# Appendix A

Duke Energy Carolinas’ Belews Creek Steam Station

## Section 1

CWA 308 Monitoring Letter and Instructions

### Enclosure 1

Instructions for Sample Collection, Packaging, and Shipment

EPA Sampling Program

The samples you will be collecting are very important. The samples will be used by the

U.S. Environmental Protection Agency (EPA) for revising th e effluent limitations

guidelines and standards for the Steam Electric Power Gen erating Industry.

These instructions are being provided to Duke Energy Carolinas’ Belews Creek Steam

Station to aid in collecting, packaging, and shipping sample s for this sampling program.

The plant must collect grab samples for all analytes a t the influent to the FGD wastewater

treatment sampling point and 24-hour composite samples for all analytes except mercury

and cyanide at the bioreactor influent and bioreactor efflue nt sampling points. At the

bioreactor influent and bioreactor effluent, the plant must collect cyanide as a single grab

sample and mercury must be collected as four individual grab samples over the 24-hour

period (i.e., a grab sample collected every six hours).

Samples will be collected once a month for four month s. The samples should be

collected and shipped to the laboratories according to the schedule provided in the cover

letter of this request. If the plant has any questions re garding the timeline or the steps

provided, please contact Mr. Ronald Jordan at (202) 566-1003 or j ordan.ronald@epa.gov.

Equipment Needed

The plant will need to obtain the following equipment to collect, pack, and ship the

samples to the laboratories:

• Sample bottles, composite containers, and tubing sets (spe cially-cleaned

according to EPA Method 1669);

• Automatic compositor;

• Powder-free gloves;

• Tyvek® coveralls or suitable alternative;

• Dust masks (for use while collecting mercury samples)

• Labels (for sample bottles and shipping samples to labora tories);

• Preservation supplies (see the “Sample Bottles and Pr eservation” Section);

• Coolers;

• Garbage bags;

• Packing material;

• Strapping tape; and

• Traffic Report (will be provided by ERG).

### Sampling Points

The plant must collect samples once per month for four months, based on the schedule

specified in the letter. Samples are to be collected fr om each of the three sampling points

included in the EPA’s sampling episode. Figure 1 identifies e ach of the sampling points

for this sampling program. The following is a description o f the three sampling points:

• 

### FGD wastewater treatment influent (FGD scrubber purge) (SP-1) : This

sampling point shall represent the FGD purge stream (e.g., hydroclone overflow)

transferred to the FGD wastewater treatment system pri or to any commingling

with other wastewaters or treatment system recycle s treams. This sample should

be collected from the sample tap on the pipe that flow s from the purge tank to the

equalization tank.

• 

### FGD bioreactor influent (SP-2) : This sampling point shall represent the effluent

from the chemical precipitation system and the influent to the biological treatment

system (prior to nutrient addition). This sampling point s hould be collected from

the sample tap on the pipe that is downstream of the sa nd filters and the hold tank,

but upstream of the heat exchanger.

• 

### FGD wastewater treatment effluent (SP-3) : This sampling point shall represent

the effluent from the biological treatment system, pri or to mixing with dilution

water or other streams. This sampling point should be col lected from the sample

tap that is located on the pipe downstream of the secon d-stage bioreactor cells.

Analytes

The analytes included in this sampling program include all ana lytes from EPA’s sampling

program, except for the dissolved metals analyses (which includes hexavalent

chromium). Table 1 contains the listing of all the an alytes included in the monitoring

program, as well as the analytical methods that will be used to analyze the samples.

### Table 1. Analytes and Analytical Methods Included in the Moni toring Program

Parameter Method Number

Classicals

Biochemical oxygen demand (BOD 5 ) SM 5210 B

Chemical oxygen demand (COD) EPA 410.4

Total suspended solids (TSS) SM 2540 D

Total dissolved solids (TDS) SM 2540 C

Sulfate EPA 300.0

Chloride EPA 300.0

Ammonia as nitrogen EPA 350.1

Nitrate/nitrate as nitrogen EPA 353.2

Total Kjeldahl nitrogen (TKN) EPA 351.2

Total phosphorus EPA 365.1

Total cyanide SM 4500 CN E

Total Metals

Total mercury EPA 1631E

Antimony, arsenic, cadmium, chromium, copper, lead, nickel,

selenium, silver, thallium, vanadium, and zinc EPA 200.8 with collision

cell

Aluminum, barium, beryllium, boron, calcium, cobalt, ir on,

magnesium, manganese, molybdenum, sodium, tin, and titani um EPA 200.7FGD Scrubber Purge(from Purge Tank)LimePolymerEqualizationTankReaction Tank 1ReactionTank 2ReactionTank 3SP-1SP-2Indicates a Sampling PointFerricChlorideFilter2HoldingTankClarifier 1SludgeStorageTankFilter PressSumpFilterBackwashFilter1Solids to FlyAsh LandfillWastewater FlowSludge FlowIntermittent Wastewater FlowClarifierSludgeMixChamberClarifier 2Filter3Cooling WaterNutrientFirst-StageBioreactors(8)First-StageEffluentStorageSecond-StageBioreactors(8)Second-StageEffluentStorageTo Ash BasinBio Reactor BackflushHydrochloricAcidSP-3Figure 1. Belews Creek FGD Wastewater Treatment System Monitoring Program Sampling Points

### Sample Bottles and Preservation

Table 2 identifies the sample bottles that are needed fo r collecting samples. The table

also identifies the on-site preservation that is requi red for the samples. Please note that

the number of sample bottles listed in Table 2 refers t o the number of bottles that will

need to be collected from each sampling point for each of the four sets of samples. For

the Group II samples, the plant can either preserve the samples with sulfuric acid after

sample collection, or the plant can order pre-preserv ed sample bottles.

For the total cyanide samples, the plant should test the wastewater from the sampling

points with lead acetate paper (turns black in the presence of sulfide) and potassium

iodide starch paper (turns blue/violet in the presence of chl orine). If sulfide is present,

the plant will need to dilute the sample with blank water until the sulfide is not detected

by the lead acetate paper. If chlorine is present, then t he plant will need to add sodium

arsenite until the chlorine is not detected by the potass ium iodide starch paper. After any

dilution and/or sodium arsenite is added to the sample, the plant will need to preserve the

sample with sodium hydroxide until the sample reaches a pH of 10 S.U. Please see

ASTM Method D 7365-09a for more details on the preservation requirements for total

cyanide.

Table 2. Summary of Sample Container and Planned Preservation

Parameter Sample Container

and Volume On-Site Preservation

BOD 5 One 1-L HDPE

bottle ≤ 6 ° C

Group I a One 1-L HDPE

bottle ≤ 6 ° C

Group II b Two 1-L HDPE

bottles H 2 SO 4 to pH <2, ≤ 6 ° C

Total cyanide One 1-L HDPE

bottle Dilution until sulfide is not detected,

NaAsO 2 until total chlorine is not

present, NaOH to pH >10, ≤ 6 ° C

Total metals (EPA Method 200.8 with

collision cell) One 500-mL HDPE

bottle None

(acid preserve at laboratory)

Total metals (EPA Method 200.7) One 500-mL HDPE

bottle None

(acid preserve at laboratory)

Total mercury:

Laboratory composite grab samples at

bioreactor influent and bioreactor effluent Four 125-mL glass

bottles

Influent samples and field blank samples Two 250-mL glass

bottles None

(acid preserve at laboratory)

(a) Group I includes TSS, TDS, sulfate, and chloride.

(b) Group II includes ammonia as nitrogen, COD, nitrate/nit rite as nitrogen, TKN, and total phosphorus.

NOTE: The number of sample bottles refers to the number of sample bottles needed for each sampling point for each of

the four sets of samples.

### Sample Labeling

Label each bottle prior to collecting the sample so i t can be identified by the laboratory.

Each self-adhesive label must be completed in indelible ink and must contain the

following information:

• Sample number (see Table 3);

• Sampling episode number (see Table 3);

• Sampling point/description (see Table 3);

• Date of sample collection;

• Analysis to be performed;

• Sample bottle type; and

• Required on-site preservation.

If any of the information is incorrect, the plant must revise the label using indelible ink.

Once applied to the sample container, the plant must co ver the labels with clear tape to

prevent tampering, abrasion, smearing, or loss during trans it. For metal and mercury

samples, do not place labels directly on the sample bot tles because of the potential for

contamination. Instead, place the label on the outer pl astic bag of the sample bottle. To

ensure that the sample label does not become separated from the bottle, the doublebagged sample bottle should be placed in an additional Zi ploc bag after collection.

Table 3 provides the sampling point descriptions, sample numbe rs, and sampling episode

number for the plant for this monitoring program. The info rmation in the table should be

provided on the sample bottle labels for the appropriate bottles. The “analysis to be

performed” should be shown on the label as the followi ng, depending on the specific

analysis:

• BOD;

• Group I;

• Group II;

• Total Cyanide;

• Total Metals – 200.8 w/ CC;

• Total Metals – 200.7;

• Total Mercury (for influent and field blank samples);

• Total Mercury – Grab 1 (for bioreactor influent and bioreacto r effluent

laboratory composite samples. The bottles should be l abeled as Grab 1,

Grab 2, Grab 3, and Grab 4 for the four respective collec tion times).

The “sample bottle type” should be shown on the label t he same as the “Sample

Container and Volume” column in Table 2, except that the quantity should not be

included. For example, for total mercury, the “sample bo ttle type” should be “250-mL

glass bottle.” The “required on-site preservation” sh ould be shown on the label the same

as the “On-Site Preservation” column in Table 2, exce pt that “(acid preserve at

laboratory)” does not need to be included for the total me tals and total mercury sample

bottles.

### Table 3. Sampling Point Descriptions and Sample Numbers for Monitoring

Program

Sampling Point Description Sample Number Sampling Episode Number

FGD Wastewater Treatment Influent – Set 1 71991 6565

FGD Wastewater Treatment Influent – Set 2 71992 6565

FGD Wastewater Treatment Influent – Set 3 71993 6565

FGD Wastewater Treatment Influent – Set 4 71994 6565

FGD Bioreactor Influent – Set 1 71995 6565

FGD Bioreactor Influent – Set 2 71996 6565

FGD Bioreactor Influent – Set 3 71997 6565

FGD Bioreactor Influent – Set 4 71998 6565

FGD Bioreactor Effluent – Set 1 71999 6565

FGD Bioreactor Effluent – Set 2 72000 6565

FGD Bioreactor Effluent – Set 3 72001 6565

FGD Bioreactor Effluent – Set 4 72002 6565

FGD Wastewater Treatment Influent Field Blank 72003 6565

FGD Bioreactor Influent Field Blank – Set 1 72004 6565

FGD Bioreactor Influent Field Blank – Set 2 72005 6565

FGD Bioreactor Influent Field Blank – Set 3 72006 6565

FGD Bioreactor Influent Field Blank – Set 4 72007 6565

FGD Bioreactor Effluent Field Blank – Set 1 72008 6565

FGD Bioreactor Effluent Field Blank – Set 2 72009 6565

FGD Bioreactor Effluent Field Blank – Set 3 72010 6565

FGD Bioreactor Effluent Field Blank – Set 4 72011 6565



### QC Samples

The plant is required to collect field blank samples as part of the sampling program. The

field blank samples should be collected at the frequency specified in Table 4.

Table 4. Field Blank Collection Frequency

Sampling Point Total Mercury Total Metals (200.8

and 200.7) Classicals 1



### FGD Wastewater

Treatment Influent Collected during one

of the four sets Collected during one

of the four sets No field blanks

required

FGD Bioreactor Influent Collected during all

four sets Collected during all

four sets No field blanks

required

FGD Bioreactor Effluent Collected during all

four sets Collected during all

four sets No field blanks

required

1 Classicals includes the analyses for BOD, Group I, Group II, and total cyanide.

### The laboratory will perform MS/MSD analyses on the total metals and total mercury

analyses; however, no additional sample volume is requi red.

Sample Collection

The plant must use clean sampling techniques when collecti ng the total metals and total

mercury samples; therefore, the sampling team should fo llow the clean hands/dirty hands

sampling techniques outlined in EPA Method 1669. Additionally, t he plant must try to

avoid significant contamination during sample collection, especially from sources such as

airborne particles, dirt, and corrosion particulates fr om piping, railing, etc.

The plant must collect grab samples for all analytes a t the influent to the FGD wastewater

treatment system. The plant must collect 24-hour compo site samples for all analytes

except cyanide and mercury at the bioreactor influent and bio reactor effluent sampling

points. The 24-hour composites must be set up to collect equa l sample aliquots every hour

over the 24-hour period. For mercury at the bioreactor infl uent and bioreactor effluent

sampling points, the plant must collect four individual gra b samples over the 24-hour

period (i.e., one mercury grab collected every six hours). For cyanide at the bioreactor

influent and bioreactor effluent sampling points, the plan t must collect a single grab

sample after the one of the mercury grab samples.

If the plant collects the samples from the same taps used for the collection of samples

during the EPA sampling episode, the plant can follow the instructions included in the

sampling plan drafted for the EPA sampling episode to colle ct the field blank samples, set

up the composite containers, and perform the composite pum p-off procedures for the

bioreactor influent and bioreactor effluent sampling points . The following instructions

can be used to collect the grab samples at the influent to the FGD wastewater treatment

system sampling point and for the mercury and cyanide grab s amples at the bioreactor

influent and bioreactor effluent sampling points: (NOTE: If a sample tap or valve is not

available to collect these samples or if the bioreacto r influent and bioreactor effluent

sampling points have intermittent flows which may inter fere with the automatic composite

collection, please contact TJ Finseth, (703) 633-1698 to dis cuss possible alternatives.)

1. Arrive at the sampling point location and prepare supplies and bottles for

the sample collection.

2. Clean hands and dirty hands put on Tyvek® suits, masks, and powder-free

gloves.

3. Dirty hands gets a clear plastic bag and opens it slightl y (touching only the

outer part of the bag) so that clean hands can place h ands in the bag and

open the bag completely.

4. Clean hands then uses the plastic bag to shroud the samp le tap (note that

there should be no flow through the sample tap at this t ime). Clean hands

will need to puncture a small hole in the bag using the ta p and dirty hands

can cable tie the bag to the tap to prevent it from fall ing during sample

collection.

5. Dirty hands opens the outer bags of the field blank wat er and total mercury

and total metals field blank sample bottles. Clean hand s opens the inner

### bag of the field blank water and unscrews the lid. Clean h ands then opens

the inner bag of the total mercury and total metals field bl ank sample

bottles. Clean hands pours the blank water into the fi eld blank sample

bottles under the shrouding, caps the bottles, and closes the inner bags.

Clean hands then places the total mercury and total met als bottles in the

outer bags and dirty hands closes the outer bag.

6. Dirty hands then opens the valve to the sample tap and pur ges the tap for at

least two minutes, then keeps the valve open until all sam ples have been

collected.

7. Dirty hands opens the outer bag for the total mercury s ample bottle. Clean

hands takes the sample bottle and inner bag and holds the m under the

shroud. Clean hands then opens the inner bag, opens the l id of the bottle

and fills the total mercury sample bottle. Clean hands caps the sample

bottle, closes the inner bag, and places the sample bo ttle in the outer bag.

Dirty hands closes the outer bag. The samplers repea t this procedure for

the collection of the total metals samples (both EPA 200.8 with collision

cell and EPA 200.7), unless the plant is collecting the met als samples as

composite samples.

8. The samplers then collect the BOD, Group I, Group II, and total cyanide

samples. NOTE: the samplers can collect these samp les using the same

technique as the mercury and metals samples, or they can remove the

plastic bag shrouding and collect directly from the tap.

9. The Group II and total cyanide samples must be preserved prio r to

shipment to the laboratories. Use the information provide d in the “Sample

Bottle and Preservation” section of these instruction f or the preservation

steps. Additionally, the BOD, Group I, Group II, and tota l cyanide samples

should be placed on ice immediately after sample coll ection/preservation.

Sample Packing and Shipment

The following steps should be used when packing and shipping the s amples to the

laboratories.

1. Make sure that each sample bottle has a label, and tha t the label correctly

specifies the sample point.

2. Tighten the lid on each filled sample bottle, being car eful not to

overtighten the lid. If bottle threads are dirty to w here the lid is impeded

from closing, clean the threads on the bottle being caref ul to not introduce

contamination into the sample. Clean the sample bottl e with a cloth rag or

paper towel.

3. Prior to packaging, place each sample bottle requiring ≤ 6°C preservation

into an ice chest with wet ice to cool.

4. When each sample requiring ≤ 6°C preservation has reached the desired

temperature, wrap each glass sample bottle with two layers of “bubble

wrap” (or place bottle in two “bubble bags”). The bubble wr ap must fit

snugly and completely cover the sample bottle. Enclose each “bubble-

### wrapped” container and plastic container in an individual sealable plastic

freezer bag.

5. Place two garbage bags inside each other in each of the coolers used to

ship samples to the laboratories.

6. Place the classicals samples in the garbage bags in th e coolers with proper

end up, close the interior garbage bag by tying, or with a tw ist-tie.

7. Add ice to the cooler to keep samples cold during shipment. Ar range blue

ice or sealed plastic freezer bags filled with wet ice on top of the sample

bottles (if samples require ≤ 6°C preservation). If using wet ice, place the

ice inside two one-gallon sealable freezer bags. Put at l east 4 × 1⁄2 gallons

of ice (4 × 2.5 pounds of ice) in each large cooler and 2 × 1⁄2 gallons of ice

(2 × 2.5 pounds of ice) in each small cooler. Use more ice when ambient

temperatures are very high. Place the ice inside the sec ond garbage bag.

8. Close the second garbage bag by tying, or with a twist-tie

. 9. Place the metals samples in the garbage bags in a diff erent cooler with

proper end up, close the interior garbage bag by tying or wit h a twist-tie.

Close the second garbage bag by tying, or with a twist-tie . NOTE: the

metals samples are not required to be cooled; however, because the metals

and classicals are being analyzed by the same laboratory, the metals can

be shipped with the classicals, but the metals samples w ould need to be

chilled prior to packing them in the cooler with the clas sicals and ice

would need to be added to the cooler between the interior a nd outer

garbage bags to keep the samples cold.

10. Fill in any free space around the bottles in the metals and classicals

coolers with additional cushioning material. Sufficient pac king material

should be used so that the sample containers will not shi ft during

shipment.

11. Fill out and print a traffic report form for the classi cals and metals samples

(provided electronically by ERG). Seal the last two pages o f the traffic

report form(s) in a plastic envelope secured to the insid e of the top of the

cooler(s). NOTE: the top page of the traffic report mus t be sent to ERG at

the following address:

Eastern Research Group

14555 Avion Parkway, Suite 200

Chantilly, VA 20151

Attn: TJ Finseth

(703) 633-1698

12. Close the cooler(s).

13. Place a completed laboratory address label on the lid o f the cooler(s). The

classicals and metals samples should be shipped to TestAme rica as

follows:

TestAmerica

4955 Yarrow Street

### Arvada, CO 80002

Attn: Elizabeth Eichelberger

(303) 736-0100

14. Make several wraps with strapping tape around the cooler pe rpendicular to

the seal to ensure that the lid will remain closed if t he latch is accidentally

released or damaged.

15. Place the mercury samples in the garbage bags in a separ ate cooler with

proper end up, close the interior garbage bag by tying, or with a twist-tie.

16. Do not add ice to the mercury cooler; simply close the second garbage bag

by tying, or with a twist-tie.

17. Fill in any free space around the bottles with additional cushioning

material. Sufficient packing material should be used so that the sample

containers will not shift during shipment.

18. Fill out and print a traffic report form for the mercury samples (provided

electronically by ERG). Seal the last two pages of the traffic report form

in a plastic envelope secured to the inside of the top o f the cooler. NOTE:

the top page of the traffic report must be sent to ERG a t the same address

provided in step 11:

19. Close the cooler.

20. Place a completed laboratory address label on the lid o f the cooler. The

mercury samples should be shipped to Frontier as follows:

Frontier GeoSciences

414 Pontius Ave. North

Seattle, WA 98109

Attn: Patrick Garcia-Strickland

(206) 957-1428

21. Make several wraps with strapping tape around the cooler pe rpendicular to

the seal to ensure that the lid will remain closed if t he latch is accidentally

released or damaged.

22. Fill out the necessary paperwork for FedEx or UPS to prepa re the

shipment for pick up or drop off. NOTE: the samples must b e shipped

priority overnight to arrive at the laboratories the following morning. Ship

the coolers to the laboratories.

23. After the coolers have been dropped off (or picked up), pleas e contact TJ

Finseth at (703) 633-1698, to notify him that the samples have b een

shipped to the laboratories.

Traffic Reports

An example traffic report will be provided to the plant by ERG for the first sample

collection event. The plant will need to make changes t o the traffic report electronically

for the other three sample collection events. Some information, such as the date and

### sample collection times must be entered by the plant after the sample collection and

therefore, will not be included in the example provided by ERG.

After the traffic report is completed by the plant, th e plant must print the four pages in the

file. The last two pages in the file must be placed in t he cooler for shipment to the

laboratories and the first page must be sent to ERG. The plant can keep the second page

of the traffic report.

Engineering Data

The plant must provide engineering data regarding the operatio n of the plant and FGD

systems during the sample collection period. Additionall y, the plant must make some

field measurements when samples are collected, including pH , temperature, and visual

observations, and provide the data to EPA after the sample collection period. The

engineering data and field measurement data requirements are in an Excel® spreadsheet

titled “Monitoring Program Engineering Data Tables,” which w ill be provided by ERG.

The tables are also included at the end of this enclosure. The plant must complete the

engineering data sheets and field measurement sheets in th e Excel® file and e-mail the

completed forms to TJ Finseth at thomas.finseth@erg.com

.

Certification Statement

The individual responsible for directing and supervising the s ample collection and the

engineering data preparation must sign the certification statement (provided in Enclosure

4) and submit it upon the completion of the sampling program . The signed certification

statement should be scanned and e-mailed to TJ Finseth at thomas.finseth@erg.com , at

the same time the engineering data is submitted.Complete the following tables for each sampling pointPlant NameSampleCollectionNumberDate of SampleCollectionSample CollectionTime Temperature (°C)pH(S.U.)Set 1Set 2Set 3Set 4Plant NameSampleCollectionNumberInfluent SamplesCollected asGrabs(Yes or No)Mercury and CyanideSamples Collected asGrabs(Yes or No)Bioreactor Influentand BioreactorEffluent SamplesCollected as 24-HourComposites(Yes or No)Tyvek Suitsused(Yes or No)Dust MasksUsed forMercury(Yes or No)Clean Hands/DirtyHands SamplingTechniques Used(Yes or No)Description of SampleCollection Technique (ifdifferent thaninstructions)Description of AbnormalConditions in FGD Systemor FGD WastewaterTreatment System that MayImpact ConcentrationsSet 1Set 2Set 3Set 4Complete the following tables based on the plant operating characteristics during each set of samplescollectedUnits OperatingDuring SamplingDayUnits Off-lineEntireSampling DaySCRs/SNCRsOperating onUnitsSet 1Set 2Set 3Set 4Flow Rate (gpm) DurationSet 1Set 2Set 3Set 4Lime Usage(tons)Ferric ChlorideUsage(Liters/day)Organosulfide Usage(Liters/day)Polymer Usage(Liters/day)Acid Usage(Liters/day)ChemicalPrecipitationSystem EffluentFlow Rate (gpd)Dilution WaterAddition Priorto BiologicalTreatmentSystem(gpd)BiologicalTreatmentSystem EffluentFlow Rate (gpd)Set 1Set 2Set 3Set 4Plant NameDate of SampleCollectionSampleCollectionNumberPlant Operation During Sample CollectionFGD Wastewater Treatment Operation During Sample CollectionPlant NameDate of SampleCollectionSampleCollectionNumberScrubber PurgeFlow Rate DuringInfluent SampleCollection(gpm)Percent HydrocloneOverflow RecycledBack to ScrubberPlant NameSampleCollectionNumberDate of SampleCollectionScrubber Slurry Blowdown FlowRateScrubber SlurryPercent SolidsPlant Operation During Sample CollectionUnit 1 Unit 2 Daily Power Generation (MW-hrs)

Plant Name Date Provide the daily power generation for each scrubbe d unit starting two weeks prior to the first set

of samples through the last set of samplesChemical

Precipitation

Effluent Dilution Water

Addition Prior to

Biological

Treatment

System Biological Treatment

System Effluent Plant Name Date FGD Wastewater Treatment System Flow Rates

(gpd) Provide the average flow rate in the FGD wastewater treatment system for each stream included in the

table starting two weeks prior to the first set of samples through the last set of samples

## Section 2

On

- Site Audit Memorandum

### DATE: 10 November 2010

TO: Steam Electric Record

FROM: Ron Jordan

Engineering and Analysis Division

SUBJECT: Notes from Audit of Industry Self-Monitoring Sampling at Duke Energy

Carolinas’ Belews Creek Steam Station on November 3-4, 2010

EPA conducted an audit of the self-monitoring sampling con ducted at Duke Energy

Carolinas’ Belews Creek Steam Station (Belews Creek) l ocated in Belews Creek, North

Carolina. This was Belews Creek’s second set (“Set 2”) o f self-monitoring sampling that was

being conducted to comply with the requirements established in a letter from Mary Smith,

Director of EPA’s Engineering and Analysis Division, dat ed July 30, 2010. EPA conducted the

audit on November 3-4, 2010. These notes summarize the sa mple collection techniques used by

Belews Creek at each of the sampling points and EPA’s ob servations/findings from the audit. A

process water diagram for the flue gas desulfurization (FG D) wastewater treatment system is

provided as Attachment 1. The treatment system is describe d in EPA’s sampling plan for the

Belews Creek plant. 1 

### The checklists that EPA completed during the audit are provided as

Attachment 2. Pictures from the audit are provided as Atta chment 3.

Both generating units and both FGD units were operating through out the period of

sampling for Set 2. The following sections describe the sample collection at each of the sampling

points and the observations/findings from each sampling poin t.

Influent to FGD Wastewater Treatment System – FGD Purge (SP -1)

Belews Creek personnel collected samples for the influen t to FGD wastewater treatment

system from a sample tap located on the wastewater pip ing downstream of the FGD purge tank

and upstream of the equalization tank. EPA specified this l ocation for the FGD purge sample

(i.e., prior to the wastewater entering the equalizati on tank) because the FGD scrubber purge is

commingled with other waste streams in the equalization tank and, therefore, the sampling point

upstream of the tank provides the best representation of t he FGD scrubber purge from the

Belews Creek FGD system. This is the same sampling point that EPA used during its sample

collection. The sample tap consisted of PVC piping with a three-way splitter with barbed ends.

Each tap was separately valved, although only one tap was used to collect all influent samples. A

picture of the sample tap is included as Figure 1 in Attachm ent 3.

Sample Collection

Set 2 samples for the FGD purge were collected on Novem ber 4, 2010. To collect the

samples of the FGD purge, Belews Creek personnel followed EPA Method 1669 protocols and

the EPA-provided instructions. Belews Creek personnel shro uded the tap with a clean plastic

1 Eastern Research Group, Inc. (ERG). Final Sampling Plan , Duke Energy Carolinas’ Belews Creek Steam Station,

Belews Creek, NC, Sampling Episode 6558. May 27, 2010.

### Page 2

bag and let the sample flow from the tap for two minute s prior to collecting any samples. All of

the mercury and metals samples were filled while the sa mplers held the bottles under the

shrouding. EPA and industry sample bottles were filled as duplicates (i.e., split samples and

multi-fill technique was not used for the influent samples ), with one bottle filled after the other

was full. After the mercury and metals samples were collected, the shrouding was pulled away

from the sample tap and Belews Creek personnel filled the bottles for classicals without the

shrouding. The flow through the sample tap continued withou t interruption until all influent

samples were collected.

No field blanks were collected for the influent sample po int during Set 2. Field blank

samples were collected during Set 1.

Preservation

Belews Creek personnel followed all method specification s when preserving the classical

samples. The Group II samples were preserved by adding H 2 

### SO 4 

### at the sample location

immediately after filling the bottles. After completi ng sample collection at the influent, the

Group II samples were then taken to the on-site labora tory and the pH was confirmed to be

below 2 S.U. The cyanide samples were checked in the la boratory for sulfides and chlorine

using lead acetate paper and potassium iodide starch paper, re spectively. The samplers did not

detect sulfides or chlorine in the samples. The cyanide samples were then preserved using

NaOH and the pH was confirmed to be above 10 S.U. The BOD , Group I, Group II, and cyanide

samples were all placed on ice after collection or p reservation.

Field Measurements

Belews Creek personnel used a pH probe and a temperature pro be in the laboratory to

measure the pH and temperature of the influent field test b ottle.

