# Appendix D

Duke Energy Carolinas’ Allen 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’ Allen Steam Station to

aid in collecting, packaging, and shipping samples for this sa mpling 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 200.7Figure 1. Allen 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 72141 6568

FGD Wastewater Treatment Influent – Set 2 72142 6568

FGD Wastewater Treatment Influent – Set 3 72143 6568

FGD Wastewater Treatment Influent – Set 4 72144 6568

FGD Bioreactor Influent – Set 1 72145 6568

FGD Bioreactor Influent – Set 2 72146 6568

FGD Bioreactor Influent – Set 3 72147 6568

FGD Bioreactor Influent – Set 4 72148 6568

FGD Bioreactor Effluent – Set 1 72149 6568

FGD Bioreactor Effluent – Set 2 72150 6568

FGD Bioreactor Effluent – Set 3 72151 6568

FGD Bioreactor Effluent – Set 4 72152 6568

FGD Wastewater Treatment Influent Field Blank 72153 6568

FGD Bioreactor Influent Field Blank – Set 1 72154 6568

FGD Bioreactor Influent Field Blank – Set 2 72155 6568

FGD Bioreactor Influent Field Blank – Set 3 72156 6568

FGD Bioreactor Influent Field Blank – Set 4 72157 6568

FGD Bioreactor Effluent Field Blank – Set 1 72158 6568

FGD Bioreactor Effluent Field Blank – Set 2 72159 6568

FGD Bioreactor Effluent Field Blank – Set 3 72160 6568

FGD Bioreactor Effluent Field Blank – Set 4 72161 6568



### 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 that will be used for the collection of

samples during the EPA sampling episode, the plant can fo llow the instructions included

in the sampling plan drafted for the EPA sampling episode to collect the field blank

samples, set up the composite containers, and perform th e composite pump-off procedures

for the bioreactor influent and bioreactor effluent sampl ing 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 samples 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 t he bioreactor influent and bioreactor

effluent sampling points have intermittent flows which may interfere with the automatic

composite collection, please contact TJ Finseth, (703) 633-1698 to discuss 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 “bubblewrapped” 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 4Percent HydrocloneOverflow RecycledBack to ScrubberPlant NameSampleCollectionNumberDate of SampleCollectionScrubber Slurry Blowdown FlowRateScrubber SlurryPercent SolidsPlant Operation During Sample CollectionFGD Wastewater Treatment Operation During Sample CollectionPlant NameDate of SampleCollectionSampleCollectionNumberScrubber PurgeFlow Rate DuringInfluent SampleCollection(gpm)Plant NameDate of SampleCollectionSampleCollectionNumberPlant Operation During Sample CollectionUnit 1 Unit 2 Unit 3 Unit 4 Unit 5Daily Power Generation (MW-hrs)Plant Name DateProvide the daily power generation for each scrubbed unit starting two weeks prior to the first set ofsamples 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

### Enclosure 2

Authority

This request for information is made under authority provided by Section 308 of the Federal

Water Pollution Control Act, as amended, 33 USC 1318. Secti on 308 provides that, "Whenever

required to carry out the objective of this Act, includi ng but not limited to . . . developing or

assisting in the development of any effluent limitation . . . pretreatment standard, or standard of

performance under this Act," the Administrator shall requ ire the owner or operator of any point

source to "establish and maintain such records, . . make s uch reports, . . install, use, and maintain

such monitoring equipment . . . sample such effluent . . . and provide such other information as

he may reasonably require."

Confidentiality

A business ("you") may not withhold information from EPA on the grounds that it is

confidential. You may, however, if you desire, assert a business confidentiality claim covering

part or all of the information that you furnish to EPA.

EPA regulations concerning confidential business informatio n are contained in 40 CFR Part 2,

Subpart B. The manner of asserting such a claim is speci fied in 40 CFR 2.203(b). Information

covered by such a claim will be disclosed by EPA only to the extent, and by means of the

procedures, set forth in Subpart B.

If you wish to claim as confidential any of the informat ion covered by the enclosed request, you

must do so at the time you submit the information to EPA. If no such claim accompanies the

information when EPA receives it, EPA may make the inf ormation available to the public

without further notice to you.

EPA will notify you in the event that a request is made for release of information that you have

claimed to be confidential or EPA otherwise decides to ma ke a determination as to whether or

not such information is entitled to confidential treatm ent. At that time, EPA will request that you

substantiate any claim you have made that information is c onfidential. Therefore, we encourage

you to consult 40 CFR Part 2, and to claim as confidential only those items that you truly believe

satisfy the criteria for confidentiality.

Note that effluent data are not eligible for confidential t reatment (see 40 CFR 2.302).

### Enclosure 3

Notice of Intent to Transfer Confidential Information to Sel ected EPA Contractors

EPA intends to grant access to confidential information collected under the sampling program to

selected EPA contractors.

In accordance with 40 CFR Sections 2.301(h)(2-3), 2.302(h)(2-3), a nd 2.305(h)(2-3), EPA may

allow those contractors identified below access to all data (including data claimed to be

confidential) collected as part of the follow-on sampli ng program. Transfer of this information

to these contractors is necessary in order for the cont ractors to assist EPA in performing

technical, statistical, and environmental analyses to support the development of effluent

limitations guidelines and standards for the Steam Electri c Power Generating industry.

The contractors and subcontractors that will be providi ng support to EPA during the

development of these regulations are listed below:

EPA Office

Receiving

Support Contractor Name EPA Contract

No. Type of Support

Eastern Research Group, Inc. 68-C-02-095 Engineering analysi s Office of Water/

Office of

Science &

Technology/

Engineering &

Analysis

Division Westat EP-C-10-023 Statistical analysis

EPA has determined that it is necessary to transfer the information described above to the

designated contractors and subcontractors in order that they may carry out the work required by

their contracts. The contracts contain all provisions necessary to implement the confidentiality

regulations (see 40 CFR 2.301(h)(2), 2.302(h)(2), and 2.305(h)(2)).

In accordance with these confidentiality regulations, yo u are entitled to provide comments to

EPA regarding this notice of contemplated disclosure. Any such comments must be received by

EPA in writing within 10 days of your receipt of this noti ce. Please send such comments to:

Ronald Jordan

USEPA Headquarters

Ariel Rios Building

1200 Pennsylvania Ave., N.W.

Mail Code: 4303T

Washington, DC 20460

jordan.ronald@epa.gov

### Enclosure 4

Certification Statement

The individual responsible for directing or supervising the sample collection and engineering

data preparation for the sampling program must read and sig n the Certification Statement listed

below. The certifying official must be a responsible co rporate official or his/her authorized

representative.

Certification Statement

I certify under penalty of law that the samples collected for the sampling program were collected

under my direction or supervision, that qualified personnel collected the samples following the

procedures described in the instructions (including the use of clean hands/di rty hands sampling

techniques described in EPA Method 1669), that qualified personnel gathered t he engineering

data required, and that the sampling and engineering data provided are complete and ref lect

normal operations for this plant. The engineering data submitted are, to the best of my

knowledge and belief, accurate and complete. In those cases where we di d not possess direct

measurement, we provided best estimates. We have to the best of our ability indicated what we

believe to be company confidential business information as defined under 40 CFR Part 2,

Subpart B. We understand that we may be required at a later time to jus tify our claim in detail

with respect to each item claimed confidential. I am aware that there are significant penalties

for submitting false information, including the possibility of fines and imprisonment as explained

in Section 308 of the Clean Water Act.

Signature of Certifying Official Date



### ( )

Printed Name of Certifying Official Telephone Numbe r of Certifying Official

Title of Certifying Official

Company Name

## Section 2

On

- Site Audit Memorandum

### DATE: 9 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’ Allen Steam Station on November 1-2, 2010

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

Carolinas’ Allen Steam Station (Allen) located in Bel mont, North Carolina. This was Allen’s

second set (“Set 2”) of self-monitoring sampling that was being conducted to comply with the

requirements established in a letter from Mary Smith, D irector of EPA’s Engineering and

Analysis Division, dated July 30, 2010. EPA conducted the audit on November 1-2, 2010.

These notes summarize the sample collection techniques used by Allen at each of the sampling

points and EPA’s observations/findings from the audit. A process water diagram for the flue gas

desulfurization (FGD) wastewater treatment system is provided as Attachment 1. The treatment

system is described in EPA’s sampling plan for the Allen plant. 1 

### The checklists that EPA

completed during the audit are provided as Attachment 2. Pic tures from the audit are provided

as Attachment 3.

Throughout the period of sampling for Set 2, Units 3 and 4 wer e operating, along with

FGD 3. Units 1, 2, and 5, along with FGD 1 were shut down fo r maintenance. The following

sections describe the sample collection at each of th e sampling points and the

observations/findings from each sampling point.

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

Allen personnel collected samples for the influent to FG D wastewater treatment system

from a sample tap located on the wastewater piping down stream of the FGD purge tank and

upstream of the equalization tank. EPA specified this locat ion for the FGD purge sample (i.e.,

prior to the wastewater entering the equalization tank) b ecause 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 Allen

FGD system. This is the same sampling point that EPA use d during its sample collection. The

sample tap consisted of a PVC fitting. A picture of the sample tap is included as Figure 1 in

Attachment 3.

Sample Collection

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

samples of the FGD purge, Allen personnel followed EPA Met hod 1669 protocols and the EPAprovided instructions. Allen personnel shrouded the tap with a clean plastic bag and let the

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

NC, Sampling Episode 6561. July 1, 2010.

### Page 2

sample flow from the tap for two minutes prior to collect ing any samples. All of the mercury

and metals samples were filled while the samplers 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 w as pulled away from the sample tap

and Allen personnel filled the bottles for classicals w ithout the shrouding. During the sample

collection for mercury and metals, wind gusts intermitte ntly caused the shroud to interfere with

the purge stream flowing from the sample tap and complicat e the sample collection. To resolve

this, an additional Allen representative not wearing T yvek® coveralls, gloves, or dust mask

stepped forward and stabilized the shroud by holding the outsi de of the plastic bag. This person

did not come in contact with the inside of the shroud or any sample bottles. The flow through the

sample tap continued without interruption until all influe nt 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

Allen personnel followed all method specifications 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

Allen personnel used a pH probe and a temperature probe in the laboratory to measure

the pH and temperature of the influent field test bottle.

Observations/Findings

EPA observed the Allen personnel setting up and collecting the Set 2 samples for the

influent to wastewater treatment system. No field bla nks were collected at this sample point

because Allen personnel previously collected field blanks duri ng Set 1. The sampling crew

followed the requirements of EPA Method 1669 (e.g., clean sa mpling protocols) while collecting

samples, with the exception that as the shroud was buf feted by wind gusts an additional Allen

representative not wearing Tyvek® coveralls, gloves, or dus t mask stepped forward and

stabilized the shroud by holding the outside of the plasti c bag. This person did not come in

contact with the inside of the shroud or any sample bott les. The flow through the sample tap

flowed without stopping during sample collection; however, after personnel began filling bottles

the flow rates slowed considerably and led the sampling cr ew to open the valve further to

maintain sufficient flow. Allen personnel collected s amples for analysis by both EPA-contracted

### Page 3

laboratories (metals and classicals) and industry labor atories (metals only). The sample bottles

were filled as duplicates, with one bottle filled after the other was full – in contrast to the multifill sample collection technique used at the other two sam ple points, and the split samples

collected during EPA’s four-day sampling episodes. The bottl es used were pre-labeled in the

laboratory.

