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: Donna Tedder, ERG

Date: 9 / 1/2011 Subject: FGS Data R eview Narrative for Total & Diss olved Mercury

– Episode 6564

Frontier Global Sciences (FGS) generated analytical data for total and dissolved mercury.
T he samples were analyzed according to E PA Method 1631E for total mercury by Cold Vapor Atomic Fluorescence Spectrometry (CVA

- FS) analy sis.

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

.

Table 1. EPA Episode 6564 Total & Dissolved Mercury

– Sample Identification

EPA Sample # Lab Sample

ID # Sample

M atrix Sample Description Sampling

Date Analysis

Date

71941 1012060

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

71941 1012060

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

71941 1012060

- 10 Solid FGD Influent, Day 1 (Solids) 12/ 6 /201 0 1/7/2011

71942 1012070

- 03 Aqueous FGD Inf luent, Day 2 12/ 7 /2010 1/6/2011

71942 1012070

- 04 Aqueous Dissolved FGD In fluent, Day 2 12/ 7 /2010 1/6/2011

71942 1012070

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

71943 1012100

- 03 Aqueous FGD In f luent, Day 3 12/ 8 /2010 1/6/2011

71943 1012100

- 04 Aqueous Dissolved FGD Influent, Day 3 12/ 8 /2010 12/2 3 /2010

71943 1012100

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

71944 1012110

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

71944 101 2110

- 05 Aqueous Dissolved FGD Influent, Day 4 12/9/2010 12/2 8 /2010

71944 1012110

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

71945 1012070

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

71945 1012070

- 06 Aqueous Dissolved FGD Ef fluent, Day 1 12/ 6 /2010 12/22/2010

71946 1012100

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

71946 1012100

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

71947 1012110

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

71947 1012110

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

71 9 48 1012120

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

71 9 48 1012120

- 07 Aqueous Dissolved FGD Effluent, Day 4 12/9/2010 12/28/20102 Table 1. EPA Episode 6564 Total & Dissolved Mercury

– Sample Identification

EPA Sample # Lab Sample

ID # Sample

M atrix Sample Description Sampling

Date Analysis

Date

71949 1012100

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

71949 1012100

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

71950 1012060

- 04 Aqueous FGD In fluent Field Blank

, Day 1 12/6/2010 12/22/2010

71951 1012060

- 06 Aqueous FGD Effluent Field Blank, Day 1 12/6/201 0 12/22/2010

71952 1012070

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

71953 1012100

- 11 Aqueous F GD Effluent Field Blank , Day 3 12/ 8 /2010 12/2 3 /2010

71954 1012110

- 08 Aqueous FGD Ef fluent Field Blank , Day 4 12/9/2010 12/28/2010

SUMM ARY

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

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

There were no findings from the data review that required additional qua lifiers in this

dataset.

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 anal ysis 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 instrument and preparation blanks met method s pecified criteria. Preparation Blanks

F0 12184

- BLK 1, F0 12184

- BLK 5, F0 12215

- BLK 5, F0 12215

– BLK 6, F0 12243

– BLK 6,

F 101058

– BLK 1, F 101058

– BLK 4, and F 101058

- BLK 5 had mercury levels of 0. 13, 0.19, 0.08, 0.09, 0.15, 0.15, 0.08, and 0. 20 ng/L , respectively. These bla nk results were greater than the MDL (0.08 ng/L), but less than the RL (0.50 ng/L). Because all of the blank results were less than the RL, no samples were qualified based on these preparation blank

results.3 DUPLICATES

A f ield duplicate

, Sample 71949 w a s collected on the S ample 71 9 46

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

The method

- suggested RPD criterion between field duplicates is 20%.

L aboratory duplicates were performed on samples 71941

, 71 9 4 1 ( solid )

, 71 9 4 2, and

71 9 4 7. All RPDs were less than 20% (the method

- suggested RPD criterion between field duplicates; the method does not require the analysis of laboratory duplicates), except for sample 71947, which had an RPD of 79.7%

. Because t he method does not require the analysis of laboratory duplicates, this result was not qualified.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

Matrix spikes (MS) and matrix spike duplicates (MSD) were performed on samples 71941, 71 9 4 1 ( solid ) , 71 9 4 2, and 71 9 4 7 for the total mercury analyse s

. MS and MSDs were performed on sample 71947 for the dissolved mercury analyse s. All aqueous MS/MSD recoveries were within method specifications of 70

- 125%

. All RPDs met

method

- specified criteria

.

Two sets of M S / MSD w ere performed on the solid sample 71941 f rom this episode.

MS/MSD1 did not me e t method

- specified criteria for recovery or RPD

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

MS/MSD2 did meet method

- specifie d criteria for recovery and RPD.1 

### MEMORANDUM

To: Ron Jordan

, Work Assignment Manager

, EPA EAD

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

Deb Bartram

, ERG

TJ Finseth

, ERG

From: Randy Mercurio, ERG

Date: 9 / 1 /2011 Subject: TestAmerica Data R eview Narrative for Total and Dissolved Metals by 200.8

– Episode 65 64

Test America generated analytical data for total and dissolved metals ( antimony, arsenic, cadmium, chromium, copper, lead, nickel, selenium, silver, thallium and v anadium ) for Sample Episode 6564

. T he samples were analyzed according to EPA Method 200.8

.

Tabl e 1 summarizes the samples Test America extracted and analyzed for total and dissolved metals by EPA Method 200.8

.