Observations/Findings

EPA observed the Belews Creek personnel setting up and co llecting the Set 2 samples for

the influent to wastewater treatment system. No fiel d blanks were collected at this sample point

because Belews Creek personnel previously collected field bla nks during Set 1. The sampling

crew followed the requirements of EPA Method 1669 (e.g., clean sampling protocols) while

collecting samples. Belews Creek personnel collected sa mples for analysis by both EPAcontracted laboratories (metals and classicals) and indus try laboratories (metals only). The

sample bottles were filled as duplicates, with one bottl e filled after the other was full – in

contrast to the multi-fill sample collection technique used at the other two sample points, and the

split samples collected during EPA’s four-day sampling epis odes. The bottles used were prelabeled in the laboratory.

Belews Creek personnel followed applicable procedures for s ample collection and

preservation. Samples were preserved within 15 minutes. Tempe rature and pH of the field test

sample were measured approximately twenty minutes after s ample collection.

### Page 3

Influent to Bioreactor System (SP-2)

Belews Creek personnel collected samples for the influen t to the bioreactor system (SP-2)

from a sample tap downstream of the sand filters afte r the wastewater from the three filters is

commingled. The sample tap is located on the wastewater piping after the three sand filter

effluent streams are commingled, downstream of the hol ding tank and upstream of the heat

exchanger. This is the same sampling point that EPA used duri ng its sample collection. The

sample tap consisted of PVC piping with a three-way spl itter with barbed ends. Each tap was

separately valved, allowing the mercury and cyanide grab samp les to be collected from a

dedicated tap without interrupting the composite sampler. Pictures of the sample tap are included

as Figures 2a and 2b in Attachment 3.

Sample Collection

Belews Creek personnel collected the influent to the biore actor system as composite

samples, except for the mercury and cyanide samples. On e ISCO automatic compositor was

programmed to collect individual sample volumes into a 20 -liter container for the composite

samples. The ISCO pump was calibrated and programmed to coll ect aliquots of equal volume in

one-hour intervals during the 24-hour composite period. Follo wing the composite period, Belews

Creek personnel pumped off the specific sample volumes int o the individual sample bottles for

all analyses except mercury and cyanide. Mercury and cyanide samples were collected as grab

samples.

To collect the composite samples, Belews Creek personn el used a T-splitter tubing set

that consisted of a short length of silicone tubing attac hed to the perpendicular end of a T-splitter

and two longer pieces of silicone tubing attached to the othe r two ends of the T-splitter. Prior to

completing the setup for the composite samples, Belews Creek personnel collected field blanks

for SP-2 by threading the short end of the tubing set thro ugh the peristaltic pump on the ISCO

Avalanche® portable sampler and attaching the end of the tubin g to a vented cap on a 10-liter

carboy and pumping reagent grade water into the carboy. To collect the composite samples,

Belews Creek personnel attached one long end of the silic one tubing to one of the barbed sample

taps and the other long end was directed to a nearby drain, and attached the vented cap and

shorter length of tubing to a 20-liter carboy. Pictures of the sampling configuration are included

as Figures 3a and 3b in Attachment 3. The samplers program med the compositor to collect 830

mL of sample every hour for a 24-hour period.

After the 24-hour period, the samplers took both carboys to the pump-off location and

pumped the sample into the individual sample bottles. B elews Creek personnel used a short

piece of Teflon® tubing connected to a length of silicone tubing and the peristaltic pump on the

ISCO Avalanche® to transfer the samples to individual sa mple bottles. The samplers first shook

the 10-liter container to homogenize the field blank sample a nd then they attached a pump-off

cap onto the carboy. The Teflon® end of the tubing was th en inserted into the carboy and the

tubing was purged with one liter of sample. Belews Creek pe rsonnel then collected the field

blank samples (metals only) while placing the bottles in a cleanbox to reduce the potential for

atmospheric contamination. The field blank bottles were f illed as multi-fill split samples (i.e.,

### Page 4

one bottle was filled one-third full, then a second and any additional bottles were filled one-third

full, and then the process was repeated until all field bl ank bottles were full).

After the field blank samples were collected, the samp lers then filled bottles for metals

and classicals using the volume collected in the 20-liter carboy. The samplers first shook the 20-

liter container to homogenize the sample, and then the y transferred the pump-off cap and tubing

from the 10-liter field blank container to the 20-liter car boy. The tubing was then purged with

two liters of sample. Belews Creek personnel then colle cted the metals samples with the bottles

placed in the clean box. The bottles were filled as m ulti-fill split samples (i.e., one bottle was

filled one-third full, then a second and any additional bot tles were filled one-third full, and then

the process was repeated until all metals bottles were full). After all the metals samples were

collected, the samplers filled the classicals samples outside the cleanbox. No classical samples

were collected for analysis by industry-contracted labor atories.

Belews Creek personnel also collected grab samples for m ercury every six hours during

the sampling. The samplers took steps to minimize atmos pheric contamination of the samples by

shrouding a second tap on the three-way splitter with a clean plastic bag. A clean shroud was

used for each grab sample (EPA observed only grabs 1 and 2). A mercury field blank sample was

collected prior to the first of the four mercury grab sam ples. The field blank was collected by

filling the bottle under the shroud with reagent grade wate r. For the field blank, one of the EPA

bottles was completely filled, then the industry samp le bottle was completely filled, and then the

second EPA field blank bottle was completely filled. The valve was then opened to allow sample

flow through the sample tap for at least two minutes prior to collecting any samples. Belews

Creek personnel filled the mercury bottles directly fro m the tap, underneath the shroud. Two

samplers collected the mercury samples under the shroud, filling the bottles as multi-fill split

samples (i.e., one sampler filled the EPA sample bottl e one-third full, then the second sampler

filled the Belews Creek sample bottle one-third full, a nd then the process was repeated until the

bottles were full). Belews Creek personnel also collec ted the cyanide sample as a grab sample

immediately after the first of the four mercury grab s amples at the sampling point.

Preservation

Belews Creek personnel followed all method specification s when preserving the classical

samples. The Group II samples were preserved by adding H 2 

### SO 4 

### at the pump-off location

immediately after filling the bottles. After completi ng pump-off of the composite samples, the

Group II samples were then taken to the on-site labora tory and the pH was confirmed to be

below 2 S.U. The cyanide samples were checked in the la boratory for sulfides and chlorine

using lead acetate paper and potassium iodide starch paper, re spectively. The samplers did not

detect sulfides or chlorine in the samples. The cyanide samples were then preserved using

NaOH and the pH was confirmed to be above 10 S.U. The BOD , Group I, Group II, and cyanide

samples were all placed on ice after collection or p reservation.

Field Measurements

Belews Creek personnel used a pH probe and a temperature pro be in the laboratory to

measure the pH and temperature of the bioreactor influent fi eld test bottle.

### Page 5

Observations/Findings

EPA observed the following activities for SP-2 during the a udit: collection of cyanide

sample and mercury grab 1 (including field blank) and grab 2; fi eld blank collection and set-up

for the composite samples; breakdown of the composite sampler; pump-off of composite

samples; and preservation.

The sampling crew followed the requirements of EPA Met hod 1669 (e.g., clean sampling

protocols) while collecting samples. Belews Creek person nel collected samples for analysis by

both EPA-contracted laboratories (metals and classica ls) and industry laboratories (metals only).

The sample bottles (except mercury field blanks) were fi lled as multi-fill split samples. Belews

Creek personnel followed applicable procedures for sample c ollection and preservation. Samples

were preserved within 15 minutes.

No clean box was used during set-up for the composite sam ple; however, clean sampling

protocols were followed. The sample tubing was provided double- bagged from the laboratory,

with all tubing ends already covered by zip-tied plastic ba gs.

During preparation for the pump-off of composite samples, the tubing was removed from

double plastics bags while outside the clean box. All tubing ends were already covered in the

laboratory by zip-tied plastic bags and clean sampling protoc ols were followed while handling

the tubing.

The ISCO pump cover was not easily removed, so during set -up of the composite sample

the tubing end was threaded through the pump. The tubing end rem ained covered while

threading. The bag on the end of the tubing was then repla ced with a clean bag prior to the clean

hands person handling the tubing end and the caps for the ca rboy. During pump-off, the

sampling crew unscrewed and removed the pump cover so they co uld “lay” the tubing into the

pump without having to thread the end of the tubing through the I SCO.

At the end of the 24-hour composite period, the carboy co ntained 20 liters. The

temperature of the field blank carboy after filling all bo ttles (measured at 9:20 a.m.) was 5° C.

The 20-liter carboy temperature after filling all sample bottles was 9.4° C (measured at 9:16

a.m.). The carboy was kept on ice throughout the composi ting period and until the carboy was

placed on the sampling table for pump-off. The elevated tem perature was unexpected and the

sampling crew speculated that the reason may be that the drain hole on the trash can allowed

water from melting ice to continuously exit the can, resul ting in an ice-only environment instead

of an ice-water bath that would have provided greater ther mal conductivity. The EPA auditor

recommended that future sampling sets either: (1) cover th e existing drain hole and create a new

drain hole at a higher level that allows the trash can to hold an ice-water mixture; or (2) cover the

drain hole and use a pump and tubing to periodically remove e xcess water from the trash can.

Mercury grabs began approximately 2 hours after compositor fo r SP-2 was started.

### Page 6

All bottles were pre-labeled by the laboratory. The fi eld blank container was a 10-liter

carboy, instead of a 20-liter carboy (a 20-liter carboy w as used to collect the 24-hour composite

samples).

Effluent from the Bioreactor System (SP-3)

Belews Creek personnel collected samples for the efflu ent from the bioreactor system

(SP-3) from a sample tap on a section of piping downstrea m of the second-stage effluent storage

tank from the second-stage bioreactor cells. This is the same sampling point that EPA used

during its sample collection. The sample tap consisted o f PVC piping with a three-way splitter

with barbed ends. Each tap was separately valved, allowing the mercury and cyanide grab

samples to be collected from a dedicated tap without in terrupting the composite sampler. Pictures

of the sample tap are included as Figures 3a, 3b and 3c in Att achment 3.

Sample Collection

Belews Creek personnel collected samples for SP-3 using t he same approach described

above for SP-2.

Preservation

Belews Creek personnel followed all method specificatio ns when preserving the

classical samples. The Group II samples were preserve d by adding H 2 

### SO 4 

### at the pump-off

location immediately after filling the bottles. After completing pump-off of the composite

samples, the Group II samples were then taken to the o n-site laboratory and the pH was

confirmed to be below 2 S.U. The cyanide samples were ch ecked in the laboratory for sulfides

and chlorine using lead acetate paper and potassium iodide star ch paper, respectively. The

samplers did not detect sulfides or chlorine in the sampl es. The cyanide samples were then

preserved using NaOH and the pH was confirmed to be above 10 S. U. The BOD, Group I,

Group II, and cyanide samples were all placed on ice af ter collection or preservation.

Field Measurements

Belews Creek personnel used a pH probe and a temperature pro be in the laboratory to

measure the pH and temperature of the bioreactor effluent field test bottle.

Observations/Findings

EPA observed the following activities for SP-3 during the a udit: collection of cyanide

sample and mercury grab 1 (including field blank) and grab 2; fi eld blank collection and set-up

for the composite samples; breakdown of the composite sampler; pump-off of composite

samples; and preservation.

The sampling crew followed the requirements of EPA Met hod 1669 (e.g., clean sampling

protocols) while collecting samples. Belews Creek person nel collected samples for analysis by

both EPA-contracted laboratories (metals and classica ls) and industry laboratories (metals only).

### Page 7

The sample bottles (except mercury field blanks) were fi lled as multi-fill split samples. Belews

Creek personnel followed applicable procedures for sample c ollection and preservation. Samples

were preserved within 15 minutes.

No clean box was used during set-up for the composite sam ple; however, clean sampling

protocols were followed. The sample tubing was provided double- bagged from the laboratory,

with all tubing ends already covered by zip-tied plastic ba gs.

During preparation for the pump-off of composite samples, the tubing was removed from

double plastics bags while outside the clean box. All tubing ends were already covered in the

laboratory by zip-tied plastic bags and clean sampling protoc ols were followed while handling

the tubing.

The ISCO pump cover was not easily removed, so during set -up of the composite sample

and pump-off the sampling crew unscrewed and removed the pump cover so they could “lay” the

tubing into the pump without having to thread the end of the tubi ng through the ISCO.

At the end of the 24-hour composite period, the carboy co ntained 20 liters (equal to the

programmed volume). The temperature of the field blank ca rboy after filling all bottles was 4.7°

C (measured at 10:35 a.m.). The 20-liter carboy temperature after filling all sample bottles was

7.6° C (measured at 10:34 a.m.). The carboy was kept on ice throughout the compositing period

and until the carboy was placed on the sampling table fo r pump-off. The elevated temperature

was unexpected and the sampling crew speculated that the r eason may be that the drain hole on

the trash can allowed water from melting ice to continuous ly exit the can, resulting in an ice-only

environment instead of an ice-water bath that would have pr ovided greater thermal conductivity.

The EPA auditor recommended that future sampling sets eit her: (1) cover the existing drain hole

and create a new drain hole at a higher level that all ows the trash can to hold an ice-water

mixture; or (2) cover the drain hole and use a pump and tubi ng to periodically remove excess

water from the trash can.

Mercury grabs began approximately 2 hours after compositor fo r SP-2 was started.

All bottles were pre-labeled by the laboratory. The fi eld blank container was a 10-liter

carboy, instead of a 20-liter carboy (a 20-liter carboy w as used to collect the 24-hour composite

samples).

### Attachment 1

Treatment System Process Water Diagram

### Attachment 2

Audit Checklists

### Attachment 3

Photographs of Sample Points

### Figure 1

– Influent to the FGD Wastewater Treatment System (FGD Purge; SP

‐ 1)

### Figure 2a

– Influent to the Bioreactor System (SP

‐ 2)

### Figure 2b

– Influent to the Bioreactor System (SP

‐ 2)

### Figure 3a

– Effluent from the Bioreactor System (SP

‐ 3)

### Figure 3b

– Effluent from the Bioreactor System (SP

‐ 3)

### Figure 3c

– Collecting Mercury Samples at the Effluent from the Bioreactor System (SP

‐ 3)

## Section 3

Signed Certification Statement

## Section 4

Engineering DataTable A4-1. Field Measurementsfor Sample Collection at the Influent to FGD Wastewater Treatment System, Belews CreekEpisode NumberSample CollectionNumberDate of SampleCollectionSample CollectionTimeTemperature(°C)pH(S.U.)6565Set 1 - Grab 1 10/6/2010112939.36.66565Set 2 - Grab 1 11/3/2010114532.76.76565Set 3-Grab 112/8/2010103834.36.76565Set 4-Grab 11/17/2011112138.26.8Table A4-2. Field Measurementsfor Sample Collection at the Influent to the Bioreactor System, Belews CreekEpisode NumberSample CollectionNumberDate of SampleCollectionSample CollectionTimeTemperature(°C)pH(S.U.)6565Set 1 - Grab 1 10/6/2010084531.76.76565Set 1-Grab 210/6/2010144233.96.36565Set 1-Grab 310/6/2010204432.76.66565Set 1 - Grab 4 10/7/2010024033.46.56565Set 2 - Grab 1 11/3/2010105531.17.16565Set 2-Grab 211/3/2010171631.37.06565Set 2-Grab 311/3/2010225632.26.66565Set 2 - Grab 4 11/4/2010045533.47.06565Set 3 - Grab 1 12/8/2010100326.97.06565Set 3-Grab 212/8/2010160627.37.06565Set 3-Grab 312/8/2010220027.97.06565Set 3 - Grab 4 12/9/2010040127.87.16565Set 4 - Grab 1 1/17/2011104827.87.26565Set 4-Grab 21/17/2011165528.07.26565Set 4-Grab 31/18/2011224827.67.16565Set 4 - Grab 4 1/18/2011044927.67.1Table A4-3. Field Measurementsfor Sample Collection at the Effluent from the Bioreactor System, Belews CreekEpisode NumberSample CollectionNumberDate of SampleCollectionSample CollectionTimeTemperature(°C)pH(S.U.)6565Set 1 - Grab 1 10/6/2010103530.26.46565Set 1-Grab 210/6/2010165030.26.36565Set 1-Grab 310/6/2010224231.16.36565Set 1 - Grab 4 10/7/2010044031.56.36565Set 2 - Grab 1 11/3/2010100729.56.86565Set 2-Grab 211/3/2010160828.56.46565Set 2-Grab 311/3/2010220928.96.56565Set 2 - Grab 4 11/4/2010040730.56.56565Set 3 - Grab 1 12/8/2010092325.46.86565Set 3-Grab 212/8/2010152625.56.86565Set 3-Grab 312/8/2010212424.96.86565Set 3 - Grab 4 12/9/2010032425.16.86565Set 4 - Grab 1 1/17/2011095626.66.76565Set 4-Grab 21/17/2011160826.66.76565Set 4-Grab 31/18/2011215626.06.86565Set 4 - Grab 4 1/18/2011035725.96.8Table A4-4. Sample Collection Procedures Used during the Sampling EpisodeEpisodeNumberSampleCollectionNumberInfluentSamplesCollected asGrabs(Yes or No)Mercuryand CyanideSamplesCollected asGrabs(Yes or No)Bioreactor Influentand BioreactorEffluent SamplesCollected as 24-Hour Composites(Yes or No)CleanHands/DirtyHands SamplingTechniques Used(Yes or No)*Description ofSampleCollectionTechnique (ifdifferent thaninstructions)Description of AbnormalConditions in FGDSystem or FGDWastewater TreatmentSystem that May ImpactConcentrations6565 Set 1 Yes YesYesYesNoneNone6565 Set 2 Yes YesYesYesNoneNone6565 Set 3 Yes YesYesYesNoneNone6565 Set 4 Yes YesYesYesNoneUnit 2 Offline* Includes the use of tyveks suits during all sampling events and dust masks during the collection of mercury samples.Table A4-5.Generating Unit Operation at Time of Sampling, Belews CreekEpisode NumberSample CollectionNumberDate of SampleCollectionPlant Operation DuringSample CollectionUnits OperatingDuring SamplingDayUnits Off-line EntireSampling DaySCRs/SNCRsOperating onUnits6565Set 110/6/10-10/7/10Unit 1/2NoneSCR6565Set 211/3/10-11/4/10Unit 1/2NoneSCR6565Set 3 12/8/10 - 12/9/10 Unit 1/2NoneSCR6565Set 4 1/17/11 - 1/18/11 Unit 1/2NoneSCRTable A4-6. FGD Scrubber Slurry Information at Time of Sampling, Belews CreekEpisodeNumberSampleCollectionNumberDate of SampleCollectionUnitsPlant Operation DuringSample CollectionScrubber Slurry BlowdownFlow RateScrubberSlurryPercentSolidsPercentHydrocloneOverflow RecycledBack to ScrubberFlow Rate(gpm)Duration6565 Set 1 10/6/10 - 10/7/101URE 17 hrs 15 - 17%0%6565Set 110/6/10-10/7/102URE17 hrs15-17%0%6565Set 211/3/10-11/4/101URE16 hrs15-17%0%6565 Set 2 11/3/10 - 11/4/102URE 10 hrs 15 - 17%0%6565 Set 3 12/8/10 - 12/9/101URE 12 hrs 15 - 17%0%6565Set 312/8/10-12/9/102URE17 hrs15-17%0%6565Set 41/17/11-1/18/111URE21 hrs15-17%0%6565 Set 4 1/17/11 - 1/18/112URE0 hrs NANANA – not applicable.URE – Unable to reasonable estimate.Table A4-7. FGD Wastewater Treatment System Operation Information, Belews CreekEpisodeNumberSampleCollectionNumberDate of SampleCollectionScrubber PurgeFlow Rate DuringInfluent SampleCollection(gpm)FGD Wastewater Treatment Operation During Sample CollectionLimeUsage(tons)FerricChlorideUsage(Liters/day)OrganosulfideUsage(Liters/day)Polymer Usage(Liters/day)Acid Usage(Liters/day)6565 Set 1 10/6/10 - 10/7/10 5621 48.9NA43.81,4756565 Set 2 11/3/10 - 11/4/10 4461 40.0NA35.81.4756565 Set 3 12/8/10 - 12/9/10 5741 45.0NA10.31.4756565 Set 4 1/17/11 - 1/18/11 4761 35.5NA31.81.475

### Table A4-8. Daily Power Generation During Sampling Period, Belews Creek

Episode Number Date Daily Power Generation

(MW-hrs)

Unit 1 Unit 2

6565 9/20/2010 27,698 26,899



### 6565 9/21/2010 27,624 26,075

6565 9/22/2010 28,111 26,848

6565 9/23/2010 27,713 25,944

6565 9/24/2010 27,180 26,463



### 6565 9/25/2010 26,143 23,956

6565 9/26/2010 27,915 902

6565 9/27/2010 27,286 0

6565 9/28/2010 28,095 2



### 6565 9/29/2010 25,967 22,135

6565 9/30/2010 23,581 22,695

6565 10/1/2010 22,823 22,552

6565 10/2/2010 23,433 21,770



### 6565 10/3/2010 22,504 19,434

6565 10/4/2010 23,484 22,153

6565 10/5/2010 25,332 22,566

6565 10/6/2010 26,918 23,872



### 6565 10/7/2010 25,717 24,425

6565 10/8/2010 25,676 23,331

6565 10/9/2010 25,740 23,570

6565 10/10/2010 24,907 22,858



### 6565 10/11/2010 27,102 25,534

6565 10/12/2010 24,980 23,013

6565 10/13/2010 26,020 24,782

6565 10/14/2010 25,499 24,297



### 6565 10/15/2010 25,865 24,575

6565 10/16/2010 26,652 23,538

6565 10/17/2010 27,283 23,495

6565 10/18/2010 26,824 25,420



### 6565 10/19/2010 27,577 24,689

6565 10/20/2010 27,198 24,889

6565 10/21/2010 26,653 24,249

6565 10/22/2010 26,305 23,873



### 6565 10/23/2010 27,329 26,267

6565 10/24/2010 27,910 25,270

6565 10/25/2010 27,930 27,085

6565 10/26/2010 27,523 26,100



### 6565 10/27/2010 28,240 26,987

6565 10/28/2010 27,229 25,175

6565 10/29/2010 26,248 24,991

6565 10/30/2010 25,096 24,643

### Table A4-8. Daily Power Generation During Sampling Period, Belews Creek

Episode Number Date 

### Daily Pow er Generation

(MW-hrs)



### Unit 1 Unit 2

6565 10/31/2010 23,212 23,076

6565 11/1/2010 27,690 23,600



### 6565 11/2/2010 27,697 24,820

6565 11/3/2010 28,186 25,557

6565 11/4/2010 27,862 25,656

6565 11/5/2010 26,534 25,724



### 6565 11/6/2010 27,628 26,178

6565 11/7/2010 27,469 28,314

6565 11/8/2010 28,322 28,010

6565 11/9/2010 27,435 26,873



### 6565 11/10/2010 25,621 27,272

6565 11/11/2010 24,804 25,564

6565 11/12/2010 25,566 27,098

6565 11/13/2010 26,156 27,811



### 6565 11/14/2010 26,800 28,056

6565 11/15/2010 25,280 26,099

6565 11/16/2010 24,560 27,342

6565 11/17/2010 9,884 24,747



### 6565 11/18/2010 0 26,792

6565 11/19/2010 0 28,122

6565 11/20/2010 0 27,715

6565 11/21/2010 0 25,458



### 6565 11/22/2010 0 26,659

6565 11/23/2010 0 23,948

6565 11/24/2010 0 25,174

6565 11/25/2010 0 25,045



### 6565 11/26/2010 0 24,221

6565 11/27/2010 118 26,284

6565 11/28/2010 21,198 26,493

6565 11/29/2010 27,689 27,921



### 6565 11/30/2010 25,812 27,749

6565 12/1/2010 25,670 25,194

6565 12/2/2010 28,297 28,097

6565 12/3/2010 25,920 28,077



### 6565 12/4/2010 25,842 28,074

6565 12/5/2010 26,531 26,616

6565 12/6/2010 28,321 28,321

6565 12/7/2010 28,314 28,260



### 6565 12/8/2010 28,310 28,279

6565 12/9/2010 28,280 28,260

6565 12/10/2010 28,119 26,690

6565 12/11/2010 28,320 27,098



### 6565 12/12/2010 25,957 27,395

### Table A4-8. Daily Power Generation During Sampling Period, Belews Creek

Episode Number Date 

### Daily Pow er Generation

(MW-hrs)



### Unit 1 Unit 2

6565 12/13/2010 26,537 28,320

6565 12/14/2010 28,330 28,319



### 6565 12/15/2010 28,329 28,323

6565 12/16/2010 21,628 28,319

6565 12/17/2010 0 28,320

6565 12/18/2010 2,334 28,296



### 6565 12/19/2010 28,048 26,794

6565 12/20/2010 28,328 28,319

6565 12/21/2010 28,321 28,320

6565 12/22/2010 25,823 26,193



### 6565 12/23/2010 25,973 27,530

6565 12/24/2010 27,370 27,855

6565 12/25/2010 25,457 27,419

6565 12/26/2010 27,998 28,328



### 6565 12/27/2010 28,002 28,240

6565 12/28/2010 27,341 28,228

6565 12/29/2010 28,320 28,320

6565 12/30/2010 28,103 28,316



### 6565 12/31/2010 26,311 28,001

6565 1/1/2011 26,100 24,947

6565 1/2/2011 21,107 24,846

6565 1/3/2011 27,647 28,320



### 6565 1/4/2011 28,320 28,320

6565 1/5/2011 28,320 28,321

6565 1/6/2011 28,009 27,244

6565 1/7/2011 27,829 28,034



### 6565 1/8/2011 27,891 25,518

6565 1/9/2011 28,311 28,320

6565 1/10/2011 28,320 28,320

6565 1/11/2011 28,320 28,319



### 6565 1/12/2011 28,320 28,284

6565 1/13/2011 28,320 28,316

6565 1/14/2011 28,320 28,321

6565 1/15/2011 26,425 26,692



### 6565 1/16/2011 28,320 414

6565 1/17/2011 28,318 0

6565 1/18/2011 28,325 11,564

### Table A 4

- 9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Belews

Creek

Episode

Number Date 

### FGD Wastewater Treatment System Flow Rates

(gpd)

Chemical

Precipitation

Effluent 

### Dilution Water

Addition Prior to

Biological Treatment

System Biological

Treatment System

Effluent



### 6565 9/20/2010 706,256 0 653,466

6565 

### 9/21/2010 639,850 0 609,509

6565 9/22/2010 677,894 0 624,325



### 6565 9/23/2010 840,951 0 760,600

6565 9/24/2010 735,328 0 370,634

6565 

### 9/25/2010 660,858 0 598,833

6565 9/26/2010 656,579 0 615,693



### 6565 9/27/2010 525,199 0 531,526

6565 9/28/2010 444,631 0 387,091

6565 

### 9/29/2010 406,171 0 374,603

6565 9/30/2010 566,207 0 501,427



### 6565 10/1/2010 660,667 0 599,597

6565 10/2/2010 684,161 0 619,025

6565 

### 10/3/2010 664,081 0 608,294

6565 10/4/2010 643,462 0 571,850



### 6565 10/5/2010 753,394 0 707,550

6565 10/6/2010 673,977 0 631,725

6565 

### 10/7/2010 715,224 0 684,285

6565 10/8/2010 701,492 0 638,531



### 6565 10/9/2010 680,179 0 550,773

6565 10/10/2010 646,665 0 537,001

6565 

### 10/11/2010 807,618 0 726,870

6565 10/12/2010 654,350 0 576,079



### 6565 10/13/2010 601,489 0 598,878

6565 10/14/2010 597,007 0 550,905

6565 

### 10/15/2010 541,134 0 518,106

6565 10/16/2010 617,902 0 518,885



### 6565 10/17/2010 646,346 0 603,260

6565 10/18/2010 601,388 0 571,273

6565 

### 10/19/2010 626,625 0 620,523

6565 10/20/2010 735,410 0 684,780



### 6565 10/21/2010 600,972 0 594,851

6565 10/22/2010 560,127 0 495,207

6565 

### 10/23/2010 686,334 0 642,367

6565 10/24/2010 676,409 0 616,462



### 6565 10/25/2010 598,526 0 589,056

6565 10/26/2010 643,249 0 580,206

### Table A 4

- 9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Belews

Creek

Episode

Number Date FGD Wastewater Treatment System Flow Rates

(gpd)

