimated values.

The solids and filtrate fraction of sample s 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 sample s 71745

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

based on the LRB result.

TestAmerica p er formed MS and MSD analys e s on sample 71747. T he 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 d id 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 pe rcent 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 ca used 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 samp le 71747.

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

MB result

The RPD between sample 71 74 6 and its field duplicate 71 749 for TSS was 27.3 %. Even

th ough 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 ( f

iltrate) Ammonia Estimated v alue Sample not preserved

immedia tely following

collection. Analyzed one

day past holding time 5.1 mg/L

71741 ( s olid) Ammonia Estimated value Sample not preserved immediately following

collection. Analyzed two

days past holding time 24 mg/kg

71742 (filtrate) Ammonia Estimated value Samp le not preserved immediately following

collection 5.3 mg/L9 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 preser ved 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

71 744 (solid) Ammonia Estimated value Sample not preserved immediately following

collection 23 mg/kg

71747 BOD 5 Minimum value GGA % recovery below

method

- specified criteria 6.9 mg/L

71748 BOD 5 Minimum value GGA % recovery and

SCB recovery below

method

- spec ified 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 0.6 0 mg/L10 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

collec tion. Analyzed two

day s 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 followin g 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 foll owing

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

717 41 (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/kg11 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

collec tion. 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

imme diately 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