Table 1. EPA Episode 6563 Total & Dissolved Metals

– Sample Identification

EPA Sample

# EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

71941 FGD Influent, Day 1 280

- 10453

- 1 Aqueous 12/06/2010 12/07/2010

71941 FGD Influent, Day 1

– S olid 280

- 10453

- 3 Solid 12/06/2010 12/07/2010

71941 FGD Influent, Day 1

– F iltrate 280

- 10453

- 4 Aqueous 12/06/2010 12/07/2010

71942 FGD Influent, Day 2 280

- 10513

- 1 Aqueous 12/07/2010 12/08/2010

71942 FGD Influent, Day 2

– S olid 280

- 10513

- 4 Solid 12/07/2010 12/08/2010

71942 FGD Influent, Day 2

– F iltrate 280

- 10513

- 5 Aqueous 12/07/2010 12/08/2010

71943 FGD Influent, Day 3 280

- 10583

- 1 Aqueous 12/08/2010 12/09/2010

71943 FGD Influent, Day 3

– S olid 280

- 10583

- 3 Solid 12/08/2010 12/09/2010

71943 FGD Influent, Day 3

– F iltrate 280

- 10583

- 4 Aqueous 12/08/2010 12/09/2010

71944 FGD Influent, Day 4 280

- 10656

- 1 Aqueous 12/09/2010 12/10/2010

71944 FGD Influent, Day 4

- S olid 280

- 10656

- 4 Solid 12/09/2010 12/10/2010

71944 FGD Influent, Day 4

- F iltrate 280

- 10656

- 5 Aqueous 12/09/2010 12/10/2010

71945 FGD Effluent, Day 1 280

- 10513

- 2 Aqueous 12/07/2010 12/08/2010

71946 FGD Effluent, Day 2 280

- 10583

- 2 Aqueous 12/08/2010 12/09/2010

71947 FGD Effluent, Day 3 280

- 10656

- 2 Aqueous 12/09/2010 12/10/2010

71948 FGD Effluent, Day 4 280

- 10724

- 1 Aqueous 12/10/2010 12/11/2010

71950 FGD Influent Field Blank, Day 1 280

- 10453

- 2 Aqueous 12/06/2010 12/07/20102 Table 1. EPA Episode 6563 Total & Dissolved Metals

– Sample Identification

EPA Sample

# EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

71951 FGD Effluent Filed Blank, Day 1 280

- 10513

- 3 Aqueous 12/07/2010 12/08/2010

71955 FGD Effluent

– D uplicate 280

- 10656

- 3 Aqueous 12/09/2010 12/10/2010

SUMMARY

The samples were prepared for total and dissolved metals analysis according to TestAmerica’s “FGD ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Element Analysis in Flue Gas Desulfurization Wastewaters,” dated October 6, 2010, based on EPA Method 200.8, by ICP/MS analysis.

Any significant findings are summarized below

. No additional data qualifiers were required.

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

the EPA Method 200.8 control limits of 70

– 130% are as follows : total and

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

MS/ MSD)

.

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

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

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

control limits of ±20%.

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

failed the method criteria of 85

– 115%.

**•** The PDS for silver in the filtrate ph ase for sample 71944 failed the method

criteria of 85

– 115%.

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

of 85

– 115%.

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

71944 failed the method criteria of 85

– 115%.

INTERNAL STANDARDIZA TION

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

Test America performed the initial calibrations on each analysis day

. The initial

calibration for the ICP

- MS analysis consisted of a blank and four calibration standards

.

I NITIAL AND CONTINUING CALIBRATION VERIFICATION (ICV/CCV)

The initial calibration verifications (ICV) and continuing calibration verifications (CCV) performed by TestAmerica all had recoveries within the method criteria.

METHOD/INSTRUMENT BLANK S

All the m ethod b lanks were less than the r eporting l imit ; however, some elements were above the MDL and flagged with a “J” qualifier

. No additiona l qualifiers were required

for m eth od b lanks.

All i nstrument b lanks ( ICB and CCB) were less tha n the r eporting l imit ; however, some elements were above the MDL and flagged with a “J” qualifier. No additional qua lifiers were required for i nstrument b lanks.

REPORTING LIMIT VERIFICATION STANDARD ( CRI )

A ll CRI samples passed Test America’s SOP control limits of 50

– 150%.

LABORATORY CONTROL SAMPLE S (LCS)

All LCS samples passed the method QC limits of 85

– 115%

.

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION (ICSA)

Based on TestAmerica’s SOP, all interference check sample A (ICSA) results had analytes of interest with concentrations less than the RL or less than five times the RL when known inherent contaminants are present in the stock solution used to make the

ICS.

All interference che ck sample B (ICSAB) synthetic s pikes recovered within

TestAmerica’s SOP criteria of 70

– 130% of the true value.

SERIAL DILUTION (SRD)

The serial dilution performed for the total and dissolved sample 71 945 FGD Effluent, Day 1 (280

- 10513

- 2 ) met Test America ’s requirement of ±10% difference.4 FIELD DUPLICATES

The RPD of the field duplicates 71947/71955 for total and dissolved results were less

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

.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

MS and MSDs were performed on samples 71945 FGD Effluent, Day 1 and 71948 FGD Effluent, Day 4 for total and dissolved analytes

. The total and dissolved selenium results

in the MS and MSD samples for samples 71945 and 71948 failed the 70

– 130% method

control l imits and were flagged with a “4” qualifier indicating concentration s in the parent sample s were greater than four times the spike amount s

. Otherwise, the MS/MSD spike recoveries were always within the control limits of 70

- 13 0 % with the exception of

total and dissolved s ilver for the MS and MSD samples for both 71945 and 71948 , which were flagged with an “F” qualifier

. The RPD for all MS/MSD samples passed the

method

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

71948 and tot al silver for 71945. The poor recoveries and RPD of s ilver ar e probably due to high sulfates in this episode’s samples t hat could form insoluble silver sulfide and/or

silver s ulfate.