Chemical

Precipitation

Effluent 

### Dilution Water

Addition Prior to

Biological Treatment

System Biological

Treatment System

Effluent



### 6565 10/27/2010 523,936 0 510,195

6565 10/28/2010 636,351 0 580,012

6565 

### 10/29/2010 702,597 0 693,348

6565 10/30/2010 695,368 0 675,872



### 6565 10/31/2010 619,118 0 613,784

6565 11/1/2010 667,227 0 628,371

6565 

### 11/2/2010 631,422 0 610,251

6565 11/3/2010 550,457 0 497,156



### 6565 11/4/2010 604,340 0 584,849

6565 11/5/2010 712,054 0 649,779

6565 

### 11/6/2010 650,251 0 630,298

6565 11/7/2010 574,075 0 524,802



### 6565 11/8/2010 643,192 0 617,130

6565 11/9/2010 701,917 0 598,526

6565 

### 11/10/2010 676,120 0 634,792

6565 11/11/2010 604,798 0 543,168



### 6565 11/12/2010 634,320 0 616,971

6565 11/13/2010 629,354 0 558,009

6565 

### 11/14/2010 657,941 0 645,981

6565 11/15/2010 672,355 0 611,759



### 6565 11/16/2010 645,042 0 617,885

6565 11/17/2010 624,574 0 573,176

6565 

### 11/18/2010 431,117 0 421,809

6565 11/19/2010 327,193 0 304,260



### 6565 11/20/2010 459,224 0 395,597

6565 11/21/2010 398,390 0 338,640

6565 

### 11/22/2010 475,493 0 453,811

6565 11/23/2010 321,053 0 287,083



### 6565 11/24/2010 360,562 0 317,463

6565 11/25/2010 212,701 0 161,533

6565 

### 11/26/2010 512,945 0 480,913

6565 11/27/2010 354,404 0 298,010



### 6565 11/28/2010 325,808 0 314,439

6565 11/29/2010 635,072 0 550,096

6565 

### 11/30/2010 613,015 0 587,347

6565 12/1/2010 682,640 0 634,207



### 6565 12/2/2010 608,521 0 591,683

6565 12/3/2010 713,763 0 638,061

6565 

### 12/4/2010 612,491 0 577,772

### Table A 4

- 9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Belews

Creek

Episode

Number Date FGD Wastewater Treatment System Flow Rates

(gpd)

Chemical

Precipitation

Effluent 

### Dilution Water

Addition Prior to

Biological Treatment

System Biological

Treatment System

Effluent



### 6565 12/5/2010 749,637 0 691,468

6565 12/6/2010 707,767 0 685,714

6565 

### 12/7/2010 670,589 0 570,605

6565 12/8/2010 634,133 0 610,976



### 6565 12/9/2010 736,413 0 677,426

6565 12/10/2010 712,877 0 662,154

6565 

### 12/11/2010 741,248 0 650,067

6565 12/12/2010 803,273 0 755,955



### 6565 12/13/2010 807,277 0 735,913

6565 12/14/2010 831,267 0 767,424

6565 

### 12/15/2010 704,652 0 640,099

6565 12/16/2010 806,653 0 778,567



### 6565 12/17/2010 555,142 0 494,520

6565 12/18/2010 567,803 0 507,245

6565 

### 12/19/2010 853,543 0 724,140

6565 12/20/2010 867,948 0 766,597



### 6565 12/21/2010 818,960 0 728,866

6565 12/22/2010 720,616 0 689,370

6565 

### 12/23/2010 729,921 0 700,263

6565 12/24/2010 819,617 0 801,906



### 6565 12/25/2010 709,825 0 634,704

6565 12/26/2010 610,361 0 603,902

6565 

### 12/27/2010 668,365 0 606,210

6565 12/28/2010 639,919 0 627,548



### 6565 12/29/2010 700,584 0 677,755

6565 12/30/2010 687,805 0 691,305

6565 

### 12/31/2010 629,254 0 573,049

6565 1/1/2011 614,054 0 602,259



### 6565 1/2/2011 735,811 0 659,125

6565 1/3/2011 740,958 0 661,823

6565 

### 1/4/2011 762,541 0 726,261

6565 1/5/2011 670,794 0 697,206



### 6565 1/6/2011 692,636 0 659,152

6565 1/7/2011 677,100 0 688,275

6565 

### 1/8/2011 620,483 0 591,875

6565 1/9/2011 664,391 0 687,862



### 6565 1/10/2011 671,873 0 637,413

6565 1/11/2011 608,396 0 591,990

6565 

### 1/12/2011 716,111 0 699,082

### Table A 4

- 9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Belews

Creek

Episode

Number Date FGD Wastewater Treatment System Flow Rates

(gpd)

Chemical

Precipitation

Effluent 

### Dilution Water

Addition Prior to

Biological Treatment

System Biological

Treatment System

Effluent



### 6565 1/13/2011 643,593 0 664,841

6565 1/14/2011 647,890 0 620,460

6565 

### 1/15/2011 687,496 0 673,236

6565 1/16/2011 575,722 0 532,612



### 6565 1/17/2011 472,513 0 469,003

6565 1/18/2011 444,255 0 392,650

## Section 5

Analytical Data1 – Based on data review, data point needs to be excluded from the data set.< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least oneresult is a J-value.* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.Exc – Excluded from data set.Table A5-1. Influent to Wastewater Treatment System, Belews CreekAnalyteUnitsMethodInfluent to FGD Wastewater Treatment System (SP-1)Set 1Set 2Set 3Set 44-SetAverageClassicalsAmmonia mg/L 350.1 1.90 NQ (1.00) 2.00 1.10 < 1.38Nitrate Nitrite as N mg/L 353.2 18.0 21.0 * 14.0 15.0 17.0Nitrogen, Total Kjeldahl mg/L 351.2 NQ (5.00) B 7.10 5.00 1.80 < 4.10Biochemical OxygenDemand mg/L 5210B ND (2.00) ND (2.00) ND (2.00) ND (2.00) ND (2.00)Chemical OxygenDemand mg/L 410.4 40.0 130 B 140 120 108Chloridemg/L 300.0 7,500 9,200 8,900 8,900 8,630Sulfatemg/L 300.0 1,100 1,100 1,200 1,100 1,130Cyanide, Total mg/L 4500 CN E NQ (0.100)NQ (0.100) ND (0.100) NQ (0.100) NQ (0.100)Total Dissolved Solids mg/L 2540C --- Exc115,000 18,000 17,000 16,700Total Suspended Solids mg/L 2540D 2,200 2,600 3,300 2,900 2,750Phosphorus, Total mg/L 365.1 0.0780 2.70 B 5.20 B NQ (0.0500) B < 2.00Total MetalsAluminum ug/L 200.7 49,000 B,^100,000B150,000 140,000 B 110,000Antimony ug/L 200.8 6.50 20.0 33.0 26.0 21.4Arsenicug/L 200.8 92.0 230 280 340 236Bariumug/L 200.7 1,100 1,200 B 1,900 1,700 1,4801 – Based on data review, data point needs to be excluded from the data set.< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least oneresult is a J-value.* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.Exc – Excluded from data set.Table A5-1. Influent to Wastewater Treatment System, Belews CreekAnalyteUnitsMethodInfluent to FGD Wastewater Treatment System (SP-1)Set 1Set 2Set 3Set 44-SetAverageBeryllium ug/L 200.7 7.70 13.0 22.0 22.0 16.2Boron ug/L200.7160,000200,000B200,000B 200,000B 190,000Cadmium ug/L 200.8 4.00 5.10 5.70 7.80 5.65Calcium ug/L200.73,300,0004,300,000B4,600,000B 4,600,000B 4,200,000Chromium ug/L 200.8 100 270 ^ 340 320 258Cobaltug/L 200.7 60.0 84.0 140 160 111Copperug/L 200.8 80.0 190 270 330 218Ironug/L 200.7 72,000 80,000 B 100,000 89,000 85,300Leadug/L 200.8 67.0 200 320 330 229Magnesium ug/L 200.7 690,000 760,000 B 740,000 B 630,000 B 705,000Manganese ug/L 200.7 7,200 7,800 B 8,200 B 6,500 B 7,430Mercuryng/L 1631E 228,000 299,000 129,000 131,000 197,000Molybdenum ug/L 200.7 NQ (40.0) 57.0 76.0 89.0 < 60.5Nickelug/L 200.8 170 270 340 370 288Selenium ug/L 200.8 3,400 5,700 7,400 6,000 5,630Silverug/L 200.8 ND (2.00) NQ (2.00)NQ (2.00) NQ (2.00) NQ (2.00)Sodium ug/L200.7 52,00048,000B50,00046,000B 49,000Thallium ug/L 200.8 5.10 8.30 8.50 11.0 8.23Tinug/L 200.7 NQ (200) NQ (200)NQ (200) NQ (200) NQ (200)1 – Based on data review, data point needs to be excluded from the data set.< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least oneresult is a J-value.* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.Exc – Excluded from data set.Table A5-1. Influent to Wastewater Treatment System, Belews CreekAnalyteUnitsMethodInfluent to FGD Wastewater Treatment System (SP-1)Set 1Set 2Set 3Set 44-SetAverageTitanium ug/L 200.7 940 2,500 B 3,800 4,700 2,990Vanadium ug/L 200.8 120 350 560 590 405Zincug/L 200.7 240 340 ^ 1,000 680 5651 – Based on data review, data point needs to be excluded from the data set.< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least oneresult is a J-value.* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.Exc – Excluded from data set.Table A5-2. Influent to Bioreactor System, Belews CreekAnalyteUnitsMethodInfluent to the Bioreactor System (SP-2)Set 1Set 2Set 3Set 44-SetAverageClassicalsAmmoniamg/L 350.1 2.20 NQ (1.00) 3.20 1.00 < 1.73Nitrate Nitrite as N mg/L 353.2 16.0 16.0 * 12.0 14.0 14.5Nitrogen, TotalKjeldahl mg/L 351.2 NQ (5.00) B 7.10 5.50 2.30 < 4.35Biochemical OxygenDemand mg/L 5210B ND (2.00) ND (2.00) NQ (2.50) ND (2.00) NQ (2.13)Chemical OxygenDemand mg/L 410.4 150 190 B 280 200 205Chloride mg/L 300.0 7,500 8,800 8,800 8,700 8,450Sulfate mg/L 300.0 1,200 1,300 1,200 1,200 1,230Cyanide, Total mg/L 4500 CN E NQ (0.100)NQ (0.100) ND (0.100) NQ (0.100) NQ (0.100)Total DissolvedSolids mg/L 2540C 13,000 14,000 14,000 12,000 13,300Total SuspendedSolids mg/L 2540D NQ (4.00) NQ (4.00)NQ (4.00) NQ (4.00) NQ (4.00)Phosphorus, Total mg/L 365.1 ND (0.0500) NQ(0.0500) B NQ (0.0500) B NQ (0.0500) B NQ (0.0500)1 – Based on data review, data point needs to be excluded from the data set.< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least oneresult is a J-value.* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.Exc – Excluded from data set.Table A5-2. Influent to Bioreactor System, Belews CreekAnalyteUnitsMethodInfluent to the Bioreactor System (SP-2)Set 1Set 2Set 3Set 44-SetAverageTotal MetalsAluminumug/L 200.7 ND (200) ^ ND (200)ND (200) ND (200) ND (200)Antimony ug/L 200.8 2.30 3.00 6.60 8.40 5.08Arsenicug/L 200.8 NQ (4.00) NQ (4.00)NQ (4.00) NQ (4.00) NQ (4.00)Barium ug/L 200.7 430 380 B 440 440 423Berylliumug/L 200.7 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Boron ug/L 200.7 150,000B 190,000B180,000B,4 180,000B 175,000Cadmiumug/L 200.8 ND (4.00) NQ (4.00)NQ (4.00) NQ (4.00) NQ (4.00)Calcium ug/L 200.7 3,700,000 3,800,000 B 3,700,000 4 4,000,000 B 3,800,000Chromiumug/L 200.8 ND (8.00) ND (8.00)^ ND (8.00) ND (8.00) ND (8.00)Cobaltug/L 200.7 NQ (20.0) NQ (20.0)NQ (20.0) NQ (20.0) NQ (20.0)Copperug/L 200.8 NQ (4.00) NQ (4.00)NQ (4.00) NQ (4.00) NQ (4.00)Ironug/L 200.7 ND (200) NQ (200) B ND (200) NQ (200) NQ (200)Leadug/L 200.8 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Magnesium ug/L 200.7 710,000 B 780,000 B 640,000 B,4 630,000 B 690,000Manganese ug/L 200.7 2,700 B 5,600 B 2,400 4 2,800 B 3,380Mercury ng/L 1631E 508 119 752 117 374Molybdenum ug/L 200.7 NQ (40.0) NQ (40.0) NQ (40.0) 45.0 < 26.3Nickel ug/L 200.8 36.0 67.0 70.0 59.0 58.01 – Based on data review, data point needs to be excluded from the data set.< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least oneresult is a J-value.* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.Exc – Excluded from data set.Table A5-2. Influent to Bioreactor System, Belews CreekAnalyteUnitsMethodInfluent to the Bioreactor System (SP-2)Set 1Set 2Set 3Set 44-SetAverageSelenium ug/L 200.8 120 89.0 900 4 110 305Silverug/L 200.8 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Sodium ug/L 200.7 48,000 B 49,000 B 49,000 46,000 B 48,000Thallium ug/L 200.8 3.50 3.70 6.00 6.60 4.95Tinug/L 200.7 ND (200) ND (200)ND (200) ND (200) ND (200)Titaniumug/L 200.7 NQ (20.0) NQ (20.0)B NQ (20.0) NQ (20.0) NQ (20.0)Vanadiumug/L 200.8 NQ (10.0) NQ (10.0)NQ (10.0) NQ (10.0) NQ (10.0)Zincug/L 200.7 NQ (40.0) ND (40.0) ^ ND (40.0) ND (40.0) NQ (40.0)1 – Based on data review, data point needs to be excluded from the data set.< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least oneresult is a J-value.* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.Exc – Excluded from data set.Table A5-3. Effluent from Bioreactor System, Belews CreekAnalyteUnitsMethodEffluent from the Bioreactor System (SP-3)Set 1Set 2Set 3Set 44-SetAverageClassicalsAmmonia mg/L 350.1 6.30 4.70 5.00 3.30 4.83Nitrate Nitrite as N mg/L 353.2 NQ (0.100) 0.150 * 0.130 0.140 < 0.118Nitrogen, Total Kjeldahl mg/L 351.2 7.40 B 10.0 7.10 3.60 7.03Biochemical OxygenDemand mg/L 5210B NQ (2.50) NQ (2.50) 3.50 ND (2.00) < 1.75Chemical OxygenDemand mg/L 410.4 160 F 200 B 220 190 F 193Chloridemg/L 300.0 7,300 8,400 9,100 8,300 8,280Sulfatemg/L 300.0 1,300 1,300 1,300 1,200 1,280Cyanide, Totalmg/L 4500 CN E NQ (0.100) FNQ (0.100) ND (0.100) NQ (0.100) F NQ (0.100)Total Dissolved Solids mg/L 2540C 15,000 13,000 11,000 14,000 F 13,300Total Suspended Solids mg/L 2540D 4.00 NQ (4.00) NQ (4.00) ND (4.00) < 2.50Phosphorus, Total mg/L 365.1 0.0840 0.120 B 0.0740 B 0.120 B,F 0.0995Total MetalsAluminumug/L 200.7 NQ (200) ^ NQ (200)B ND (200) ND (200) NQ (200)Antimonyug/L 200.8 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Arsenicug/L 200.8 NQ (4.00) NQ (4.00)NQ (4.00) NQ (4.00) NQ (4.00)Barium ug/L200.7 450420B4504804501 – Based on data review, data point needs to be excluded from the data set.< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least oneresult is a J-value.* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.Exc – Excluded from data set.Table A5-3. Effluent from Bioreactor System, Belews CreekAnalyteUnitsMethodEffluent from the Bioreactor System (SP-3)Set 1Set 2Set 3Set 44-SetAverageBerylliumug/L 200.7 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Boron ug/L200.7160,000B 170,000B170,000B 170,000B,4 168,000Cadmiumug/L 200.8 ND (4.00) ND (4.00)ND (4.00) ND (4.00) ND (4.00)Calcium ug/L200.73,200,0003,800,000B4,000,0004,100,000B,4 3,780,000Chromiumug/L 200.8 ND (8.00) ND (8.00)^ ND (8.00) ND (8.00) ND (8.00)Cobaltug/L 200.7 ND (20.0) ND (20.0)ND (20.0) ND (20.0) ND (20.0)Copperug/L 200.8 ND (4.00) ND (4.00)ND (4.00) ND (4.00) ND (4.00)Ironug/L 200.7 NQ (200) NQ (200) B NQ (200) NQ (200) NQ (200)Leadug/L 200.8 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Magnesium ug/L 200.7 740,000B 790,000B710,000B 670,000B,4 728,000Manganese ug/L 200.7 2,400B 5,200B3,500 2,800 B,4 3,480Mercuryng/L 1631E 403 162 24.2 2.99 148Molybdenumug/L 200.7 NQ (40.0) NQ (40.0)NQ (40.0) NQ (40.0) NQ (40.0)Nickelug/L 200.8 ND (4.00) NQ (4.00)ND (4.00) ND (4.00) NQ (4.00)Seleniumug/L 200.8 NQ (4.00) NQ (10.0) 32.0 NQ (4.00) < 10.3Silverug/L 200.8 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Sodium ug/L200.753,000B 49,000B51,00047,000B50,000Thalliumug/L 200.8 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Tinug/L 200.7 ND (200) ND (200)ND (200) ND (200) ND (200)1 – Based on data review, data point needs to be excluded from the data set.< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least oneresult is a J-value.* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.Exc – Excluded from data set.Table A5-3. Effluent from Bioreactor System, Belews CreekAnalyteUnitsMethodEffluent from the Bioreactor System (SP-3)Set 1Set 2Set 3Set 44-SetAverageTitaniumug/L 200.7 NQ (20.0) NQ (20.0)B NQ (20.0) NQ (20.0) NQ (20.0)Vanadiumug/L 200.8 ND (10.0) NQ (10.0)NQ (10.0) ND (10.0) NQ (10.0)Zincug/L 200.7 ND (40.0) NQ (40.0) ^ ND (40.0) ND (40.0) NQ (40.0)< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least oneresult is a J-value.Table A5-4. Classical Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment System, BelewsCreekAnalyteUnitMethodInfluent to FGDWastewater TreatmentSystem (SP-1)4-Set AverageInfluent toBioreactor System(SP-2)4-Set AverageEffluent fromBioreactor System(SP-3)4-Set AverageClassicalsAmmoniamg/L 350.1< 1.38< 1.734.83Nitrate Nitrite as Nmg/L 353.217.014.5< 0.118Nitrogen, Total Kjeldahl mg/L 351.2< 4.10< 4.357.03Biochemical Oxygen Demand mg/L 5210B ND (2.00) NQ (2.13) < 1.75Chemical Oxygen Demand mg/L 410.4108205193Chloride mg/L 300.0 8,630 8,450 8,280Sulfate mg/L 300.0 1,130 1,230 1,280Cyanide, Totalmg/L 4500 CN E NQ (0.100)NQ (0.100) NQ (0.100)Total Dissolved Solids mg/L 2540C16,70013,30013,300Total Suspended Solids mg/L 2540D2,750NQ (4.00)< 2.50Phosphorus, Totalmg/L 365.1< 2.00NQ (0.0500) 0.0995< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least oneresult is a J-value.Table A5-5. Metal Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment System, Belews CreekAnalyteUnitMethodInfluent to FGDWastewater TreatmentSystem (SP-1)4-Set AverageInfluent to BioreactorSystem (SP-2)4-Set AverageEffluent from BioreactorSystem (SP-3)4-Set AverageTotal MetalsAluminum ug/L 200.7110,000ND (200)NQ (200)Antimony ug/L 200.8 21.45.08ND (2.00)Arsenic ug/L 200.8236NQ (4.00)NQ (4.00)Barium ug/L 200.7 1,480423450Beryllium ug/L 200.716.2ND (2.00)ND (2.00)Boron ug/L 200.7 190,000 175,000 168,000Cadmium ug/L 200.85.65NQ (4.00)ND (4.00)Calcium ug/L 200.7 4,200,000 3,800,000 3,780,000Chromium ug/L 200.8258ND (8.00)ND (8.00)Cobalt ug/L 200.7111NQ (20.0)ND (20.0)Copper ug/L 200.8218NQ (4.00)ND (4.00)Ironug/L 200.785,300NQ (200)NQ (200)Lead ug/L 200.8229ND (2.00)ND (2.00)Magnesium ug/L 200.7 705,000690,000728,000Manganese ug/L 200.7 7,4303,3803,480Mercury ng/L 1631E 197,000374148Molybdenum ug/L 200.7< 60.5< 26.3NQ (40.0)Nickel ug/L 200.8 28858.0 NQ (4.00)Selenium ug/L 200.8 5,630305< 10.3Silver ug/L 200.8NQ (2.00)ND (2.00)ND (2.00)< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least oneresult is a J-value.Table A5-5. Metal Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment System, Belews CreekAnalyteUnitMethodInfluent to FGDWastewater TreatmentSystem (SP-1)4-Set AverageInfluent to BioreactorSystem (SP-2)4-Set AverageEffluent from BioreactorSystem (SP-3)4-Set AverageSodium ug/L 200.7 49,00048,00050,000Thallium ug/L 200.8 8.234.95ND (2.00)Tinug/L 200.7NQ (200)ND (200)ND (200)Titanium ug/L 200.72,990NQ (20.0)NQ (20.0)Vanadium ug/L 200.8405NQ (10.0)NQ (10.0)Zincug/L 200.7565NQ (40.0)NQ (40.0)

