# Appendix K

Appalachian Power Company’s Mountaineer Plant

# 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 colle cting are very important. The samples will be used by the

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

guidelines and standards for the Steam Electric Power Generating Industry.

These instructions are bei ng provided to Appalachian Po wer Company’s Mountaineer

Plant to aid in collecting, packaging, and sh ipping samples for this sampling program.

The plant must collect grab samples for a ll analytes at the untreated carbon capture

wastewater sampling point a nd 24-hour composite sample s for all analytes except

mercury and cyanide at the carbon capture wast ewater treatment effl uent sampling point,

if the plant treats the carbon cap ture wastewater on site. If the plant does not treat the

carbon capture wastewater on site, the pl ant must provide the name of the

company/facility that treats the carbon captu re wastewater and provi de a description of

the wastewater treatment system used at the facility to treat the carbon capture

wastewater. At the carbon capture wastewat er treatment effluent sampling point, the

plant must collect cyanide as a single grab sa mple and mercury must be collected as four

individual grab samples over the 24-hour peri od (i.e., a grab sample collected every six

hours).

Samples must be collected Monday through T hursday during the week of November 29,

2010. If the plant has any questions regarding the timeline or the steps provided, please

contact Mr. Ronald Jordan at ( 202) 566-1003 or jordan.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 (specially-cleaned

according to EPA Method 1669);

• Automatic compositor;

• Powder-free gloves;

• Tyvek® coveralls or su itable alternative;

• Dust masks (for use while collecting mercury samples)

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

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

• Coolers;

• Garbage bags;

• Packing material;

• Strapping tape; and

• Traffic Report (will be provided by ERG).

# Sampling Points

The plant must collect samples Monday thr ough Thursday during the week of November

29, 2010 from each of the two sampling points specified below. The following is a

description of the two sampling points:

• 

# Untreated Carbon Capture Wastewater (SP-1) : This sampling point(s) shall

represent the untreated ca rbon capture wastewater generated from the carbon

capture process prior to a ny dilution from other waste streams or any chemical

addition for treatment.

• 

# Carbon Capture Wastewater Treatment Effluent (SP-2) : This sampling point

shall represent the effluent from the car bon capture wastewater treatment system,

if the carbon capture wastewater is tr eated on site. The sample should be

collected prior to any commingling with ot her process wastewaters. (NOTE: This

effluent sample should only be collected if the wastewater treatment system is

located on site and the treatment syst em is treating only the carbon capture

wastewater.

The plant must contact Mr. Ronald Jordan at (202) 566-1003, to di scuss all sources of

carbon capture wastewater gene ration, the carbon capture wa stewater treatment system,

and the potential sample collection points in the process.

Analytes

Table 1 contains the listing of all the analytes included in this sampling program, as well

as the analytical methods that EPA will use to analyze the samples.

# Table 1. Analytes and Anal ytical Methods Included in the Sampling 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, ch romium, copper, lead, nickel,

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

cell

Aluminum, barium, beryllium, boron, calcium, cobalt, iron,

magnesium, manganese, molybdenum, sodium, tin, titanium, and

zinc EPA 200.7



# Sample Bottles and Preservation

Table 2 identifies the sample bottles that ar e needed for collecting samples. The table

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

the number of sample bottles listed in Table 2 refers to 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 pres erve the samples with sulfuric acid after

sample collection, or the plant can orde r pre-preserved 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 pr esence of chlorine). If sulfide is present,

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

by the lead acetate paper. If chlorine is pr esent, then the plant w ill need to add sodium

arsenite until the chlorine is not detected by the potassium iodi de starch paper. After any

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

sample with sodium hydroxide until the samp le 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

the carbon capture wastewater treatment

effluent Four 125-mL glass

bottles

Untreated carbon capture wastewater

samples and field blank samples Two 250-mL glass

bottles None

(acid preserve at laboratory)

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

(b) Group II includes ammonia as nitrogen, COD, nitr ate/nitrite 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 it can be identified by the laboratory.