POST DIGESITON SPIKE S

PDSs were performed on sample 71945 FGD Ef fluent, Day 1 (280

- 10513

- 2 PD S ) and the

solid and aqueous sample of 71944 FGD Influent, Day 4 (280

- 10656

- 4 PDS ; 280

- 10656

- 5 PDS respectively ). Total and dissolved s ilver fail ed Test America’s aqueous control

limits of 8 5

– 11 5% for sample 71945

, total silver failed the filtrate of sample 71944

, and

total silver failed the solid control limits of 75

– 115% for sample 71944 . All failures were all flagged “W”

. The poor recoveries of s ilver ar e probably due to high sulfates in this episode’s sam ples that could form insoluble silver sulfide and/or silver s ulfate. The

aqueous s ample 71944 also failed Test America’s 85

- 115% control limits for total

cadm ium and total nickel, which were flagged “W”.

D ETECTION LIMITS

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead of reagent water.1 

### MEMORANDUM

To: Ron Jordan

, Work Assignment Manager

, EPA EAD

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

Deb Bartram

, ERG

TJ Finseth

, ERG

From: Randy Mercurio, ERG

Date: 9 / 1 /2011 Subject: TestAmerica Data R eview Narrative for Total and Dissolved Metals by 200.7

– Episode 65 64

Test America generated analytical data for total and dissolved metals ( aluminum, boron, barium, beryllium, calcium, cobalt, iron, magnesium, manganese, molybdenum, sodium, tin, titanium

, and z inc)

. T he samples were analyzed according to EPA Method 200. 7

.

Table 1 summarizes the s ample s Test America extracted and analy zed for total and dissolved metals by EPA Method 200.7.

Table 1. EPA Episode 6564 Total & Dissolved Metals

– Sample Identification

EPA Sample

# EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

71941 FGD Influent, Day 1 280

- 10453

- 1 Aqueous 12/06 /2010 12/07 /2010

7 1941 FGD Influent, Day 1

– Solid 280

- 10453

- 3 Solid 12/06/2010 12/07/2010

7 1941 FGD Influent, Day 1

- Filtrate 280

- 10453

- 4 Aqueous 12/06/2010 12/07/2010

7 1942 FGD Influent, Day 2 280

- 10513

- 1 Aqueous 12/07 /2010 12/ 08 /2010

7 1942 FGD Influent, Day 2

– Solid 280

- 10513

- 4 Solid 12/07 /2010 12/ 08 /2010

7 1942 FGD Influent, Day 2

– Filtrate 28 0

- 10513

- 5 Aqueous 12/07 /2010 12/ 08 /2010

71943 FGD Influent , Day 3 2 80

- 10583

- 1 Aqueous 12/08 /2010 12/ 0 9 /2010

7 1943 FGD Influent, Day 3

– S olid 280

- 10583

- 3 Solid 12/08 /2010 12/ 0 9 /2010

7 1943 FGD Influent, Day 3

– F iltrate 280

- 10583

- 4 Aqueous 12/08 /2010 12/ 0 9 /2010

7 1944 FGD Influent

, Day 4 280

- 10656

- 1 Aqueous 12/ 0 9 /2010 12 /1 0 /2010

71944 FGD Influent

, Day 4

– Solid 280

- 10656

- 4 Solid 12/ 0 9 /2010 12 /1 0 /2010

71944 FGD Influent

, Day 4

- Filtrate 280

- 10656

- 5 Aqueous 12/ 0 9 /2010 12 /1 0 /2010

7 1945 FGD Effluent, Day 1 280

- 10513

- 2 Aqueous 12/07 /2010 12/ 08 /2010

7 1946 FGD Effluent, Day 2 280

- 10583

- 2 Aqueous 12/08 /2010 12/ 0 9 /2010

71947 FGD Effluent, Day 3 280

- 10656

- 2 Aqueous 12/ 0 9 /2010 12 /1 0 /2010

71948 FGD Effluent, Day 4 280

- 10724

- 1 Aqueous 12/10 /2010 12 /1 1 /2010

71950 FGD Influent Field Blank, Day 1 280

- 10453

- 2 Aqueous 12/06/2010 12/07/20102 Table 1. EPA Episode 6564 Total & Dissolved Metals

– Sample Identification

EPA Sample

# EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

7 1951 FGD Effluent Filed Blank

, Day 1 280

- 10513

- 3 Aqueous 12/07 /2010 12/ 08 /2010

71955 FGD Ef fluent

– D uplicate 280

- 10656

- 3 Aqueous 12/ 0 9 /2010 12 /1 0 /2010

SUMMARY

The sample s were prepared for total and dissolved metals analysis according to

Test America’s SOP for ICP Analysis for Trace Metals by Method 200.7

. Any significant findings are summarized below

. No additional data qualifiers were required.

**•** The serial dilution analysis for dissolved manganese, dissolved molybdenum, and dissolved sodium for sample 71945 did not meet TestAmerica’s requirement of

± 10% difference

.

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

and zinc in the soli d phase of sample 71944 did not meet TestAmerica’s requirement of ± 10% difference

.

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

the EPA Method 200.7 control limits of 70

– 130% are as follows : dissolved barium (71945 MS/MSD) ; dissolved barium (71948 MS/ MSD); and total iron (71945 MSD).

**•** The MS/MSD relative percent difference ( RPD ) for dissolved barium for sample s 71945 and 71948 failed TestAmerica’s SOP control limits of ±20%.

**•** The post digestion spikes (PDS) for total barium for sample 71 945 failed the

method criteria of 85

– 115%.

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

method criteria of 85

– 115%.

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

method crite ria of 85

– 115%.

SAMPLE RECEIPT, HANDLING, AND STORAGE

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

The initial c alibration v erifications (ICV) and c ontinuing c alibration v erifications (CCV) performed by Test America all had recoveries within the method criteria.