### Table A5-6. Field Blank Analytical Results, Belews Creek

Analyte Sample Point Method Unit Concentration

Total Metals

Boron Influent to FGD Wastewater Treatment System

Field Blank - Set 1 200.7 ug/L 2001 – Based on data review, data point needs to be excluded from the data set.ND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.Exc – Excluded from data set.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-7. Influent to FGD Wastewater TreatmentSystem, Set 1 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia 350.1mg/L 10.05511.9Nitrate Nitrite as N353.2 mg/L 2 0.038 0.2 18Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.38 5 3.6 J,BBiochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) UChemical Oxygen Demand 410.4 mg/L 2 8.1 40 40Chloride 300.0mg/L 5001301,5007,500Sulfate 300.0mg/L 50122501,100Cyanide, Total4500 CN E mg/L 1 0.02 0.1 0.039 JTotal Dissolved Solids 2540C mg/L 1 4.7 10 --- Exc1Total Suspended Solids 2540D mg/L 1 18 67 2,200Phosphorus, Total365.1 mg/L 1 0.005 0.05 0.078Total MetalsAluminum 200.7ug/L29.420049,000B,^Antimony 200.8ug/L20.7226.5Arsenic 200.8ug/L21.2492Barium 200.7ug/L22.5201,100Beryllium 200.7ug/L20.7127.7Boron 200.7ug/L25083025,000160,000Cadmium 200.8ug/L21.244Calcium 200.7ug/L501,70010,0003,300,0001 – Based on data review, data point needs to be excluded from the data set.ND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.Exc – Excluded from data set.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-7. Influent to FGD Wastewater TreatmentSystem, Set 1 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationChromium 200.8ug/L23.38100Cobalt 200.7ug/L21.12060Copper 200.8ug/L20.96480Iron 200.7ug/L23220072,000Lead 200.8ug/L20.73267Magnesium 200.7ug/L221400690,000Manganese 200.7ug/L20.51207,200Mercury 1631Eng/L40,0009,94020,800228,000Molybdenum 200.7ug/L2 1.6 40 36JNickel 200.8ug/L20.894170Selenium 200.8ug/L51.6103,400Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00052,000Thallium 200.8ug/L20.4725.1Tin 200.7ug/L24.82006.6JTitanium 200.7ug/L21.620940Vanadium 200.8ug/L21.710120Zinc 200.7ug/L29.140240ND – Not detected (number in parentheses is the quantitation limit).* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-8. Influent to FGD Wastewater TreatmentSystem, Set 2 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia 350.1mg/L 10.05510.97JNitrate Nitrite as N353.2 mg/L 5 0.095 0.5 21 *Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 7.1Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) UChemical Oxygen Demand 410.4 mg/L 2 8.1 40 130 BChloride 300.0mg/L 5001301,5009,200Sulfate 300.0mg/L 100235001,100Cyanide, Total4500 CN E mg/L 1 0.02 0.1 0.079 JTotal Dissolved Solids 2540C mg/L 1 94 200 15,000Total Suspended Solids 2540D mg/L 1 11 40 2,600Phosphorus, Total 365.1 mg/L 5 0.025 0.25 2.7 BTotal MetalsAluminum 200.7ug/L29.4200100,000BAntimony 200.8ug/L20.72220Arsenic 200.8ug/L53.110230Barium 200.7ug/L22.5201,200BBeryllium 200.7ug/L20.71213Boron200.7 ug/L 50 170 5,000 200,000 BCadmium 200.8ug/L21.245.1Calcium 200.7ug/L501,70010,0004,300,000BChromium 200.8ug/L23.38270^ND – Not detected (number in parentheses is the quantitation limit).* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-8. Influent to FGD Wastewater TreatmentSystem, Set 2 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationCobalt 200.7ug/L21.12084Copper 200.8ug/L20.964190Iron 200.7ug/L23220080,000BLead 200.8ug/L20.732200Magnesium 200.7ug/L221400760,000BManganese 200.7ug/L20.51207,800BMercury 1631Eng/L10,0002,4805,200299,000Molybdenum 200.7ug/L2 1.6 40 57Nickel 200.8ug/L20.894270Selenium 200.8ug/L51.6105,700Silver 200.8ug/L20.5920.62JSodium 200.7ug/L218010,00048,000BThallium 200.8ug/L20.4728.3Tin 200.7ug/L24.820013JTitanium 200.7ug/L21.6202,500BVanadium 200.8ug/L21.710350Zinc 200.7ug/L29.140340^ND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-9. Influent to FGD Wastewater TreatmentSystem, Set 3 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia 350.1mg/L10.0551 2Nitrate Nitrite as N353.2 mg/L 2 0.038 0.2 14Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 15Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) UChemical Oxygen Demand 410.4 mg/L 2 8.1 40 140Chloride 300.0mg/L200516008,900Sulfate 300.0mg/L100235001,200Cyanide, Total4500 CN E mg/L 1 0.02 0.1 ND (0.1) UTotal Dissolved Solids 2540C mg/L 1 240 500 18,000Total Suspended Solids 2540D mg/L 1 11 40 3,300Phosphorus, Total365.1 mg/L 10 0.05 0.5 5.2 BTotal MetalsAluminum 200.7ug/L502405,000150,000Antimony 200.8ug/L20.72233Arsenic 200.8ug/L21.24280Barium 200.7ug/L22.5201,900Beryllium 200.7ug/L20.71222Boron 200.7ug/L501705,000200,000BCadmium 200.8ug/L21.245.7Calcium 200.7ug/L501,70010,0004,600,000BChromium 200.8ug/L23.38340Cobalt 200.7ug/L21.120140ND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-9. Influent to FGD Wastewater TreatmentSystem, Set 3 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationCopper 200.8ug/L20.964270Iron 200.7ug/L232200100,000Lead 200.8ug/L20.732320Magnesium 200.7ug/L5054010,000740,000BManganese 200.7ug/L50135008,200BMercury 1631Eng/L50,00012,10025,200129,000Molybdenum 200.7ug/L2 1.6 40 76Nickel 200.8ug/L20.894340Selenium 200.8ug/L50161007,400Silver 200.8ug/L20.5920.76JSodium 200.7ug/L218010,00050,000Thallium 200.8ug/L20.4728.5Tin 200.7ug/L24.820021JTitanium 200.7ug/L21.6203,800Vanadium 200.8ug/L21.710560Zinc 200.7ug/L29.1401,000ND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-10. Influent to FGD Wastewater TreatmentSystem, Set 4 AnalyticalResults, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia 350.1mg/L10.05511.1Nitrate Nitrite as N353.2 mg/L 2 0.038 0.2 15Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 11.8Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) UChemical Oxygen Demand 410.4 mg/L 2 8.1 40 120Chloride 300.0mg/L200516008,900Sulfate 300.0mg/L50122501,100Cyanide, Total4500 CN E mg/L 1 0.02 0.1 0.029 JTotal Dissolved Solids2540C mg/L 1 240 500 17,000Total Suspended Solids 2540D mg/L 1 11 40 2,900Phosphorus, Total365.1 mg/L 1 0.005 0.05 0.036 J,BTotal MetalsAluminum 200.7ug/L29.4200140,000BAntimony 200.8ug/L20.72226Arsenic 200.8ug/L21.24340Barium 200.7ug/L22.5201,700Beryllium 200.7ug/L20.71222Boron200.7 ug/L 50 170 5,000 200,000 BCadmium 200.8ug/L21.247.8Calcium 200.7ug/L501,70010,0004,600,000BChromium 200.8ug/L23.38320Cobalt 200.7ug/L21.120160ND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-10. Influent to FGD Wastewater TreatmentSystem, Set 4 AnalyticalResults, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationCopper 200.8ug/L20.964330Iron 200.7ug/L23220089,000Lead 200.8ug/L20.732330Magnesium 200.7ug/L221400630,000BManganese 200.7ug/L20.51206,500BMercury 1631Eng/L10,0002,4105,050131,000Molybdenum 200.7ug/L21.6 40 89Nickel 200.8ug/L20.894370Selenium 200.8ug/L103.1206,000Silver 200.8ug/L20.5921.4JSodium200.7 ug/L 2 180 10,000 46,000 BThallium 200.8ug/L20.47211Tin 200.7ug/L24.820020JTitanium 200.7ug/L21.6204,700Vanadium 200.8ug/L21.710590Zinc 200.7ug/L29.140680ND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-11. Influent to Bioreactor System, Set 1 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia 350.1mg/L 10.05512.2Nitrate Nitrite as N353.2 mg/L 2 0.038 0.2 16Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.38 5 3.6 J,BBiochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) UChemical Oxygen Demand 410.4 mg/L 2 8.1 40 150Chloride 300.0mg/L 5001301,5007,500Sulfate 300.0mg/L 50122501,200Cyanide, Total4500 CN E mg/L 1 0.02 0.1 0.042 JTotal Dissolved Solids 2540C mg/L 1 47 100 13,000Total Suspended Solids 2540D mg/L 1 1.1 4 2.8 JPhosphorus, Total365.1 mg/L 1 0.005 0.05 ND (0.05) UTotal MetalsAluminum 200.7ug/L29.4200ND(200)U,^Antimony 200.8ug/L20.7222.3Arsenic 200.8ug/L21.242JBarium200.7 ug/L 2 2.5 20 430Beryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L25083025,000150,000BCadmium 200.8ug/L21.24ND(4)UCalcium 200.7ug/L501,70010,0003,700,000Chromium 200.8ug/L23.38ND(8)UND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-11. Influent to Bioreactor System, Set 1 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationCobalt 200.7ug/L21.1203JCopper 200.8ug/L20.9641.2JIron 200.7ug/L232200ND(200)ULead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L221400710,000BManganese 200.7ug/L20.51202,700BMercury 1631Eng/L10024.451508Molybdenum 200.7ug/L2 1.6 40 23 JNickel 200.8ug/L20.89436Selenium200.8 ug/L 5 1.6 10 120Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00048,000BThallium 200.8ug/L20.4723.5Tin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.6209.2JVanadium 200.8ug/L21.7101.7JZinc 200.7ug/L29.1409.5JND – Not detected (number in parentheses is the quantitation limit).* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-12. Influent to Bioreactor System, Set 2 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia 350.1mg/L10.05510.92JNitrate Nitrite as N353.2 mg/L 2 0.038 0.2 16 *Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 7.1Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) UChemical Oxygen Demand 410.4 mg/L 5 20 100 190 BChloride 300.0mg/L5001301,5008,800Sulfate 300.0mg/L100235001,300Cyanide, Total4500 CN E mg/L 1 0.02 0.1 0.065 JTotal Dissolved Solids 2540C mg/L 1 47 100 14,000Total Suspended Solids 2540D mg/L 1 1.1 4 3.2 JPhosphorus, Total365.1 mg/L 1 0.005 0.05 0.018 J,BTotal MetalsAluminum 200.7ug/L29.4200ND(200)UAntimony 200.8ug/L20.7223Arsenic 200.8ug/L21.243.2JBarium 200.7ug/L22.520380BBeryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L501705,000190,000BCadmium 200.8ug/L21.242JCalcium 200.7ug/L501,70010,0003,800,000BChromium 200.8ug/L23.38ND(8)U,^ND – Not detected (number in parentheses is the quantitation limit).* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-12. Influent to Bioreactor System, Set 2 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationCobalt 200.7ug/L21.12012JCopper 200.8ug/L20.9641.2JIron 200.7ug/L23220047J,BLead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L221400780,000BManganese 200.7ug/L20.51205,600BMercury 1631Eng/L10024.150.5119Molybdenum 200.7ug/L21.640 23JNickel 200.8ug/L52.21067Selenium 200.8ug/L51.61089Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00049,000BThallium 200.8ug/L20.4723.7Tin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.62012J,BVanadium 200.8ug/L21.7104.1JZinc 200.7ug/L29.140ND(40)U,^ND – Not detected (number in parentheses is the quantitation limit).4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-13. Influent to Bioreactor System, Set 3 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia350.1 mg/L 1 0.055 1 3.2Nitrate Nitrite as N353.2 mg/L 2 0.038 0.2 12Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 5.5Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 1.8 JChemical Oxygen Demand 410.4 mg/L 5 20 100 280Chloride 300.0mg/L200516008,800Sulfate 300.0mg/L100235001,200Cyanide, Total4500 CN E mg/L 1 0.02 0.1 ND (0.1) UTotal Dissolved Solids 2540C mg/L 1 94 200 14,000Total Suspended Solids 2540D mg/L 1 1.1 4 3.2 JPhosphorus, Total365.1 mg/L 1 0.005 0.05 0.045 J,BTotal MetalsAluminum 200.7ug/L29.4200ND(200)UAntimony 200.8ug/L20.7226.6Arsenic 200.8ug/L21.242.1JBarium 200.7ug/L22.520440Beryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L501705,000180,000B,4Cadmium 200.8ug/L21.242.4JCalcium 200.7ug/L501,70010,0003,700,0004Chromium 200.8ug/L23.38ND(8)UND – Not detected (number in parentheses is the quantitation limit).4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-13. Influent to Bioreactor System, Set 3 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationCobalt 200.7ug/L21.12010JCopper 200.8ug/L20.9641.3JIron 200.7ug/L232200ND(200)ULead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L5054010,000640,000B,4Manganese 200.7ug/L20.51202,4004Mercury1631E ng/L 500 122 255 752Molybdenum 200.7ug/L21.640 28JNickel 200.8ug/L20.89470Selenium 200.8ug/L51.6109004Silver 200.8ug/L20.592ND(2)USodium200.7 ug/L 2 180 10,000 49,000Thallium 200.8ug/L20.4726Tin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.62015JVanadium 200.8ug/L21.7103.7JZinc 200.7ug/L29.140ND(40)UND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-14. Influent to Bioreactor System, Set 4 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia 350.1mg/L 10.05511Nitrate Nitrite as N353.2 mg/L 5 0.095 0.5 14Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 2.3Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) UChemical Oxygen Demand 410.4 mg/L 2 8.1 40 200Chloride 300.0mg/L 200516008,700Sulfate 300.0mg/L 50122501,200Cyanide, Total4500 CN E mg/L 1 0.02 0.1 0.04 JTotal Dissolved Solids 2540C mg/L 1 94 200 12,000Total Suspended Solids 2540D mg/L 1 1.1 4 1.2 JPhosphorus, Total365.1 mg/L 1 0.005 0.05 0.031 J,BTotal MetalsAluminum 200.7ug/L29.4200ND(200)UAntimony 200.8ug/L20.7228.4Arsenic 200.8ug/L21.242.6JBarium 200.7ug/L22.520440Beryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L501705,000180,000BCadmium 200.8ug/L21.241.8JCalcium 200.7ug/L501,70010,0004,000,000BChromium 200.8ug/L23.38ND(8)UCobalt 200.7ug/L21.1207.6JND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-14. Influent to Bioreactor System, Set 4 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationCopper 200.8ug/L20.9641.7JIron 200.7ug/L23220036JLead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L221400630,000BManganese 200.7ug/L20.51202,800BMercury 1631Eng/L10024.150.5117Molybdenum 200.7ug/L21.6 40 45Nickel 200.8ug/L20.89459Selenium 200.8ug/L20.624110Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00046,000BThallium 200.8ug/L20.4726.6Tin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.62017JVanadium 200.8ug/L21.7103.6JZinc 200.7ug/L29.140ND(40)UND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.F – MS and/or MSD not within laboratory control limits.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-15. Effluent from Bioreactor System, Set 1 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia 350.1mg/L 10.05516.3Nitrate Nitrite as N353.2 mg/L 1 0.019 0.1 0.061 JNitrogen, Total Kjeldahl 351.2 mg/L 2 0.15 2 7.4 BBiochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 2.2 JChemical Oxygen Demand 410.4 mg/L 2 8.1 40 160 FChloride 300.0mg/L 5001301,5007,300Sulfate 300.0mg/L 50122501,300Cyanide, Total4500 CN E mg/L 1 0.02 0.1 0.036 J,FTotal Dissolved Solids 2540C mg/L 1 47 100 15,000Total Suspended Solids 2540D mg/L 1 1.1 44Phosphorus, Total365.1 mg/L 1 0.005 0.05 0.084Total MetalsAluminum 200.7ug/L29.420079J,^Antimony 200.8ug/L20.722ND(2)UArsenic 200.8ug/L21.242JBarium 200.7ug/L22.520450Beryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L25083025,000160,000BCadmium 200.8ug/L21.24ND(4)UCalcium 200.7ug/L2694003,200,000Chromium 200.8ug/L23.38ND(8)UND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.F – MS and/or MSD not within laboratory control limits.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-15. Effluent from Bioreactor System, Set 1 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationCobalt 200.7ug/L21.120ND(20)UCopper 200.8ug/L20.964ND(4)UIron 200.7ug/L232200110JLead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L221400740,000BManganese 200.7ug/L20.51202,400BMercury 1631Eng/L10024.451403Molybdenum 200.7ug/L21.640 1.8JNickel 200.8ug/L20.894ND(4)USelenium 200.8ug/L20.6243.9JSilver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00053,000BThallium 200.8ug/L20.472ND(2)UTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.6207.9JVanadium 200.8ug/L21.710ND(10)UZinc 200.7ug/L29.140ND(40)UND – Not detected (number in parentheses is the quantitation limit).* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-16. Effluent from Bioreactor System, Set 2 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia 350.1mg/L 10.05514.7Nitrate Nitrite as N353.2 mg/L 1 0.019 0.1 0.15 *Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.15 2 10Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 2 JChemical Oxygen Demand 410.4 mg/L 5 20 100 200 BChloride300.0 mg/L 500 130 1,500 8,400Sulfate 300.0mg/L 100235001,300Cyanide, Total4500 CN E mg/L 1 0.02 0.1 0.052 JTotal Dissolved Solids 2540C mg/L 1 47 100 13,000Total Suspended Solids 2540D mg/L 1 1.1 4 2 JPhosphorus, Total365.1 mg/L 1 0.005 0.05 0.12 BTotal MetalsAluminum 200.7ug/L29.420039J,BAntimony 200.8ug/L20.722ND(2)UArsenic 200.8ug/L21.242JBarium 200.7ug/L22.520420BBeryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L501705,000170,000BCadmium 200.8ug/L21.24ND(4)UCalcium 200.7ug/L501,70010,0003,800,000BChromium 200.8ug/L23.38ND(8)U,^ND – Not detected (number in parentheses is the quantitation limit).* - LCS or LCSD is outside the laboratory control limits.^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-16. Effluent from Bioreactor System, Set 2 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationCobalt 200.7ug/L21.120ND(20)UCopper 200.8ug/L20.964ND(4)UIron 200.7ug/L232200170J,BLead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L221400790,000BManganese 200.7ug/L20.51205,200BMercury 1631Eng/L204.8310.1162Molybdenum 200.7ug/L21.6 40 1.9JNickel 200.8ug/L20.8941.2JSelenium 200.8ug/L51.6101.8JSilver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00049,000BThallium 200.8ug/L20.472ND(2)UTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.62012J,BVanadium 200.8ug/L21.7102.3JZinc 200.7ug/L29.1409.4J,^ND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-17. Effluent from Bioreactor System, Set 3 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia 350.1mg/L 10.05515Nitrate Nitrite as N353.2 mg/L 1 0.019 0.1 0.13Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 7.1Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 3.5Chemical Oxygen Demand 410.4 mg/L 5 20 100 220Chloride 300.0mg/L 200516009,100Sulfate 300.0mg/L 100235001,300Cyanide, Total4500 CN E mg/L 1 0.02 0.1 ND (0.1) UTotal Dissolved Solids 2540C mg/L 1 94 200 11,000Total Suspended Solids 2540D mg/L 1 1.1 4 1.6 JPhosphorus, Total365.1 mg/L 1 0.005 0.05 0.074 BTotal MetalsAluminum 200.7ug/L29.4200ND(200)UAntimony 200.8ug/L20.722ND(2)UArsenic 200.8ug/L21.242.7JBarium 200.7ug/L22.520450Beryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L501705,000170,000BCadmium 200.8ug/L21.24ND(4)UCalcium 200.7ug/L501,70010,0004,000,000Chromium 200.8ug/L23.38ND(8)UCobalt 200.7ug/L21.120ND(20)UND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-17. Effluent from Bioreactor System, Set 3 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationCopper 200.8ug/L20.964ND(4)UIron 200.7ug/L23220065JLead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L5054010,000710,000BManganese 200.7ug/L20.51203,500Mercury 1631Eng/L204.8710.224.2Molybdenum 200.7ug/L21.640 2.3JNickel 200.8ug/L20.894ND(4)USelenium 200.8ug/L51.61032Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00051,000Thallium 200.8ug/L20.472ND(2)UTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.62013JVanadium 200.8ug/L21.7101.9JZinc 200.7ug/L29.140ND(40)UND – Not detected (number in parentheses is the quantitation limit).4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.F – MS and/or MSD not within laboratory control limits.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-18. Effluent from Bioreactor System, Set 4 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia 350.1mg/L 10.05513.3Nitrate Nitrite as N353.2 mg/L 1 0.019 0.1 0.14Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 3.6Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) UChemical Oxygen Demand 410.4 mg/L 2 8.1 40 190 FChloride 300.0mg/L 200516008,300Sulfate 300.0mg/L 50122501,200Cyanide, Total4500 CN E mg/L 1 0.02 0.1 0.032 J,FTotal Dissolved Solids 2540C mg/L 1 94 200 14,000 FTotal Suspended Solids 2540D mg/L 1 1.1 4 ND (4) UPhosphorus, Total365.1 mg/L 1 0.005 0.05 0.12 B,FTotal MetalsAluminum 200.7ug/L29.4200ND(200)UAntimony 200.8ug/L20.722ND(2)UArsenic 200.8ug/L21.241.6JBarium 200.7ug/L22.520480Beryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L501705,000170,000B,4Cadmium 200.8ug/L21.24ND(4)UCalcium 200.7ug/L501,70010,0004,100,000B,4Chromium 200.8ug/L23.38ND(8)UND – Not detected (number in parentheses is the quantitation limit).4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.F – MS and/or MSD not within laboratory control limits.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-18. Effluent from Bioreactor System, Set 4 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationCobalt 200.7ug/L21.120ND(20)UCopper 200.8ug/L20.964ND(4)UIron 200.7ug/L232200150JLead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L221400670,000B,4Manganese200.7 ug/L 2 0.51 20 2,800 B,4Mercury 1631Eng/L10.240.52.99Molybdenum 200.7ug/L21.640 2.5JNickel 200.8ug/L20.894ND(4)USelenium 200.8ug/L20.6240.9JSilver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00047,000BThallium 200.8ug/L20.472ND(2)UTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.62016JVanadium 200.8ug/L21.710ND(10)UZinc 200.7ug/L29.140ND(40)UND – Not detected (number in parentheses is the quantitation limit).J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-19. Influent to FGD Wastewater Treatment System Field Blank AnalyticalResults, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND(200) UAntimony 200.8 ug/L 2 0.72 2 ND(2) UArsenic 200.8ug/L 2 1.2 4 ND(4) UBarium 200.7ug/L 2 2.5 20 ND(20) UBeryllium 200.7 ug/L 2 0.71 2 ND(2) UBoron 200.7ug/L 2 6.7 200 200Cadmium 200.8 ug/L 2 1.2 4 ND(4) UCalcium 200.7ug/L 2 69 400 360 JChromium 200.8 ug/L 2 3.3 8 ND(8) UCobalt 200.7ug/L 2 1.1 20 ND(20)UCopper 200.8ug/L 2 0.96 4 ND(4) UIron 200.7ug/L 2 32 200 ND(200)ULead 200.8ug/L 2 0.73 2 ND(2)UMagnesium 200.7 ug/L 2 21 400 41 JManganese 200.7 ug/L 2 0.51 20 ND(20) UMercury 1631Eng/L 1 0.24 0.5 ND(0.5) UMolybdenum 200.7 ug/L 2 1.6 40 ND (40) UNickel 200.8ug/L 2 0.89 4 ND(4) USelenium 200.8 ug/L 2 0.62 4 ND(4) USilver 200.8ug/L 2 0.59 2 ND(2)USodium 200.7ug/L 2 180 10,000 ND(10,000)UThallium 200.8ug/L 2 0.47 2 ND(2) UTin 200.7ug/L 2 4.8 200 ND(200)UTitanium 200.7ug/L 2 1.6 20 ND(20) UND – Not detected (number in parentheses is the quantitation limit).J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-19. Influent to FGD Wastewater Treatment System Field Blank AnalyticalResults, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationVanadium 200.8 ug/L 2 1.7 10 ND(10) UZinc 200.7ug/L 2 9.1 40 9.7 JND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-20. Influent to Bioreactor System Field Blank, Set 1 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTotal MetalsAluminum 200.7ug/L 2 9.4 200 ND(200)U,^Antimony 200.8ug/L 2 0.72 2 ND(2)UArsenic 200.8ug/L 2 1.2 4 ND(4)UBarium 200.7ug/L 2 2.5 20ND(20)UBeryllium 200.7ug/L 2 0.71 2 ND(2)UBoron 200.7ug/L 26.7 20018J,BCadmium 200.8ug/L 2 1.2 4 ND(4)UCalcium 200.7ug/L 2 69 400 360JChromium 200.8ug/L 2 3.3 8 ND(8)UCobalt 200.7ug/L 2 1.1 20ND(20)UCopper 200.8ug/L 2 0.96 4ND(4)UIron 200.7ug/L 232200ND(200)ULead 200.8ug/L 20.73 2ND(2)UMagnesium 200.7ug/L 2 21 400 150J,BManganese 200.7ug/L 2 0.51 20 1.1J,BMercury 1631Eng/L 1 0.24 0.5ND(0.5)UMolybdenum 200.7ug/L 2 1.6 40 ND(40)UNickel 200.8ug/L 20.89 4ND(4)USelenium 200.8ug/L 2 0.62 4 ND(4)USilver 200.8ug/L 20.59 2ND(2)USodium 200.7ug/L 2 180 10,000250J,BThallium 200.8ug/L 2 0.47 2 ND(2)UND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-20. Influent to Bioreactor System Field Blank, Set 1 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTin 200.7ug/L 24.8200ND(200)UTitanium 200.7ug/L 2 1.6 20 ND(20)UVanadium 200.8ug/L 2 1.7 10 ND(10)UZinc 200.7ug/L 29.1 40ND(40)UND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-21. Influent to Bioreactor System Field Blank, Set 2 AnalyticalResults, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTotal MetalsAluminum 200.7ug/L 2 9.4 200 11J,BAntimony 200.8ug/L 2 0.72 2 ND(2)UArsenic 200.8ug/L 2 1.2 4 ND(4)UBarium 200.7ug/L 2 2.5 20ND(20)UBeryllium 200.7ug/L 2 0.71 2 ND(2)UBoron 200.7ug/L 26.7 200 32J,BCadmium 200.8ug/L 2 1.2 4 ND(4)UCalcium 200.7ug/L 2 69 400 230J,BChromium 200.8ug/L 2 3.3 8 ND(8)U,^Cobalt 200.7ug/L 2 1.1 20ND(20)UCopper 200.8ug/L 2 0.96 4 ND(4)UIron 200.7ug/L 232 200ND(200)ULead 200.8ug/L 20.73 2ND(2)UMagnesium 200.7ug/L 2 21 400 98J,BManganese 200.7ug/L 2 0.51 20 2.1J,BMercury 1631Eng/L 1 0.24 0.5 ND(0.5)UMolybdenum 200.7ug/L 2 1.6 40 ND(40)UNickel 200.8ug/L 20.89 4 ND(4)USelenium 200.8ug/L 2 0.62 4 1.2JSilver 200.8ug/L 20.59 2ND(2)USodium 200.7ug/L 2 180 10,000ND(10,000)UThallium 200.8ug/L 2 0.47 2 ND(2)UND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-21. Influent to Bioreactor System Field Blank, Set 2 AnalyticalResults, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTin 200.7ug/L 24.8200ND(200)UTitanium 200.7ug/L 2 1.6 20 ND(20)UVanadium 200.8ug/L 2 1.7 10 3.3JZinc 200.7ug/L 29.1 4015J,^ND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-22. Influent to Bioreactor System Field Blank, Set 3 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTotal MetalsAluminum 200.7ug/L 2 9.4 200 ND(200)UAntimony 200.8ug/L 2 0.72 2 ND(2)UArsenic 200.8ug/L 2 1.2 4ND(4)UBarium 200.7ug/L 2 2.5 20ND(20)UBeryllium 200.7ug/L 2 0.71 2 ND(2)UBoron 200.7ug/L 26.7 20069J,BCadmium 200.8ug/L 2 1.2 4 ND(4)UCalcium 200.7ug/L 2 69 400 290JChromium 200.8ug/L 2 3.3 8 ND(8)UCobalt 200.7ug/L 2 1.1 20ND(20)UCopper 200.8ug/L 2 0.96 4ND(4)UIron 200.7ug/L 232200ND(200)ULead 200.8ug/L 20.73 2ND(2)UMagnesium 200.7ug/L 2 21 400 50J,BManganese 200.7ug/L 2 0.51 20 ND(20)UMercury 1631Eng/L 1 0.25 0.52ND(0.52)UMolybdenum 200.7ug/L 2 1.6 40 ND(40)UNickel 200.8ug/L 20.89 4ND(4)USelenium 200.8ug/L 2 0.62 4 ND(4)USilver 200.8ug/L 20.59 2ND(2)USodium 200.7ug/L 2 180 10,000300JThallium 200.8ug/L 2 0.47 2 ND(2)UTin 200.7ug/L 24.8200ND(200)UND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-22. Influent to Bioreactor System Field Blank, Set 3 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTitanium 200.7ug/L 2 1.6 20 ND(20)UVanadium 200.8ug/L 2 1.7 10 2.3JZinc 200.7ug/L 29.1 40ND(40)UND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-23. Influent to Bioreactor System Field Blank, Set 4 AnalyticalResults, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTotal MetalsAluminum 200.7ug/L 2 9.4 200 ND(200)UAntimony 200.8ug/L 2 0.72 2 ND(2)UArsenic 200.8ug/L 2 1.2 4ND(4)UBarium 200.7ug/L 2 2.5 20ND(20)UBeryllium 200.7ug/L 2 0.71 2 ND(2)UBoron 200.7ug/L 26.7 20028J,BCadmium 200.8ug/L 2 1.2 4 ND(4)UCalcium 200.7ug/L 2 69 400ND(400)UChromium 200.8ug/L 2 3.3 8 ND(8)UCobalt 200.7ug/L 2 1.1 20ND(20)UCopper 200.8ug/L 2 0.96 4ND(4)UIron 200.7ug/L 232200ND(200)ULead 200.8ug/L 20.73 2ND(2)UMagnesium 200.7ug/L 2 21 400 ND(400)UManganese 200.7ug/L 2 0.51 20 ND(20)UMercury 1631Eng/L 1 0.24 0.5ND(0.5)UMolybdenum 200.7ug/L 2 1.6 40 ND(40)UNickel 200.8ug/L 20.89 4ND(4)USelenium 200.8ug/L 2 0.62 4 ND(4)USilver 200.8ug/L 20.59 2ND(2)USodium 200.7ug/L 2 180 10,000220J,BThallium 200.8ug/L 2 0.47 2 ND(2)UTin 200.7ug/L 24.8200ND(200)UND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-23. Influent to Bioreactor System Field Blank, Set 4 AnalyticalResults, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTitanium 200.7ug/L 2 1.6 20 ND(20)UVanadium 200.8ug/L 2 1.7 10 ND(10)UZinc 200.7ug/L 29.1 40ND(40)UND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-24. Effluent from Bioreactor System Field Blank, Set 1 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTotal MetalsAluminum 200.7ug/L 2 9.4 200 ND(200)U,^Antimony 200.8ug/L 2 0.72 2 ND(2)UArsenic 200.8ug/L 2 1.2 4 ND(4)UBarium 200.7ug/L 2 2.5 20ND(20)UBeryllium 200.7ug/L 2 0.71 2 ND(2)UBoron 200.7ug/L 26.7 20023J,BCadmium 200.8ug/L 2 1.2 4 ND(4)UCalcium 200.7ug/L 2 69 400ND(400)UChromium 200.8ug/L 2 3.3 8 ND(8)UCobalt 200.7ug/L 2 1.1 20ND(20)UCopper 200.8ug/L 2 0.96 4ND(4)UIron 200.7ug/L 232200ND(200)ULead 200.8ug/L 20.73 2ND(2)UMagnesium 200.7ug/L 2 21 400 55J,BManganese 200.7ug/L 2 0.51 20 1.2J,BMercury 1631Eng/L 1 0.24 0.5ND(0.5)UMolybdenum 200.7ug/L 2 1.6 40 ND(40)UNickel 200.8ug/L 20.89 4ND(4)USelenium 200.8ug/L 2 0.62 4 ND(4)USilver 200.8ug/L 20.59 2ND(2)USodium 200.7ug/L 2 180 10,000210J,BThallium 200.8ug/L 2 0.47 2 ND(2)UND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-24. Effluent from Bioreactor System Field Blank, Set 1 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTin 200.7ug/L 24.8200ND(200)UTitanium 200.7ug/L 2 1.6 20 ND(20)UVanadium 200.8ug/L 2 1.7 10 ND(10)UZinc 200.7ug/L 29.1 40ND(40)UND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-25. Effluent fromBioreactor System Field Blank, Set2 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTotal MetalsAluminum 200.7ug/L 2 9.4 200 ND(200)U,^Antimony 200.8ug/L 2 0.72 2 ND(2)UArsenic 200.8ug/L 2 1.2 4ND(4)UBarium 200.7ug/L 2 2.5 20ND(20)UBeryllium 200.7ug/L 2 0.71 2 ND(2)UBoron 200.7ug/L 26.7 20023J,BCadmium 200.8ug/L 2 1.2 4 ND(4)UCalcium 200.7ug/L 2 69 400ND(400)UChromium 200.8ug/L 2 3.3 8 ND(8)UCobalt 200.7ug/L 2 1.1 20ND(20)UCopper 200.8ug/L 2 0.96 4ND(4)UIron 200.7ug/L 232200ND(200)ULead 200.8ug/L 20.73 2ND(2)UMagnesium 200.7ug/L 2 21 400 55J,BManganese 200.7ug/L 2 0.51 20 1.2J,BMercury 1631Eng/L 1 0.24 0.5ND(0.5)UMolybdenum 200.7ug/L 2 1.6 40 ND(40)UNickel 200.8ug/L 20.89 4ND(4)USelenium 200.8ug/L 2 0.62 4 ND(4)USilver 200.8ug/L 20.59 2ND(2)USodium 200.7ug/L 2 180 10,000210J,BThallium 200.8ug/L 2 0.47 2 ND(2)UND – Not detected (number in parentheses is the quantitation limit).^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-25. Effluent fromBioreactor System Field Blank, Set2 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTin 200.7ug/L 24.8200ND(200)UTitanium 200.7ug/L 2 1.6 20ND(20)UVanadium 200.8ug/L 2 1.7 10 ND(10)UZinc 200.7ug/L 29.1 40ND(40)UND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-26. Effluent from Bioreactor System Field Blank, Set 3 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTotal MetalsAluminum 200.7ug/L 2 9.4 200ND(200)UAntimony 200.8ug/L 2 0.72 2 ND(2)UArsenic 200.8ug/L 2 1.2 4ND(4)UBarium 200.7ug/L 2 2.5 20ND(20)UBeryllium 200.7ug/L 2 0.71 2 ND(2)UBoron 200.7ug/L 26.7 20075J,BCadmium 200.8ug/L 2 1.2 4 ND(4)UCalcium 200.7ug/L 2 69 400ND(400)UChromium 200.8ug/L 2 3.3 8 ND(8)UCobalt 200.7ug/L 2 1.1 20ND(20)UCopper 200.8ug/L 2 0.96 4ND(4)UIron 200.7ug/L 232200ND(200)ULead 200.8ug/L 20.73 2ND(2)UMagnesium 200.7ug/L 2 21 400 ND(400)UManganese 200.7ug/L 2 0.51 20 ND(20)UMercury 1631Eng/L 1 0.24 0.5 0.3JMolybdenum 200.7ug/L 2 1.6 40 ND(40)UNickel 200.8ug/L 20.89 4ND(4)USelenium 200.8ug/L 2 0.62 4 ND(4)USilver 200.8ug/L 20.59 2ND(2)USodium 200.7ug/L 2 180 10,000270JThallium 200.8ug/L 2 0.47 2 ND(2)UTin 200.7ug/L 24.8200ND(200)UND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-26. Effluent from Bioreactor System Field Blank, Set 3 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTitanium 200.7ug/L 2 1.6 20ND(20)UVanadium 200.8ug/L 2 1.7 10 2.1JZinc 200.7ug/L 29.1 40ND(40)UND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-27. Effluent from Bioreactor System Field Blank, Set 4 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTotal MetalsAluminum 200.7ug/L 2 9.4 200 ND(200)UAntimony 200.8ug/L 2 0.72 2 ND(2)UArsenic 200.8ug/L 2 1.2 4ND(4)UBarium 200.7ug/L 2 2.5 20ND(20)UBeryllium 200.7ug/L 2 0.71 2 ND(2)UBoron 200.7ug/L 26.7 20017J,BCadmium 200.8ug/L 2 1.2 4 ND(4)UCalcium 200.7ug/L 2 69 400ND(400)UChromium 200.8ug/L 2 3.3 8 ND(8)UCobalt 200.7ug/L 2 1.1 20ND(20)UCopper 200.8ug/L 2 0.96 4ND(4)UIron 200.7ug/L 232200ND(200)ULead 200.8ug/L 20.73 2ND(2)UMagnesium 200.7ug/L 2 21 400 ND(400)UManganese 200.7ug/L 2 0.51 20 ND(20)UMercury 1631Eng/L 1 0.24 0.5ND(0.5)UMolybdenum 200.7ug/L 2 1.6 40 ND(40)UNickel 200.8ug/L 20.89 4ND(4)USelenium 200.8ug/L 2 0.62 4 ND(4)USilver 200.8ug/L 20.59 2ND(2)USodium 200.7ug/L 2 180 10,000240J,BThallium 200.8ug/L 2 0.47 2 ND(2)UTin 200.7ug/L 24.8200ND(200)UND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table A5-27. Effluent from Bioreactor System Field Blank, Set 4 Analytical Results, Belews CreekAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-SpecificQLConcentrationTitanium 200.7ug/L 2 1.6 20 ND(20)UVanadium 200.8ug/L 2 1.7 10 ND(10)UZinc 200.7ug/L 29.1 40ND(40)U

## Section 6

Data Review Narratives

[A concentration noted as “XXX” indicates that the sample result applies to a different power plant and has been

removed.]