Each self-adhesive label must be complete d 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 plan t must revise the labe l using indelible ink.

Once applied to the sample container, the plan t must cover the labels with clear tape to

prevent tampering, abrasion, smearing, or loss during transit. For metals and mercury

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

contamination. Instead, place the label on the ou ter plastic bag of the sample bottle. To

# ensure that the sample label does not b ecome separated from the bottle, the doublebagged sample bottle should be placed in an additional Ziploc bag after collection.

Please note however, that the labels can be placed directly on the metals and mercury

sample bottles ONLY IF they are placed directly on the bottles in a clean laboratory

environment. HOWEVER, any revisions to the labels by the plant must be made on a

label placed on the outer plastic bag for the double-bagged sample bottle, and the changes

noted in the traffic report.

Table 3 provides the sampling point descrip tions, sample numbers, and sampling episode

number for the plant for this monitoring program. NOTE: if multiple untreated carbon

capture wastewater streams are identified, EPA will need to provide additional sample

numbers. The information in the table shoul d be provided on the sample bottle labels for

the appropriate bottles. The “an alysis to be performed” should be shown on the label as

the following, 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 untreated carbon capture wastewater and field blank

samples); and

• Total Mercury – Grab 1 (for carbon captu re wastewater treatment effluent

laboratory composite samples. The bo ttles should be labeled as Grab 1,

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

The “sample bottle type” should be shown on the label the 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 bottle type” should be “250-mL

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

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

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

bottles.

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

Sampling Point Description Sample

Number Sampling Episode

Number

Untreated Carbon Capture Wast ewater - Set 1 72491 6575

Untreated Carbon Capture Wast ewater - Set 2 72492 6575

Untreated Carbon Capture Wast ewater - Set 3 72493 6575

Untreated Carbon Capture Wast ewater - Set 4 72494 6575

Carbon Capture Wastewater Treatment Effluent - Set 1 72495 6575

Carbon Capture Wastewater Treatment Effluent - Set 2 72496 6575

Carbon Capture Wastewater Treatment Effluent - Set 3 72497 6575

Carbon Capture Wastewater Treatment Effluent - Set 4 72498 6575

Untreated Carbon Capture Wastewater Field Blank - Set 1 72499 6575

Carbon Capture Wastewater Treatment Effluent Field Blank - Set 1 72500 6575

Carbon Capture Wastewater Treatment Effluent Field Blank - Set 2 72501 6575

Carbon Capture Wastewater Treatment Effluent Field Blank - Set 3 72502 6575

Carbon Capture Wastewater Treatment Effluent Field Blank - Set 4 72503 6575



# 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



# Untreated Carbon

Capture Wastewater Collected during one

of the four sets Collected during one

of the four sets No field blanks

required

Carbon Capture

Wastewater Treatment

Effluent Collected once during

each of the four sets Collected during one

of the four sets 2 

# No field blanks

required

1 

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

2 

# The field blank can be collected during any of the sa mple sets, but the plant must use the sample number

and sampling point description associated with the co rrect sample set (e.g., Carbon Capture Wastewater

Treatment Effluent Field Blank – Set 2 – sample number 72501 if the field is collected during set 2).



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

analyses; however, no additional sample volume is required.

Sample Collection

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

mercury samples; therefore, the sampling t eam should follow the clean hands/dirty hands

sampling techniques outlined in EPA Method 166 9. Additionally, the plant must try to

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

airborne particles, dirt, and corrosion pa rticulates from pipi ng, railing, etc.