METHOD/INSTRUMENT BLANK S

All the m ethod b lanks were less than the r eporting l imit ; however, some had levels above

th e MDL and were flagged with the “J” qualifier.

All i nstrument b lanks ( ICB and CCB) were less than the r eporting l imit; however, some

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

.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

All CRI samples passed Test America’s SOP control limits of 50

– 150%.

LABORATORY CONTROL SAMPLES (LCS)

All LCS passed the method control limits of 85

– 115%.

INTERFERENCE CHECK SOLUTION S

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

recoveries met the method

- specified criteria.

SERIAL DILUTION (SRD)

Serial dilutions were performed for each batch of total and dissolved samples. The serial dilution results for dissolved manganese, dissolved molybdenum and dissolved sodi um for sample 71945 FGD Effluent, Day 1 (280

- 10513

- 2) had percent differences of 25%, 22% and 20% respectively, which were appropriately flagged. The serial dilution results for total barium, total cobalt, total magnesium, total manganese, total titanium a nd total zinc of the solid fraction for sample 71944 FGD Influent, Day 4 (280

- 10656

- 4) had4 percent differences of 41%, 53%, 51%, 50%, 44% and 43% respectively, which were also appropriately flagged. No additional qualifiers were required.

FIELD DUPLICATES

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

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

.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

MS and MSD were performed on the total and dissolved sample s of 71945 FGD Effluent, Day1 (280

- 10513

- 2) and 71948 FGD Effluent, Day 4 (280

- 10724

- 1)

. Some elements with high concentrations frequently failed the EPA 200.7 Method spike recovery control

limits of 70

– 130% but were flagged with a “4” qualifier indicating tha t the concentration in the parent sample was greater than 4 times the spike and could not be reliably

calculated

. Otherwise, the MS/MSD spike recoveries were always within the control

limits of 70

- 130% with the exception of d issolved barium for both the MS and MSD for sample s 71945 and 71948 and the total iron MSD for sample 71945. All relative percent differences (RPDs) were within ± 20% with the exception of dissolved barium for both samples 71945 and 71948

. N o additional data qualifiers were needed

.

POST DIGESTION SPIKE

The PDS of sample 71945 FGD Effluent, Day 1 (280

- 10513

- 2 PDS) failed the method

criteria of 85

– 115% for total barium, which was flagged. The solid fraction PDS of sample 71944 FGD Influent, Day 4 (280

- 10656

- 4 PDS) failed for magnesium and tin, which were flagged

. The filtrate fraction PDS of sample 71944 FGD Influent, Day 5 (280

- 10656

- 5 PDS) failed for titanium and zinc, which were flagged. No additional qualifiers were required.

D ETECTION LIMITS

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead of reagent water.1 

### MEMORANDUM

To: Ron Jordan

, Work Assignment Manager

, EPA EAD

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

Deb Bartram

, ERG

TJ Finseth

, ERG

From: Donna Tedder, ERG

Date: 9 / 1 /201 1 Subject: FGS Data R eview Narrative for Dissolved Hexavalent Chromium

– Episode

65 6 4

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

chromium for Sample Episode 6564

. T he samples were analyzed according to a

m odified EPA Method 2 18. 6 for dissolved hexavalent chromium by Liquid Chromatography

– Inductively Coupled Plasma Mass Spectrometry (LC

- ICP

- MS)

.

Table 1 summarizes the s amples FGS prepared and analyzed for dissolved hexavalent

chromium

.

Table 1. EPA Episode 6564 Dissolved Hexavalent Chromium

– Sample

Identification

EPA Sample # Sample

Matrix Sample Description Sampling

Date Analysis

Date

71 9 4 1 Aqueous FGD Influent Day 1 12 / 6 / 10 1 2 / 29 /10

7 1943 Aqueous FGD Influent Day 3 12/8/10 12/29/10

7 1944 Aqueous FGD Influent Day 4 12/9/10 12/29/10

7 1945 Aqueous FGD Effluent Day 1 12/7/10 12/29/10

7 1946 Aqueous FGD Effluent Day 2 12/8/10 12/29/10

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

7 1950 Aqueous FGD In fluent Field Blank Day 1 12/6/10 12/29/10

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

7 1955 Aqueous FGD Effluent Dup Day 3 12/9/10 12/29/10

SUMMARY

The samples were prepared for dissolved hexavalent chromium analysis according to

FGS

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

. S amples 71 9 4 1, 71 9 4 3, and 71 9 4 4 were diluted prior to analysis due to the presence of high levels of nontarget chloride interferences

. T here were no issues requiring additional

data qualifiers for the hexavalent chromium data in this episode.2 SAMPLE REC E IPT, HANDLING, AND STORAGE ISSUES

The collection date and time were not recorded on the chain of custody for s ample s 71945 and 71951

.

I NITIAL P RECISION AND ACCURACY/ R ECOVERY

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

method criteria.

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 blank and eight calibration standards with a

correlation factor ≥ 0.995 as re quired by the method

.

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

of true value required by the analytical method

.

C ONTINUING C ALIBRATION V ERIFICATION

All CCVs met method

- specified criteria

, ± 10% of true value with recoveries ranging

from 9 4.9 to 95.5 %.

BLANK

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

- specified requirements

.

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 96 % and 95 %

. The method suggested that a second source quality control sample (QCS) must be analyzed by the laborator y at least once a quarter. The second

source ICV meets this recommendation

.

D ETECTION LIMITS

The laboratory method detection limit (MDL) in the synthetic matrix was 0.392 ug/L. Results below this MDL were reported as not detected.3 DUPLICATES

There were no laboratory duplicates performed in this episode other than a duplicate of

the LCSD and a duplicate of the matrix spike ( MS ).