Allen personnel followed applicable procedures for sample collection and preservation.

Samples were preserved within 15 minutes. Temperature and pH o f the field test sample were

measured approximately eleven minutes after sample collecti on.

Influent to Bioreactor System (SP-2)

Allen personnel collected samples for the influent to th e bioreactor system (SP-2) from a

sample tap downstream of the sand filters after the w astewater 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. A picture of the sample tap is included

as Figure 2 in Attachment 3.

Sample Collection

Allen personnel collected the influent to the bioreactor system as composite samples,

except for the mercury and cyanide samples. One ISCO auto matic compositor was programmed

to collect individual sample volumes into a 20-liter con tainer for the composite samples. The

ISCO pump was calibrated and programmed to collect aliquots of equal volume in one-hour

intervals during the 24-hour composite period. Following the composite period, Allen personnel

pumped off the specific sample volumes into the indivi dual sample bottles for all analyses except

mercury and cyanide. Mercury and cyanide samples were colle cted as grab samples.

To collect the composite samples, Allen personnel used a T-splitter tubing set that

consisted of a short length of silicone tubing attached t o 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, Allen pe rsonnel collected field blanks for SP-2

by threading the short end of the tubing set through the per istaltic 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,

Allen personnel attached one long end of the silicone tubi ng to one of the barbed sample taps and

the other long end was directed to a nearby drain, and att ached the vented cap and shorter length

of tubing to a 20-liter carboy. A picture of the sampling configuration is included as Figure 3 in

Attachment 3. The samplers programmed the compositor to collect 830 mL of sample every

hour for a 24-hour period.

### Page 4

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

pumped the sample into the individual sample bottles. A llen 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 sample bottles. The samplers first shook the

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

onto the carboy. The Teflon® end of the tubing was then inserted into the carboy and the tubing

was purged with one liter of sample. Allen personnel the n 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 filled as mu lti-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 field blank bottles wer e 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. Allen personnel then collected th e metals samples with the bottles placed in

the clean box. The bottles were filled as multi-fillsplit samples (i.e., one bottle was filled onethird full, then a second and any additional bottles were filled one-third full, and then the process

was repeated until all metals bottles were full). Aft er all the metals samples were collected, the

samplers filled the classical samples outside the cl eanbox. No classical samples were collected

for analysis by industry-contracted laboratories.

Allen personnel also collected grab samples for mercury every six hours during the

sampling. The samplers took steps to minimize atmospheric 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. Allen

personnel filled the mercury bottles directly from 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 bottle one-third fu ll, then the second sampler filled the Allen

sample bottle one-third full, and then the process was repeated until the bottles were full). Allen

personnel also collected the cyanide sample as a grab sa mple immediately after the first of the

four mercury grab samples at the sampling point.

Preservation

Allen personnel followed all method specifications 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

### Page 5

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

Allen personnel used a pH probe and a temperature probe in the laboratory to measure

the pH and temperature of the bioreactor influent field tes t bottle.

Observations/Findings

EPA did not observe the field blank collection and set- up for the composite samples.

EPA observed the following activities for SP-2 during the aud it: collection of cyanide sample

and mercury grab 1 (including field blank) and grab 2; breakdown o f 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. Allen personnel col lected samples for analysis by both

EPA-contracted laboratories (metals and classicals) an d industry laboratories (metals only). The

sample bottles (except mercury field blanks) were filled as multi-fill split samples. Allen

personnel followed applicable procedures for sample collec tion 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 the tubin g end was threaded through

the pump. The tubing end remained covered while threading. Durin g pump-off, the bag on the

end of the tubing was replaced with a clean bag prior to pl acing the tubing in the clean box.

Allen staff did not use a clean box during the set-up for the composite sample. At the end of the

24-hour composite period, the carboy contained 15.5 liters (i nstead of the programmed 20 liters

total volume).

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

inner bags for the first EPA mercury field blank bottle a nd the UWAG mercury field blank bottle

were sealed outside the shroud. The inner bag for the sec ond EPA field blank bottle was sealed

under the shroud. The EPA auditor informed the sampling person nel that the inner bag for all

### Page 6

bottles should be sealed while under the shroud, which was done for all remaining samples that

were observed.

All bottles were pre-labeled by the laboratory. During pum p-off of the composite

samples, Allen personnel marked the outer bags for the s ample bottles. While doing so, an inner

bag was mistakenly written on with a marker (prior to fi lling the bottle). Since this would violate

clean sampling protocols, the sample bottle for the Met hod 200.7 field blank (sample 72155) was

replaced with a spare double-bagged clean bottle (pre-labele d in the laboratory as NN-7625).

The field blank container was a 10-liter carboy, instea d of a 20-liter carboy (a 20-liter

carboy was used to collect the 24-hour composite samples).

Effluent from the Bioreactor System (SP-3)

Allen personnel collected samples for the effluent fro m the bioreactor system (SP-3) from

a sample tap on a section of piping downstream of the s econd-stage effluent storage tank from

the second-stage bioreactor cells. This is the same sam pling point that EPA used during its

sample collection. The sample tap consisted of PVC pi ping 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 interrupting the c omposite sampler. A picture of the

sample tap is included as Figure 3 in Attachment 3.

Sample Collection

Allen personnel collected samples for SP-3 using the sa me approach described above for

SP-2.

Preservation

Allen personnel followed all method specifications whe n 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

Allen personnel used a pH probe and a temperature probe in the laboratory to measure

the pH and temperature of the bioreactor effluent field tes t bottle.

Observations/Findings

### Page 7

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. Allen personnel col lected samples for analysis by both

EPA-contracted laboratories (metals and classicals) an d industry laboratories (metals only). The

sample bottles (except mercury field blanks) were filled as multi-fill split samples. Allen

personnel followed applicable procedures for sample collec tion 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 the tubin g end was threaded through

the pump during set-up for the composite sample and while prepar ing for pump-off. The tubing

end remained covered while threading. During pump-off, the bag o n the end of the tubing was

replaced with a clean bag prior to placing the tubing in the clean box. At the end of the 24-hour

composite period, the carboy contained 20 liters (equal to the programmed volume).

While filling mercury grab 2, the EPA bottle was complete ly filled – then, since the

samplers had intended to fill both EPA and industry sample bottles as multi-fill split samples, the

contents of the EPA bottle was dumped and both EPA and in dustry bottles were filled together

(multi-fill). Per the request of the EPA auditor, both sample bottles were dumped and replaced

with new bottles. The new bottles for grab 2 were coll ected as multi-fill split samples.

All bottles were pre-labeled by the laboratory. The f ield 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 2

– Influent to the Bioreactor System (SP

‐ 2)

### Figure 3

– Effluent from the Bioreactor System (SP

‐ 3)

## Section 3

Signed Certification Statement

## Section 4

Engineering DataTable D4-1. Field Measurementsfor Sample Collection at the Influent to FGD Wastewater Treatment System,AllenEpisode NumberSample CollectionNumberDate of SampleCollectionSample CollectionTimeTemperature(°C)pH(S.U.)6568Set 1 - Grab 1 10/5/2010080038.197.026568Set 2 - Grab 1 11/1/2010111832.616.96568Set 3-Grab 112/6/2010105337.76.86568Set 4-Grab 11/12/2011151136.96.8Table D4-2. Field Measurementsfor Sample Collection at the Influent to the Bioreactor System,AllenEpisode NumberSample CollectionNumberDate of SampleCollectionSample CollectionTimeTemperature(°C)pH(S.U.)6568Set 1 - Grab 1 10/4/2010112829.96.76568Set 1-Grab 210/4/2010172631.06.76568Set 1-Grab 310/4/2010233529.16.76568Set 1 - Grab 4 10/5/2010051828.76.66568Set 2 - Grab 1 11/1/2010102623.46.16568Set 2-Grab 211/1/2010163024.16.66568Set 2-Grab 311/1/2010222923.86.96568Set 2 - Grab 4 11/2/2010043023.96.66568Set 3 - Grab 1 12/6/2010100823.37.36568Set 3-Grab 212/6/2010161223.57.56568Set 3-Grab 312/6/2010220723.07.16568Set 3 - Grab 4 12/7/2010040922.96.76568Set 4 - Grab 1 1/12/2011143923.85.86568Set 4-Grab 21/12/2011204224.06.76568Set 4-Grab 31/13/2011023924.16.66568Set 4 - Grab 4 1/13/2011083724.26.7Table D4-3. Field Measurementsfor Sample Collection at the Effluent from the Bioreactor System,AllenEpisode NumberSample CollectionNumberDate of SampleCollectionSample CollectionTimeTemperature(°C)pH(S.U.)6568Set 1 - Grab 1 10/4/2010125529.27.36568Set 1-Grab 210/4/2010185128.17.46568Set 1-Grab 310/5/2010005228.37.46568Set 1 - Grab 4 10/5/2010064727.27.36568Set 2 - Grab 1 11/1/2010094322.07.36568Set 2-Grab 211/1/2010155322.27.36568Set 2-Grab 311/1/2010215322.17.36568Set 2 - Grab 4 11/2/2010034721.87.36568Set 3 - Grab 1 12/6/2010092519.86.96568Set 3-Grab 212/6/2010152720.27.06568Set 3-Grab 312/6/2010212919.37.16568Set 3 - Grab 4 12/7/2010032719.87.26568Set 4 - Grab 1 1/12/2011140420.16.36568Set 4-Grab 21/12/2011200520.17.26568Set 4-Grab 31/13/2011020721.07.26568Set 4 - Grab 4 1/13/2011080620.07.2Table D4-4. 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 ImpactConcentrations6568 Set 1 Yes YesYesYesNoneNone6568 Set 2 Yes YesYesYesNoneNone6568 Set 3 Yes YesYesYesNoneUnit 3&4 burning IllinoisBasin Coal6568 Set 4 Yes YesYesYesNoneNone* Includes the use of tyveks suits during all sampling events and dust masks during the collection of mercury samples.Table D4-5.Generating Unit Operation at Time of Sampling,AllenEpisode NumberSample CollectionNumberDate of SampleCollectionPlant OperationDuring Sample CollectionUnits OperatingDuring SamplingDayUnits Off-line EntireSampling DaySCRs/SNCRsOperating onUnits6568Set 110/4/10-10/5/10Units3,41,2,5SNCR6568Set 211/1/10-11/2/10Units3,41,2,5SNCR6568Set 3 12/6/10 - 12/7/10 Units 1,2,3,4,5NoneSNCR6568Set 4 1/12/11 - 1/13/11 Units 1,2,3,4,5NoneSNCRTable D4-6. FGD Scrubber Slurry Information at Time of Sampling,AllenEpisodeNumberSampleCollectionNumberDate of SampleCollectionFGDSystemPlant Operation During Sample CollectionScrubber Slurry BlowdownFlow RateScrubberSlurryPercentSolidsPercentHydrocloneOverflow RecycledBack to ScrubberFlow Rate(gpm)Duration6568 Set 1 10/4/10 - 10/5/101URE0 hrs NANA6568Set110/4/10-10/5/103URE13 hrs14-16%0%6568Set 211/1/10-11/2/101URE0 hrsNANA6568 Set 2 11/1/10 - 11/2/103URE8 hrs 14 -16%0%6568 Set 3 12/6/10 - 12/7/101URE7 hrs 14 -16%0%6568Set 312/6/10-12/7/103URE9 hrs14-16%0%6568Set 41/12/11-1/13/111URE11 hrs14-16%0%6568 Set 4 1/12/11 - 1/13/113URE9 hrs 14 -16%0%NA – not applicable.URE – Unable to reasonable estimate.Table D4-7. FGD Wastewater Treatment System Operation Information,AllenEpisodeNumberSampleCollectionNumberDate 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)6568 Set 1 10/4/10 - 10/5/10 3581 38NA203296568 Set 2 11/1/10 - 11/2/10 3511 30NA163296568 Set 3 12/6/10 - 12/7/10 3801 36NA179886568 Set 4 1/12/11 - 1/13/11 3761 55NA20659