The plant must collect grab samples for a ll analytes at the untreated carbon capture

wastewater sampling point. The plant must collect 24-hour composite samples for all

analytes except cyanide and mercury at the carbon capture wastewater treatment effluent

sampling point. The 24-hour composites must be set up to collect equal sample aliquots

every hour over the 24-hour period. For me rcury at the carbon capture wastewater

treatment effluent sampling point, the plant must collect four individual grab samples over

the 24-hour period (i.e., one merc ury grab collected every si x hours). For cyanide at the

carbon capture wastewater treatment effluent sampling point, the plant must collect a

single grab sample after one of the mercury grab samples.

If the plant is able to collect the sample s from a valve or tap, the plant can use the

instructions provided in this section to set up and collect the composite samples at the

carbon capture wastewater treatm ent effluent sampling point. This section also provides

instructions to collect the grab samples at the untreated carbon capture wastewater

sampling point and for the mercury and cyan ide grab samples at the carbon capture

wastewater treatment effluent sampling point . Please note that th e plant will need to

install a two-way splitter on the tap to allow for the composite tubing to be connected to

the tap and also have a tap available for th e grab sample collection of the cyanide and

mercury samples. Additionally, the descripti on below assumes that the sample lines are

pressurized and therefore would not allow the compositor to backflush the composite

tubing directly into the sample line. (NOTE: If a sample tap or valve is not available to

collect these samples or if the carbon capture wastewater treatment ef fluent sampling point

has intermittent flow which may interfere with the automatic composite collection, please

contact TJ Finseth, (703) 633-1698 to discuss possible alternatives.)

Composite Sample Collection

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

the sample collection.

2. Clean hands and dirty hands put on T yvek® suits and powder-free gloves.

3. Dirty hands opens the outer bag of the cleanbox and clean hands opens the

clear inner bags and secures the cl eanbox open with the clips located

inside the box.

4. Dirty hands opens the outer bag contai ning a length of precleaned silicone

tubing, a “T” splitter, and two additi onal pieces of silicone tubing. Clean

hands takes the inner bag containing the tubing and moves it into the

cleanbox. Clean hands opens the inner bag and removes the tubing. Clean

hands places a clean plastic bag over each end of the silicone tubing. The

tubing configuration will be set up such that one end will be connected to

the sample tap, one end will be thre aded through the automatic compositor

and connected to the large composite container, and one end will be

placed next to a sump/drain near the sampling point. To collect the

samples, the sample tap will be left open during the entire sample

collection time period and will flow di rectly to the sump/drain; however,

# the automatic compositor will pull sample from the flowing stream as

dictated by the sampling program. Additionally, the automatic compositor

will be capable of purging the line back to the flowing stream between

each individual sample aliquot.

5. Dirty hands threads one portion of the silicone tubing through the

peristaltic pump portion of the automatic compositor.

6. Dirty hands opens the outer bag of th e metals field blank water and the

field blank composite container. Clea n hands opens the inner bag for the

field blank water, unscrews the lid and places it in the inner bag. Clean

hands then places one end of the silicone tubing into the blank water.

Clean hands also opens the inner bag for the field blank composite

container and loosens the lid. Clean hands holds the silicone tubing with

the plastic bag covering the end out of the cleanbox and over a bucket and

dirty hands operates the pump to pump blank water through the tubing.

After the tubing has been purged with sufficient volume, clean hands

holds the silicone tubing at the m outh of the field blank composite

container and fills the composite container with sufficient volume to

collect the total metals field blank samples at the pump -off location. Dirty

hands stops the pump. During the purgi ng of the tubing and collection of

the field blank sample volume, di rty hands pinches a portion of the

silicone tubing that will be placed by the sump/drain. Clean hands places

the plastic bag over the end of the si licone tubing, replaces the lid on the

field blank composite cont ainer, places the silicone tubing back in the

cleanbox, and closes the inner bag of th e field blank composite container.

Dirty hands closes the outer bag of th e field blank composite container.

7. Clean hands holds the end of the si licone tubing outside the cleanbox over

a bucket, with the plastic bag still covering the end of the tubing. Dirty

hands places the end of the silicone tubing near the sump/drain and opens

the sample tap valve to allow the wa stewater to flow through the tubing.