One field duplicate w as collected and analyzed. Sample 719 55

, was a duplicate of

effluent sample 719 47

, with an RPD of 8 %.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

The M S and matrix spike duplicate ( MSD ) were performed using a secondary source spike on sample 71 9 48

. Two set of MS/MSD were performed at two different

concentration levels. The MS/MSD 1 (spiked at 50 ug /L) r ecoveries were within criteria,

9 2

. 5 % and 91.0 %, with an RPD of 1.59 %. The MS/MSD 2 (spiked at 250 ug/L)

r ecoveries were within criteria

, 96. 2 % and 9 6

. 8 %, with an RPD of 0.56 %.1 

### MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD Deb Bartram, ERG TJ Finseth, ERG

From: Donna Tedder , ERG

Date: 9 / 1 / 20 11 Subject: TestAmerica Data Review Narrative for Cla ssicals Analyses

– Episode 65 64

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry analyses for Sample Episode 65 64

. All samples were tested for the following analytes:

**•** Ammonia by EPA method 350.1,

**•** Biochemical Oxygen De mand

– 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 an d liquid portions of the samples and

a nalyzed both portion s separately for the following analytes :

**•** Ammonia,

**•** Chloride

**•** Cyanide,

**•** Nitrate/Nitrite,

**•** Phosphorus,

**•** Sulfate, and

**•** TKN.

Table 1 summarizes the nine field sampl es analyzed by TestAmerica and partic ularly highlights how the laboratory split and analyzed the influent samples

.2 Table 1. EPA Episode 65 6 4 Classical Analytes

– Sample Identification

EPA Sample # Sample Description Sampling

Date Sample

Matrix Portion of Sample Analytes

719 41 FGD Influen t, Day 1 12/06 /10 Water Entire

Fraction BOD 5 , COD, TDS, and

TSS

Water Filtrate Ammonia, Chloride, Cyanide, Nitrate/Nitrite, Phosphorus, Sulfate, and

TKN

Solids Solids Ammonia, Chloride, Cyanide, Nitrate/Nitrite, Phosphorus, Sulfate, and

TKN

719 42 FGD Influent, Day 2 12/07 /10 Water Entire

Fraction BOD 5 , COD, TDS, and

TSS

Water Filtrate Ammonia, Chloride, Cyanide, Nitrate/Nitrite, Phosphorus, Sulfate, and

TKN

Solids Solids Ammonia, Chloride, Cyanide, Nitrate/Nitrite, Phosphorus, Sulfate, and

TKN

719 43 FGD Influent, Day 3 12/08 /10 Water Entire

Fraction BOD 5 , COD, TDS, and

TSS

Water Filtrate Ammonia, Chloride, Cyanide, Nitrate/Nitrite, Phosphorus, Sulfate, and

TKN

Solids Solids Ammonia, Chloride, Cyanide, Nitrate/Nitrite, Phosphorus , Sulfate, and

TKN

719 44 FGD Influent, Day 4 12/09 /10 Water Entire

Fraction BOD 5 , COD, TDS, and

TSS

Water Filtrate Ammonia, Chloride, Cyanide, Nitrate/Nitrite, Phosphorus, Sulfate, and

TKN

Solids Solids Ammonia, Chloride, Cyanide, Nitrate/Nitrite, Phosphorus, Sulfate, and

TKN

719 45 FGD Effluent, Day 1 12/07 /10 Water Entire

Fraction All analytes3 EPA Sample # Sample Description Sampling

Date Sample

Matrix Portion of Sample Analytes

719 46 FGD Effluent, Day 2 12/08 /10 Water Entire

Fraction All analytes

719 47 FGD Effluent, Day 3 12/09 /10 Water Entire

Fraction All analytes

719 48 FGD Ef fluent, Day 4 12/10 /10 Water Entire

Fraction All analytes

71955 FGD Effluent

- Duplicate 12/09 /10 Water Entire

Fraction All analytes

SUMMARY

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

unless otherwise noted below

.

TestAmerica could not use a preserved sample volume for phase separation. Therefore, they combined two of the unpreserved 250 mL metal sample volumes and phase separated this volume. After phase separation, TestAmerica preserved the samples accordingly. Because of this process, ammonia, nitrate/nitrite, TKN, phosphorus, and cyanide influent samples were not preserved immediately following sample collection as required by the method.

One field duplicate sample was collected and analyzed for each analyt e. The 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 high est 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 calibration blanks and calibration verification samples met the criteria sp ecified 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 det ected 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 c riteria specified in the method unless specified

below

.

If required by the method, a matrix spike (M S) analysis was run on sample 71 948 (FGD

effluent ) for each analyte to check for matrix interferences

. For some analytes,

TestAmerica s piked more than one sample

. All MS samples analyzed met the criteria specified in the method unless described below.4 DATA NOTES /ISSUES

Ammonia

As stated above, filtrate and solid aliquots of samples 71 9 41

- 71 9 44 were not preserved immediately after sample collection. Ins tead

, TestAmerica preserved the sample after phase separation. The filtrate volume of samples 71941

- 71944 were already qualified by

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

less than the RL, so there was no n eed to further qualify these samples. The solid aliquot

of s amples 71941

- 71944 were qualified as estimated value s because the samples were not preserved immediately following sample collection

.

The filtrate and solid aliquots of sample s 71 9 41 , 71 9 42, 71 9 43, and 71 9 44 were analyzed 9, 8, 7, and 6 day s , respectively, after the 28

- day hold time. These samples were already qualified as estimated values either because their result was less than the RL or because they were not preserved immediately following s ample collection, so no further action

was necessary.