### Table D4-8. Daily Power Generation During Sampling Period, Allen

Episode

Number Date Daily Power Generation

(MW-hrs)

Unit 1 Unit 2 

### Unit 3 Unit 4 Unit 5

6568 9/20/2010 3,001 2,896 5,548 5,688 5,402



### 6568 9/21/2010 3,054 2,977 5,755 6,000 5,655

6568 9/22/2010 3,469 3,398 6,338 6,622 6,238

6568 9/23/2010 3,442 3,156 6,233 6,540 6,105

6568 9/24/2010 3,425 2,574 6,296 6,541 6,150



### 6568 9/25/2010 3,149 2,499 5,666 6,092 5,757

6568 9/26/2010 2,641 2,448 5,924 6,352 5,911

6568 9/27/2010 3,328 3,246 6,350 6,580 6,218

6568 9/28/2010 3,384 3,349 6,389 6,414 6,110



### 6568 9/29/2010 521 1,773 4,668 4,890 3,771

6568 9/30/2010 0 2,544 5,229 5,245 5,205

6568 10/1/2010 0 0 6,326 6,624 2,914

6568 10/2/2010 0 0 6,371 5,510 0



### 6568 10/3/2010 0 0 6,226 6,333 0

6568 10/4/2010 0 0 6,457 6,635 0

6568 10/5/2010 0 0 6,355 6,317 0

6568 10/6/2010 0 0 6,349 6,268 0



### 6568 10/7/2010 0 0 7,079 7,056 0

6568 10/8/2010 0 0 6,619 6,613 0

6568 10/9/2010 0 0 3,732 3,948 0

6568 10/10/2010 0 0 4,080 4,083 0



### 6568 10/11/2010 0 0 4,696 5,079 2,794

6568 10/12/2010 0 0 4,174 4,790 3,940

6568 10/13/2010 0 0 4,625 5,223 0

6568 10/14/2010 0 0 3,338 2,492 0



### 6568 10/15/2010 0 0 0 0 0

6568 10/16/2010 0 0 0 0 0

6568 10/17/2010 0 0 0 0 0

6568 10/18/2010 0 0 0 0 0



### 6568 10/19/2010 0 0 0 0 0

6568 10/20/2010 0 0 0 0 0

6568 10/21/2010 0 0 0 0 0

6568 10/22/2010 0 0 0 0 0



### 6568 10/23/2010 0 0 0 0 0

6568 10/24/2010 0 0 0 0 0

6568 10/25/2010 0 0 0 0 0

6568 10/26/2010 0 0 2,287 0 0



### 6568 10/27/2010 0 0 5,009 3,336 0

6568 10/28/2010 0 0 5,227 5,502 0

6568 10/29/2010 0 0 4,043 4,288 0

6568 10/30/2010 0 0 3,616 3,899 0

### Table D4-8. Daily Power Generation During Sampling Period, Allen

Episode

Number Date 

### Daily Pow er Generation

(MW-hrs)



### Unit 1 Unit 2 Unit 3 Unit 4 Unit 5

6568 10/31/2010 0 0 3,360 3,816 0

6568 11/1/2010 0 0 5,969 6,281 0



### 6568 11/2/2010 0 0 6,188 6,194 0

6568 11/3/2010 0 0 5,593 5,694 0

6568 11/4/2010 0 0 6,163 5,545 0

6568 11/5/2010 0 0 5,694 5,802 0



### 6568 11/6/2010 0 0 5,035 5,833 0

6568 11/7/2010 994 660 5,373 6,237 0

6568 11/8/2010 2,850 3,077 4,658 5,810 0

6568 11/9/2010 1,526 1,410 4,854 2,575 0



### 6568 11/10/2010 0 0 0 0 0

6568 11/11/2010 0 0 0 0 0

6568 11/12/2010 0 0 0 0 0

6568 11/13/2010 0 0 0 0 0



### 6568 11/14/2010 0 0 0 0 0

6568 11/15/2010 0 0 0 0 0

6568 11/16/2010 0 0 0 0 11

6568 11/17/2010 0 0 14 4 38



### 6568 11/18/2010 0 0 4,758 5,087 4,719

6568 11/19/2010 0 0 4,963 5,172 5,849

6568 11/20/2010 0 0 5,154 5,393 5,068

6568 11/21/2010 0 0 3,362 3,646 4,853



### 6568 11/22/2010 0 0 0 0 4,062

6568 11/23/2010 0 0 0 0 0

6568 11/24/2010 0 0 0 0 0

6568 11/25/2010 0 0 0 0 0



### 6568 11/26/2010 0 0 0 0 0

6568 11/27/2010 0 0 0 0 0

6568 11/28/2010 0 0 135 0 0

6568 11/29/2010 0 0 6,284 5,500 3,753



### 6568 11/30/2010 0 0 6,513 6,551 3,103

6568 12/1/2010 0 0 6,275 6,368 0

6568 12/2/2010 0 0 6,668 6,875 0

6568 12/3/2010 0 0 7,078 7,082 0



### 6568 12/4/2010 0 0 6,592 6,936 0

6568 12/5/2010 26 58 6,346 6,762 1,441

6568 12/6/2010 3,472 3,401 6,683 6,634 6,800

6568 12/7/2010 4,220 3,868 6,705 4,488 7,076



### 6568 12/8/2010 4,152 3,990 7,077 0 7,072

6568 12/9/2010 3,396 2,596 6,529 0 6,500

6568 12/10/2010 2,828 2,933 5,220 0 5,361

6568 12/11/2010 2,706 158 5,357 0 5,253



### 6568 12/12/2010 37 2,289 4,251 2,863 4,542

### Table D4-8. Daily Power Generation During Sampling Period, Allen

Episode

Number Date 

### Daily Pow er Generation

(MW-hrs)