Dirty hands operates the pump to pur ge the pump portion of the tubing for

a minimum of 2 minutes.

8. Dirty hands programs the automatic co mpositor to collect the 20 liters of

sample over a 24-hour time period in one-hour intervals (i.e., collect 830

mL of sample every hour). Dirty hand s calibrates the compositor to ensure

that 830 mL is being collected for each individual grab.

9. Dirty hands opens the outer bag of th e large composite container. Clean

hands opens the inner bag and connect s the silicone tubing to the port on

the composite container, securing th e connection with a cable tie. Clean

hands closes the inner bag around the composite bottle, and dirty hands

closes the outer bag. The samplers put ice around the composite container

to keep the samples cold during the compositing time period.

10. At the end of the composite sampling period, dirty hands stops each of the

automatic compositors and opens the outer bag of each composite

container. For each container, clean hands opens the inner bag and

detaches the used tubing from the co mposite container and covers the port

with a closed lid or small plastic ba g. The samplers transport each of the

# composite containers, including the fiel d blank composite container, to the

pump-off area to pump off the samples into the specified sample

containers.

11. The samplers then repeat steps 1 th rough 10 (skipping step 6) to collect

the composite samples for the next day of sample collection.

After the composite samples have been collected, the sampling team will then

transfer the sample into the individual sample containers at the pump-off area.

Sample Pump-Off Procedures

12. Arrive at the pump-off location and prepare suppl ies and bottles for the

sample collection.

13. Clean hands and dirty hands put on T yvek® suits and powder-free gloves.

14. Dirty hands opens the outer bag of the cleanbox and clean hands opens the

clear inner bags and secures the cl eanbox open with the clips located

inside the box.

15. Dirty hands opens the opening on the pe ristaltic pump head so the tubing

can be placed in the pump head. Dirty hands opens the outer bag

containing a length of precleaned Teflon® tubing connected to a length of

precleaned silicone tubing. Clean hands moves the tubing into the

cleanbox and opens the inner bag and removes the tubing. Clean hands

places a clean plastic bag over the end of the Teflon® and silicone tubing.

16. Dirty hands threads the silicone tubi ng into the peristaltic pump head.

17. Dirty hands shakes the field blank co mposite container to mix the sample

and then opens the outer bag of the field blank composite container and

total metals field blank sample bottle. Clean hands removes the total

metals field blank sample bottle and places it in the cleanbox. Clean hands

opens the inner bag of the field blank composite container, removes the lid

from the container, and places the end of the Teflon® tubing in the blank

water. Clean hands holds the end of the silicone tubing outside the

cleanbox over a bucket, with the plastic bag still covering the end of the

tubing and dirty hands operates the pump to pump about two liters of

blank water from the field blank com posite container. Clean hands places

the end of the silicone tubing in th e cleanbox, opens the inner bag of the

total metals field blank sample bottle, and removes the lid. Dirty hands

operates the pump to collect the total metals field blank sample and then

stops the pump. Clean hands closes the lid on the sample bottle and closes

the inner bag. Clean hands places the i nner bag and bottle in the outer bag

and dirty hands clos es the outer bag.

18. Dirty hands shakes the large composite container to mix the sample and

then opens the outer bag of the larg e composite container for the metals

samples and clean hands opens the in ner bag. Clean hands transfers the

Teflon® tubing from the field blank composite container to the metals

sample composite container. Clean ha nds holds the end of the silicone

tubing outside the cleanbox over a buck et, with the plastic bag still

# covering the end of the tubing and dirt y hands operates the pump to pump

about two liters of sample through the tubing and then stops the pump.

19. Dirty hands opens the outer bag of the total metals by EPA Method 200.8

sample bottle. Clean hands removes th e inner bag and bottle and places it

in the cleanbox. Clean hands opens the inner bag and removes the lid.