Ammonia was detected at 0.0610 mg/L in the LRB associated with samples 71945 and 71946. The blank result was above the MDL (0.055 mg/L), but below the RL (1.0 mg/L),

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

BOD 5

TestAmerica analyzed five dilutions, but no dilutions had a dissolved oxygen (DO) depletion greater than 2.0 mg/L for sample 71 945

. 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.

BOD was not detected above the RL in any method blanks. However, for batch 44128, the results for the three water/unseeded blanks were 0.23 mg/L, 0.21 mg/L, and 0.19 mg/L. Two of these water blanks were above the method control criteria of 0.20 mg/L.

Because of th ese blank results, sample 71 9 4 1 was qualified with a “B” meaning the analyte was detected in the sample and the blank.

The glucose

- glutamic acid (GGA) s tandards associated with sample 71948 h ad percent

recover ies of 8 4% and 86 %

. The perce nt recovery of the first GGA standard was below

the meth od and laboratory criteria of 85

- 115%. TestAmerica flagged sample 71948 with a “*” meaning the laboratory control sample was not within laboratory control limits. Sample 71 94 8 w as additionally qualifi ed as a minimum value.5 Chloride and Sulfate

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

d ays, respectively, after the 28

- day hold time. Additionally, f iltrate aliquots of samples 71941, 71942, 71943, and 71944 we r e analyzed 8, 7, 6, and 5 days , respectively, outside

of the 28

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

The laboratory diluted the MS and MSD sample s for 71 941 and 71948 by 200 , but the

diluted result s for sulfate and chloride w e re still above the highest calibration standard. The laboratory did not reanalyze these sample s with a higher dilution factor, because the

MS and MSD percent recover ies w ere within the control limits specified by EPA method 300.0. Therefore, if the MS and MSD result s for sample 71 941 for chloride and sulfate

are reported, they will be qualified as estimated value s

. The results for samples 71941 and 71948 were within the calibration range, so there was no need to qualify these samples. The LFB associated wit h sample 71941 and 71948 met the method criteria.

COD

Sample s 71941, 71943, and 71944 were preserved to pH less than 2 S.U. after sample collection. However, when the laboratory received the sample s
, the p H was neutral. The sample s w ere preserved again b y the laboratory. These samples were qualified as

estimated values.

T he percent recoveries for the MS and MSD samples associated with 71 948 were 93%

and 79%

, respectively. Only the MS sample was within the control limits of 90

- 11 0% specified in the meth od. However, since the method does not require an MSD analysis

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

. Also

, the MS

and MSD results associated with sample 71948 were above 150 mg/L. COD is calculated using a reverse curve m eaning that the 200 mg/L calibration point represents the zero in the curve and the 0 mg/L calibration point represents the highest absorbance.

TestAmerica has noticed that results in the 150

- 200 mg/L range yield inconsistent results, so typically the lab dilutes these samples and reanalyzes. The MS and MSD samples

associated with 71948 were not diluted further and reanalyzed, so TestAmerica flagged them with an “E” meaning that the results exceeded the calibration range. If reported, the

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

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

and 71 %

, respectively. Both the MS and MSD sample results for this sample were not
within the control limits specifi ed in the method. Sample 71941 was already qualified as an estimated value because the sample was not preserved appropriately, so there was no need to further qualify the sample as a minimum value. The LFB associated with sample

71941 and 71948 met the met hod criteria.6 Cyanide

As stated above, filtrate and solid aliquots of samples 71 941

- 719 44 were not preserved immediately after sample collection. Instead

, TestAmerica preserved the sample after phase separation. Filtrate aliquots of samples 71 9 41 and 71944 were already qualified by the laboratory with a “J” meaning the sample result was an estimated value because it

was less than the RL, so there was no need to further qualify these samples. Because the filtrate aliquots of samples 71942 and 71943 and the solid aliquots of samples 71 9 41

- 71 9 44 were not preserved immediately following sample collection as required by the method, these samples were qualified as estimated values.

Solid and filtrate aliquots of s ample s 71941, 71942, 71943, and 71944 were analyzed 25, 24, 23, and 22 days , respectively, outside of the 14

- day holding time. These samples were already qualified as estimated values because they were not preserved immediately following sample collection as required by the method, so no further qu alification was

necessary.

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

interferences

. The laboratory stated that the samples foamed during preparation and in order to protect the instruments, the samples needed t o be diluted. T he diluted result s for the filtrate aliquot of sample s 71 941 and 71944 w ere less than the lowe st calibration

standard. However , these samples were already qualified by the laboratory with a “J” meaning the sample result was an estimated valu e because it was less than the RL, so there was no need to further qualify these samples.

The percent recoveries for the MS and MSD samples associated with sample 71948 were 79% and 78%, respectively. These percent recoveries were not within the laborator y control criteria of 90

- 110%. Additionally, t he percent recoveries for the MS and MSD samples associated with sample 71955 were 67% and 69%, respectively. These percent recoveries were also not within the laboratory control criteria. Since there are no MS or MSD criteria specified in SM 4500 CN - E

, samples 71948 and 71955 were not qualified based on the low MS and MSD percent recoveries. The LFBs associated with samples

71948 and 71955 met the method criteria.

The RPD between sample 71947 and its field d uplicate 71 9 55 for cyanide was 46.2 %. Even though the RPD was greater than 20%, the sample was not qualified because there are no control limits for field duplicates specified in SM 4500 CN - E.

Nitrate/ Nitrite

As stated above, filtrate and solid aliqu ots of samples 71 9 41

- 71 9 44 were not preserved immediately after sample collection. Instead

, TestAmerica preserved the sample after phase separation. Because these samples were not preserved immediately following sample collection as required by the metho d, these samples were qualified as estimated

values.7 The filtrate and solid aliquots of s amples 71941, 71942, 71943, and 71944 were analyzed 11, 10, 9, and 8 days , respectively, outside of the 28

- day hold time. These samples were already qualified as esti mated values because they were not preserved immediately following sample collection, so no further action was necessary.