### 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: 2/9/2012

Subject: FGS Data Review Narrative for Total Mercury – Long-Term M onitoring

Month 1 (Part 2)

Frontier Global Sciences (FGS) generated analytical da ta for total mercury. FGS

analyzed the samples according to EPA Method 1631E for merc ury by Cold Vapor

Atomic Fluorescence Spectrometry (CVAFS) analysis.

Table 1 summarizes the 20 samples (excluding laboratory pre p blanks) FGS extracted

and analyzed for total mercury.

Table 1. 

### Long-Term Monitoring Month 1 (Part 2) Mercury – Sample Identification

EPA

Sample # Lab Sample

ID # Sample

Matrix Sample Description Sampling

Date

71991 1010066-05 Aqueous FGD Influent, Set 1 10/6/2010

71995 1010066-06 Aqueous FGD Bioreactor Influent, Set 1 10/6/2010

71999 1010066-07 Aqueous FGD Bioreactor Effluent, Set 1 10/6/2010

72003 1010066-10 Aqueous FGD Influent Field Blank 10/6/2010

72004 1010066-08 Aqueous FGD Bioreactor Influent Field Blank, Set 1 10/ 6/2010

72008 1010066-09 Aqueous FGD Bioreactor Effluent Field Blank, Set 1 10/6 /2010

72141 1010048-01 Aqueous FGD Influent, Set 1 10/5/2010

72145 1010048-02 Aqueous FGD Bioreactor Influent, Set 1 10/4/2010

72149 1010048-03 Aqueous FGD Bioreactor Effluent, Set 1 10/4/2010

72153 1010048-06 Aqueous FGD Influent Field Blank 10/5/2010

72154 1010048-04 Aqueous FGD Bioreactor Influent Field Blank, Set 1 10/ 4/2010

72158 1010048-05 Aqueous FGD Bioreactor Effluent Field Blank, Set 1 10/4 /2010

72241 1010066-01 Aqueous FGD Influent, Set 1 10/7/2010

72245 1010066-02 Aqueous FGD Effluent, Set 1 10/7/2010

72249 1010066-04 Aqueous FGD Influent Field Blank 10/7/2010

72250 1010066-03 Aqueous FGD Effluent Field Blank, Set 1 10/6/2010

72291 1010046-01 Aqueous FGD Influent Set 1 10/5/2010

72295 1010046-05 Aqueous FGD Effluent, Set 1 10/5/2010

72299 1010046-07 Aqueous FGD Influent Field Blank 10/5/2010

### 2

Table 1. 

### Long-Term Monitoring Month 1 (Part 2) Mercury – Sample Identification

EPA

Sample # Lab Sample

ID # Sample

Matrix Sample Description Sampling

Date

72300 1010046-06 Aqueous FGD Effluent, Field Blank, Set 1 10/4/2010



### SUMMARY

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

There were no findings from the data review that required a dditional qualifiers in this

dataset.

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES

There were no sample receipt issues in this data package.

INITIAL CALIBRATION

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

the CVAFS analysis consisted of a blank and five calibrat ion standards with a correlation

coefficient ≥ 0.995. All method-specified criteria were met.

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

All initial and continuing calibration verifications (I CVs, CCVs) met method-specified

criteria.

BLANKS

All the preparation blanks or laboratory reagent blanks (L RBs) and the continuing

calibration blanks (CCBs) met method-specified criteria. Because all of the blank results

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

results.

DUPLICATES

No field duplicate samples were collected with these sa mpling episodes. One sample was

analyzed in duplicate at the laboratory, sample 71999. The r elative percent difference

(RPD) for sample 71999 was 1.31%. The laboratory’s RPD cr iteria between analytical

duplicates is 24%.

LABORATORY CONTROL SAMPLES

All laboratory control samples were within FGS’s contr ol limits of 80-120% recovery

and 24% RPD.

### 3

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

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

71995 and 71999. MS/MSD were also performed on samples 72199 and 72195 in the

same preparatory batch but discussed in a previous narrative. All aqueous MS/MSD

recoveries were within method specifications of 71-125%. All RPDs met methodspecified criteria.

DETECTION LIMITS

The laboratory MDL in the synthetic matrix was 0.239 ng/ L. Results below this MDL

were reported as not detected (ND).

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A EAD

Deb Bartram, ERG

TJ Finseth, ERG

From: Randy Mercurio, ERG

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.8 – Long- Term

Monitoring: Month 1 (Part 2)

TestAmerica generated analytical data for total metals (antimony, arsenic, cadmium,

chromium, copper, lead, nickel, selenium, silver, thalliumand vanadium) for these longterm monitoring samples. The samples were analyzed accor ding to EPA Method 200.8.

Table 1 summarizes the samples TestAmerica extracted a nd analyzed for total metals by

EPA Method 200.8.

Table 1. 

### Long-Term Monitoring Month 1 (Part 2) Total Metals – Sample

Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

71991 FGD Influent, Set 1 280

- 8121

- 1 Aqueous 10/6/2010 10/7/2010

71995 FGD Bioreactor Influent, Set 1 280

- 8194

- 1 Aqueous 10/7/2010 10/8/2010

71999 FGD Bioreactor Effluent, Set 1 280

- 8194

- 2 Aqueous 10/7/2010 10/8/2010

72003 FGD Influent Field Blank 280

- 8121

- 2 Aqueous 10/6/2010 10/7/2010

72004 FGD Bioreactor Influent Field

Blank, Set 1 280

- 8194

- 3 Aqueous 10/7/2010 10/8/2010

72008 FGD Bioreactor Effluent Field

Blank, Set 1 280

- 8194

- 4 Aqueous 10/7/2010 10/8/2010

72141 FGD Influent, Set 1 280

- 8061

- 1 Aqueous 10/5/2010 10/6/2010

72145 FGD Bioreactor Influent, Set 1 280

- 8061

- 2 Aqueous 10/5/2010 10/6/2010

72149 FGD Bioreactor Effluent, Set 1 280

- 8061

- 3 Aqueous 10/5/2010 10/6/2010

72154 FGD Bioreactor Influent Field

Blank, Set 1 280

- 8061

- 4 Aqueous 10/5/2010 10/6/2010

72153 FGD Influent Field Blank 280

- 8061

- 6 Aqueous 10/5/2010 10/6/2010

72158 FGD Bioreactor Effluent Field

Blank, Set 1 280

- 8061

- 5 Aqueous 10/5/2010 10/6/2010

72241 FGD Influent, Set 1 280

- 8195

- 1 Aqueous 10/7/2010 10/8/2010

72245 FGD Effluent, Set 1 280

- 8195

- 2 Aqueous 10/7/2010 10/8/2010

72249 FGD Bioreactor Influent Field

Blank, Set 1 280

- 8195

- 4 Aqueous 10/7/2010 10/8/2010

### 2 Table 1. 

### Long-Term Monitoring Month 1 (Part 2) Total Metals – Sample

Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

72250 FGD Effluent Field Blank, Set 1 280

- 8195

- 3 Aqueous 10/7/2010 10/8/2010

72291 FGD Influent, Set 1 280

- 8058

- 1 Aqueous 10/5/2010 10/6/2010

72295 FGD Effluent, Set 1 280

- 8058

- 2 Aqueous 10/5/2010 10/6/2010

72300 FGD Effluent Field Blank, Set 1 280

- 8058

- 3 Aqueous 10/5/2010 10/6/2010

72299 FGD Influent Field Blank, Set 1 280

- 8058

- 4 Aqueous 10/5/2010 10/6/2010



### SUMMARY

The samples were prepared for total metals analysis accor ding to TestAmerica’s “FGD

ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Elements

Analysis in Flue Gas Desulfurization Wastewaters,” date d October 6, 2010, based on

EPA Method 200.8, by ICP/MS analysis.

Any significant findings are summarized below. No addition al data qualifiers were

required.

• The post digestion spike (PDS) recoveries for the follo wing analytes failed

TestAmerica’s control limits of 85–115%: arsenic, antimony, and vanadium.

INTERNAL STANDARDIZATION

All internal standards used by TestAmerica were within th e method criteria.

INITIAL CALIBRATION

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

calibration for the ICP-MS analysis consisted of a bla nk and four calibration standards.

INITIAL AND CONTINUING CALIBRATION VERIFICATION (IC V/CCV)

The initial calibration verifications (ICV) and continu ing calibration verifications (CCV)

performed by TestAmerica all had recoveries within the m ethod criteria.

METHOD/INSTRUMENT BLANKS

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

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

required for method blanks.

### 3

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

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

flagged with a “J” qualifier. No additional qualifiers were required for instrument blanks.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

All CRI samples passed TestAmerica’s SOP control limi ts of 50–150% recovery.

LABORATORY CONTROL SAMPLES (LCS)

All LCS samples passed the method QC limits of 85–115% recov ery.

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION

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

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

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

ICS.

All interference check sample B (ICSAB) synthetic sp ikes recovered within

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

SERIAL DILUTION

The serial dilution performed on sample 72149 passed TestAmer ica’s criteria of ±10%

difference.

FIELD DUPLICATES

No field duplicate samples were collected with these sa mpling episodes.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

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

72149 and 72241. All MS/MSD spike recoveries were within the me thod control criteria

of 70-130% for all analytes. The relative percent differenc e (RPD) for all MS/MSDs were

within the FGD ICP/MS SOP ±20% control limits for both samples. No additional data

qualifiers were required.

POST DIGESTION SPIKES (PDS)

The PDS performed on sample 72149 passed TestAmerica’s cont rol limits of 85–115%

recovery for all analytes, except for arsenic, antimo ny, and vanadium, which were

flagged with a “W”. No additional data qualifiers were require d for PDS samples.

### 4

DETECTION LIMITS

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

of reagent water.

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A EAD

Deb Bartram, ERG

TJ Finseth, ERG

From: Randy Mercurio, ERG

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.7 – Long-Term

Monitoring: Month 1 (Part 2)

TestAmerica generated analytical data for total metals (aluminum, boron, barium,

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

titanium and zinc) for these long-term monitoring samples. The samples were analyzed

according to EPA Method 200.7.

Table 1 summarizes the samples TestAmerica extracted a nd analyzed for total metals by

EPA Method 200.7.

Table 1. 

### Long-Term Monitoring Month 1 (Part 2) Total Metals – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

7 199 1 FGD Influent, Set 1 280

- 8121

- 1 Aqueous 10/6 /2010 10/7 /2010

71995 FGD Bioreactor Influent, Set 1 280

- 8194

- 1 Aqueous 10/7 /2010 10/8 /2010

71999 FGD Bioreactor Effluent, Set 1 280

- 8194

- 2 Aqueous 10/7 /2010 10/8 /2010

7 2003 FGD Influent Field Blank 280

- 8121

- 2 Aqueous 10/6 /2010 10/7 /2010

72004 FGD Bioreactor Influent Field

Blank, Set 1 280

- 8194

- 3 Aqueous 10/7 /2010 10/8 /2010

72008 FGD Bioreactor Ef fluent Field

Blank, Set 1 280

- 8194

- 4 Aqueous 10/7 /2010 10/8 /2010

7 214 1 FGD Influent, Set 1 280

- 8061

- 1 Aqueous 10/5 /2010 10/6 /2010

721 4 5 FGD Bioreactor Influent, Set 1 280

- 8061

- 2 Aqueous 10/5 /2010 10/6 /2010

7 214 9 FGD Bioreactor Effluent, Set 1 280

- 8061

- 3 Aqueous 10/5 /2010 10/6 /2010

7 215 3 FGD Influent Field Blank 2 80

- 8061

- 6 Aqueous 10/5 /2010 10/6 /2010

7 215 4 FGD Bioreactor Influent Field

Blank, Set 1 280

- 8061

- 4 Aqueous 10/5 /2010 10/6 /2010

7 215 8 FGD Bioreactor Effluent Field

Blank, Set 1 280

- 8061

- 5 Aqueous 10/5 /2010 10/6 /2010

72241 FGD Influent, Set 1 280

- 8195

- 1 Aqueous 10/7 /2010 10/8 /2010

72245 FGD Ef fluent, Set 1 280

- 8195

- 2 Aqueous 10/7 /2010 10/8 /2010

72249 FGD Bioreactor Influent Field

Blank, Set 1 280

- 8195

- 4 Aqueous 10/7 /2010 10/8 /2010

### 2

Table 1. 

### Long-Term Monitoring Month 1 (Part 2) Total Metals – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

72250 FGD Effluent Field Blank, Set 1 280

- 8195

- 3 Aqueous 10/7 /2010 10/8 /2010

72291 FGD Influent, Set 1 280

- 8058

- 1 Aqueous 10/5 /2010 10/6 /2010

7 2295 FGD Effluent, Set 1 280

- 8058

- 2 Aqueous 10/5 /2010 10/6 /2010

7 2299 FGD Influent Field Blank, Set 1 280

- 8058

- 4 Aqueous 10/5 /2010 10/6 /2010

7 2300 FGD Ef

fluent Field Blank

, Set 1 280

- 8058

- 3 Aqueous 10/5 /2010 10/6 /2010



### SUMMARY

The samples were prepared for total metals analysis acc ording to TestAmerica’s SOP for

ICP Analysis for Trace Metals by Method 200.7. Any signific ant findings are

summarized below. No additional data qualifiers were requir ed.

• The serial dilution for cobalt, iron, molybdenum, sodium , and titanium for sample

72241 failed TestAmerica’s SOP control limit of percent di fferences less than

10%.

• The matrix spike (MS) and matrix spike duplicate (MSD) r ecoveries for barium,

beryllium, cobalt, iron, manganese, molybdenum, sodium, tin, titanium, and zinc

for sample 72149 failed the method spike recovery limits of 70-130%.

• The MS/MSD recoveries for barium and tin for sample 72241 failed the method

spike recovery limits of 70-130%. The MS recovery for co balt for sample 72241

also failed the method spike recovery limits.

• The post digestion spike (PDS) for barium and sodium for sample 72149 failed

TestAmerica’s control limits of 85-115% recovery.

• The PDS for cobalt and tin for sample 72241 failed TestAme rica’s control limits

of 85–115% recovery.

SAMPLE RECEIPT, HANDLING AND STORAGE ISSUES

There were no sample receipt issues in this data package.

INTERNAL STANDARDIZATION

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

ISTD recoveries within the ±30% criterion of the calibra tion blank as per Section 9.11 of

the SOP were seen. All ISTD were within TestAmerica’ s SOP control limits.

### 3

INITIAL CALIBRATION

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

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

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

The initial calibration verifications (ICV) and continu ing calibration verifications (CCV)

performed by TestAmerica all had recoveries within the m ethod criteria.

METHOD/INSTRUMENT BLANKS

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

were above the method detection limit (MDL) and were f lagged with the “J” qualifier.

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

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

flagged with the “J” qualifier.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

All CRI samples passed TestAmerica’s SOP control limi ts of 50–150% recovery.

LABORATORY CONTROL SAMPLES (LCS)

All LCSs passed the method control limits of 85–115% recover y.

INTERFERENCE CHECK SOLUTIONS

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

data quality objectives met TestAmerica’s SOP criteria.

SERIAL DILUTION (SRD)

Serial dilutions were performed for each batch of total samples. All serial dilution percent

differences were less than 10% as required by TestAmeric a’s SOP, except for cobalt,

iron, molybdenum, sodium, and titanium for Sample 72241.

FIELD DUPLICATES

No field duplicate samples were collected with these sa mpling episodes.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

MS and MSDs were performed on the total samples of 72149 and 72241.

### 4

The MS/MSD of sample 72149 failed the method spike recovery limits of 70-130% for

all elements except aluminum. Boron, calcium and magnes ium had high concentrations

and failed the EPA 200.7 Method spike recovery control limits of 70–130% but were

flagged with a “4” qualifier indicating that the concentra tion in the parent sample was

greater than 4 times the spike and could not be reliably calculated. These data were

considered acceptable based on the LCS passing the method con trol limits.

The MS/MSD recoveries of sample 72241 failed the method sp ike recovery limits of 70-

130% for all elements except beryllium, molybdenum, and titanium, as well as the MSD

recovery for cobalt. Aluminum, boron, calcium, iron, magnesium, manganese, sodium

and zinc had high concentrations and failed the EPA 200.7 Metho d spike recovery

control limits of 70–130% but were flagged with a “4” qualifier indicating that the

concentration in the parent sample was greater than 4 times the spike and could not be

reliably calculated. These data were considered acceptable based on the LCS passing the

method control limits.

All RPDs of the MS/MSDs were within ± 20%. No additional data qualifiers were

needed.

POST DIGESTION SPIKE (PDS)

The PDS performed on sample 72149 failed the method criteria of 85–115% for barium

and sodium, which were qualified with a “W”. The PDS perf ormed on sample 72241

failed the method criteria of 85–115% recovery for cobalt a nd tin, which were qualified

with a “W”. No additional data qualifiers were required.

DETECTION LIMITS

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

of reagent water.

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Deb Bartram, ERG

TJ Finseth, ERG

From: Jennifer Colby, ERG

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Classicals Ana lyses – Long-Term

Monitoring: Month 1 (Part 2)

TestAmerica Denver Laboratory generated analytical data f or classical wet chemistry

analyses for these long-term monitoring samples. All s amples were tested for the

following analytes:

• Ammonia by EPA method 350.1,

• Biochemical Oxygen Demand – 5 day (BOD 5 

### ) by SM 5210B,

• Chloride and Sulfate by EPA method 300.0,

• Chemical Oxygen Demand (COD) by EPA method 410.4,

• Cyanide (total) by SM 4500 CN

- 

### E,

• Nitrate/Nitrite by EPA method 353.2

• Phosphorus (total) by EPA method 365.1,

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

• Total Kjeldakl Nitrogen (TKN) by EPA method 351.2, and

• Total Suspended Solids (TSS) by SM 2540D.

Table 1 summarizes the ten samples analyzed by TestAmer ica for the above analytes.

Table 1. Long-Term Monitoring Month 1 (Part 2) Classical Analytes – Sample

Identification

EPA

Sample # Sample

Matrix Sample Description Sampling

Date

72291 Water FGD Influent, Set 1 10/05/10

72295 Water FGD Effluent, Set 1 10/05/10

72141 Water FGD Influent, Set 1 10/05/10

72145 Water FGD Bioreactor Influent, Set 1 10/05/10

72149 Water FGD Bioreactor Effluent, Set 1 10/05/10

71991 Water FGD Influent, Set 1 10/06/10

71995 Water FGD Bioreactor Influent, Set 1 10/07/10

71999 Water FGD Bioreactor Effluent, Set 1 10/07/10

72241 Water FGD Influent, Set 1 10/07/10

### 2

Table 1. Long-Term Monitoring Month 1 (Part 2) Classical Analytes – Sample

Identification

EPA

Sample # Sample

Matrix Sample Description Sampling

Date

72245 Water FGD Effluent, Set 1 10/07/10

SUMMARY

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

unless otherwise noted below. All samples were preserved a ppropriately unless otherwise

specified below.

Field duplicate samples were not collected for these ep isodes. Depending on the method,

a laboratory duplicate was analyzed, instead. The Relati ve Percent Difference (RPD)

between the sample and its duplicate was less than 20% unl ess otherwise noted below.

If applicable, the appropriate number of standards was used to create a calibration curve.

If sample results were above the highest standard used t o create the curve, the sample was

diluted and reanalyzed. All sample results were between the lowest and highest standards

unless noted below. Additionally, unless otherwise noted, a ll calibration blanks and

calibration verification samples met the criteria sp ecified in the method.

If required by the method, the quality control sample (QC S), a secondary source standard

used to verify calibration, was always within the cont rol limits specified by the method.

As described below, the analyte of interest was detecte d 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 spec ified in the method unless specified

below.

If required by the method, a matrix spike (MS) analysis was run on sample 72149 for

each analyte to check for matrix interferences. For so me analytes, TestAmerica spiked

more samples than required. All MS samples analyzed met the criteria specified in the

method unless described below.

DATA NOTES/ISSUES

Ammonia

MS and matrix spike duplicates (MSD) were performed on sa mples 71999 and 72149.

The percent recoveries for the MS and MSD for both of these samples were within the

method criteria; however the MS and MSD results for s ample 71999 were above the

calibration range. Only one set of MS/MSD are required pe r the method; therefore, the

results from sample 72149 meet the requirements. No further action is required.

### 3

BOD 5



### The traffic reports for the following samples did not ind icate the receipt temperature for

the following samples: 72291, 72295, 72141, 71995, 71999, 72241, and 72245. The

sample receipt checklist provided by TestAmerica did note that the receipt temperatures

were appropriate; however, this cannot be verified. 40 CFR 136 Table II requires that all

samples must be stored and shipped at temperatures no greate r than 6°C.

TestAmerica analyzed five dilutions; the dilutions had d issolved oxygen (DO) depletion

greater than 2.0 mg/L for samples 72291, 71999, and 72241. As required in the method,

the final result was calculated by taking the average o f the results for all dilutions with a

DO depletion greater than 2.0 mg/L and a final DO greater t han 1.0 mg/L.

The seed correction factor was lower than 0.6 mg/L, at 0. 531 mg/L for one of the batches.

The samples were flagged with an “s” indicating the see d correction blank (SCB)

recovery was low. This low seed correction factor suggest s that the sample results may be

biased low.

Chloride and Sulfate

MS and MSD were performed on samples 71999 and 72149. All chloride and sulfate MS

and MSD recoveries for these samples met the method c riteria; however, for sample

71999, the MS/MSD results for sulfate exceeded the calibra tion range and for sample

72149, the MS/MSD results for chloride exceeded the calibra tion range. These MS/MSD

results were qualified as estimated values. No further a ction is required.

COD

MS and MSD were performed on samples 71999 and 72149. The percent recoveries for

the MS and MSD for samples 72149 were within the method cont rol criteria. The percent

recoveries for the MS and MSD for sample 71999 were 25% an d 44%, respectively,

which are outside the method control criteria of 90-110% and t herefore, the MS/MSD

results were flagged with “F” qualifiers. The LCS/LCSD results were acceptable for this

sample indicating the analytical system was operating w ithin control.

Cyanide

Because of the nature of the sample matrix, all of th e samples in this sampling episode

used a lower volume, which resulted in elevated RLs being ca lculated and reported by

TestAmerica with the sample results.

MS and MSD were performed on samples 71999 and 72149. The percent recoveries for

the MS and MSD for samples 71999 were both 88%, which is outs ide the method control

criteria of 90-110% and therefore, the MS and MSD results were flagged with an “F”

qualifier. The percent recoveries for the MS and MSD f or sample 72149 were 89% and

### 4

88%, respectively, which are outside the method control c riteria and therefore, the MS

and MSD results were flagged with “F” qualifiers. The LCS /LCSD results were

acceptable for these samples indicating the analytical s ystem was operating within

control. Additionally, there is no method requirement f or the analysis of a MS/MSD and

no corrective action is necessary.

Nitrate/Nitrite

No issues were identified by the data reviewer.

Phosphorus

MS and MSD were performed on samples 71999 and 72149. The percent recoveries for

the MS and MSD for sample 71999 were within the method cont rol criteria. The percent

recoveries for the MS and MSD for sample 72149 were 77% an d 79%, respectively,

which are outside the method control criteria, but did m eet the laboratory control criteria

and therefore, were not flagged by the laboratory. The LCS/LCSD recoveries for this

batch were acceptable and indicate that the analytical s ystem was operating within

control.

TDS

The method blank associated with one of the batches detec ted TDS at a level greater than

the MDL, but less than the RL. All affected samples w ere flagged with a “B” qualifier,

which includes samples 72141, 72145, 72149, 72291, and 72295.

Because of the nature of the sample matrix, some of t he samples in this sampling episode

used a lower volume, which resulted in elevated RLs being c alculated and reported by

TestAmerica with the sample results.

TA reports that constant weight was not achieved after 3 drying cycles for the following

samples: 71991, 72241, and 72245. Review of the general chemistry wo rksheets

indicates that constant weight was achieved for all thr ee samples. No further action was

necessary.

The result for sample 71991 was two orders of magnitude lower than the concentrations

for similar samples in this episode; therefore, TestAm erica reviewed the analyses and

determined that the sample should have been run with a di lution factor of 10 or 20, but

was run with a dilution of one. The laboratory has n o way of confirming how the

analysis was run and the issue was identified after the hold time had expired; therefore,

this result is unreliable and should be excluded from the da ta set.

### 5

TKN

Method blank results associated with one of the batches w ere greater than the MDL, but

less than the RL. The blank results were flagged with a “J” qualifier. All associated

samples were flagged with a “B” qualifier. No additional corrective action is necessary.

TSS

Because of the nature of the sample matrix, some of t he samples in this sampling episode

used a lower volume, which resulted in elevated RLs being c alculated and reported by

TestAmerica with the sample results.

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level

Detected

72291 BOD s SCB recovery low XXX mg/L

71991 TDS EXCLUDE Dilution factor cannot be

confirmed 510 mg/L

### 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: 2/9/2012

Subject: FGS Data Review Narrative for Total Mercury – Long-Term M onitoring:

Month 2 (Part 1)

Frontier Global Sciences (FGS) generated analytical da ta for total mercury. FGS

analyzed the samples according to EPA Method 1631E for merc ury by Cold Vapor

Atomic Fluorescence Spectrometry (CVAFS) analysis.

Table 1 summarizes the 19 samples (excluding laboratory pre p blanks) FGS extracted

and analyzed for total mercury.

Table 1. 