Dirty hands operates the pump to collect the total metals sample and then

stops the pump. Clean hands closes the lid on the sample bottle and closes

the inner bag. Clean hands places the i nner bag and bottle in the outer bag

and dirty hands closes the outer bag. The samplers repeat the procedure to

collect the total metals by EPA Method 200.7 sample.

20. The samplers operate the pump to collect the BOD 5 

# , Group I, and Group II

samples. NOTE: The samplers do not need to use the cleanbox while

collecting these samples.

Grab Sample Colletion

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

the sample collection.

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

gloves.

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

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

open the bag completely.

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

there should be no flow through the samp le tap at this time). Clean hands

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

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

collection.

5. Dirty hands opens the outer bags of th e field blank water and total mercury

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

bag of the field blank water and unscrew s the lid. Clean hands then opens

the inner bag of the total mercury an d total metals field blank sample

bottles. Clean hands pours the blank water into the field blank sample

bottles under the shrouding, caps the bottles, and clos es the inner bags.

Clean hands then places the total mercury and total metals bottles in the

outer bags and dirty hands closes the outer bags.

6. Dirty hands then opens the valve to th e sample tap and purges the tap for at

least two minutes, then keeps the valv e open until all samples have been

collected.

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

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

shroud. Clean hands then opens the i nner bag, opens the lid of the bottle

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

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

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

the collection of the to tal metals samples (both EPA 200.8 with collision

# cell and EPA 200.7), unless the plant is collecting the metals 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 samples 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 prior to

shipment to the laboratories. Use th e information provided in the “Sample

Bottles and Preservation” section of th ese instruction for the preservation

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

should be placed on ice immediately afte r sample collection/preservation.

Sample Packing and Shipment

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

laboratories.

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

specifies the sample point.

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

overtighten the lid. If bo ttle threads are dirty to where the lid is impeded

from closing, clean the threads on th e bottle being careful to not introduce

contamination into the sample. Clean the sample bottle 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 wrap must fit

snugly and completely cover the sa mple bottle. Enclose each “bubblewrapped” container and pl astic container in an in dividual sealable plastic

freezer bag.

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

ship samples to the laboratories.

6. Place the classicals samples in the garb age bags in the coolers with proper

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

7. Add ice to the cooler to keep sample s cold during shipment. Arrange blue

ice or sealed plastic freezer bags fill ed 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 fre ezer bags. Put at least 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 second 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 different cooler with

proper end up, close the interior garbag e bag by tying or with 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 th e metals samples would need to be

chilled prior to packing them in the cooler with the classicals and ice

would need to be added to the cool er between the interior and outer

garbage bags to keep the samples cold.

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

coolers with additional cushioning mate rial. Sufficient packing material

should be used so that the sample containers will not shift during

shipment.

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

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

report form(s) in a plastic envelope secu red to the inside of the top of the

cooler(s). NOTE: the top page of the tr affic report must 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 labe l on the lid of the cooler(s). The

classicals and metals samples shoul d be shipped to TestAmerica 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 perpendicular to

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

released or damaged.

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

proper end up, close the interior garbag e 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 bot tles 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 in side of the top of the cooler. NOTE:

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

provided in step 11:

19. Close the cooler.

20. Place a completed laboratory address la bel on the lid of 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 perpendicular to

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

released or damaged.

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

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

priority overnight to arri ve at the laboratories the following morning. Ship

the coolers to the laboratories.

23. After the coolers have been dropped o ff (or picked up), please contact TJ

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

shipped to the laboratories.