### Unit 1 Unit 2 Unit 3 Unit 4 Unit 5

6568 12/13/2010 3,690 3,788 6,567 6,553 6,402

6568 12/14/2010 4,345 4,190 6,999 7,080 6,962



### 6568 12/15/2010 4,106 3,936 6,993 7,116 6,167

6568 12/16/2010 4,123 4,024 7,046 7,184 718

6568 12/17/2010 3,457 3,304 6,610 6,686 6,558

6568 12/18/2010 4,107 3,945 7,091 7,244 7,075



### 6568 12/19/2010 2,749 2,439 5,745 6,009 5,511

6568 12/20/2010 3,424 3,204 6,720 6,908 6,682

6568 12/21/2010 2,208 1,993 5,044 5,227 4,861

6568 12/22/2010 0 0 4,125 3,635 4,318



### 6568 12/23/2010 0 0 5,154 5,478 5,276

6568 12/24/2010 0 0 4,248 4,409 4,612

6568 12/25/2010 0 0 3,483 3,948 3,794

6568 12/26/2010 1,241 827 5,837 6,553 5,947



### 6568 12/27/2010 3,104 3,429 6,738 7,008 6,536

6568 12/28/2010 2,644 2,383 5,737 6,160 5,777

6568 12/29/2010 0 0 3,036 6,341 5,669

6568 12/30/2010 0 0 0 5,854 5,216



### 6568 12/31/2010 0 0 0 2,439 4,848

6568 1/1/2011 0 0 0 0 3,935

6568 1/2/2011 0 0 0 0 4,510

6568 1/3/2011 2,668 6 3,517 5,638 6,039



### 6568 1/4/2011 2,888 2,245 6,019 6,050 5,913

6568 1/5/2011 2,837 2,786 6,008 6,351 6,050

6568 1/6/2011 2,402 2,274 5,021 4,946 4,915

6568 1/7/2011 2,330 2,153 5,173 5,083 1,467



### 6568 1/8/2011 3,005 2,797 6,143 5,985 3,826

6568 1/9/2011 3,631 3,447 7,171 7,013 6,888

6568 1/10/2011 3,629 3,371 7,069 6,911 6,749

6568 1/11/2011 3,112 2,916 6,856 6,977 6,207



### 6568 1/12/2011 3,729 3,680 6,473 7,231 6,884

6568 1/13/2011 3,826 4,028 7,110 7,246 7,018

### Table D4-9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Allen

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

6568 9/20/2010 394,755 0 327,041

6568 9/21/2010 406,835 0 317,768



### 6568 9/22/2010 401,508 0 364,620

6568 9/23/2010 370,408 0 295,826

6568 9/24/2010 411,894 0 363,881

6568 9/25/2010 498,120 0 410,783



### 6568 9/26/2010 498,274 0 452,038

6568 9/27/2010 601,574 0 495,121

6568 9/28/2010 533,971 0 545,144

6568 9/29/2010 570,844 0 474,409



### 6568 9/30/2010 482,214 0 412,593

6568 10/1/2010 442,078 0 331,515

6568 10/2/2010 179,125 0 153,032

6568 10/3/2010 269,978 0 211,384



### 6568 10/4/2010 416,434 0 306,375

6568 10/5/2010 345,221 0 231,940

6568 10/6/2010 265,856 0 226,597

6568 10/7/2010 176,693 0 132,938



### 6568 10/8/2010 221,500 0 173,740

6568 10/9/2010 190,709 0 136,145

6568 10/10/2010 169,302 0 93,937

6568 10/11/2010 121,306 0 101,672



### 6568 10/12/2010 259,230 0 179,607

6568 10/13/2010 363,336 0 283,061

6568 10/14/2010 151,931 0 105,415

6568 10/15/2010 141,883 0 82,831



### 6568 10/16/2010 0 0 0

6568 10/17/2010 0 0 0

6568 10/18/2010 0 0 0

6568 10/19/2010 189,361 0 54,434



### 6568 10/20/2010 0 0 0

6568 10/21/2010 0 0 0

6568 10/22/2010 259,968 0 138,028

6568 10/23/2010 323,485 0 218,595



### 6568 10/24/2010 0 0 5,016

6568 10/25/2010 161,237 0 69,142

6568 10/26/2010 99,227 0 80,190

6568 10/27/2010 0 0 0

### Table D4-9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Allen

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



### 6568 10/28/2010 0 0 0

6568 10/29/2010 303,223 0 216,676

6568 10/30/2010 171,894 0 113,845



### 6568 10/31/2010 254,540 0 215,427

6568 11/1/2010 341,589 0 237,183

6568 11/2/2010 353,628 0 262,881

6568 11/3/2010 32,271 0 24,038



### 6568 11/4/2010 292,694 0 193,023

6568 11/5/2010 276,421 0 207,921

6568 11/6/2010 190,455 0 140,688

6568 11/7/2010 153,000 0 81,813



### 6568 11/8/2010 394,354 0 311,834

6568 11/9/2010 140,852 0 102,324

6568 11/10/2010 203,446 0 173,379

6568 11/11/2010 25 0 0



### 6568 11/12/2010 0 0 0

6568 11/13/2010 19,219 0 178

6568 11/14/2010 89,419 0 53,341

6568 11/15/2010 0 0 0



### 6568 11/16/2010 214,076 0 173,217

6568 11/17/2010 0 0 0

6568 11/18/2010 119,364 0 78,151

6568 11/19/2010 199,916 0 139,575



### 6568 11/20/2010 260,326 0 189,335

6568 11/21/2010 401,208 0 220,392

6568 11/22/2010 377,734 0 237,488

6568 11/23/2010 180,120 0 100,020



### 6568 11/24/2010 133,413 0 80,131

6568 11/25/2010 0 0 0

6568 11/26/2010 0 0 0

6568 11/27/2010 124,035 0 94,218



### 6568 11/28/2010 0 0 0

6568 11/29/2010 17,559 0 9,268

6568 11/30/2010 352,713 0 194,895

6568 12/1/2010 358,402 0 246,711



### 6568 12/2/2010 370,869 0 284,436

6568 12/3/2010 341,607 0 243,410

6568 12/4/2010 314,082 0 209,303

6568 12/5/2010 325,374 0 229,708



### 6568 12/6/2010 351,928 0 194,694

### Table D4-9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Allen

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



### 6568 12/7/2010 392,999 0 278,143

6568 12/8/2010 352,677 0 157,463

6568 12/9/2010 331,819 0 249,881



### 6568 12/10/2010 308,580 0 230,573

6568 12/11/2010 308,956 0 225,891

6568 12/12/2010 387,525 0 263,495

6568 12/13/2010 391,199 0 301,453



### 6568 12/14/2010 375,836 0 285,785

6568 12/15/2010 375,311 0 275,071

6568 12/16/2010 388,144 0 232,024

6568 12/17/2010 377,519 0 255,041



### 6568 12/18/2010 448,323 0 321,297

6568 12/19/2010 427,734 0 290,575

6568 12/20/2010 509,617 0 372,818

6568 12/21/2010 486,186 0 229,059



### 6568 12/22/2010 451,479 0 318,963

6568 12/23/2010 409,104 0 251,070

6568 12/24/2010 382,800 0 213,055

6568 12/25/2010 231,392 0 154,139



### 6568 12/26/2010 389,183 0 227,204

6568 12/27/2010 480,374 0 390,018

6568 12/28/2010 386,082 0 257,109

6568 12/29/2010 379,136 0 238,540



### 6568 12/30/2010 330,727 0 251,349

6568 12/31/2010 369,461 0 286,830

6568 1/1/2011 349,544 0 223,944

6568 1/2/2011 139,395 0 78,811



### 6568 1/3/2011 335,072 0 241,903

6568 1/4/2011 358,368 0 268,186

6568 1/5/2011 344,716 0 253,380

6568 1/6/2011 369,418 0 282,493



### 6568 1/7/2011 399,467 0 294,291

6568 1/8/2011 253,736 0 171,222

6568 1/9/2011 407,705 0 300,985

6568 1/10/2011 372,938 0 289,353



### 6568 1/11/2011 378,593 0 272,812

6568 1/12/2011 403,793 0 307,012

6568 1/13/2011 481,009 0 355,707

## Section 5

Analytical Data< - 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 D5-7 through D5-27 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.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.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.MI – Matrix interferences present.Table D5-1. Influent to FGD Wastewater Treatment System, AllenAnalyteUnitsMethodInfluent to FGD Wastewater Treatment System (SP-1)Set 1Set 2Set 3Set 44-SetAverageClassicalsAmmonia mg/L 350.1 1.50 5.10 9.00 B 25.0 10.2Nitrate Nitrite as N mg/L 353.2 51.0 48.0 * 47.0 37.0 45.8Nitrogen, TotalKjeldahl mg/L 351.2 NQ (5.00) B 8.60 15.0 25.0 < 12.8BiochemicalOxygen Demand mg/L 5210B ND (2.00) 7.70 ND (2.00) 4.60 < 3.58Chemical OxygenDemand mg/L 410.4 71.0 160 B 140 180 138Chloride mg/L 300.0 3,800 5,100 3,700 6,800 4,850Sulfate mg/L 300.0 1,500 1,600 2,100 1,400 1,650Cyanide, Total mg/L 4500 CN E NQ (0.100) 0.590 0.110 0.370 < 0.280Total DissolvedSolids mg/L 2540C 12,000 B 13,000 12,000 F 14,000 12,800Total SuspendedSolids mg/L 2540D 3,000 2,600 Est 4,500 4,100 3,550Phosphorus, Total mg/L 365.1 0.180 NQ (0.0500) B NQ (0.0500) B 2.60 B < 0.708< - 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 D5-7 through D5-27 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.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.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.MI – Matrix interferences present.Table D5-1. Influent to FGD Wastewater Treatment System, AllenAnalyteUnitsMethodInfluent to FGD Wastewater Treatment System (SP-1)Set 1Set 2Set 3Set 44-SetAverageTotal MetalsAluminum ug/L 200.7 67,000 B,^ 110,000 B 79,000 4 110,000 B 91,500Antimony ug/L 200.8 12.0 17.0 8.90 13.0 12.7Arsenic ug/L 200.8 150 230 180 200 190Barium ug/L 200.7 920 930 B 830 1,500 1,050Beryllium ug/L 200.7 11.0 15.0 11.0 17.0 13.5Boron ug/L 200.7 110,000 160,000 B 210,000 B,4 100,000 B 145,000Cadmium ug/L 200.8 4.80 6.60 7.10 6.00 6.13Calcium ug/L 200.7 2,000,000 2,400,000 B 1,700,000 4 3,200,000 B 2,330,000Chromium ug/L 200.8 150 230 ^ 210 190 195Cobalt ug/L 200.7 67.0 100 100 100 91.8Copper ug/L 200.8 140 220 200 220 195Ironug/L 200.7 86,000 110,000 B 110,000 4, MI 100,000 102,000Lead ug/L 200.8 110 150 140 140 135Magnesium ug/L 200.7 760,000 940,000 B 990,000 4 990,000 B 920,000Manganese ug/L 200.7 4,000 7,000 B 8,900 4 7,500 B 6,850Mercury ng/L 1631E 36,000 120,000 27,600 49,700 58,300Molybdenum ug/L 200.7 NQ (40.0) 51.0 NQ (40.0) NQ (40.0) < 27.8< - 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 D5-7 through D5-27 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.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.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.MI – Matrix interferences present.Table D5-1. Influent to FGD Wastewater Treatment System, AllenAnalyteUnitsMethodInfluent to FGD Wastewater Treatment System (SP-1)Set 1Set 2Set 3Set 44-SetAverageNickel ug/L 200.8 260 430 350 310 338Selenium ug/L 200.8 1,500 2,300 1,900 1,700 1,850Silver ug/L 200.8 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Sodium ug/L 200.7 45,000 55,000 B 52,000 B 51,000 B 50,800Thallium ug/L 200.8 NQ (2.00) 4.50 4.70 5.20 < 3.85Tinug/L 200.7 NQ (200) NQ (200)NQ (200) NQ (200) NQ (200)Titanium ug/L 200.7 1,300 2,400 B 2,300 2,600 2,150Vanadium ug/L 200.8 150 200 170 200 180Zinc ug/L 200.7 460 480 ^ 460 MI 390 448< - 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 D5-7 through D5-27 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.