### Long-Term Monitoring Month 2 (Part 1) Mercury – Sample Identification

EPA

Sample # Lab Sample

ID # Sample

Matrix Sample Description Sampling

Date

71992 1011064-01 Aqueous FGD Influent, Set 2 11/3/2010

71996 1011064-06 Aqueous FGD Bioreactor Influent, Set 2 11/3/2010

72000 1011064-11 Aqueous FGD Bioreactor Effluent, Set 2 11/3/2010

72005 1011064-12 Aqueous FGD Bioreactor Influent Field Blank, Set 2 11/ 3/2010

72009 1011064-13 Aqueous FGD Bioreactor Effluent Field Blank, Set 2 11/3 /2010

72042 1011043-01 Aqueous FGD Influent, Set 2 11/3/2010

72046 1011043-02 Aqueous FGD Effluent, Set 2 11/2/2010

72051 1011043-03 Aqueous FGD Effluent Field Blank, Set 2 11/2/2010

72092 1011031-01 Aqueous FGD Influent, Set 2 11/2/2010

72096 1011031-02 Aqueous FGD Effluent, Set 2 11/2/2010

72101 1011031-03 Aqueous FGD Effluent, Field Blank, Set 2 11/1/2010

72142 1011032-01 Aqueous FGD Influent, Set 2 11/1/2010

72146 1011032-02 Aqueous FGD Bioreactor Influent, Set 2 11/1/2010

72150 1011032-03 Aqueous FGD Bioreactor Effluent, Set 2 11/1/2010

72155 1011032-04 Aqueous FGD Bioreactor Influent Field Blank, Set 2 11/ 1/2010

72159 1011032-05 Aqueous FGD Bioreactor Effluent Field Blank, Set 2 11/1 /2010

72242 1011061-01 Aqueous FGD Influent, Set 2 11/4/2010

72246 1011061-06 Aqueous FGD Effluent, Set 2 11/4/2010

72251 1011061-07 Aqueous FGD Effluent Field Blank, Set 2 11/3/2010

### 2

SUMMARY

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

There were no findings from the data review that required a dditional qualifiers in this

dataset. The following summarizes the findings from the data review:

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES

There were no sample receipt issues in this data package.

INITIAL CALIBRATION

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

the CVAFS analysis consisted of a blank and five calibrat ion standards with a correlation

coefficient ≥ 0.995. All method-specified criteria were met.

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

All initial and continuing calibration verifications (I CVs, CCVs) met method-specified

criteria.

BLANKS

All the preparation blanks or laboratory reagent blanks (L RBs) and the continuing

calibration blanks (CCBs) met the method-specified crite ria. Because all of the blank

results were less than the RL, no samples were quali fied based on these preparation blank

results.

DUPLICATES

No field duplicate samples were collected with these sa mpling episodes. Two samples

were analyzed in duplicate at the laboratory, samples 72046 a nd 72246. The relative

percent difference (RPD) for samples 72046 and 72246 were 4.25% an d 0.84%,

respectively. The laboratory’s RPD criteria between an alytical duplicates is 24%.

LABORATORY CONTROL SAMPLES

All laboratory control samples were within FGS’s contr ol limits of 80-120% recovery

and 24% RPD.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

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

71996, 72046, 72150, and 72246. All aqueous MS/MSD recoveries were within th e

### 3

method specifications of 71-125%, except for the MS samples for 72046 and 72150,

which had recoveries of 20.1% and 54.5%, respectively. All RPD s met method-specified

criteria of less than or equal to 24%, except for samples 72046 and 72150, which had

RPDs of 72.2% and 24.5%, respectively. Because the MSDs an d the associated LCSs

were within the method specifications, no data qualificati on is required for these samples.

DETECTION LIMITS

The laboratory MDL in the synthetic matrix was 0.239 ng/ L. Results below this MDL

were reported as not detected (ND).

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

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

Deb Bartram, ERG

TJ Finseth, ERG

From: Randy Mercurio, ERG

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.8 – Long-Term

Monitoring: Month 2 (Part 1)

TestAmerica generated analytical data for total metals (antimony, arsenic, cadmium,

chromium, copper, lead, nickel, selenium, silver, thallium and vanadium) for these longterm monitoring samples. The samples were analyzed according to EPA Method 200.8.

Table 1 summarizes the samples TestAmerica extracted and analyzed for total metals by

EPA Method 200.8.

Table 1. 

### Long-Term Monitoring Month 2 (Part 1) Total Metals – Sample

Identification



### EPA

Sample # 

### EPA Sample

Description 

### Lab Sample

ID # 

### Sample

Matrix 

### Sampling

Date 

### Receipt

Date

71992 FGD Influent, Set 2 280

- 9327

- 1 Aqueous 11/03/2010 11/04/2010

71996 FGD Bioreactor Influent,

Set 2 280

- 9389

- 1 Aqueous 11/04/2010 11/05/2010

72000 FGD Bioreactor Effluent,

Set 2 280

- 9389

- 2 Aqueous 11/04/2010 11/05/2010

72005 FGD Bioreactor Influent

Field Blank, Set 2 280

- 9389

- 3 Aqueous 11/04/2010 11/05/2010

72009 FGD Bioreactor Effluent

Field Blank, Set 2 280

- 9389

- 4 Aqueous 11/04/2010 11/05/2010

72042 FGD Influent, Set 2 280

- 9326

- 1 Aqueous 11/03/2010 11/04/2010

72046 FGD Effluent, Set 2 280

- 9326

- 2 Aqueous 11/03/2010 11/04/2010

72051 FGD Bioreactor Effluent

Field Blank, Set 2 280

- 9326

- 3 Aqueous 11/03/2010 11/04/2010

72092 FGD Influent, Set 2 280

- 9249

- 1 Aqueous 11/02/2010 11/03/2010

72096 FGD Effluent, Set 2 280

- 9249

- 2 Aqueous 11/02/2010 11/03/2010

72101 FGD Effluent Field

Blank, Set 2 280

- 9249

- 3 Aqueous 11/02/2010 11/03/2010

72142 FGD Influent, Set 2 280

- 9202

- 1 Aqueous 11/01/2010 11/02/2010

72146 FGD Bioreactor Influent,

Set 2 280

- 9250

- 1 Aqueous 11/02/2010 11/03/2010

### 2 Table 1. 

### Long-Term Monitoring Month 2 (Part 1) Total Metals – Sample

Identification



### EPA

Sample # 

### EPA Sample

Description 

### Lab Sample

ID # 

### Sample

Matrix 

### Sampling

Date 

### Receipt

Date

72150 FGD Bioreactor Effluent,

Set 2 280

- 9250

- 2 Aqueous 11/02/2010 11/03/2010

72155 FGD Bioreactor Influent

Field Blank, Set 2 280

- 9250

- 3 Aqueous 11/02/2010 11/03/2010

72159 FGD Bioreactor Effluent

Field Blank, Set 2 280

- 9250

- 4 Aqueous 11/02/2010 11/03/2010

72242 FGD Influent, Set 2 280

- 9388

- 1 Aqueous 11/04/2010 11/05/2010

72246 FGD Effluent, Set 2 280

- 9388

- 2 Aqueous 11/04/2010 11/05/2010

72251 FGD Bioreactor Effluent

Field Blank, Set 2 280

- 9388

- 3 Aqueous 11/04/2010 11/05/2010



### SUMMARY

The samples were prepared for total metals analysis according to TestAmerica’s “FGD

ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Elements

Analysis in Flue Gas Desulfurization Wastewaters,” dated October 6, 2010, based on

EPA Method 200.8, by ICP/MS analysis.

Any significant findings are summarized below. No additional data qualifiers were

required.

• The serial dilution for selenium for sample 72096 failed TestAmerica’s criteria of

±10% difference.

• The matrix spike (MS) and matrix spike duplicate (MSD) recoveries for silver for

sample 72096 failed the EPA Method 200.8 control limits of 70–130%.

• The MS and MSD recoveries for selenium and silver for sample 72246 failed the

EPA Method 200.8 control limits of 70–130%.

• The MS/MSD relative percent difference (RPD) for silver for sample 72246 failed

the FGD ICP/MS SOP control limits of ±20%.

• The post digestion spike (PDS) recoveries for silver failed TestAmerica’s control

limits of 85–115%.

INTERNAL STANDARDIZATION

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

INITIAL CALIBRATION

### 3

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

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

INITIAL AND CONTINUING CALIBRATION VERIFICATION (ICV/CCV)

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

performed by TestAmerica all had recoveries within the method criteria.

METHOD/INSTRUMENT BLANKS

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

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

required for method blanks.

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

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

flagged with a “J” qualifier. No additional qualifiers were required for instrument blanks.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

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

LABORATORY CONTROL SAMPLES (LCS)

All LCS samples passed the method QC limits of 85–115% recovery.

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION

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

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

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

ICS.

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

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

The ICSA solution for the method 200.8 analysis exceeded the acceptance limits for

Chromium in analytical batch 280-40682. The lab has confirmed with the vendor that

Chromium is a trace impurity in the ICSA solution. Therefore, corrective action was

deemed unnecessary; the associated data have been flagged “^”.

### 4

SERIAL DILUTION

The serial dilution performed on sample 72096 passed TestAmerica’s criteria of ±10%

difference for all analytes except selenium, which was flagged “V.” No further data

qualifiers were needed for the serial dilution.

FIELD DUPLICATES

No field duplicate samples were collected with these sampling episodes.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

MS and MSD were performed on samples 72096 and 72246. The MS/MSD for sample

72096 failed the method control limits of 70–130% recovery for selenium and silver.

Selenium was flagged for the MS/MSD with a “4” qualifier indicating that the

concentration in the parent sample was greater than 4 times the spike and could not be

reliably calculated. This result was considered acceptable based on the LCS passing the

method control limits. Silver was flagged for the MS/MSD with an “F” qualifier and it is

likely that silver failed due to matrix interference from the high concentration of sulfates,

which can form insoluble silver sulfide and/or silver sulfate. The silver recoveries in the

associated LCS/LCSD were acceptable.

The MS/MSD for sample 72246 failed the method control limits of 70–130% recovery

for selenium and silver, which were flagged with an “F” qualifier. The RPD failed the

FGD ICP/MS SOP control limits of ±20% for silver for sample 72246. No additional data

qualifiers were required for MS/MSD samples.

Otherwise, all MS/MSD spike recoveries were within the method control limits of 70-

130% and the RPD for the MS/MSDs were within the FGD ICP/MS SOP control limits

of ±20 percent. No additional data qualifiers were required.

POST DIGESTION SPIKES (PDS)

The PDS performed on sample 72096 passed TestAmerica’s control limits of 85–115%

recovery for all analytes, except for silver, which was flagged with a “W” qualifier. It is

likely that silver failed due to matrix interference from the high concentration of sulfates,

which can form insoluble silver sulfide and/or silver sulfate. The silver recoveries in the

associated LCS/LCSD were acceptable. No additional data qualifiers were required.

DETECTION LIMITS

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

of reagent water.

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A EAD

Deb Bartram, ERG

TJ Finseth, ERG

From: Randy Mercurio, ERG

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.7 – Long-Term

Monitoring: Month 2 (Part 1)

TestAmerica generated analytical data for total metals (aluminum, boron, barium,

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

titanium and zinc). The samples were analyzed according t o EPA Method 200.7.

Table 1 summarizes the samples TestAmerica extracted a nd analyzed for total metals by

EPA Method 200.7.

Table 1. 

### Long-Term Monitoring Month 2 (Part 1) Total Metals – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

7199 2 FGD Influent, Set 2 280

- 9327

- 1 Aqueous 11/03 /2010 11/04 /2010

71996 FGD Bioreactor Influent, Set 2 280

- 9389

- 1 Aqueous 11/04 /2010 11/05 /2010

72000 FGD Bioreactor Effluent, Set 2 280

- 9389

- 2 Aqueous 11/04 /2010 11/05 /2010

72005 FGD Bioreactor Influent Field

Blank, Set 2 280

- 9389

- 3 Aqueous 11/04 /2010 11/05 /2010

72009 FGD Bioreactor Effluent Field

Blank, Set 2 280

- 9389

- 4 Aqueous 11/04 /2010 11/05 /2010

7 2042 FGD Influent, Set 2 280

- 9326

- 1 Aqueous 11/03 /2010 11/04 /2010

7 2046 FGD Effluent, Set 2 280

- 9326

- 2 Aqueous 11/03 /2010 11/04 /2010

72051 FGD Bioreactor Effluent Field

Blank, Set 2 280

- 9326

- 3 Aqueous 11/03 /2010 11/04 /2010

7 2092 FGD Influent, Set 2 280

- 9249

- 1 Aqueous 11/02 /2010 11/03 /2010

72 101 FGD Ef

fluent Field Blank , Set 2 280

- 9249

- 3 Aqueous 11/02 /2010 11/03 /2010

72142 FGD Influent, Set 2 280

- 9202

- 1 Aqueous 11/01 /2010 11/02 /2010

7 2146 FGD Bioreactor Influent, Set 2 280

- 9250

- 1 Aqueous 11/02 /2010 11/03 /2010

7 2150 FGD Bioreactor Effluent, Set 2 280

- 9250

- 2 Aqueous 11/02 /2010 11/03 /2010

7 2155 FGD Bioreactor In fluent Field

Blank, Set 2 280

- 9250

- 3 Aqueous 11/02 /2010 11/03 /2010

7 2159 FGD Bioreactor Ef fluent Field

Blank, Set 2 2 80

- 9250

- 4 Aqueous 11/02 /2010 11/03 /2010

72242 FGD Influent, Set 2 280

- 9388

- 1 Aqueous 11/04 /2010 11/05 /2010

### 2

Table 1. 

### Long-Term Monitoring Month 2 (Part 1) Total Metals – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

72251 FGD Bioreactor Effluent Field

Blank, Set 2 280

- 9388

- 3 Aqueous 11/04 /2010 11/05 /2010



### SUMMARY

The samples were prepared for total metals analysis acc ording to TestAmerica’s SOP for

ICP Analysis for Trace Metals by Method 200.7. Any signific ant findings are

summarized below. No additional data qualifiers were requir ed for this data set.

• Aluminum, calcium, iron, magnesium, and manganese wer e measured above the

reporting limit (RL) in a method blank; however, the conc entration of these

elements in the samples associated with this method blank were at least 10 times

the blank result or below the RL.

• The matrix spike (MS)/matrix spike duplicate (MSD) rel ative percent difference

(RPD) for boron, calcium, and magnesium for sample 72096 failed TestAmerica’s

± 20% requirement.

• The post digestion spike (PDS) for calcium, manganese, t itanium, and zinc for

sample 72096 failed TestAmerica’s control limits of 85-115% re covery.

SAMPLE RECEIPT, HANDLING AND STORAGE ISSUES

There were no sample receipt issues in this data package.

INTERNAL STANDARDIZATION

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

ISTD recoveries within the ±30% criterion of the calibra tion blank as per Section 9.11 of

the SOP were seen. All ISTD were within TestAmerica’ s SOP control limits.

INITIAL CALIBRATION

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

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

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

The initial calibration verifications (ICV) and continu ing calibration verifications (CCV)

performed by TestAmerica all had recoveries within the m ethod criteria.

### 3

METHOD/INSTRUMENT BLANKS

All the method blanks were less than the RL, except for MB 280-40683/1-A. Aluminum,

calcium, iron, magnesium, and manganese were measured ab ove the RL in this method

blank; however, the concentration of these elements in the samples associated with this

method blank were at least 10 times the blank result or b elow the RL. Therefore, no data

needed qualification regarding the method blank result. In the other method blanks, some

elements were above the method detection limit (MDL), but less than the RL; therefore,

these blanks and were flagged with the “J” qualifier.

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

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

flagged with the “J” qualifier.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

All CRI samples passed TestAmerica’s SOP control limi ts of 50–150% recovery.

LABORATORY CONTROL SAMPLES (LCS)

All LCSs passed the method control limits of 85–115% recover y.

INTERFERENCE CHECK SOLUTIONS

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

data quality objectives met TestAmerica’s SOP criteria.

SERIAL DILUTION (SRD)

All serial dilution percent differences were less tha n 10% as required by TestAmerica’s

SOP.

FIELD DUPLICATES

No field duplicate samples were collected with these sa mpling episodes.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

Matrix spikes (MS) and matrix spike duplicates (MSD) w ere performed on the total

samples of 72096 and 72246. Some elements with high concentrat ions failed the EPA

200.7 Method spike recovery control limits of 70–130% but were f lagged with a “4”

qualifier indicating that the concentration in the paren t sample was greater than 4 times

the spike and could not be reliably calculated. These da ta were considered acceptable

based on the LCS passing the method criteria. Otherwi se, all MS/MSD spike recoveries

were within the method control criteria of 70-130%. The RPD for all MS/MSDs were

### 4

within TestAmerica’s ± 20% requirement, except for boron, calcium, and magnesium for

sample 72096. These elements were flagged with an “F” qualif ier.

POST DIGESTION SPIKE (PDS)

The PDS performed on sample 72096 passed TestAmerica’s contr ol limits of 85-115%

recovery for all analytes except boron, calcium, man ganese, sodium, titanium, and zinc.

Calcium, manganese, titanium, and zinc were qualified wit h a “W;” however, Because

the spike level in the MS/MSD analyses for these ele ments was less than 4 times the

sample concentration, there is no evidence of matrix in terferences. Additionally, these

elements passed TestAmerica’s requirement of percent d ifferences less than 10% for the

serial dilution for sample 72096. Boron and sodium failed t he PDS; however, the percent

recoveries were not calculated by the laboratory becaus e their concentrations were

greater than 4 times the PDS spike level. Boron and sodiu m also passed the serial dilution

for sample 72096 demonstrating no significant matrix interfe rences.

DETECTION LIMITS

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

of reagent water.

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A EAD

Deb Bartram, ERG

TJ Finseth, ERG

From: Ariel Atkinson, ERG

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Classicals Ana lyses – Long Term

Monitoring: Month 2 (Part 1)

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry

analyses for these long-term monitoring samples. All s amples were tested for the

following analytes:

• Ammonia by EPA method 350.1,

• Biochemical Oxygen Demand – 5 day (BOD 5 

### ) by SM 5210B,

• Chloride and Sulfate by EPA method 300.0,

• Chemical Oxygen Demand (COD) by EPA method 410.4,

• Cyanide (total) by SM 4500 CN

- 

### E,

• Nitrate/Nitrite by EPA method 353.2,

• Phosphorus (total) by EPA method 365.1,

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

• Total Kjeldahl Nitrogen (TKN) by EPA method 351.2, and

• Total Suspended Solids (TSS) by SM 2540D.

Table 1 summarizes the 12 samples that TestAmerica anal yzed for the above analytes.

Table 1. Long-Term Monitoring Month 2 (Part 1) Classical Analytes – Sample

Identification

EPA

Sample # Sample

Matrix Sample Description Sampling

Date

71992 Water FGD Influent, Set 2 11/3/10

71996 Water FGD Bioreactor Influent, Set 2 11/3/10(CN)

11/4/10(All other

analytes)

72000 Water FGD Bioreactor Effluent, Set 2 11/3/10(CN)

11/4/10(All other

analytes)

72042 Water FGD Influent, Set 2 11/3/2010

72046 Water FGD Effluent, Set 2 11/3/2010

### 2

Table 1. Long-Term Monitoring Month 2 (Part 1) Classical Analytes – Sample

Identification

EPA

Sample # Sample

Matrix Sample Description Sampling

Date

72092 Water FGD Influent, Set 2 11/2/2010

72096 Water FGD Effluent, Set 2 11/2/2010

72142 Water FGD Influent, Set 2 11/1/2010

72146 Water FGD Bioreactor Influent, Set 2 11/2/2010

72150 Water FGD Bioreactor Effluent, Set 2 11/1/10(CN)

11/2/10(All other

analytes)

72242 Water FGD Influent, Set 2 11/4/10

72246 Water FGD Effluent, Set 2 11/4/10

SUMMARY

All samples were analyzed within the holding time specif ied in 40 CFR 136 Table II. All

samples were preserved appropriately unless otherwise speci fied below.

Field duplicate samples were not collected for these ep isodes. Depending on the method,

a laboratory duplicate was analyzed, instead. The Relati ve Percent Difference (RPD)

between the sample and its duplicate was less than 20% unl ess otherwise noted below.

If applicable, the appropriate number of standards was used to create a calibration curve.

If sample results were above the highest standard used t o create the curve, the sample was

diluted and reanalyzed unless otherwise specified below. Al l sample results were between

the lowest and highest standards unless noted below. Additi onally, unless otherwise

noted, all calibration blanks and calibration verificat ion samples met the criteria specified

in the method.

If required by the method, the quality control sample (QC S), a secondary source standard

used to verify calibration, was always within the cont rol limits specified by the method

unless otherwise noted below.

As described below, the analyte of interest was detecte d 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 spec ified in the method unless specified

below.

If required by the method, a matrix spike (MS) sample wa s analyzed on samples 72042,

72096, and/or 72246 for each analyte to check for matrix interf erences. For some

analytes, TestAmerica spiked more samples than require d. MS samples analyzed met the

criteria specified in the method unless described below.

### 3

DATA NOTES/ISSUES

Ammonia

The MS result failed criteria at 111% recovery and was qualified with an “F” flag. The

MSD and LCS recoveries demonstrate that the analysis was under control. No additional

qualifiers were required.

BOD 5



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

depletion greater than 2.0 mg/L for samples 72092, 72146, 72150 72042, 72046, 71992,

71996, and 72246. Therefore, BOD 5 

### was reported as not detected for these samples. 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 calculat ed by taking the average of the

results for all dilutions with a DO depletion greater t han 2.0 mg/L and a final DO greater

than 1.0 mg/L.

One of the three batches had a seed correction factor lower than 0.6 mg/L. The seed

correction factors were 0.632 mg/L, 0.5533 mg/L, and 0.6267 mg/L for batches 38776,

39101, and 39326 respectively. The samples in batch 39101 should be flagg ed with an

“s” indicating the seed correction blank (SCB) recovery was low. This low seed

correction factor suggests that samples 72042, 72046, and 71992 may be biased low;

however all these samples had a result of ND and ther efore do not require qualification.

All glucose-glutamic acid standards and laboratory duplicat es were analyzed

appropriately and met the criteria specified in SM 5210B.

Chloride and Sulfate

The MS/MSD results of samples 72246 for sulfate and chlori de were above the

calibration curve. TestAmerica did not reanalyze the s amples with a higher dilution factor

because the percent recoveries were within EPA method 300. 0 control limits. If reported,

these MS/MSD results will be qualified as estimated val ues. The LFB associated with

this sample met the method criteria. The analyzed resu lt for sample 72246 was within the

calibration curve, so there was no need to qualify this s ample.

COD

Several LRB and Calibration Blanks (CB) had results gr eater than the MDL; however, all

the LRB and CB results less than the RL and were flagge d with a “J” qualifier. No further

qualifications are necessary.

One LFB, LCSD from batch 41304, had a percent recovery grea ter that the 90-110%

criteria. The LFB was flagged with a “*” qualifier indic ating the LCS or LCSD exceeds

### 4

the control limits. The sample 72046, which is associated with this LFB, was also flagged

with “*” qualifier.

The percent recovery for the MS/MSD analyses for sam ples 72096 and 72246 were

above the control limits of 90-110% required by EPA method 410.4. The percent

recoveries for the MS and MSD analyses for sample 72096 were 115% and 118%,

respectively and the recoveries for sample 72246 were 131% and 132%, respectively.

These results were flagged with an “F” qualifier because t hey exceed control limits. The

LFB percent recoveries associated with samples 72096 and 72246 m et the method

criteria.

MS/MSDs were not performed in batches 41739 and 41304. The sampl es associated with

these batches include 72042 and 72046. These sample results were qualified with an “F”

qualifier because there were no MS/MSD results.

Cyanide

The calibration was performed using standards ranging from 0.00 ppb to 400.0 ppb. The

method states that the appropriate calibration range of s tandard concentrations for this

method are between 5 ppb and 20 ppb. Samples 72142, 72092, 72096, 72046, 72242, a ll

had results ≥ 20 ug/L; but were not diluted because they were within the ca libration range

performed by the laboratory.

The MS/MSD results for sample 72246 passed the recovery cr iteria; however, the

MS/MSD results for sample 72096 failed recovery criteria. The MS/MSD results for

72096 were qualified with an “F” flag. The associated LCS/LC SD recoveries were

within control limits.

Nitrate/Nitrite

The RPD between the LFB and a duplicate LFB from batch 280-40320 is 10.7%. This

does not meet the control limits, and therefore the LF B, LFB duplicate, and associated

samples are flagged with a “*” qualifier meaning RPD of the LCS and LCSD exceeds the

control limit. The RPD for the MS/MSD in this batch was 1 percent; therefore the system

appears to be in control. No further qualifiers were nee ded.

The MS/MSD results for samples 72042, 72096, and 72246 were above t he calibration

curve. TestAmerica did not reanalyze these MS/MSDs with a higher dilution factor, but

the MS/MSD results for samples 72246 and 72042 were flagged with an “E” qualifier

because the results exceeded calibration range. The MS/MSD results for sample 72096

were not flagged with “E” qualifier because the percent re coveries for the MS/MSD

analysis of sample 72096 were not within the method control limits of 90-110 percent;

therefore, these MS/MSD results were flagged with an “ F” qualifier. The percent

recoveries for the MS/MSD of 72096 were 118% and 121%, respectiv ely. Additionally,

the MS of sample 72042, and the MSD of sample 72246 were not wi thin the method

control limits of 90-110%. The percent recovery of the MS D for sample 72246 was 89%

### 5

and the percent recovery of the MS of sample 72042 was 88 pe rcent; however neither

MS/MSDs were flagged with an “F’ qualifier because they d id meet the laboratory

control limits. If reported, the 72042 MS should be flagged w ith an “F” qualifier, the

72096 MS/MSD should be qualified as estimated, and the 72246 MS sho uld be flagged

with an “F” qualifier.

Phosphorus

The LRB was greater than the MDL at 0.0141 mg/L, however th e result was less than the

RL. The LRB results were flagged with a “J” qualifier b ecause the result was less than

the RL but greater than the MDL. No further qualifiers are needed. All samples that

contained the analyte were also flagged with a “B” qualif ier because the compound was

found in the blank and the sample. All calibration blank r esults were also above the MDL

but less than the RL, and therefore are also flagged wi th a “J” qualifier.

The percent recoveries for the MS/MSD analysis of sa mples 72096 and 72246 were not

within the control limits of 90-110% specified in EPA Method 365. 1. However the

MS/MSD of sample 72096 were within the laboratory control limits of 71-128%. The

percent recoveries of the MS and MSD for sample 72096 were 87% and 84%,

respectively, and the MS and MSD recoveries for sample 72246 were 26% and 31%,

respectively. Because the MS/MSD of sample 72096 met labo ratory control limits it was

not flagged by the laboratory, but if the MS/MSD results for sample 72096 are reported,

they should be flagged with an “F” qualifier.

Samples 72146, 72150, 72046, 72242, 71996, 72000, and the LRB had results that were

lower than the lowest calibration standard. Each of th ese results was flagged with a “J”

qualifier because each result was less than the RL but greater than or equal to the MDL,

and therefore the concentrations are approximate values. N o further qualifiers are needed.

TDS

Constant weight was not achieved after 3 drying cycles fo r all samples. It should be noted

that the weight increased from the first weighing to th e second weighing for all samples

except 72042, 72046, 71992, 72242, 72246, 71996, and 72000. Method 2540C warns that

samples which contain high levels of calcium, magnesiu m, chloride, and sulfate may be

hygroscopic meaning they absorb moisture from the air. FGD wastewater contains high

concentrations of all of these species. This was likely the cause for the inconsistent

weight calculations. Samples 72142, 72092, 72096, 72146, and 72150 were not qua lified,

but results may be biased high.

The RPD for the laboratory duplicate from sample 72096 was 12%, which is not less than

10% as required by SM 2540C. The laboratory control limits a re 20%; therefore, the

laboratory did not qualify the sample. The sample resu lt will be qualified as an estimated

value as shown in Table 2. Laboratory duplicates were n ot performed in the other

batches.

### 6

TKN

TestAmerica performed MS/MSD analysis on samples 72096 and 72246. The percent

recoveries for the MS and MSD for sample 72096 were 161% an d 147%, respectively,

and 145% and 149% for the MS and MSD for sample 72246. These samp les did not meet

the method control limits of 90-110%, nor the laboratory co ntrol 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 recove ries and RPDs could not be

reliably calculated. The associated LCS/LCSD were also acceptable, therefore, no

additional data qualifiers are required.

TKN was detected in the calibration blanks. The results were greater than the MDL

(0.077 mg/L), but less than the RL (1.0 mg/L). Because the re sults were less than the RL,

no samples were qualified, but the CBs were flagged with a “J” qualifier.

TSS

The RPDs for the laboratory duplicates performed on sam ples 72142, 72096, 72046, and

72246 were greater than the method control criteria of 10%, at 11%, 18%, 22%, and 18%,

respectively. The laboratory control criterion is 20 perc ent; therefore, samples 72142,

72096, and 72246 were not qualified by the laboratory. Sample 72046 and its duplicate

were already qualified by TestAmerica with a “J” meaning t hat the result is an estimated

value because the result is below the RL, so no further qualification was necessary for

this sample. Because the RPD was greater than the meth od control limits, sample 72142,

72096, and 72246 were qualified as estimated values.