Traffic Reports

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

collection event. The plant will need to make changes to 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, the plant must print the four pages in the

file. The last two pages in the file must be placed in the 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 and Process Flow Diagram

The plant must provide engine ering data regarding the opera tion of the plant, the carbon

capture system, and the carbon capture wastew ater treatment system during the sample

collection period. Additionally, the plant mu st make some field measurements when

samples are collected, including pH, temperatur e, and visual observations, and provide

the data to EPA after the sample collecti on period. The engine ering data and field

measurement data requirements are in an Excel® spreadsheet titled “Monitoring Program

Engineering Data Tables.” The tables are also included at the end of this enclosure. The

# plant must also submit a detailed process fl ow diagram for the carbon capture process and

the carbon capture wastewater treatment syst em, annotated to indi cate the location of

each sampling point. The process flow diagram must present sufficient detail to depict

each process flow stream (influent, effluent , and recycle streams) associated with or

contributing directly or indirectly to th e generation and treatm ent of carbon capture

wastewater. The plant must complete the e ngineering data sheets and field measurement

sheets in the Excel® file and e-mail the comp leted forms, along with the process flow

diagram, to TJ Finseth at thomas.finseth@erg.com . Note that any information claimed as

confidential business information (CBI) must not be sent by e-mail and must instead be

sent via U.S. postal service or by courier (e.g., Federal Express).

Certification Statement

The individual responsible for directing a nd supervising the sample collection and the

engineering data preparation must sign the ce rtification 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 1 - Grab 1Set 1 - Grab 2Set 1 - Grab 3Set 1 - Grab 4Set 2 - Grab 1Set 2 - Grab 2Set 2 - Grab 3Set 2 - Grab 4Set 3 - Grab 1Set 3 - Grab 2Set 3 - Grab 3Set 3 - Grab 4Set 4 - Grab 1Set 4 - Grab 2Set 4 - Grab 3Set 4 - Grab 4NOTE: For influent samples, only the grab 1 row needs to be completed.Plant NameSampleCollectionNumberUntreated CarbonCaptureWastewaterSamplesCollected asGrabs(Yes or No)Mercury and CyanideSamples Collected asGrabs(Yes or No)Carbon Capture WWTEffluent Samples(Except Mercury &Cyanide) Collected as24-Hour Composites(Yes or No)Tyvek Suits used(Yes or No)Dust MasksUsed forMercury(Yes or No)CleanHands/DirtyHands SamplingTechniques Used(Yes or No)Description of SampleCollection Technique(if different thaninstructions)Description of AbnormalConditions in Carbon CaptureSystem or Carbon CaptureWastewater Treatment Systemthat May Impact WastewaterCharacteristicsSet 1Set 2Set 3Set 4Complete the following tables based on the plant operating characteristics during each set of samples collectedUnits OperatingDuring SamplingDayUnits Off-lineEntireSampling DaySCRs/SNCRsOperating onUnits FGD OperatingSet 1Set 2Set 3Set 4(Liters/day) (Liters/day) (Liters/day) (Liters/day) (Liters/day)Set 1Set 2Set 3Set 4NOTE: If the plant does not treat the carbon capture wastewater on site, the plant must provide the name of the company/facility that treats the wastewater, aswell as a description of the treatment system. (See the "Off Site Treatment" tab in this Excel file).Insert the Names of the Chemicals Used in Treatment in the Cells Below and Provide the AmountUsed During Each Set of Sampling and UsagePlant NameSampleCollectionNumberDate of SampleCollectionPlant NameSampleCollectionNumberDate of SampleCollectionCarbon Capture Wastewater Treatment Chemical Usage During Sample Collection (if on site)Plant Operation During Sample Collection

# Flue Gas Flow Through Carbon Capture

System (scf/min) MW-Equivalent Power Generation

Treated by the Carbon Capture System

(MW-hr)

Unit 1 Unit 1 Plant Name Date Provide the daily flue gas flowrate (and MW equivalent) for the carbon capture system starting two weeks prior to the first set

of samples through the last set of samples

# Untreated Carbon

Capture Wastewater Dilution Water Flow

Rate (if added prior

to Effluent) Carbon Capture

Wastewater Treatment

Effluent Plant Name Date Provide the average flow rate of the untreated carbon capture wastewater and the associated wastewater

treatment system (if applicable) for each stream included in the table starting two weeks prior to the first

set of samples through the last set of samples.