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.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.MI – Matrix interferences present.Table D5-2. Influent toBioreactor System, AllenAnalyteUnitsMethodInfluent to the Bioreactor System (SP-2)Set 1Set 2Set 3Set 44-SetAverageClassicalsAmmonia mg/L 350.1 5.00 5.20 8.20 B 18.0 9.10Nitrate Nitrite as N mg/L 353.2 39.0 30.0 * 29.0 29.0 31.8Nitrogen, TotalKjeldahl mg/L 351.2 5.10 B 5.80 14.0 4 17.0 10.5Biochemical OxygenDemand mg/L 5210B ND (2.00) ND (2.00) NQ (2.50) 3.90 < 1.79Chemical OxygenDemand mg/L 410.4 100 67.0 B 110 F 190 117Chloride mg/L 300.0 4,400 3,500 4,600 6,600 4,780Sulfate mg/L 300.0 1,500 1,700 1,600 1,500 1,580Cyanide, Total mg/L 4500 CN E NQ (0.100) NQ (0.100) NQ (0.100) F 0.140 < 0.0725Total DissolvedSolids mg/L 2540C 11,000 B 8,300 9,100 13,000 10,400Total SuspendedSolids mg/L 2540D ND (4.00) NQ (4.00) 6.40 4.00 < 3.60Phosphorus, Total mg/L 365.1 ND (0.0500) NQ (0.0500) B NQ (0.0500) B,F 0.0500 B < 0.0313< - 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 D5-7 through D5-27 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.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.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.MI – Matrix interferences present.Table D5-2. Influent toBioreactor System, AllenAnalyteUnitsMethodInfluent to the Bioreactor System (SP-2)Set 1Set 2Set 3Set 44-SetAverageTotal MetalsAluminumug/L 200.7 ND (200) NQ (200)B NQ (200) ND (200) NQ (200)Antimonyug/L 200.8 NQ (2.00) NQ (2.00) 2.00 2.00 < 1.50Arsenicug/L 200.8 NQ (4.00) NQ (4.00)NQ (4.00) NQ (4.00) NQ (4.00)Barium ug/L 200.7 220 95.0 B 200 320 209Berylliumug/L 200.7 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Boronug/L 200.7 69,000 100,000 B 130,000 B,4 85,000 B 96,000Cadmiumug/L 200.8 ND (4.00) ND (4.00)ND (4.00) ND (4.00) ND (4.00)Calcium ug/L 200.7 2,000,000 1,500,000 B 1,800,000 42,800,000B 2,030,000Chromiumug/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) NQ (20.0)NQ (20.0) NQ (20.0) NQ (20.0)Copperug/L 200.8 NQ (4.00) NQ (4.00) 10.0 15.0 < 7.25Ironug/L 200.7 ND (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 200.7 740,000 690,000 B 750,000 B,4 780,000 B 740,000Manganese ug/L 200.7 230 2,200 B 940 2,600 B 1,490Mercury ng/L 1631E 105 330 320 360 279Molybdenum ug/L 200.7 NQ (40.0) NQ (40.0)NQ (40.0) NQ (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 D5-7 through D5-27 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.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.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.MI – Matrix interferences present.Table D5-2. Influent toBioreactor System, AllenAnalyteUnitsMethodInfluent to the Bioreactor System (SP-2)Set 1Set 2Set 3Set 44-SetAverageNickel ug/L 200.8 11.0 50.0 26.0 37.0 31.0Selenium ug/L 200.8 630 100 96.0 69.0 224Silverug/L 200.8 ND (2.00) NQ (2.00)ND (2.00) F ND (2.00) NQ (2.00)Sodium ug/L 200.7 44,000 41,000 B 51,000 47,000 B 45,800Thalliumug/L 200.8 NQ (2.00) NQ (2.00)NQ (2.00) NQ (2.00) NQ (2.00)Tinug/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 ND (10.0) ND (10.0)NQ (10.0) ND (10.0) NQ (10.0)Zincug/L 200.7 ND (40.0) ND (40.0) ^ ND (40.0) ND (40.0) ND (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 D5-7 through D5-27 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.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.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.MI – Matrix interferences present.Table D5-3. Effluent fromBioreactor System, AllenAnalyteUnitsMethodEffluent from the Bioreactor System (SP-3)Set 1Set 2Set 3Set 44-SetAverageClassicalsAmmonia mg/L 350.1 14.0 8.70 13.0 B 18.0 13.4Nitrate Nitrite as N mg/L 353.2 NQ (0.100)NQ (0.100) * NQ (0.100) NQ (0.100) NQ (0.100)Nitrogen, TotalKjeldahl mg/L 351.2 15.0 B,4 12.0 24.0 21.0 18.0Biochemical OxygenDemand mg/L 5210B ND (2.00) ND (2.00)ND (2.00) NQ (2.50) NQ (2.13)Chemical OxygenDemand mg/L 410.4 100 84.0 B 170 170 131Chloride mg/L 300.0 4,500 3,900 4,900 6,300 4,900Sulfate mg/L 300.0 1,500 1,700 1,500 1,600 1,580Cyanide, Total mg/L 4500 CN E 0.120 F NQ (0.100) 0.110 0.120 < 0.100Total DissolvedSolids mg/L 2540C 11,000 B 9,300 10,000 11,000 10,300Total SuspendedSolids mg/L 2540D ND (4.00) ND (4.00)NQ (4.00) NQ (4.00) NQ (4.00)Phosphorus, Total mg/L 365.1 0.170 0.190 B 0.120 B NQ (0.0500) B < 0.126< - 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 D5-7 through D5-27 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.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.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.MI – Matrix interferences present.Table D5-3. Effluent fromBioreactor System, AllenAnalyteUnitsMethodEffluent from the Bioreactor System (SP-3)Set 1Set 2Set 3Set 44-SetAverageTotal MetalsAluminumug/L 200.7 NQ (100) B ND (200)ND (200) ND (200) NQ (175)Antimony ug/L 200.8 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Arsenicug/L 200.8 5.30 NQ (4.00) NQ (4.00) 4.10 < 3.35Barium ug/L 200.7 260 F 130 B 200 250 210Berylliumug/L 200.7 ND (2.00) F ND (2.00) ND (2.00) ND (2.00) ND (2.00)Boron ug/L 200.7 76,000 4 120,000B77,000B 77,000 B 87,500Cadmium ug/L 200.8 ND (4.00) ND (4.00)ND (4.00) ND (4.00) ND (4.00)Calcium ug/L 200.7 2,200,000 4 1,600,000 B 2,100,000 2,600,000 B 2,130,000Chromium ug/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) F ND (20.0)ND (20.0) ND (20.0) ND (20.0)Copper ug/L 200.8 ND (4.00) ND (4.00)ND (4.00) ND (4.00) ND (4.00)Ironug/L 200.7 NQ (200) F 340 870 290 < 400Leadug/L 200.8 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Magnesium ug/L 200.7 740,000 4 820,000 B 650,000 B 740,000 B 738,000Manganese ug/L 200.7 570 F 650 B 1,700 2,000 B 1,230Mercury ng/L 1631E 7.42 8.16 20.2 13.0 12.2Molybdenum ug/L 200.7 NQ (40.0) F NQ (40.0)NQ (40.0) NQ (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 D5-7 through D5-27 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.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.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.MI – Matrix interferences present.Table D5-3. Effluent fromBioreactor System, AllenAnalyteUnitsMethodEffluent from the Bioreactor System (SP-3)Set 1Set 2Set 3Set 44-SetAverageNickelug/L 200.8 ND (4.00) ND (4.00)NQ (4.00) NQ (4.00) NQ (4.00)Selenium ug/L 200.8 NQ (4.00) NQ (4.00)NQ (4.00) ^ NQ (4.00) NQ (4.00)Silverug/L 200.8 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Sodium ug/L 200.7 44,000 F 45,000 B 50,000 44,000 B 45,800Thallium ug/L 200.8 ND (2.00) ND (2.00)ND (2.00) ND (2.00) ND (2.00)Tinug/L 200.7 ND (200) F ND (200)ND (200) ND (200) ND (200)Titaniumug/L 200.7 NQ (20.0) F ND (20.0)NQ (20.0) NQ (20.0) NQ (20.0)Vanadium ug/L 200.8 ND (10.0) ND (10.0)ND (10.0) ND (10.0) ND (10.0)Zincug/L 200.7 ND (40.0) F 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).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 D5-7 through D5-27 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 D5-4. Classical Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment System, AllenAnalyteUnitMethodInfluent to FGDWastewater TreatmentSystem (SP-1)4-Set AverageInfluent toBioreactor System(SP-2)4-Set AverageEffluent fromBioreactor System(SP-3)4-Set AverageClassicalsAmmonia mg/L350.1 10.2 9.10 13.4Nitrate Nitrite as Nmg/L 353.245.831.8NQ (0.100)Nitrogen, Total Kjeldahl mg/L 351.2< 12.810.518.0Biochemical Oxygen Demand mg/L 5210B< 3.58< 1.79NQ (2.13)Chemical Oxygen Demand mg/L 410.4138117131Chloride mg/L300.0 4,850 4,780 4,900Sulfate mg/L300.0 1,650 1,580 1,580Cyanide, Totalmg/L 4500 CN E < 0.280< 0.0725< 0.100Total Dissolved Solids mg/L 2540C12,80010,40010,300Total Suspended Solids mg/L 2540D3,550< 3.60NQ (4.00)Phosphorus, Totalmg/L 365.1< 0.708< 0.0313< 0.126< - 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 D5-7 through D5-27 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 D5-5. Metal Pollutants 4-Set Average DataSummary for FGD Wastewater Treatment System, AllenAnalyteUnitMethodInfluent 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 200.791,500NQ (200)NQ (175)Antimony ug/L 200.812.7< 1.50ND (2.00)Arsenic ug/L 200.8190NQ (4.00)< 3.35Barium ug/L 200.7 1,050209210Beryllium ug/L 200.713.5ND (2.00)ND (2.00)Boron ug/L 200.7 145,000 96,000 87,500Cadmium ug/L 200.86.13ND (4.00)ND (4.00)Calcium ug/L200.7 2,330,000 2,030,000 2,130,000Chromium ug/L 200.8195ND (8.00)ND (8.00)Cobalt ug/L 200.791.8NQ (20.0)ND (20.0)Copper ug/L 200.8195< 7.25ND (4.00)Ironug/L 200.7102,000NQ (200)< 400Leadug/L 200.8135ND (2.00)ND (2.00)Magnesiumug/L200.7 920,000 740,000 738,000Manganeseug/L200.7 6,850 1,490 1,230Mercury ng/L 1631E 58,30027912.2Molybdenum ug/L 200.7< 27.8NQ (40.0)NQ (40.0)Nickel ug/L 200.8 33831.0 NQ (4.00)Selenium ug/L 200.8 1,850224NQ (4.00)Silverug/L 200.8 ND (2.00)NQ (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 D5-7 through D5-27 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 D5-5. Metal Pollutants 4-Set Average DataSummary for FGD Wastewater Treatment System, AllenAnalyteUnitMethodInfluent to FGDWastewater TreatmentSystem (SP-1)4-Set AverageInfluent to BioreactorSystem (SP-2)4-Set AverageEffluent from BioreactorSystem (SP-3)4-Set AverageSodium ug/L200.7 50,800 45,800 45,800Thallium ug/L 200.8< 3.85NQ (2.00)ND (2.00)Tinug/L 200.7NQ (200)ND (200)ND (200)Titanium ug/L 200.72,150NQ (20.0)NQ (20.0)Vanadium ug/L 200.8180NQ (10.0)ND (10.0)Zincug/L 200.7448ND (40.0)NQ (40.0)