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Ac

tion Reason Level Detected

72042 COD F MS/MSD not

performed in batch X XX mg/L



### 72046 COD F MS/MSD not

performed in batch X XX mg/L



### 72096 TDS Estimated

Value Lab duplicate RPD >

method-specified

criteria Sample: X XX

mg/L

Dup: XXX

mg/L,12%RPD



### 72142 TSS Estimated

Value Lab duplicate RPD >

method-specified

criteria Sample: X XX

mg/L Dup: XXX

mg/L; 11%RPD



### 72096 TSS Estimated

Value Lab duplicate RPD >

method-specified

criteria Sample: X XX

mg/L

Dup: XXX

mg/L; 18% RPD

### 7 Table 2. Data Review Summary Table

Sample Analyte Qualifier/Ac

tion Reason Level Detected

72246 TSS Estimated

Value Lab duplicate RPD >

method-specified

criteria Sample: X XX

mg/L

Dup: XXX

mg/L; 18% 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: Donna Tedder, ERG

Date: 2/9/2012

Subject: FGS Data Review Narrative for Total Mercury – Long-Term M onitoring:

Month 3

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

analyzed the samples according to EPA Method 1631E for merc ury by Cold Vapor

Atomic Fluorescence Spectrometry (CVAFS) analysis.

Table 1 summarizes the 24 samples (excluding laboratory pre p blanks) FGS extracted

and analyzed for total mercury.

Table 1. 

### Long-Term Monitoring Month 3 Mercury – Sample Identification

EPA

Sample # Lab Sample

ID # Sample

Matrix Sample Description Sampling

Date

71993 1012119-01 Aqueous FGD Influent, Set 3 12/8/2010

71997 1012119-06 Aqueous FGD Bioreactor Influent, Set 3 12/8/2010

72001 1012119-11 Aqueous FGD Bioreactor Effluent, Set 3 12/8/2010

72006 1012119-12 Aqueous FGD Bioreactor Influent Field Blank, Set 3 12/ 8/2010

72010 1012119-13 Aqueous FGD Bioreactor Effluent Field Blank, Set 3 12/8 /2010

72043 1012094-01 Aqueous FGD Influent, Set 3 12/8/2010

72047 1012094-02 Aqueous FGD Effluent, Set 3 12/7/2010

72052 1012094-03 Aqueous FGD Effluent Field Blank, Set 3 12/7/2010

72093 1012077-01 Aqueous FGD Influent Set 3 12/7/2010

72097 1012077-02 Aqueous FGD Effluent, Set 3 12/7/2010

72102 1012077-03 Aqueous FGD Effluent Field Blank, Set 3 12/7/2010

72143 1012080-01 Aqueous FGD Influent, Set 3 12/6/2010

72147 1012080-06 Aqueous FGD Bioreactor Influent, Set 3 12/6/2010

72151 1012080-11 Aqueous FGD Bioreactor Effluent, Set 3 12/6/2010

72156 1012080-12 Aqueous FGD Bioreactor Influent Field Blank, Set 3 12/ 6/2010

72160 1012080-13 Aqueous FGD Bioreactor Effluent Field Blank, Set 3 12/6/2010

72192 1012105-01 Aqueous FGD Influent, Set 1 12/8/2010

72196 1012105-02 Aqueous FGD SBR Influent, Set 1 12/8/2010

72200 1012105-03 Aqueous FGD SBR Effluent, Set 1 12/8/2010

### 2 Table 1. 

### Long-Term Monitoring Month 3 Mercury – Sample Identification

EPA

Sample # Lab Sample

ID # Sample

Matrix Sample Description Sampling

Date

72205 1012105-04 Aqueous FGD SBR Influent Field Blank, Set 1 12/8/2010

72209 1012105-05 Aqueous FGD SBR Effluent Field Blank, Set 1 12/8/2010

72243 1012117-01 Aqueous FGD Influent, Set 3 12/9/2010

72247 1012117-06 Aqueous FGD Effluent, Set 3 12/9/2010

72252 1012117-07 Aqueous FGD Effluent Field Blank, Set 3 12/8/2010



### SUMMARY

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

There were no findings from the data review that required a dditional qualifiers in this

dataset.

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES

There were no sample receipt issues in this data package.

INITIAL CALIBRATION

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

the CVAFS analysis consisted of a blank and five calibrat ion standards with a correlation

coefficient ≥ 0.995. All method-specified criteria were met.

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

All initial and continuing calibration verifications (I CVs, CCVs) met method-specified

criteria.

BLANKS

All the preparation blanks or laboratory reagent blanks (L RBs) and the continuing

calibration blanks (CCBs) met method-specified criteria. Some preparation blanks had

mercury levels greater than the MDL (0.24 ng/L), but less t han the RL associated with

each individual blank (different RLs based on preparation) . Because all of the blank

results were less than the RL, no samples were quali fied based on these preparation blank

results.

DUPLICATES

No field duplicate samples were collected with these sa mpling episodes. Three samples

were analyzed in duplicate at the laboratory, Bioreacto r Influent sample 72147, SBR

Influent sample 72196, and Effluent sample 72247. The relative pe rcent difference (RPD)

### 3

for samples 72147, 72196, and 72247 were 9.74%, 4.36%, and 9.10%, respectiv ely. A

sample from another work order was analyzed in duplica te with these batches that

resulted in an RPD of 79.7%, which is outside of the laborat ory’s criteria. The

laboratory’s RPD criteria between analytical duplicates is 24%. No sample qualifications

were needed based on these analytical duplicate results.

LABORATORY CONTROL SAMPLES

All laboratory control samples were within FGS’s contr ol limits of 80-120% recovery

and 24% RPD.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

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

72097, 72147, and 72196. Additionally, an MS/MSD was performed on samp le 72296,

which was a rerun from the long-term monitoring, month 2 set of samples. All aqueous

MS/MSD recoveries were within method specifications of 71-125%. All RPDs met

method-specified criteria.

DETECTION LIMITS

The laboratory MDL in the synthetic matrix was 0.239 ng/ L. Results below this MDL

were reported as not detected (ND).

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A EAD

Deb Bartram, ERG

TJ Finseth, ERG

From: Randy Mercurio, ERG

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.8 – Long-Term

Monitoring: Month 3

TestAmerica generated analytical data for total metals (antimony, arsenic, cadmium,

chromium, copper, lead, nickel, selenium, silver, thalliumand vanadium) for these longterm monitoring samples. The samples were analyzed accor ding to EPA Method 200.8.

Table 1 summarizes the samples TestAmerica extracted a nd analyzed for total metals by

EPA method 200.8.

Table 1. 

### Long-Term Monitoring Month 3 Total Metals – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

71993 FGD Influent, Set 3 280

- 10586

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

71997 FGD Bioreactor Influent, Set 3 280

- 10586

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

71997 FGD Bioreactor Influent, Set 3 280

- 10654

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

72001 FGD Bioreactor Effluent, Set 3 280

- 10654

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

72006 FGD Bioreactor Influent Field

Blank, Set 3 280

- 10654

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

72010 FGD Bioreactor Effluent Field

Blank, Set 3 280

- 10654

- 4 Aqueous 12/09/2010 12/10/2010

72043 FGD Influent, Set 3 280

- 10584

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

72047 FGD Effluent, Set 3 280

- 10584

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

72052 FGD Bioreactor Effluent Field

Blank, Set 3 280

- 10584

- 3 Aqueous 12/08/2010 12/09/2010

72093 FGD Influent, Set 3 280

- 10515

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

72097 FGD Effluent, Set 3 280

- 10515

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

72102 FGD Effluent Field Blank, Set 3 280

- 10515

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

72143 FGD Influent, Set 3 280

- 10455

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

72147 FGD Bioreactor Influent, Set 3 280

- 10517

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

72151 FGD Bioreactor Effluent, Set 3 280

- 10517

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

72156 FGD Bioreactor Influent Field

Blank, Set 3 280

- 10517

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

72160 FGD Bioreactor Effluent Field 280

- 10517

- 4 Aqueous 12/07/2010 12/08/2010

### 2

Table 1. 

### Long-Term Monitoring Month 3 Total Metals – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

Blank, Set 3

72192 FGD Influent, Set 1 280

- 10585

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

72196 FGD SBR Influent, Set 1 280

- 10585

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

72200 FGD SBR Effluent, Set 1 280

- 10585

- 3 Aqueous 12/08/2010 12/09/2010

72205 FGD SBR Influent Field Blank,

Set 1 280

- 10585

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

72209 FGD SBR Effluent Field Blank,

Set 1 280

- 10585

- 5 Aqueous 12/08/2010 12/09/2010

72243 FGD Influent, Set 3 280

- 10655

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

72247 FGD Effluent, Set 3 280

- 10655

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

72252 FGD Effluent Field Blank, Set 3 280

- 10655

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



### SUMMARY

The samples were prepared for total metals analysis accor ding to TestAmerica’s “FGD

ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Elements

Analysis in Flue Gas Desulfurization Wastewaters,” date d October 6, 2010, based on

EPA Method 200.8, by ICP/MS analysis.

Any significant findings are summarized below. No addition al data qualifiers were

required.

• One of the continuing calibration verifications (CCV) per formed on 12/21/2010

failed the method criteria for selenium.

• The matrix spike (MS) and matrix spike duplicate (MSD) rec overies for total

silver for sample 72196 failed the EPA Method 200.8 control lim its of 70-130%.

The MSD recovery for total silver for sample 72147 also fa iled the method

control limits.

• The MS/MSD relative percent difference (RPD) for tota l silver for samples 72147

and 72196 failed the FGD ICP/MS SOP control limits of ±20%.

• The post digestion spike (PDS) recoveries for copper, nic kel, and silver for

sample 72147 failed TestAmerica’s control limits of 85–115%. The PDS

recovery for silver for sample 71997 also failed TestAmeri ca’s control limits.

INTERNAL STANDARDIZATION

All internal standards used by TestAmerica were within th e method criteria.

### 3

INITIAL CALIBRATION

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

calibration for the ICP-MS analysis consisted of a bla nk and four calibration standards.

INITIAL AND CONTINUING CALIBRATION VERIFICATION (IC V/CCV)

The initial calibration verifications (ICV) and CCV perf ormed by TestAmerica all had

recoveries within the method criteria, except for seleniu m for one CCV on 12/21/2010.

Samples associated with this CCV that had selenium value s less than the reporting limit

were reported. Any samples with selenium values above the reporting limit were

reanalyzed.

METHOD/INSTRUMENT BLANKS

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

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

required for method blanks.

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

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

flagged with a “J” qualifier. No additional qualifiers were required for instrument blanks.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

All CRI samples passed TestAmerica’s SOP control limi ts of 50–150% recovery.

LABORATORY CONTROL SAMPLES (LCS)

All LCS samples passed the method QC limits of 85–115% recov ery.

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION

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

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

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

ICS.

All interference check sample B (ICSAB) synthetic sp ikes recovered within

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

SERIAL DILUTION

The serial dilution performed on samples 72147 and 72196 passed Te stAmerica’s criteria

of ±10% difference.

### 4

FIELD DUPLICATES

No field duplicate samples were collected with these sa mpling episodes.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

MS and MSD were performed on samples of 72147, 72196, and 71997. The M SD of

sample 72147 failed the method control limits of 70–130% recover y for silver at 69%,

which was flagged with an “F” qualifier. The MS/MSD of sam ple 72196 failed the

method control limits of 70–130% recovery for silver, which was flagged with an “F”

qualifier. These silver failures are likely due to matrix interference from the high

concentration of sulfates, which can form insoluble si lver sulfide and/or silver sulfate.

The silver recoveries in the associated LCS/LCSDs were acceptable. The RPD for the

MS/MSDs for samples 72147 and 72196 failed the FGD ICP/MS SOP ± 20% control

limits for silver.

Otherwise, all MS/MSD spike recoveries were within th e method control limits of 70-

130% and the RPD for the MS/MSDs were within the FGD ICP /MS SOP control limits

of ±20 percent. No additional data qualifiers were required.

POST DIGESTION SPIKES (PDS)

The PDS performed on samples 72147 and 71997 passed TestAmerica’s control limits of

85–115% recovery for all analytes, except for copper, nickel, and silver for PDS sample

72147 and silver for PDS sample 71997, which were flagged with a “W ” qualifier. No

additional data qualifiers were required.

DETECTION LIMITS

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

of reagent water.

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A EAD

Deb Bartram, ERG

TJ Finseth, ERG

From: Randy Mercurio, ERG

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.7 – Long-Term

Monitoring: Month 3

TestAmerica generated analytical data for total metals (aluminum, boron, barium,

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

titanium and zinc). The samples were analyzed according t o EPA Method 200.7.

Table 1 summarizes the samples TestAmerica extracted a nd analyzed for total metals by

EPA Method 200.7

Table 1. 

### Long-Term Monitoring Month 3 Total Metals – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

71993 FGD Influent , Set 3 280

- 10586

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

71997 FGD Bioreactor Influent , Set 3 280

- 10654

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

72001 FGD Bioreactor Effluent , Set 3 280

- 10654

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

72006 FGD Bioreactor Influent Field

Blank, Set 3 280

- 10654

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

72010 FGD Bioreactor Effluent Field

Blank, Set 3 280

- 10654

- 4 Aqueous 12/09 /2010 12/10 /2010

7 2043 FGD Influent, Set 3 280

- 10584

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

7 2047 FGD Effluent, Set 3 280

- 10584

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

72052 FGD Bioreactor Effluent Field

Blank, Set 3 280

- 10584

- 3 Aqueous 12/08 /2010 12/09 /2010

7 2093 FGD Influent, Set 3 280

- 10515

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

7 2097 FGD Ef fluent, Set 3 280

- 10515

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

72 102 FGD Ef

fluent Field Blank , Set 3 280

- 10515

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

72143 FGD Influent, Set 3 280

- 10455

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

7 2147 FGD Bioreactor Influent, Set 3 280

- 10517

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

7 2151 FGD Bioreactor Effluent, Set 3 280

- 10517

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

7 2156 FGD Bioreactor In fluent Field

Blank, Set 3 280

- 10517

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

7 2160 FGD Bioreactor Ef fluent Field

Blank, Set 3 2 80

- 10517

- 4 Aqueous 12/07 /2010 12/08 /2010

7 2192 FGD Influent, Set 1 280

- 10585

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

### 2 Table 1. 

### Long-Term Monitoring Month 3 Total Metals – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

72196 FGD SBR Influent, Set 1 280

- 10585

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

72200 FGD SBR Effluent, Set 1 280

- 10585

- 3 Aqueous 12/08 /2010 12/09 /2010

72205 FGD SBR Influent Field Blank

, Set 1 280

- 10585

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

72209 FGD SBR Effluent Field Blank

, Set 1 280

- 10585

- 5 Aqueous 12/08 /2010 12/09 /2010

72243 FGD Influent, Set 3 280

- 10655

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

72247 FGD Effluent, Set 3 280

- 10655

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

72252 FGD Effluent Field Blank, Set 3 280

- 10655

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



### SUMMARY

The samples were prepared for total metals analysis acc ording to TestAmerica’s SOP for

ICP Analysis for Trace Metals by Method 200.7. Any signific ant findings are

summarized below. Additional data qualifiers were require d (see Table 2).

• The serial dilution for cobalt, iron, and zinc for sa mple 72143 failed

TestAmerica’s SOP control limit of percent differenc es less than 10%.

• The post digestion spike (PDS) for calcium, iron, magn esium, and zinc for sample

72143 failed TestAmerica’s control limits of 85–115% recovery.

• The PDS for manganese for sample 72147 failed TestAmerica ’s control limits of

85–115% recovery.

SAMPLE RECEIPT, HANDLING AND STORAGE ISSUES

The samples associated with Episode 6569 (72192, 72196, 72200, 72205, and 72209) did

not have a sample date or time on the traffic report.

INTERNAL STANDARDIZATION

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

ISTD recoveries within the ±30% criterion of the calibra tion blank as per Section 9.11 of

the SOP were seen. All ISTD were within the control limits.

INITIAL CALIBRATION

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

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

### 3

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

The initial calibration verifications (ICV) and continu ing calibration verifications (CCV)

performed by TestAmerica all had recoveries within the m ethod criteria.

METHOD/INSTRUMENT BLANKS

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

were above the method detection limit (MDL) and were f lagged with the “J” qualifier.

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

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

flagged with the “J” qualifier.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

All CRI samples passed TestAmerica’s SOP control limi ts of 50–150% recovery.

LABORATORY CONTROL SAMPLES (LCS)

All LCSs passed the method control limits of 85–115% recover y.

INTERFERENCE CHECK SOLUTIONS

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

data quality objectives met TestAmerica’s SOP criteria.

SERIAL DILUTION (SRD)

Serial dilutions were performed for each batch of total samples. All serial dilution percent

differences were less than 10% as required by TestAmeric a’s SOP, except for cobalt,

iron, and zinc for sample 72143, which were flagged with a “ V” qualifier.

FIELD DUPLICATES

No field duplicate samples were collected with these sa mpling episodes.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

Matrix spikes (MS) and matrix spike duplicates (MSD) w ere performed on the total

samples of 72143, 72147, and 72196. Some elements with high concent rations failed the

EPA 200.7 Method spike recovery control limits of 70–130% but w ere flagged with a “4”

qualifier indicating that the concentration in the paren t sample was greater than 4 times

the spike and could not be reliably calculated. These data were considered acceptable

based on the LCS passing the method control limits. Othe rwise, all MS/MSD spike

recoveries were within the method control criteria of 70-130%. The RPD for all

### 4

MS/MSDs were within TestAmerica’s ± 20% requirement. No additional data qualifiers

were needed.

POST DIGESTION SPIKE (PDS)

The PDS performed on sample 72143 passed TestAmerica’s cont rol limits of 85–115%

recovery for all analytes except aluminum, boron, calc ium, iron, magnesium, titanium,

and zinc. Calcium, magnesium, and zinc were qualified with a “W”. Calcium and

magnesium did pass in the matrix spike for this sample. Aluminum, boron, iron and

titanium failed the PDS; however, the percent recoveri es were not calculated by the

laboratory because their concentrations were greater than 4 times the PDS spike level.

Aluminum, boron, and titanium passed TestAmerica’s requir ement of percent differences

less than 10% for the serial dilution for this sample demo nstrating that there were no

significant matrix interference with these elements. Iron and zinc failed TestAmerica’s

requirements for the serial dilution; therefore, based on these cumulative results, iron and

zinc are being qualified as suspect due to matrix interfere nce. These additional qualifiers

appear in Table 2.

The PDS performed on sample 72147 passed TestAmerica’s cont rol limits of 85–115%

recovery for all analytes except boron and manganese. Manganese was qualified with a

“W”. Boron failed the PDS; however, the percent recov ery was not calculated by the

laboratory because its concentration was greater the 4 times the PDS spike level. Both

boron and manganese passed TestAmerica’s requirement of percent differences less than

10% for the serial dilution for sample 72147 demonstrating th at there were no significant

matrix interferences. No additional qualifier is requir ed due to this PDS.

The PDS performed on sample 72196 passed TestAmerica’s cont rol limits of 85–115%

recovery for all analytes except boron and manganese; however, the percent recoveries

were not calculated by the laboratory because their co ncentrations were greater than 4

times the PDS spike level. Both boron and manganese passed TestAmerica’s requirement

of percent differences less than 10% for the serial dil ution for sample 72196

demonstrating that there were no significant matrix int erferences. No additional qualifier

is required due to this PDS.

DETECTION LIMITS

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

of reagent water.

Table 2. Data Review Summary

Sample Analyte Qualifier/Action Reason Level Detected

72143 Iron (total) Matrix

Interference PDS and SD Failed XXX μ g/L

72143 Zinc (total) Matrix

Interference PDS and SD Failed XXX ug/L

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Deb Bartram, ERG

TJ Finseth, ERG

From: Jennifer Colby, ERG

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Classicals Ana lyses – Long-Term

Monitoring: Month 3

TestAmerica Denver Laboratory generated analytical data f or classical wet chemistry

analyses for these long-term monitoring samples. All s amples were tested for the

following analytes:

• Ammonia by EPA method 350.1,

• Biochemical Oxygen Demand – 5 day (BOD 5 

### ) by SM 5210B,

• Chloride and Sulfate by EPA method 300.0,

• Chemical Oxygen Demand (COD) by EPA method 410.4,

• Cyanide (total) by SM 4500 CN

- 

### E,

• Nitrate/Nitrite by EPA method 353.2

• Phosphorus (total) by EPA method 365.1,

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

• Total Kjeldakl Nitrogen (TKN) by EPA method 351.2, and

• Total Suspended Solids (TSS) by SM 2540D.

Table 1 summarizes the 15 samples that TestAmerica anal yzed for the above analytes.

Table 1. Long-Term Monitoring Month 3 Classical Analytes – Sample

Identification

EPA

Sample # Sample

Matrix Sample Description Sampling

Date

71993 Water FGD Influent, Set 3 12/08/2010

71997 Water FGD Bioreactor Influent, Set 3 12/09/2010

72001 Water FGD Bioreactor Effluent, Set 3 12/09/2010

72043 Water FGD Influent, Set 3 12/08/2010

72047 Water FGD Effluent, Set 3 12/08/2010

72093 Water FGD Influent, Set 3 12/07/2010

72097 Water FGD Effluent, Set 3 12/07/2010

72143 Water FGD Influent, Set 3 12/06/2010

72147 Water FGD Bioreactor Influent, Set 3 12/07/2010

### 2 Table 1. Long-Term Monitoring Month 3 Classical Analytes – Sample

Identification

EPA

Sample # Sample

Matrix Sample Description Sampling

Date

72151 Water FGD Bioreactor Effluent, Set 3 12/07/2010

72192 Water FGD Influent, Set 1 12/08/2010

72196 Water FGD SBR Influent, Set 1 12/08/2010

72200 Water FGD SBR Effluent, Set 1 12/08/2010

72243 Water FGD Influent, Set 3 12/09/2010

72247 Water FGD Effluent, Set 3 12/09/2010

SUMMARY

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

unless otherwise noted below. All samples were preserve d appropriately unless

otherwise specified below. Samples 72192, 72196, and 72200 had no colle ction dates or

times listed on the traffic report, and were given the date of relinquishment. Many of the

traffic reports did not have receipt temperatures.

Field duplicate samples were not collected for this epis ode. Depending on the method, a

laboratory duplicate was analyzed instead. The Relative Percent Difference (RPD)

between the sample and its duplicate was less than 20% unl ess otherwise noted below.

If applicable, the appropriate number of standards was used to create a calibration curve.

If sample results were above the highest standard used t o create the curve, the sample was

diluted and reanalyzed. All sample results were between the lowest and highest standards

unless noted below. Additionally, unless otherwise noted, a ll calibration blanks and

calibration verification samples met the criteria sp ecified in the method.

If required by the method, the quality control sample (QC S), a secondary source standard

used to verify calibration, was always within the cont rol limits specified by the method.

As described below, the analyte of interest was detecte d 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 spec ified in the method unless specified

below.

If required by the method, a matrix spike (MS) analysis was run on sample 72147 and

sample 72196 for each analyte to check for matrix interfe rences. All MS samples

analyzed met the criteria specified in the method unless described below.

### 3

DATA NOTES/ISSUES

Ammonia

The result for the method blank associated with one of the batches was greater than the

MDL. All associated samples were flagged with a “B” qualif ier. This affects samples

72147, 72143, 72093, 72097, and 72151. No further action is required.

The percent recoveries for the MS and matrix spike dupli cate (MSD) for sample 72147

were 93% and 102%, respectively, which is within the method co ntrol criteria; however,

the results exceeded the calibration range. These MS a nd MSD and results were flagged

with an “E” qualifier.

BOD 5



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

depletion greater than 2.0 mg/L for samples 72143, 72151, 72043, 71993, a nd 72247.

Therefore, BOD 5 

### was reported as not detected for these samples. Additiona lly, for sample

72200, the dilutions did not have a residual DO criteria of gre ater than 1.0 mg/L;

therefore, BOD 5 

### was reported as not detected for this sample. The rest of the samples had

at least one dilution with a DO depletion greater than 2.0 mg/L. As required in the

method, the final result was calculated by taking the av erage 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.

Chloride and Sulfate

MS and MSD were performed on samples 72147 and 72196. The MS/MS D recoveries

for both samples were within the method control for both chloride and sulfate; however,

the MS and MSD results for chloride exceeded the calibra tion range. Both sets of

MS/MSD results were flagged with “E” qualifiers.

COD

MS and MSD were performed on samples 72147 and 72196. The MS a nd MSD

recoveries for sample 72147 were 66% and 71%, respectively, w hich is outside the

method control criteria. These MS/MSD results were flagged with an “F” qualifier. The

MS and MSD recoveries for sample 72196 were 72% and 70%, respec tively, which is

outside the method control criteria. These MS/MSD re sults were flagged with an “F”

qualifier.

Cyanide

Because of the nature of the sample matrix, all of th e samples in this sampling episode

used a lower volume, which resulted in elevated RLs being ca lculated and reported by

TestAmerica with the sample results.

### 4

MS and MSD were performed on samples 72147 and 72196. The MS a nd MSD

recoveries for sample 72147 were 76% and 75%, respectively. T he MS and MSD

recoveries for sample 72196 were 59% and 57%, respectively. Th e LCS/LCSD

recoveries associated with these batches were acceptabl e, which indicates the analytical

system was operating within control. Additionally, ther e is no method requirement for the

analysis of a MS/MSD and therefore, no corrective ac tion is necessary.

Nitrate/Nitrite

No MS/MSD data was reported for batch 45200 in the sample a nd QC sample report

summary. The method requires that a known amount of ana lyte be added to 10% of

samples per batch. The general chemistry worksheet indi cates that MS samples were

performed on a sample outside of these episodes, but no spiking concentrations or percent

recoveries are indicated. The MS/MSD recoveries for the other batches were within

control limits.

Phosphorus

The results for the method blanks associated with two of the batches was greater than the

MDL, but less than the RL. The blank results were flagge d with a “J” qualifier. All

associated samples were qualified with a “B” flag. No additional corrective action is

necessary.

MS and MSD were performed on sample 72001, 72147 and 72196. The percen t

recoveries for the MS and MSD for sample 72147 were 69% an d 70%, respectively,

which is outside the method control criteria. These MS /MSD results were flagged with

an “F” qualifier. The LCS/LCSD recoveries for this ba tch were acceptable and indicate

that the analytical system was operating within control . The percent recoveries for the

MS and MSD for sample 72196 were 91% and 85%, respectively. The MSD recovery is

outside the method control criteria, but within the labor atory criteria and therefore, was

not flagged. If reported, the MSD result should be flagge d with an “F” qualifier. The

LCS/LCSD recoveries for this batch were acceptable and ind icate that the analytical

system was operating within control. Additionally, the MS/MSD performed on sample

72001 was in the same batch as the MS/MSD for 72196 and the pe rcent recoveries for the

MS and MSD were 96% and 97%, respectively, with are within th e method control

criteria.

TDS

TA reports that constant weight was not achieved after 3 drying cycles for the following

samples: 72097, 72143, 72147, 72151, 71993, 72196, 72200, 71997, 72004, and 72243.

Review of the general chemistry worksheets indicates th at constant weight was achieved

for all samples. No further action was necessary.

### 5

Because of the nature of the sample matrix, some of t he samples in this sampling episode

used a lower volume, which resulted in elevated RLs being ca lculated and reported by

TestAmerica with the sample results.

The analytical duplicate associated with sample 72143 excee ded the recovery criteria.

The duplicate result was qualified with an “F” flag. Beca use an analytical duplicate was

not required by the method, no further corrective action i s necessary.

TKN

MS and MSD were performed on samples 72147 and 72196. The MS a nd MSD

recoveries for sample 72147 were 76% and 57%, respectively. The concentration in the

original sample was greater than four times the spike a mount; therefore, the recoveries

cannot be reliably calculated and the results were flagge d with a “4” qualifier. The MS

and MSD recoveries for sample 72196 were 81% and 78%, respecti vely, which do not

meet the method control criteria, but do meet the labo ratory control criteria and therefore,

these results were not flagged by the laboratory. If r eported, the MS and MSD results

should be flagged with “F” qualifiers. The LCS/LCSD reco veries associated with these

batches were acceptable, which indicates the analytical system was operating within

control.

TSS

Because of the nature of the sample matrix, some of t he samples in this sampling episode

used a lower volume, which resulted in elevated RLs being ca lculated and reported by

TestAmerica with the sample results.

### 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: 2/9/2012

Subject: FGS Data Review Narrative for Total Mercury – Long-Term M onitoring:

Month 4 and 5

Frontier Global Sciences (FGS) generated analytical da ta for total mercury. FGS

analyzed the samples according to EPA Method 1631E for merc ury by Cold Vapor

Atomic Fluorescence Spectrometry (CVAFS) analysis.

Table 1 summarizes the 30 samples (excluding laboratory pre p blanks) FGS extracted

and analyzed for total mercury.

Table 1. 