TestAmerica diluted the MS and MSD samples for 71948 by 20 fold , but the analyzed result was still above the highest calibration stan dard. The samples were not diluted and reanalyzed because the percent recoveries were within the control limits spe cified in the

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

values. The result for sample 71948 was wit hin the calibration range, so there was no need to qualify this sample. The LFB associated with sample 71948 met the method

criteria.

Phosphorus

As stated above, filtrate and solid aliquots of samples 71 9 41

- 71 9 44 were not preserved immediately after sample collection. Instead

, TestAmerica preserved the sample after phase separation. The solid aliquot of sample 719 44 was already qualified by the laboratory with a “J” meaning the sample result was an estimated value because it was

less than the RL, so t here wa s no need to further qualify this sample. Phosphorus was not detected in the solid aliquot for sample 71941, so there was no need to further qualify this sample. Solid samples 719 42 and 71943 and filtrate samples 71941

- 71944 were qualified as esti mated values because they were not preserved immediately following sample collection as required by the method

.

Filtrate and solid aliquots of s amples 71941, 71942, 71943, and 71944 were analyzed 10, 9, 8, and 7 days, respectively, past the 28

- day ho ld ti me. These samples were not
detect ed

, already qualified with a “J”, or qualified as estimated values because they were not preserved immediately following sample collection, so no further action was

necessary.

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

of samples 71941

- 71944

. Phosphorus was also detected at 0.0103 mg/L in the LRB

associated with sample 71948

. Additionally, p hosphorus was detected at 0.0103 mg/L in

the LRB associated with sample s 71945, 71946, 71 947, and 71955. Since all of these

blank results were less than the RL (0.050 mg/L)

, no samples were qualified based on

these LRB results.

The percent recoveries for the MS and MSD anal ys e s for sample 71948 were not within

the method control limits of 90

- 110% or within the laboratory control limits of 71

- 128%

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

. Sample 71 948 was already qualified by the laboratory with a “J” meaning the sample

result was an estimated value beca use it was less than the RL, so there was no need to further qualify this sample as a minimum value. The LFB associated with sample 71948

met the method criteria.8 TDS

One l aboratory duplicate was analyzed on sample 71948

. The RPD between this sample

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

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

Samples 71941, 71942, 71943, 71945, 71946, 71947, 71948, and 71955 did not achieve a constant weight after thr ee drying cycles. The weight increased from the first weighing to the second weighing for sample 71948. SM 2540C warns that samples that contain high levels of calcium, magnesium, chloride, and sulfate may be hygroscopic, meaning they

absorb moisture from the air. FGD wastewater contains high concentrations of all of these species, so this may be the cause for the inconsistent weight calculations. These samples were not qualified , but results may be biased high

.

The RPD between sample 71947 and its field d uplicate 71 9 55 for TDS was 24 %. Even though the RPD was greater than 20%, the sample was not qualified because there are no control limits for field duplicates specified in SM 2540C

.

TKN

As stated above, filtrate and solid aliquots of samples 71 941

- 71 9 44 were not preserved immediately after sample collection. Instead

, TestAmerica preserved the sample after phase separation. Because these samples were not preserved immediately following sample collection as required by the method, these samples were qua lified as estimated

values.

Filtrate and solid aliquots of samples 71941, 71942, 71943, and 71944 were analyzed 10, 9, 8, and 7 days

, respectively , past the 28

- day hold time. These samples were already qualified as estimated values because they were not p reserved immediately following sample collection, so no further action was necessary.

TKN was detected at 0.264 mg/L in the laboratory reagent blank associated with the filtrate aliquot of samples 71941

- 71944

. Because this blank result was less than th e RL (1.0 mg/L) , no samples were qualified based on th is LRB result.

TestAmerica preformed MS and MSD analysis on sample 71 948 . T he percent recoveries

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

control limits of 90

- 11 0% , but did meet the laboratory control limits of 54

- 131%. The sample concentration was greater than 4 times the spike amount in the MS and MSD samples , so TestAmerica stated that the percent recoveries and RPDs could not be reliably calculated. Sample 71 9 48 was not qualified because it is not possible to

determine if the MS and MSD failure s w ere a result of matrix interferences or the low spiking level. The LFB associated with sample 71948 met the method criteria.9 TSS

Two laboratory du plicates were anal yzed for TSS . The RPD for sample 71941 and its duplicate was less than 10% as required by the method ; h owever, the RPD for sample 71948 and its duplicate was 50%. The result for 71948 was at the RL (4.0 mg/L) and the result for the laboratory duplicate was 2.40 mg/L, which was less than the RL. The low concentration of TSS was likely the cause for the high RPD value. Sample 71948 was qualified as an estimated value.10 Table 2 . Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level

Detecte d 71941 (solid) Ammonia H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 9 days past holding

time. 15 mg/Kg

71942 (solid) Ammonia H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 8 days past holding

time. 12 mg/Kg

71943 (solid) Ammonia H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 7 days past holding

time. 11 mg/Kg

71944 (solid) Ammonia H, Estimated

Value Sample not preserved immediately following

co llection. Analyzed 6 days past holding

time. 15 mg/Kg

71941 BOD B Unseeded water blank

> method

- specified

criteria 3.0 mg/L

71948 BOD Minimum Value GGA % recovery

below method

specified criteria 2.6 mg/L

71941 (solid) Chloride H, Estimate d

Value Analyze d 9 days past holding time. 1,500 mg/Kg 71942 (solid) Chloride H, Estimate d