### Table D5-6. Field Blank Analytical Results, Allen

Analyte Sample Point Method Unit Concentration

Total Metals

Mercury Influent to Bioreactor System

Field Blank - Set 3 1631E ng/L 0.610

Zinc Influent to Bioreactor System

Field Blank - Set 2 200.7 ug/L 66.0ND – 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 D5-7. Influent to FGD Wastewater Treatment System, Set 1 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L10.05511.5Nitrate Nitrite as N353.2 mg/L 100.191 51Nitrogen, Total Kjeldahl351.2 mg/L 10.385 2.4 J,BBiochemical Oxygen Demand5210B mg/L 10.242 ND (2) UChemical Oxygen Demand410.4 mg/L 28.140 71Chloride 300.0mg/L100253003,800Sulfate 300.0mg/L100235001,500Cyanide, Total4500 CN E mg/L 10.020.1 0.028 JTotal Dissolved Solids2540C mg/L 1160330 12,000 BTotal Suspended Solids2540D mg/L 128100 3,000Phosphorus, Total365.1 mg/L 10.005 0.05 0.18Total MetalsAluminum 200.7ug/L29.420067,000B,^Antimony 200.8ug/L20.72212Arsenic 200.8ug/L21.24150Barium 200.7ug/L22.520920Beryllium 200.7ug/L20.71211Boron 200.7ug/L25083025,000110,000Cadmium 200.8ug/L21.244.8Calcium 200.7ug/L501,70010,0002,000,000Chromium 200.8ug/L23.38150Cobalt 200.7ug/L21.12067ND – 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 D5-7. Influent to FGD Wastewater Treatment System, Set 1 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCopper 200.8ug/L20.964140Iron 200.7ug/L23220086,000Lead 200.8ug/L20.732110Magnesium 200.7ug/L221400760,000Manganese 200.7ug/L20.51204,000Mercury 1631Eng/L4,0009942,08036,000Molybdenum 200.7ug/L21.64029JNickel 200.8ug/L20.894260Selenium 200.8ug/L20.6241,500Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00045,000Thallium 200.8ug/L20.4720.7JTin 200.7ug/L24.82008.5JTitanium 200.7ug/L21.6201,300Vanadium 200.8ug/L21.710150Zinc 200.7ug/L29.140460ND – 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.Est – Estimated value.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 D5-8. Influent to FGD Wastewater Treatment System, Set 2 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L10.05515.1Nitrate Nitrite as N353.2 mg/L 5 0.095 0.5 48 *Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.152 8.6Biochemical Oxygen Demand 5210B mg/L 1 0.32.5 7.7Chemical Oxygen Demand 410.4 mg/L 2 8.140 160 BChloride300.0 mg/L 200 51 600 5,100Sulfate 300.0mg/L50122501,600Cyanide, Total4500 CN E mg/L 1 0.02 0.1 0.59Total Dissolved Solids2540C mg/L 1 47100 13,000Total Suspended Solids 2540D mg/L 1 1140 2,600 EstPhosphorus, Total365.1 mg/L 1 0.005 0.05 0.04 J,BTotal MetalsAluminum 200.7ug/L29.4200110,000BAntimony 200.8ug/L20.72217Arsenic 200.8ug/L53.110230Barium 200.7ug/L22.520930BBeryllium 200.7ug/L20.71215Boron 200.7ug/L501705,000160,000BCadmium 200.8ug/L21.2 46.6Calcium 200.7ug/L501,70010,0002,400,000 BND – 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.Est – Estimated value.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 D5-8. Influent to FGD Wastewater Treatment System, Set 2 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationChromium 200.8ug/L23.3 8230^Cobalt 200.7ug/L21.120100Copper 200.8ug/L20.964220Iron 200.7ug/L232200110,000BLead 200.8ug/L20.732150Magnesium 200.7ug/L2 21 400940,000BManganese 200.7ug/L20.51 207,000BMercury 1631Eng/L5,0001,2402,600120,000Molybdenum 200.7ug/L2 1.6 40 51Nickel 200.8ug/L20.894430Selenium 200.8ug/L20.6242,300Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00055,000BThallium 200.8ug/L20.4724.5Tin 200.7ug/L24.820013JTitanium 200.7ug/L21.6202,400BVanadium 200.8ug/L21.7 10200Zinc 200.7ug/L29.140480^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.F – MS and/or MSD not within laboratory control limits.J – Result measured above the MDL, but less than the quantitation limit.MI – Matrix interferences present.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table D5-9. Influent to FGD Wastewater Treatment System, Set 3 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L10.05519BNitrate Nitrite as N353.2 mg/L 5 0.095 0.5 47Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.152 15Biochemical Oxygen Demand 5210B mg/L 1 0.242 ND (2) UChemical Oxygen Demand 410.4 mg/L 28.140 140Chloride 300.0mg/L100253003,700Sulfate 300.0mg/L100235002,100Cyanide, Total4500 CN E mg/L 1 0.02 0.1 0.11Total Dissolved Solids 2540C mg/L 1 470 1,000 12,000 FTotal Suspended Solids 2540D mg/L 128100 4,500Phosphorus, Total365.1 mg/L 1 0.005 0.05 0.014 J,BTotal MetalsAluminum 200.7ug/L2 9.4 20079,0004Antimony 200.8ug/L20.72 28.9Arsenic 200.8ug/L21.24180Barium 200.7ug/L22.520830Beryllium 200.7ug/L20.71 211Boron 200.7ug/L501705,000210,000B,4Cadmium 200.8ug/L2 1.2 47.1Calcium 200.7ug/L501,70010,0001,700,000 4ND – 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.MI – Matrix interferences present.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table D5-9. Influent to FGD Wastewater Treatment System, Set 3 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationChromium 200.8ug/L2 3.3 8210Cobalt 200.7ug/L21.120100Copper 200.8ug/L20.964200Iron 200.7ug/L232200110,0004,MILead 200.8ug/L20.732140Magnesium 200.7ug/L50 54010,000990,0004Manganese 200.7ug/L50 13 5008,9004Mercury 1631Eng/L4,0009942,08027,600Molybdenum 200.7ug/L2 1.6 40 32JNickel 200.8ug/L20.894350Selenium 200.8ug/L20.6241,900Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00052,000BThallium 200.8ug/L20.4724.7Tin 200.7ug/L24.820010JTitanium 200.7ug/L21.6202,300Vanadium 200.8ug/L2 1.7 10170Zinc 200.7ug/L29.140460MIND – 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 D5-10. Influent to FGD Wastewater Treatment System, Set 4 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L50.27 525Nitrate Nitrite as N353.2 mg/L 10 0.19137Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38525Biochemical Oxygen Demand 5210B mg/L 1 0.32.5 4.6Chemical Oxygen Demand 410.4 mg/L 2 8.140 180Chloride 300.0mg/L200516006,800Sulfate 300.0mg/L50122501,400Cyanide, Total4500 CN E mg/L 1 0.020.1 0.37Total Dissolved Solids 2540C mg/L 1 240500 14,000Total Suspended Solids 2540D mg/L 155200 4,100Phosphorus, Total365.1 mg/L 5 0.025 0.25 2.6 BTotal MetalsAluminum 200.7ug/L2 9.4 200110,000BAntimony 200.8ug/L20.72 2 13Arsenic 200.8ug/L21.24200Barium 200.7ug/L22.5201,500Beryllium 200.7ug/L20.71 2 17Boron 200.7ug/L501705,000100,000BCadmium 200.8ug/L21.2 4 6Calcium200.7 ug/L 50 1,700 10,000 3,200,000 BChromium 200.8ug/L2 3.3 8 190Cobalt 200.7ug/L21.120100ND – 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 D5-10. Influent to FGD Wastewater Treatment System, Set 4 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCopper 200.8ug/L20.964220Iron 200.7ug/L232200100,000Lead 200.8ug/L20.732140Magnesium 200.7ug/L50 540 10,000990,000BManganese 200.7ug/L2 0.51 207,500BMercury 1631Eng/L20,0004,83010,10049,700Molybdenum 200.7ug/L2 1.6 40 37JNickel 200.8ug/L20.894310Selenium 200.8ug/L20.62 41,700Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00051,000BThallium 200.8ug/L20.47 25.2Tin 200.7ug/L24.820011JTitanium 200.7ug/L21.6 202,600Vanadium 200.8ug/L21.7 10200Zinc 200.7ug/L29.140390ND – 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 D5-11. Influent to Bioreactor System, Set 1 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L10.05515Nitrate Nitrite as N353.2 mg/L 10 0.191 39Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.152 5.1 BBiochemical Oxygen Demand 5210B mg/L 1 0.242 ND (2) UChemical Oxygen Demand 410.4 mg/L 2 8.140 100Chloride 300.0mg/L100253004,400Sulfate 300.0mg/L100235001,500Cyanide, Total4500 CN E mg/L 1 0.020.1 0.058 JTotal Dissolved Solids 2540C mg/L 11940 11,000 BTotal Suspended Solids 2540D mg/L 1 1.14 ND (4) UPhosphorus, Total365.1 mg/L 1 0.005 0.05 ND (0.05) UTotal MetalsAluminum 200.7ug/L29.4 200ND(200)UAntimony 200.8ug/L20.72 21.9JArsenic 200.8ug/L21.242.4JBarium 200.7ug/L22.520220Beryllium 200.7ug/L20.71 2ND(2)UBoron 200.7ug/L501705,00069,000Cadmium 200.8ug/L21.2 4ND(4)UCalcium 200.7ug/L501,70010,0002,000,000Chromium 200.8ug/L23.3 8ND(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 D5-11. Influent to Bioreactor System, Set 1 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCopper 200.8ug/L20.9641.1JIron 200.7ug/L232200ND(200)ULead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L2 21 400740,000Manganese 200.7ug/L20.51 20230Mercury 1631Eng/L10024.150.5105Molybdenum 200.7ug/L2 1.6 40 14JNickel 200.8ug/L20.89411Selenium 200.8ug/L20.624630Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00044,000Thallium 200.8ug/L20.4721.1JTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.6202.3JVanadium 200.8ug/L21.7 10ND(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 D5-12. Influent to Bioreactor System, Set 2 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L10.05515.2Nitrate Nitrite as N353.2 mg/L 5 0.095 0.5 30 *Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.0771 5.8Biochemical Oxygen Demand 5210B mg/L 1 0.242 ND (2) UChemical Oxygen Demand 410.4 mg/L 28.140 67 BChloride 300.0mg/L200516003,500Sulfate 300.0mg/L50122501,700Cyanide, Total4500 CN E mg/L 1 0.020.1 0.053 JTotal Dissolved Solids2540C mg/L 147100 8,300Total Suspended Solids 2540D mg/L 11.142 JPhosphorus, Total365.1 mg/L 1 0.005 0.05 0.02 J,BTotal MetalsAluminum 200.7ug/L2 9.4 20037J,BAntimony 200.8ug/L20.72 21.9JArsenic 200.8ug/L21.241.6JBarium 200.7ug/L22.52095BBeryllium 200.7ug/L20.71 2ND(2)UBoron 200.7ug/L501705,000100,000BCadmium 200.8ug/L21.2 4ND(4)UCalcium 200.7ug/L501,70010,0001,500,000 BChromium 200.8ug/L2 3.3 8ND(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 D5-12. Influent to Bioreactor System, Set 2 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCobalt 200.7ug/L21.1204.5JCopper 200.8ug/L20.9642JIron 200.7ug/L23220066J,BLead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L2 21 400690,000BManganese 200.7ug/L20.51 202,200BMercury 1631Eng/L10024.150.5330Molybdenum 200.7ug/L2 1.6 40 22JNickel 200.8ug/L20.89450Selenium 200.8ug/L20.624100Silver 200.8ug/L20.5920.99JSodium 200.7ug/L218010,00041,000BThallium 200.8ug/L20.4721.2JTin200.7 ug/L 2 4.8 200 ND (200) UTitanium 200.7ug/L21.6203.4J,BVanadium 200.8ug/L21.7 10ND(10)UZinc 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.