### Long-Term Monitoring Month 4 and 5 Mercury – Sample Identification

EPA

Sample # Lab Sample

ID # Sample

Matrix Sample Description Sampling

Date

71994 1101223-48 Aqueous FGD Influent, Set 4 1/17/2011

71998 1101223-53 Aqueous FGD Bioreactor Influent, Set 4 1/17/2011

72002 1101223-58 Aqueous FGD Bioreactor Effluent, Set 4 1/17/2011

72007 1101223-59 Aqueous FGD Bioreactor Influent Field Blank, Set 4 1/17/2011

72011 1101223-60 Aqueous FGD Bioreactor Effluent Field Blank, Set 4 1/17/2011

72044 1101308-01 Aqueous FGD Influent, Set 4 1/26/2011

72048 1101308-06 Aqueous FGD Effluent, Set 4 1/25/2011

72053 1101308-07 Aqueous FGD Effluent Field Blank, Set 4 1/25/2011

72094 1101223-41 Aqueous FGD Influent, Set 4 1/14/2011

72098 1101223-46 Aqueous FGD Effluent, Set 4 1/14/2011

72103 1101223-47 Aqueous FGD Effluent Field Blank, Set 4 1/13/2011

72144 1101223-21 Aqueous FGD Influent, Set 4 1/12/2011

72148 1101223-26 Aqueous FGD Bioreactor Influent, Set 4 1/12/2011

72152 1101223-31 Aqueous FGD Bioreactor Effluent, Set 4 1/12/2011

72157 1101223-32 Aqueous FGD Bioreactor Influent Field Blank, Set 4 1/12/2011

72161 1101223-33 Aqueous FGD Bioreactor Effluent Field Blank, Set 4 1/12/2011

72193 1101223-08 Aqueous FGD Influent, Set 3 1/12/2011

72197 1101223-13 Aqueous FGD SBR Influent, Set 3 1/12/2011

72201 1101223-18 Aqueous FGD SBR Effluent, Set 3 1/12/2011

### 2

Table 1. 

### Long-Term Monitoring Month 4 and 5 Mercury – Sample Identification

EPA

Sample # Lab Sample

ID # Sample

Matrix Sample Description Sampling

Date

72206 1101223-19 Aqueous FGD SBR Influent Field Blank, Set 3 1/12/2011

72210 1101223-20 Aqueous FGD SBR Effluent Field Blank, Set 3 1/12/2011

72244 1101223-34 Aqueous FGD Influent, Set 4 1/12/2011

72248 1101223-39 Aqueous FGD Effluent, Set 4 1/13/2011

72253 1101223-40 Aqueous FGD Effluent Field Blank, Set 4 1/12/2011

72293 1101223-01 Aqueous FGD Influent, Set 3 1/12/2011

72297 1101223-06 Aqueous FGD Effluent, Set 3 1/12/2011

72302 1101223-07 Aqueous FGD Effluent, Field Blank, Set 3 1/12/2011

72294 1102108-01 Aqueous FGD Influent, Set 4 2/9/2011

72298 1102108-06 Aqueous FGD Effluent, Set 4 2/9/2011

72303 1102108-07 Aqueous FGD Effluent Field Blank, Set 4 2/9/2011



### SUMMARY

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

There were no findings from the data review that required a dditional qualifiers in this

dataset. The following summarizes the findings from the data review:

• The sample number for Sample 72157 was labeled incorrectly o n the traffic

report.

• The sample description for Sample 72148 was entered incorrec tly by FGS at the

time of sample receipt.

• Two laboratory duplicates were out of the method-suggested relative percent

difference (RPD) criteria.

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES

Sample 72157 was labeled incorrectly as Sample 721557 in the tra ffic report submitted to

the laboratory. The error was identified and correct ed during the data review based on

the sample description. FGS incorrectly labeled Sampl e 72148 as the FGD Bioreactor

Effluent, Set 4, when the correct sample description is FGD Bioreactor Influent, Set 4.

This error was identified and corrected during the data review and confirmed based on

the traffic report.

### 3

INITIAL CALIBRATION

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

the CVAFS analysis consisted of a blank and five calibrat ion standards with a correlation

coefficient ≥ 0.995. All method-specified criteria were met.

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

All initial and continuing calibration verifications (I CVs, CCVs) met method-specified

criteria.

BLANKS

All the preparation blanks or laboratory reagent blanks (L RBs) and the continuing

calibration blanks (CCBs) met the method-specified crite ria. Because all of the blank

results were less than the RL, no samples were quali fied based on these preparation blank

results.

DUPLICATES

No field duplicate samples were collected with these sa mpling episodes. Four samples

were analyzed in duplicate at the laboratory, Influent s amples 72144 and 71994 and

Effluent samples 72048 and 72298. The relative percent differenc e (RPD) for samples

72144, 71994, 72048, and 72298 were 30.6%, 7.66%, 19.4% and 43.9%, respectively.

Two of these RPDs were outside of laboratory criteria . The samples from another

sampling episode were also analyzed in duplicate with RPD s of 13.3%, 22.4%, and

3.03%. The laboratory’s RPD criteria between analytica l duplicates is 24%. Analytical

duplicates are not a method requirement; therefore, no samples were qualified based on

analytical duplicates.

LABORATORY CONTROL SAMPLES

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

and 24% RPD.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

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

sample 72144 and Effluent samples 72048 and 72298. MS/MSDs were also performed

on samples from another sampling episode. All aqueous MS /MSD recoveries were

within method specifications of 71-125%. All RPDs met metho d-specifiec criteria.

DETECTION LIMITS

The laboratory MDL in the synthetic matrix was 0.239 ng/ L. Results below this MDL

were reported as not detected (ND).

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A EAD

Deb Bartram, ERG

TJ Finseth, ERG

From: Randy Mercurio, ERG

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.8 – Long-Term

Monitoring: Month 4

TestAmerica generated analytical data for total metals (antimony, arsenic, cadmium,

chromium, copper, lead, nickel, selenium, silver, thalliumand vanadium) for these longterm monitoring samples. The samples were analyzed accor ding to EPA Method 200.8.

Table 1 summarizes the samples TestAmerica extracted a nd analyzed for total metals by

EPA Method 200.8.

Table 1. 

### Long-Term Monitoring Month 4 Total Metals – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

71994 FGD Influent, Set 4 280

- 11658

- 1 Aqueous 1/17/2011 1/18/2011

71998 FGD Bioreactor Influent, Set 4 280

- 11690

- 1 Aqueous 1/18/2011 1/19/2011

72002 FGD Bioreactor Effluent, Set 4 280

- 11690

- 2 Aqueous 1/18/2011 1/19/2011

72007 FGD Bioreactor Influent Field

Blank, Set 4 280

- 11690

- 3 Aqueous 1/18/2011 1/19/2011

72011 FGD Bioreactor Effluent Field

Blank, Set 4 280

- 11690

- 4 Aqueous 1/18/2011 1/19/2011

72094 FGD Influent, Set 4 280

- 11635

- 1 Aqueous 1/14/2011 1/15/2011

72098 FGD Effluent, Set 4 280

- 11635

- 2 Aqueous 1/14/2011 1/15/2011

72103 FGD Effluent Field Blank, Set 4 280

- 11635

- 3 Aqueous 1/14/2011 1/15/2011

72144 FGD Influent, Set 4 280

- 11555

- 1 Aqueous 1/12/2011 1/13/2011

72148 FGD Bioreactor Influent, Set 4 280

- 11597

- 1 Aqueous 1/13/2011 1/14/2011

72152 FGD Bioreactor Effluent, Set 4 280

- 11597

- 2 Aqueous 1/13/2011 1/14/2011

72157 FGD Bioreactor Influent Field

Blank, Set 4 280

- 11597

- 3 Aqueous 1/13/2011 1/14/2011

72161 FGD Bioreactor Effluent Field

Blank, Set 4 280

- 11597

- 4 Aqueous 1/13/2011 1/14/2011

72193 FGD Influent, Set 3 280

- 11552

- 1 Aqueous 1/12/2011 1/13/2011

72197 FGD SBR Influent, Set 3 280

- 11552

- 2 Aqueous 1/12/2011 1/13/2011

72201 FGD SBR Effluent, Set 3 280

- 11552

- 3 Aqueous 1/12/2011 1/13/2011

### 2

Table 1. 

### Long-Term Monitoring Month 4 Total Metals – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

72206 FGD SBR Influent Field Blank,

Set 3 280

- 11552

- 4 Aqueous 1/12/2011 1/13/2011

72210 FGD SBR Effluent Field Blank,

Set 3 280

- 11552

- 5 Aqueous 1/12/2011 1/13/2011

72244 FGD Influent, Set 4 280

- 11598

- 1 Aqueous 1/13/2011 1/14/2011

72248 FGD Effluent, Set 4 280

- 11598

- 2 Aqueous 1/13/2011 1/14/2011

72253 FGD Effluent Field Blank, Set 4 280

- 11598

- 3 Aqueous 1/13/2011 1/14/2011

72293 FGD Influent, Set 3 280

- 11553

- 1 Aqueous 1/12/2011 1/13/2011

72297 FGD Effluent, Set 3 280

- 11553

- 3 Aqueous 1/12/2011 1/13/2011

72302 FGD Effluent Field Blank, Set 3 280

- 11553

- 4 Aqueous 1/12/2011 1/13/2011



### SUMMARY

The samples were prepared for total metals analysis accor ding to TestAmerica’s “FGD

ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Elements

Analysis in Flue Gas Desulfurization Wastewaters,” date d October 6, 2010, based on

EPA Method 200.8, by ICP/MS analysis.

Any significant findings are summarized below. No addition al data qualifiers were

required.

• The sample for FGD Effluent, Set 3 associated with Epi sode 6571 was incorrectly

labeled as sample 72295 on the traffic report. The correc t sample number (72297)

was found on the sample bottle label and confirmed with E RG prior to analysis.

• The matrix spike (MS) and matrix spike duplicate (MSD) rec overies for total

silver for sample 72248 failed the EPA Method 200.8 control lim its of 70-130%.

The MSD recovery for total silver for sample 72201 also fa iled the method

control limits.

• The MS/MSD relative percent difference (RPD) for tota l silver for samples 72201

and 72248 failed the FGD ICP/MS SOP control limits of ±20%.

• The post digestion spike (PDS) recoveries for silver for samples 72201 and 72002

failed TestAmerica’s control limits of 85–115%.

INTERNAL STANDARDIZATION

All internal standards used by TestAmerica were within th e method criteria.

### 3

INITIAL CALIBRATION

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

calibration for the ICP-MS analysis consisted of a bla nk and four calibration standards.

INITIAL AND CONTINUING CALIBRATION VERIFICATION (IC V/CCV)

The initial calibration verifications (ICV) and continu ing calibration verifications (CCV)

performed by TestAmerica all had recoveries within the m ethod criteria.

METHOD/INSTRUMENT BLANKS

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

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

required for method blanks.

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

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

flagged with a “J” qualifier. No additional qualifiers were required for instrument blanks.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

All CRI samples passed TestAmerica’s SOP control limi ts of 50–150% recovery.

LABORATORY CONTROL SAMPLES (LCS)

All LCS samples passed the method QC limits of 85–115% recov ery.

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION

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

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

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

ICS.

All interference check sample B (ICSAB) synthetic sp ikes recovered within

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

SERIAL DILUTION

The serial dilution performed on samples 72201 and 72002 passed Te stAmerica’s criteria

of ±10% difference.

FIELD DUPLICATES

No field duplicate samples were collected with these sa mpling episodes.

### 4

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

MS and MSD were performed on samples of 72201, 72248, and 72002. The MSD of

sample 72201 failed the method control limits of 70–130% recover y for silver at 61%,

which was flagged with an “F” qualifier. The MS/MSD of sam ple 72248 failed the

method control limits of 70–130% recovery for silver at 66% a nd 45% respectively,

which were flagged with an “F” qualifier. These silver fa ilures are likely due to matrix

interference from the high concentration of sulfates , which can form insoluble silver

sulfide and/or silver sulfate. The silver recoveries in the associated LCS/LCSDs were

acceptable. The RPD for the MS/MSDs for samples 72201 and 72248 failed the FGD

ICP/MS SOP ±20% control limits for silver.

Otherwise, all MS/MSD spike recoveries were within th e method control limits of 70-

130% and the RPD for the MS/MSDs were within the FGD ICP /MS SOP control limits

of ±20 percent. No additional data qualifiers were required.

POST DIGESTION SPIKES (PDS)

The PDS performed on samples 72201 and 72002 passed TestAmerica’s control limits of

85–115% recovery for all analytes, except for silver for b oth PDS samples, which were

flagged with a “W” qualifier. Additional data qualifiers wo uld be required; however

silver was not detected in these samples.

DETECTION LIMITS

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

of reagent water.

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A EAD

Deb Bartram, ERG

TJ Finseth, ERG

From: Randy Mercurio, ERG

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.7 – Long-Term

Monitoring: Month 4

TestAmerica generated analytical data for total metals (aluminum, boron, barium,

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

titanium and zinc) for these long-term monitoring samples. The samples were analyzed

according to EPA Method 200.7.

Table 1 summarizes the samples TestAmerica extracted a nd analyzed for total metals by

EPA Method 200.7.

Table 1. 

### Long-Term Monitoring Month 4 Total Metals – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

71994 FGD Influent, Set 4 280

- 11658

- 1 Aqueous 1/17/2011 1/18/2011

71998 FGD Bioreactor Influent, Set 4 280

- 11690

- 1 Aqueous 1/18/2011 1/19/2011

72002 FGD Bioreactor Effluent, Set 4 280

- 11690

- 2 Aqueous 1/18/2011 1/19/2011

72007 FGD Bioreactor Influent Field

Blank, Set 4 280

- 11690

- 3 Aqueous 1/18/2011 1/19/2011

72011 FGD Bioreactor Effluent Field

Blank, Set 4 280

- 11690

- 4 Aqueous 1/18/2011 1/19/2011

72094 FGD Influent , Set 4 280

- 11635

- 1 Aqueous 1/14/2011 1/15 /201 1

72098 FGD Effluent , Set 4 280

- 11635

- 2 Aqueous 1/14/2011 1/15 /201 1

72103 FGD Effluent Field Blank, Set 4 280

- 11635

- 3 Aqueous 1/14/2011 1/15 /201 1

7 2144 FGD Influent, Set 4 280

- 11555

- 1 Aqueous 1/12 /201 1 1/13 /201 1

7 2148 FGD Bioreactor Influent, Set 4 280

- 11597

- 1 Aqueous 1/13/2011 1/14/2011

72152 FGD Bioreactor Effluent, Set 4 280

- 11597

- 2 Aqueous 1/13/2011 1/14/2011

72157 FGD Bioreactor Influent Field

Blank, Set 4 280

- 11597

- 3 Aqueous 1/13/2011 1/14/2011

72161 FGD Bioreactor Effluent Field

Blank, Set 4 280

- 11597

- 4 Aqueous 1/13/2011 1/14/2011

72193 FGD Influent, Set 3 280

- 11552

- 1 Aqueous 1/12 /201 1 1/13 /201 1

7 2197 FGD SBR Influent, Set 3 280

- 11552

- 2 Aqueous 1/12 /201 1 1/13 /201 1

7 2201 FGD SBR Effluent, Set 3 280

- 11552

- 3 Aqueous 1/12 /201 1 1/13 /201 1

### 2 Table 1. 

### Long-Term Monitoring Month 4 Total Metals – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

72 206 FGD SBR Influent Field Blank,

Set 3 280

- 11552

- 4 Aqueous 1/12 /201 1 1/13 /201 1

7 2210 FGD SBR Effluent Field Blank,

Set 3 280

- 11552

- 5 Aqueous 1/12 /201 1 1/13 /201 1

72244 FGD Influent, Set 4 280

- 11598

- 1 Aqueous 1/13/2011 1/14/2011

72248 FGD Effluent , Set 4 280

- 11598

- 2 Aqueous 1/13/2011 1/14/2011

72253 FGD Effluent Field Blank, Set 4 280

- 11598

- 3 Aqueous 1/13/2011 1/14/2011

7 2293 FGD Influent, Set 3 280

- 11553

- 1 Aqueous 1/12 /201 1 1/13 /201 1

7 2297 FGD Effluent, Set 3 280

- 11553

- 3 Aqueous 1/12 /201 1 1/13 /201 1

7 2302 FGD Ef

fluent Field Blank, Set 3 2 80

- 11553

- 4 Aqueous 1/12 /201 1 1/13 /201 1



### SUMMARY

The samples were prepared for total metals analysis acc ording to TestAmerica’s SOP for

ICP Analysis for Trace Metals by Method 200.7. Any signific ant findings are

summarized below. No additional data qualifiers were require d for this set of data.

• Several samples did not have the date and time of sampl e collection listed on the

traffic reports.

• One sample was listed with the wrong sample number on the traffic report.

• The post digestion spike (PDS) for sodium for sample 72002 fai led

TestAmerica’s control limits of 85–115% recovery.

SAMPLE RECEIPT, HANDLING AND STORAGE ISSUES

Samples associated with Episode 6569 (72193, 72197, 72201, 72206, and 72210) did n ot

have a sample date or time on the traffic report or s ample labels.

Samples associated with Episode 6571 (72293, 72297, and 72302) did not hav e a sample

date or time on the traffic report or sample labels. Add itionally, a field sampler name was

not present on the traffic report. The sample FGD Ef fluent, Set3 was listed on the traffic

report as sample 72295, which is incorrect; however, the sam ple bottle was labeled

correctly as sample 72297. TestAmerica used 72297 for processing the sample.

Samples of 72144 FGD Influent, Set 4 did not have a sample dat e or time listed on the

sample bottles.

### 3

INTERNAL STANDARDIZATION

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

ISTD recoveries within the ±30% criterion of the calibra tion blank as per Section 9.11 of

the SOP were seen. All ISTD were within the control limits.

INITIAL CALIBRATION

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

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

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

The initial calibration verifications (ICV) and continu ing calibration verifications (CCV)

performed by TestAmerica all had recoveries within the m ethod criteria.

METHOD/INSTRUMENT BLANKS

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

were above the method detection limit (MDL) and were f lagged with the “J” qualifier.

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

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

flagged with the “J” qualifier.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

All CRI samples passed TestAmerica’s SOP control limi ts of 50–150% recovery.

LABORATORY CONTROL SAMPLES (LCS)

All LCSs passed the method control limits of 85–115% recover y.

INTERFERENCE CHECK SOLUTIONS

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

data quality objectives met TestAmerica’s SOP criteria.

SERIAL DILUTION (SRD)

Serial dilutions were performed for each batch of total samples. All serial dilution percent

differences were less than 10% as required by TestAmerica ’s SOP.

FIELD DUPLICATES

No field duplicate samples were collected with these sa mpling episodes.

### 4

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

Matrix spikes (MS) and matrix spike duplicates (MSD) w ere performed on the total

samples of 72201, 72248, and 72002. Some elements with high concent rations failed the

EPA 200.7 Method spike recovery control limits of 70–130% but w ere flagged with a “4”

qualifier indicating that the concentration in the paren t sample was greater than 4 times

the spike and could not be reliably calculated. These data were considered acceptable

based on the LCS passing the method control limits. Othe rwise, all MS/MSD spike

recoveries were within the method control criteria of 70-130%. The relative percent

difference (RPD) for all MS/MSDs were within TestAme rica’s ± 20% requirement,

except for magnesium for sample 72095. No additional data quali fiers were needed.

POST DIGESTION SPIKE (PDS)

The PDS performed on sample 72201 failed the method criteria of 85–115% recovery for

boron; however, the result was not qualified with a “ W” because the sample

concentration was greater than 4 times the spike amoun t.

The PDS performed on sample 72002 failed the method criteria of 85–115% recovery for

boron, magnesium and manganese; however, these result s were not qualified with a “W”

because their sample concentrations were greater than 4 times the spike amount. Sodium

also failed the method criteria and was flagged with a “W ” qualifier. All elements passed

the serial dilution for this sample demonstrating that there were no significant matrix

interferences. No additional data qualifiers are required.

DETECTION LIMITS

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

of reagent water.

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A EAD

Deb Bartram, ERG

TJ Finseth, ERG

From: Jennifer Colby, ERG

Donna Tedder, ERG

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Classicals Ana lyses – Long-Term

Monitoring: Month 4

TestAmerica Denver Laboratory generated analytical data f or classical wet chemistry

analyses for these long-term monitoring samples. All s amples were tested for the

following analytes:

• Ammonia by EPA method 350.1,

• Biochemical Oxygen Demand – 5 day (BOD 5 

### ) by SM 5210B,

• Chloride and Sulfate by EPA method 300.0,

• Chemical Oxygen Demand (COD) by EPA method 410.4,

• Cyanide (total) by SM 4500 CN

- 

### E,

• Nitrate/Nitrite by EPA method 353.2

• Phosphorus (total) by EPA method 365.1,

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

• Total Kjeldakl Nitrogen (TKN) by EPA method 351.2, and

• Total Suspended Solids (TSS) by SM 2540D.

Table 1 summarizes the 15 samples that TestAmerica anal yzed for the above analytes.

Table 1. Long-Term Monitoring Month 4 Classical Analytes – Sample

Identification

EPA

Sample # Sample

Matrix Sample Description Sampling

Date

71994 Water FGD Influent, Set 4 1/21/2011

71998 Water FGD Bioreactor Influent, Set 4 1/21/2011

72002 Water FGD Bioreactor Effluent, Set 4 1/21/2011

72094 Water FGD Influent, Set 4 1/18/2011

72098 Water FGD Effluent, Set 4 1/18/2011

72144 Water FGD Influent, Set 4 1/14/2011

72148 Water FGD Bioreactor Influent, Set 4 1/17/2011

### 2 Table 1. Long-Term Monitoring Month 4 Classical Analytes – Sample

Identification

EPA

Sample # Sample

Matrix Sample Description Sampling

Date

72152 Water FGD Bioreactor Effluent, Set 4 1/17/2011

72193 Water FGD Influent, Set 3 1/14/2011

72197 Water FGD SBR Influent, Set 3 1/14/2011

72201 Water FGD SBR Effluent, Set 3 1/14/2011

72244 Water FGD Influent, Set 4 1/17/2011

72248 Water FGD Effluent, Set 4 1/17/2011

72293 Water FGD Influent, Set 3 1/14/2011

72297 Water FGD Effluent, Set 3 1/14/2011

SUMMARY

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

unless otherwise noted below. All samples were preserve d appropriately unless

otherwise specified. Group II samples 72293 and 72297 were receiv ed at the laboratory

at a neutral pH. The laboratory preserved the volume and proceeded with the requested

analyses.

Field duplicate samples were not collected for this epis ode. Depending on the method, a

laboratory duplicate was analyzed instead. The Relative Percent Difference (RPD)

between the sample and its duplicate was less than 20% unl ess otherwise noted below.

If applicable, the appropriate number of standards was used to create a calibration curve.

If sample results were above the highest standard used t o create the curve, the sample was

diluted and reanalyzed. All sample results were between the lowest and highest standards

unless noted below. Additionally, unless otherwise noted, a ll calibration blanks and

calibration verification samples met the criteria sp ecified in the method.

If required by the method, the quality control sample (QC S), a secondary source standard

used to verify calibration, was always within the cont rol limits specified by the method.

As described below, the analyte of interest was detecte d 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 spec ified in the method unless specified

below.

If required by the method, a matrix spike (MS) analysis was run on samples 72002,

72094, 72193, 72201, 72244, and 72297 for each analyte to check for matrix

interferences. All MS samples analyzed met the crite ria specified in the method unless

described below.

### 3

DATA NOTES/ISSUES

Ammonia

Samples 72293 and 72297 were received by the laboratory at a neutra l pH. Sample

72293 was qualified as an estimated, as shown in Table 2. Samp le 72297 had a result

greater than the MDL, but less than the RL, so the re sult was already flagged with a ”J”

qualifier, so further qualification was not necessary.

The percent recoveries for the MS and MSD performed on sample 72094 were 77% and

76%, respectively, which is outside of method control cri teria. Additionally, the MS and

MSD results exceeded the calibration range. The MS/MSD results for sample 72094 were

flagged with “E” and “F” qualifiers. No further qualificatio n is needed.

BOD 5



### No issues were identified by the data reviewer.

Chloride and Sulfate

MS and MSD were performed on samples 72002, 72094, and 72201. The perce nt

recoveries for the MS and MSD for all chloride and sul fate results were within the

method control criteria; however, all the MS and MSD results exceeded the exceeded the

calibration range, except for the MSD sulfate result f or sample 72002. All these chloride

and sulfate MS and MSD results were qualified with “E” qualifiers, except for the MSD

sulfate result for sample 72002.

COD

Samples 72293 and 72297 were received by the laboratory at neutral pH. These results

were qualified as estimated values, as shown in Table 2.

MS and MSD were performed on samples 72002 and 72098. The percent recoveries for

the MS and MSD for sample 72002 were 91% and 87%, respectively. The percent

recoveries for the MS and MSD for sample 72098 were 90% an d 88%, respectively.

Both the MSD results are outside the method control c riteria. These MSD results were

flagged with “F” qualifiers.

Cyanide

MS and MSD were performed on samples 72193 and 72002. The percent recoveries for

the MS and MSD for sample 72193 were 74% and 78%, respectively . The percent

recoveries for the MS and MSD for sample 72002 were both 88%. The LCS/LCSD

recoveries were acceptable, indicating that the analyti cal system was operating within

control. Additionally, there is no method requirement f or the analysis of a MS/MSD and

no corrective action is necessary.

### 4

Nitrate/Nitrite

Samples 72293 and 72297 were received by the laboratory at neutral pH. These results

were qualified as estimated values, as shown in Table 2.

Phosphorus

Samples 72293 and 72297 were received by the laboratory at neutral pH. These results

were qualified as estimated values, as shown in Table 2.

The method blank associated with two of the batches detec ted phosphorus at levels

greater than the MDL, but less than the RL. All affec ted samples were flagged with a “B”

qualifier. No additional corrective action is necessary

.

MS and MSD were performed on samples 72002 and 72297. The percent recoveries for

the MS and MSD for sample 72002 were 72% and 56%, respectively, which are outside

the method control criteria. The MS result was withi n the laboratory control criteria and

therefore, was not flagged by the laboratory; however, the MSD result was outside the

laboratory control criteria and was flagged with an “F” qualifier. The LCS/LCSD

recoveries for this batch were acceptable, indicating the analytical system was operating

within control. If reported, the MS result should be fl agged with an “F” qualifier.

The percent recoveries for the MS and MSD for sample 72297 were 66% and 58%,

respectively, which are outside the method control crite ria. There results were flagged

with “F” qualifiers. The LCS/LCSD recoveries for this batch were acceptable, indicating

the analytical system was operating within control.

TDS

TA reports that constant weight was not achieved after 3 drying cycles for the following

samples: 72293, 72244, 71994, 72152, and 72248. Review of the general chemist ry

worksheets indicates that constant weight was achieve d for all. No further action was

necessary.

The analytical duplicate performed on sample 72002 exceeded t he recovery criteria. The

duplicate result was flagged with an “F” qualifier. Becaus e an analytical duplicate was

not required by the method, no further corrective action i s necessary.

TKN

Samples 72293 and 72297 were received by the laboratory at neutral pH. These results

were qualified as estimated values, as shown in Table 2.

MS and MSD were performed on samples 72001 and 72002. The percent recoveries for

the MS and MSD for sample 72002 were both 93%, which is withi n the method control

### 5

criteria. The percent recoveries for the MS and MSD for sample 72001 were 48% and

46%, respectively, which are outside the method control cri teria. There results were

flagged with “F” qualifiers. The LCS/LCSD recoveries fo r this batch were acceptable,

indicating that the analytical system was operating wit hin control.

TSS

Because of the nature of the sample matrix, some of t he samples in this sampling episode

used a lower volume, which resulted in elevated RLs being c alculated and reported by

TestAmerica with the sample results.

The analytical duplicate performed on sample 72248 exceeded t he recovery criteria.

Because the sample result is below the RL, further qual ification was not necessary.

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Ac

tion Reason Level Detected

72293 Ammonia Estimated

Value Received at neutral pH XXX mg/L

72293 COD Estimated

Value Received at neutral pH XXX mg/L

72297 COD Estimated

Value Received at neutral pH XXX mg/L

72293 Nitrate/Nitrite Estimated

Value Received at neutral pH XXX mg/L

72297 Nitrate/Nitrite Estimated

Value Received at neutral pH XXX mg/L

72293 Phosphorus Estimated

Value Received at neutral pH XXX mg/L

72297 Phosphorus Estimated

Value Received at neutral pH XXX mg/L

72293 TKN Estimated

Value Received at neutral pH XXX mg/L



### 72297 TKN Estimated

Value Received at neutral pH XXX mg/L