Value Analyzed 8 days past holding time. 3,000 mg/Kg 71943 (solid) Chloride H, Estimate d

Value Analyzed 7 days past holding time. 1,900 mg/Kg 71944 (solid) Chloride H, Estimate d

Value Analyzed 6 days past holding time. 2,200 mg/Kg 71941 (filtrate) Chloride H, Estimate d

Value Analyzed 8 days past holding time. 6,100 mg/L

71942 (filtrate) Chloride H, Estimate d

Value Analyzed 7 days past holding time. 9,400 mg/L

71943 (filtrate) Chloride H, Estimate d

Value Analyzed 6 days past holding time. 8,700 mg/L11 Table 2 . Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level

Detecte d 71944 (filtrate) Chloride H, Estimate d

Value Analyzed 5 days past holding time. 6,800 mg/L

71941 (solid) Sulfate H, Estimate d

Value Analyzed 9 days past holding time. 27,000 mg/Kg 71942 (solid) Sulfate H, Estimate d

Value Analyzed 8 days past holding time. 29,000 mg/Kg 71943 (solid) Sulfate H, Estimate d

Value Analyzed 7 days past holding time. 24,000 mg/Kg 71944 (solid) Sulfate H, Estimate d

Value Analyzed 6 days past holding time. 27,000 mg/Kg 71941 (filtrate) Sulfate H, Estimate d

Value Analyzed 8 days past holding time. 9,700 mg/L

71942 (filtrate) Sulfate H, Estimate d

Value Analyzed 7 days past holding time. 11,000 mg/L 71943 (filtrate) Sulfate H, Estimate d

Value Analyzed 6 day s past holding time. 9,300 mg/L

71944 (filtrate) Sulfate H, Estimate d

Value Analyzed 5 days past holding time. 9,800 mg/L

71941 COD Estimated Value pH upon receipt > 2

S.U. , MS % recovery

below method

specified criteria 250 mg/L

71943 COD Estimated Val ue pH upon receipt > 2

S.U. 350 mg/L

71944 COD Estimated Value pH upon receipt > 2

S.U. 280 mg/L

71942 (filtrate) Cyanide H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 24 days past holding

time. 0.19 mg/L

71943 (fi ltrate) Cyanide H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 23 days past holding

time. 0.16 mg/L

71941 (solid) Cyanide H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 25 days past h olding

time. 0.54 mg/Kg12 Table 2 . Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level

Detecte d 71942 (solid) Cyanide H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 24 days past holding

time. 0.69 mg/Kg

71943 (solid) Cyanide H, Estimated

Value Sample not preserved immediately following

col lection. Analyzed 23 days past holding

time. 0.73 mg/Kg

71944 (solid) Cyanide H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 22 days past holding

time. 0.96 mg/Kg

71941 (solid) Nitrate/Nitrite H, Estimated

Value Sample not preserved immediately following

collection. Analyzed

11 days past holding

time. 34 mg/Kg

71942 (solid) Nitrate/Nitrite H, Estimated

Value Sample not preserved immediately following

collection. Analyzed

10 days past holding

time. 69 mg/Kg

71943 (soli d) Nitrate/Nitrite H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 9 days past holding

time. 39 mg/Kg

71944 (solid) Nitrate/Nitrite H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 8 day s past holding

time. 49 mg/Kg

71941 (filtrate) Nitrate/Nitrite H, Estimated

Value Sample not preserved immediately following

collection. Analyzed

11 days past holding

time. 140 mg/L13 Table 2 . Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level

Detecte d 71942 (filtrate) Nitrate/Nitrite H, Estimated

Value Sample not preserved immediately following

collection. Analyzed

10 days past holding

time. 230 mg/L

71943 (filtrate) Nitrate/Nitrite H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 9 days past holding

time. 170 mg/L

71944 (filtrate) Nitrat e/Nitrite H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 8 days past holding

time. 140 mg/L

71942 (solid) Phosphorus H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 9 days past holding

time. 250 mg/Kg

71943 (solid) Phosphorus H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 8 days past holding

time. 190 mg/Kg

71941 (filtrate) Phosphorus H, Estimated

Value Sample not preserved immediately following

col lection. Analyzed

10 days past holding

time. 0.12 mg/L

71942 (filtrate) Phosphorus H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 9 days past holding

time. 0.14 mg/L

71943 (filtrate) Phosphorus H, Estimated

Value Sampl e not preserved immediately following

collection. Analyzed 8 days past holding

time. 0.13 mg/L14 Table 2 . Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level

Detecte d 71944 (filtrate) Phosphorus H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 7 days past holding

time. 0.11 mg/L

71948 TDS Es timated Value Laboratory duplicate

RPD > method

specified criteria 15,000 mg/L

71941 (solid) TKN H, Estimated

Value Sample not preserved immediately following

collection. Analyzed

10 days past holding

time. 560 mg/Kg

71942 (solid) TKN H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 9 days past holding

time. 500 mg/Kg

71943 (solid) TKN H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 8 days past holding

time. 83 mg/Kg

71944 (solid) TKN H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 7 days past holding

time. 620 mg/Kg

71941 (filtrate) TKN H, Estimated

Value Sample not preserved immediately following

collection. Analyzed

10 days past holding

time. 14 mg /L

71942 (filtrate) TKN H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 9 days past holding

time. 25 mg/L15 Table 2 . Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level

Detecte d 71943 (filtrate) TKN H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 8 days pa st holding

time. 36 mg/L

71944 (filtrate) TKN H, Estimated

Value Sample not preserved immediately following

collection. Analyzed 7 days past holding

time. 14 mg/L

71948 TSS Estimated Value Laboratory duplicate

RPD > method

specified criteria 4.0 mg/L