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 D5-13. Influent to Bioreactor System, Set 3 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L10.055 18.2BNitrate Nitrite as N353.2 mg/L 10 0.191 29Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.152 14 4Biochemical Oxygen Demand 5210B mg/L 10.32.5 2.3 JChemical Oxygen Demand 410.4 mg/L 28.140 110 FChloride 300.0mg/L100253004,600Sulfate 300.0mg/L100235001,600Cyanide, Total4500 CN E mg/L 1 0.020.1 0.092 J,FTotal Dissolved Solids 2540C mg/L 147100 9,100Total Suspended Solids 2540D mg/L 11.14 6.4Phosphorus, Total365.1 mg/L 1 0.005 0.05 0.022 J,B,FTotal MetalsAluminum 200.7ug/L2 9.4 20051JAntimony 200.8ug/L20.72 2 2Arsenic 200.8ug/L21.241.9JBarium 200.7ug/L22.520200Beryllium 200.7ug/L20.71 2ND(2)UBoron 200.7ug/L501705,000130,000B,4Cadmium 200.8ug/L21.2 4ND(4)UCalcium 200.7ug/L501,70010,0001,800,000 4Chromium 200.8ug/L2 3.3 8ND(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 D5-13. Influent to Bioreactor System, Set 3 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCobalt 200.7ug/L21.1203JCopper 200.8ug/L20.96410Iron 200.7ug/L23220093JLead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L50 540 10,000750,000B,4Manganese 200.7ug/L2 0.51 20940Mercury 1631Eng/L10024.150.5320Molybdenum 200.7ug/L2 1.6 40 19JNickel 200.8ug/L20.89426Selenium 200.8ug/L20.62 496Silver 200.8ug/L20.592ND(2)U,FSodium 200.7ug/L218010,00051,000Thallium 200.8ug/L20.47 21.8JTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.6 206.7JVanadium 200.8ug/L21.7 102.5JZinc 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 D5-14. Influent to Bioreactor System, Set 4 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L50.27 518Nitrate Nitrite as N353.2 mg/L 5 0.095 0.5 29Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.385 17Biochemical Oxygen Demand 5210B mg/L 10.32.5 3.9Chemical Oxygen Demand 410.4 mg/L 28.140 190Chloride 300.0mg/L200516006,600Sulfate 300.0mg/L200461,0001,500Cyanide, Total4500 CN E mg/L 1 0.020.1 0.14Total Dissolved Solids2540C mg/L 147100 13,000Total Suspended Solids 2540D mg/L 11.14 4Phosphorus, Total365.1 mg/L 1 0.005 0.05 0.05 BTotal MetalsAluminum 200.7ug/L2 9.4 200ND(200)UAntimony 200.8ug/L20.72 22Arsenic 200.8ug/L21.242.4JBarium 200.7ug/L22.520320Beryllium 200.7ug/L20.71 2ND(2)UBoron 200.7ug/L501705,00085,000BCadmium 200.8ug/L21.2 4ND(4)UCalcium 200.7ug/L501,70010,0002,800,000 BChromium 200.8ug/L2 3.3 8ND(8)UCobalt 200.7ug/L21.1205JND – 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 D5-14. Influent to Bioreactor System, Set 4 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCopper 200.8ug/L20.96415Iron 200.7ug/L23220098JLead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L2 21 400780,000BManganese 200.7ug/L2 0.51 202,600BMercury 1631Eng/L10024.150.5360Molybdenum 200.7ug/L2 1.6 40 19JNickel 200.8ug/L20.89437Selenium 200.8ug/L20.62469Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00047,000BThallium 200.8ug/L20.4721.6JTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.6209.7JVanadium 200.8ug/L21.7 10ND(10)UZinc 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 D5-15. Effluent fromBioreactor System, Set 1Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L20.11214Nitrate Nitrite as N353.2 mg/L 1 0.019 0.1 0.099 JNitrogen, Total Kjeldahl 351.2 mg/L 2 0.152 15 B,4Biochemical Oxygen Demand 5210B mg/L 1 0.242 ND (2) UChemical Oxygen Demand 410.4 mg/L 28.140 100Chloride 300.0mg/L100253004,500Sulfate 300.0mg/L100235001,500Cyanide, Total4500 CN E mg/L 1 0.020.1 0.12 FTotal Dissolved Solids2540C mg/L 11940 11,000 BTotal Suspended Solids2540D mg/L 11.14 ND (4) UPhosphorus, Total365.1 mg/L 1 0.005 0.05 0.17Total MetalsAluminum 200.7ug/L14.710019J,BAntimony 200.8ug/L20.722ND(2)UArsenic 200.8ug/L21.245.3Barium 200.7ug/L22.520260FBeryllium 200.7ug/L20.712ND(2)U,FBoron 200.7ug/L501705,00076,0004Cadmium 200.8ug/L21.24ND(4)UCalcium 200.7ug/L501,70010,0002,200,000 4Chromium 200.8ug/L23.3 8ND(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 D5-15. Effluent fromBioreactor System, Set 1Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCobalt 200.7ug/L21.120ND(20)U,FCopper 200.8ug/L20.964ND(4)UIron 200.7ug/L232200170J,FLead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L2 21 400740,0004Manganese 200.7ug/L20.51 20570FMercury 1631Eng/L10.240.57.42Molybdenum 200.7ug/L2 1.6 4037J,FNickel 200.8ug/L20.894ND(4)USelenium 200.8ug/L20.6242JSilver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00044,000FThallium 200.8ug/L20.472ND(2)UTin 200.7ug/L24.8200ND(200)U,FTitanium 200.7ug/L21.6202.2J,FVanadium 200.8ug/L21.710ND(10)UZinc 200.7ug/L29.140ND(40)U,FND – 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 D5-16. Effluent fromBioreactor System, Set 2Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L10.05518.7Nitrate Nitrite as N353.2 mg/L 1 0.019 0.1 0.062 J,*Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.152 12Biochemical Oxygen Demand 5210B mg/L 1 0.242 ND (2) UChemical Oxygen Demand 410.4 mg/L 2 8.140 84 BChloride 300.0mg/L200516003,900Sulfate 300.0mg/L50122501,700Cyanide, Total4500 CN E mg/L 1 0.02 0.1 0.061 JTotal Dissolved Solids2540C mg/L 1 47100 9,300Total Suspended Solids 2540D mg/L 1 1.14 ND (4) UPhosphorus, Total365.1 mg/L 1 0.005 0.05 0.19 BTotal MetalsAluminum 200.7ug/L29.4200ND(200)UAntimony 200.8ug/L20.722ND(2)UArsenic 200.8ug/L21.242.9JBarium 200.7ug/L22.520130BBeryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L501705,000120,000BCadmium 200.8ug/L21.24ND(4)UCalcium 200.7ug/L501,70010,0001,600,000 BChromium 200.8ug/L23.3 8ND(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 D5-16. Effluent fromBioreactor System, Set 2Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCobalt 200.7ug/L21.120ND(20)UCopper 200.8ug/L20.964ND(4)UIron 200.7ug/L232200340Lead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L2 21 400820,000BManganese 200.7ug/L20.51 20650BMercury 1631Eng/L10.240.58.16Molybdenum 200.7ug/L2 1.6 40 35JNickel 200.8ug/L20.894ND(4)USelenium 200.8ug/L20.6240.98JSilver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00045,000BThallium 200.8ug/L20.472ND(2)UTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.620ND(20)UVanadium 200.8ug/L21.710ND(10)UZinc 200.7ug/L29.1409.3J,^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.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 D5-17. Effluent fromBioreactor System, Set 3Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L20.11 213BNitrate Nitrite as N353.2 mg/L 1 0.019 0.1 0.092 JNitrogen, Total Kjeldahl 351.2 mg/L 5 0.385 24Biochemical Oxygen Demand 5210B mg/L 1 0.242 ND (2) UChemical Oxygen Demand 410.4 mg/L 28.140 170Chloride 300.0mg/L100253004,900Sulfate 300.0mg/L100235001,500Cyanide, Total4500 CN E mg/L 1 0.020.1 0.11Total Dissolved Solids 2540C mg/L 147100 10,000Total Suspended Solids 2540D mg/L 11.14 2.4 JPhosphorus, Total365.1 mg/L 1 0.005 0.05 0.12 BTotal MetalsAluminum 200.7ug/L2 9.4 200ND(200)UAntimony 200.8ug/L20.72 2ND(2)UArsenic 200.8ug/L21.242JBarium 200.7ug/L22.520200Beryllium 200.7ug/L20.71 2ND(2)UBoron 200.7ug/L501705,00077,000BCadmium 200.8ug/L2 1.2 4ND(4)UCalcium 200.7ug/L501,70010,0002,100,000Chromium 200.8ug/L2 3.3 8ND(8)UCobalt 200.7ug/L21.120ND(20)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 D5-17. Effluent fromBioreactor System, Set 3Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCopper 200.8ug/L20.964ND(4)UIron 200.7ug/L232200870Lead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L50 540 10,000650,000BManganese 200.7ug/L2 0.51 201,700Mercury 1631Eng/L204.8310.120.2Molybdenum 200.7ug/L2 1.6 40 18JNickel 200.8ug/L20.8941.6JSelenium 200.8ug/L20.62 41.6J,^Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00050,000Thallium 200.8ug/L20.47 2ND(2)UTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.6 205JVanadium 200.8ug/L2 1.7 10ND(10)UZinc 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 D5-18. Effluent fromBioreactor System, Set 4Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L50.27 518Nitrate Nitrite as N353.2 mg/L 1 0.019 0.1 0.065 JNitrogen, Total Kjeldahl 351.2 mg/L 5 0.385 21Biochemical Oxygen Demand 5210B mg/L 10.32.5 1.7 JChemical Oxygen Demand 410.4 mg/L 28.140 170Chloride 300.0mg/L200516006,300Sulfate 300.0mg/L200461,0001,600Cyanide, Total4500 CN E mg/L 1 0.020.1 0.12Total Dissolved Solids2540C mg/L 147100 11,000Total Suspended Solids 2540D mg/L 11.14 3.6 JPhosphorus, Total365.1 mg/L 1 0.005 0.05 0.041 J,BTotal MetalsAluminum 200.7ug/L2 9.4 200ND(200)UAntimony 200.8ug/L20.72 2ND(2)UArsenic 200.8ug/L21.244.1Barium 200.7ug/L22.520250Beryllium 200.7ug/L20.71 2ND(2)UBoron 200.7ug/L501705,00077,000BCadmium 200.8ug/L21.2 4ND(4)UCalcium 200.7ug/L501,70010,0002,600,000 BChromium 200.8ug/L2 3.3 8ND(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 D5-18. Effluent fromBioreactor System, Set 4Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCopper 200.8ug/L20.964ND(4)UIron 200.7ug/L232200290Lead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L2 21 400740,000BManganese 200.7ug/L2 0.51 202,000BMercury 1631Eng/L10.240.513Molybdenum 200.7ug/L2 1.6 40 24JNickel 200.8ug/L20.8942.1JSelenium 200.8ug/L20.6241.7JSilver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00044,000BThallium 200.8ug/L20.472ND(2)UTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.6208.2JVanadium 200.8ug/L21.7 10ND(10)UZinc 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.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 D5-19. Influent to FGD Wastewater Treatment System Field Blank, Set 1 AnalyticalResults, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) U,^Antimony 200.8 ug/L 2 0.72 2 ND (2) UArsenic 200.8 ug/L 2 1.2 4 ND (4) UBarium 200.7 ug/L 2 2.5 20 3.5 JBeryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 2 6.7 200 12 JCadmium 200.8 ug/L 2 1.2 4 ND (4) UCalcium 200.7 ug/L 2 69 400 ND (400) UChromium 200.8 ug/L 2 3.3 8 ND (8) UCobalt 200.7 ug/L 2 1.1 20 ND(20) UCopper 200.8 ug/L 2 0.96 4 ND(4) UIron 200.7 ug/L 2 32 200 57 JLead 200.8 ug/L 2 0.73 2 ND(2) UMagnesium 200.7 ug/L 2 21 400 ND (400) UManganese 200.7 ug/L 2 0.51 20 ND (20) UMercury 1631E ng/L 1 0.24 0.5 ND (0.5) UMolybdenum 200.7 ug/L 2 1.6 40 ND (40) UNickel 200.8 ug/L 2 0.89 4 ND(4) USelenium 200.8 ug/L 2 0.62 4 ND (4) USilver 200.8 ug/L 2 0.59 2 ND(2) USodium 200.7 ug/L 2 180 10,000 ND (10,000) 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.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 D5-19. Influent to FGD Wastewater Treatment System Field Blank, Set 1 AnalyticalResults, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationThallium 200.8 ug/L 2 0.47 2 ND (2) UTin 200.7ug/L 2 4.8 200 ND(200)UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 ND (10) UZinc 200.7 ug/L 2 9.1 40 ND(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 D5-20. Influent to Bioreactor System Field Blank, Set 1 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) UAntimony 200.8 ug/L 2 0.72 2 ND (2) UArsenic 200.8 ug/L 2 1.2 4 ND (4) UBarium 200.7 ug/L 2 2.5 20 ND (20) UBeryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 2 6.7 200 160 JCadmium 200.8 ug/L 2 1.2 4 ND (4) UCalcium 200.7 ug/L 2 69 400 ND (400) UChromium 200.8 ug/L 2 3.3 8 ND (8) UCobalt 200.7 ug/L 2 1.1 20 ND (20) UCopper 200.8 ug/L 2 0.96 4 2.1 JIron 200.7 ug/L 2 32 200 ND(200) ULead 200.8 ug/L 2 0.73 2 ND(2) UMagnesium 200.7 ug/L 2 21 400 ND (400) UManganese 200.7 ug/L 2 0.51 20 ND (20) UMercury 1631E ng/L 1 0.24 0.5 ND (0.5) UMolybdenum 200.7 ug/L 2 1.6 40 ND (40) UNickel 200.8 ug/L 2 0.89 4 ND (4) USelenium 200.8 ug/L 2 0.62 4 ND (4) USilver 200.8 ug/L 2 0.59 2 ND(2) USodium 200.7 ug/L 2 180 10,000 ND (10,000) UThallium 200.8 ug/L 2 0.47 2 ND (2) UTin 200.7 ug/L 2 4.8 200 ND(200) 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 D5-20. Influent to Bioreactor System Field Blank, Set 1 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 ND (10) UZinc 200.7 ug/L 2 9.1 40 9.2 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 D5-21. Influent to Bioreactor System Field Blank, Set 2 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 13 J,BAntimony 200.8 ug/L 2 0.72 2 ND (2) UArsenic 200.8 ug/L 2 1.2 4 ND(4) UBarium 200.7 ug/L 2 2.5 20 ND(20) UBeryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 2 6.7 200 40 J,BCadmium 200.8 ug/L 2 1.2 4 ND (4) UCalcium 200.7 ug/L 2 69 400 79 J,BChromium 200.8 ug/L 2 3.3 8 ND (8) U,^Cobalt 200.7 ug/L 2 1.1 20 ND(20) UCopper 200.8 ug/L 2 0.96 4 ND (4) UIron 200.7ug/L 2 32 200 ND(200) ULead 200.8 ug/L 2 0.73 2 ND (2) UMagnesium 200.7 ug/L 2 21 400 100 J,BManganese 200.7 ug/L 2 0.51 20 1.5 J,BMercury 1631E ng/L 1 0.24 0.5 ND (0.5) UMolybdenum 200.7 ug/L 2 1.6 40 ND (40) UNickel 200.8 ug/L 2 0.89 4 ND (4) USelenium 200.8 ug/L 2 0.62 4 ND (4) USilver 200.8 ug/L 2 0.59 2 ND (2) USodium 200.7 ug/L 2 180 10,000 ND(10,000) UThallium 200.8 ug/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 D5-21. Influent to Bioreactor System Field Blank, Set 2 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTin 200.7ug/L 2 4.8 200 ND(200)UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 1.9 JZinc 200.7 ug/L 2 9.1 40 66 ^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.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 D5-22. Influent to Bioreactor System Field Blank, Set 3 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) UAntimony 200.8 ug/L 2 0.72 2 ND (2) UArsenic 200.8 ug/L 2 1.2 4 ND (4) UBarium 200.7 ug/L 2 2.5 20 ND (20) UBeryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 2 6.7 200 110 J,BCadmium 200.8 ug/L 2 1.2 4 ND (4) UCalcium 200.7 ug/L 2 69 400 130 JChromium 200.8 ug/L 2 3.3 8 ND (8) UCobalt 200.7 ug/L 2 1.1 20 ND (20) UCopper 200.8 ug/L 2 0.96 4 ND (4) UIron 200.7 ug/L 2 32 200 ND(200) ULead 200.8 ug/L 2 0.73 2 ND(2) UMagnesium 200.7 ug/L 2 21 400 32 J,BManganese 200.7 ug/L 2 0.51 20 ND (20) UMercury 1631E ng/L 1 0.24 0.5 0.61Molybdenum 200.7 ug/L 2 1.6 40 ND (40) UNickel 200.8 ug/L 2 0.89 4 ND (4) USelenium 200.8 ug/L 2 0.62 4 ND (4) U,^Silver 200.8 ug/L 2 0.59 2 ND(2) USodium 200.7 ug/L 2 180 10,000 270 JThallium 200.8 ug/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 D5-22. Influent to Bioreactor System Field Blank, Set 3 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTin 200.7 ug/L 2 4.8 200 ND(200) UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 ND (10) UZinc 200.7 ug/L 2 9.1 40 ND(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 D5-23. Influent to Bioreactor System Field Blank, Set 4 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND(200) UAntimony 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 20 ND(20)UBeryllium 200.7ug/L 2 0.71 2 ND(2) UBoron 200.7ug/L 2 6.7 200 29J,BCadmium 200.8ug/L 2 1.2 4 ND(4) UCalcium 200.7ug/L 2 69 400 86 J,BChromium 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 200ND(200)ULead 200.8ug/L 2 0.73 2 ND(2)UMagnesium 200.7 ug/L 2 21 400 25 J,BManganese 200.7 ug/L 2 0.51 20 ND(20) UMercury 1631Eng/L 1 0.24 0.5 0.38 JMolybdenum 200.7 ug/L 2 1.6 40 ND(40) UNickel 200.8ug/L 2 0.89 4 ND(4)USelenium 200.8ug/L 2 0.62 4 ND(4) USilver 200.8ug/L 2 0.59 2 ND(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).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 D5-23. Influent to Bioreactor System Field Blank, Set 4 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTin 200.7ug/L 2 4.8 200ND(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 2 9.1 40 ND(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 D5-24. Effluent from Bioreactor System Field Blank, Set 1 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND(200) UAntimony 200.8 ug/L 2 0.72 2 ND(2) UArsenic 200.8 ug/L 2 1.2 4 ND(4) UBarium 200.7 ug/L 2 2.5 20 ND(20) UBeryllium 200.7 ug/L 2 0.71 2 ND(2) UBoron 200.7ug/L 2 6.7 200 110 JCadmium 200.8 ug/L 2 1.2 4 ND(4) UCalcium 200.7 ug/L 2 69 400 ND(400) UChromium 200.8 ug/L 2 3.3 8 ND(8) UCobalt 200.7ug/L 2 1.1 20 ND(20) UCopper 200.8 ug/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 ND (400) UManganese 200.7 ug/L 2 0.51 20 ND (20) UMercury 1631E ng/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 200.7 ug/L 2 180 10,000 ND(10,000) UThallium 200.8 ug/L 2 0.47 2 ND(2) UTin 200.7ug/L 2 4.8 200 ND(200)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 D5-24. Effluent from Bioreactor System Field Blank, Set 1 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTitanium 200.7 ug/L 2 1.6 20 ND(20) UVanadium 200.8 ug/L 2 1.7 10 ND(10) UZinc 200.7ug/L 2 9.1 40 9.3 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 D5-25. Effluent from Bioreactor System Field Blank, Set 2 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) UAntimony 200.8 ug/L 2 0.72 2 ND(2) UArsenic 200.8 ug/L 2 1.2 4 ND(4) UBarium 200.7 ug/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 18 J,BCadmium 200.8 ug/L 2 1.2 4 ND(4) UCalcium 200.7 ug/L 2 69 400 ND(400) UChromium 200.8 ug/L 2 3.3 8 ND (8) U,^Cobalt 200.7ug/L 2 1.1 20 ND(20) UCopper 200.8 ug/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 51 J,BManganese 200.7 ug/L 2 0.51 20 0.9 J,BMercury 1631E ng/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 200.7 ug/L 2 180 10,000 ND(10,000) UThallium 200.8 ug/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 D5-25. Effluent from Bioreactor System Field Blank, Set 2 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTin 200.7ug/L2 4.8 200 ND(200)UTitanium 200.7 ug/L 2 1.6 20 ND(20) UVanadium 200.8 ug/L 2 1.7 10 2 JZinc 200.7ug/L 2 9.1 40 ND(40)U,^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.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 D5-26. Effluent from Bioreactor System Field Blank, Set 3 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) UAntimony 200.8 ug/L 2 0.72 2 ND (2) UArsenic 200.8 ug/L 2 1.2 4 ND(4) UBarium 200.7 ug/L 2 2.5 20 ND(20) UBeryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 2 6.7 200 77 J,BCadmium 200.8 ug/L 2 1.2 4 ND (4) UCalcium 200.7 ug/L 2 69 400 ND(400) UChromium 200.8 ug/L 2 3.3 8 ND (8) UCobalt 200.7 ug/L 2 1.1 20 ND(20) UCopper 200.8 ug/L 2 0.96 4 ND(4) UIron 200.7ug/L 2 32 200 ND(200) ULead 200.8 ug/L 2 0.73 2 ND(2)UMagnesium 200.7 ug/L 2 21 400 ND (400) UManganese 200.7 ug/L 2 0.51 20 ND (20) UMercury 1631E ng/L 1 0.24 0.5 0.25 JMolybdenum 200.7 ug/L 2 1.6 40 ND (40) UNickel 200.8 ug/L 2 0.89 4 ND(4) USelenium 200.8 ug/L 2 0.62 4 ND (4) U,^Silver 200.8 ug/L 2 0.59 2 ND(2) USodium 200.7 ug/L 2 180 10,000 230 JThallium 200.8 ug/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 D5-26. Effluent from Bioreactor System Field Blank, Set 3 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTin 200.7ug/L 2 4.8 200 ND(200) UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 1.7 JZinc 200.7ug/L 2 9.1 40 ND(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 D5-27. Effluent from Bioreactor System Field Blank, Set 4 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) UAntimony 200.8 ug/L 2 0.72 2 ND (2) UArsenic 200.8 ug/L 2 1.2 4 ND (4) UBarium 200.7 ug/L 2 2.5 20 ND(20) UBeryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 2 6.7 200 26 J,BCadmium 200.8 ug/L 2 1.2 4 ND (4) UCalcium 200.7 ug/L 2 69 400 ND (400) UChromium 200.8 ug/L 2 3.3 8 ND (8) UCobalt 200.7 ug/L 2 1.1 20 ND(20) UCopper 200.8 ug/L 2 0.96 4 ND(4) UIron 200.7ug/L 2 32 200 ND(200) ULead 200.8 ug/L 2 0.73 2 ND(2) UMagnesium 200.7 ug/L 2 21 400 ND (400) UManganese 200.7 ug/L 2 0.51 20 ND (20) UMercury 1631E ng/L 1 0.24 0.5 ND (0.5) UMolybdenum 200.7 ug/L 2 1.6 40 ND (40) UNickel 200.8 ug/L 2 0.89 4 ND(4) USelenium 200.8 ug/L 2 0.62 4 ND (4) USilver 200.8 ug/L 2 0.59 2 ND(2) USodium 200.7 ug/L 2 180 10,000 ND (10,000) 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 D5-27. Effluent from Bioreactor System Field Blank, Set 4 Analytical Results, AllenAnalyteMethodUnitDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationThallium 200.8 ug/L 2 0.47 2 ND (2) UTin 200.7ug/L 2 4.8 200 ND(200) UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 ND (10) UZinc 200.7 ug/L 2 9.1 40 ND(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 XXX 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:2600

mg/L Dup: 2920

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: 2 mg/L

Dup: 2.4 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 110,000 μ g/L

72143 Zinc (total) Matrix

Interference PDS and SD Failed 460 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