Carbon Capture Wastewater Generation and Treatment System

Flow Rates

# Carbon Capture Wastewater Treatment System (if located off site)

Does the plant ship the carbon capture wastewater off site for treatment or disposal?

If the plant answered yes to the question above, please answer the following questions:

Provide the name of the company and facility where the carbon capture wastewater is transferred.

Company

Facility

Address line 1

Address line 2

City

State

Zip

Provide a description of the wastewater treatment or disposal system used for the carbon capture wastewater.

# Enclosure 2

Authority

This request for information is made under auth ority provided by Secti on 308 of the Federal

Water Pollution Control Act, as amended, 33 US C 1318. Section 308 provides that, "Whenever

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

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

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

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

such monitoring equipment . . . sample such efflue nt . . . and provide such other information as

he may reasonably require."

Confidentiality

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

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

part or all of the informati on that you furnish to EPA.

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

Subpart B. The manner of asserting such a clai m is specified 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 th e information 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 information 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 deci des to make a determination as to whether or

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

substantiate any claim you have ma de that information is confiden tial. Therefore, we encourage

you to consult 40 CFR Part 2, and to claim as c onfidential only those item s that you truly believe

satisfy the criteria for confidentiality.

Note that effluent data ar e not eligible for confiden tial treatment (see 40 CFR 2.302).

# Enclosure 3

Notice of Intent to Transfer Confidential Information to Selected EPA Contractors

EPA intends to grant access to confidential information collected under this wastewater sampling

program to selected EPA contractors.

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

allow those contractors identif ied below access to all data (i ncluding data claimed to be

confidential) collected as part of the sampling 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 Stea m Electric Power Generating industry.

The contractors and subcontractor s that will be providing suppor t 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 analysis 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 tr ansfer the information described above to the

designated contractors and subcont ractors in order that they ma y 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 regulati ons, you are entitled to provide comments to EPA

regarding this notice of contempl ated disclosure. Any such co mments must be received by EPA

in writing within 10 days of your receipt of this notice. 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 di recting or supervising the sample collection and engineering data

preparation for the sampling program must read a nd sign the Certification Statement listed below.

The certifying official must be a responsible corporate 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 supervis ion, that qualified personnel colle cted the samples following the

procedures described in the in structions (including the use of clean hands/dirty hands sampling

techniques described in EPA Me thod 1669), that qualified pers onnel gathered the engineering

data required, and that the sampling and engineeri ng data provided are complete and reflect

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

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

measurement, we provided best estimates. We ha ve to the best of our ab ility indicated what we

believe to be company confiden tial business information as de fined under 40 CFR Part 2, Subpart

B. We understand that we may be required at a later time to just ify 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 possibili ty 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 Number of Certifying Official

Title of Certifying Official

Company Name

# Section 2

On

- Site Audit Memorandum

# An on

- site audit was not performed at the Mountaineer Plant.

# Section 3

Signed Certification Statement

# Section 4

Engineering DataTable K4-1. Field Measurements for Sample Collection at the PVF Bleed Stream, MountaineerEpisode NumberSample CollectionNumberDate of SampleCollectionSample CollectionTimeTemperature(°C)pH(S.U.)6575PVF Set 1 - Grab 1 1/31/2011 0904 16.4 7.956575PVF Set 2 - Grab 1 2/1/2011 0825 35.7 3.666575PVF Set 3 - Grab 1 2/2/2011 0915 30.5 5.16575PVF Set 4 - Grab 1 2/3/2011 0933 32.1 3.5Table K4-2. Field Measurements for Sample Collection at the Flue Gas Condensate Stream, MountaineerEpisode NumberSample CollectionNumberDate of SampleCollectionSample CollectionTimeTemperature(°C)pH(S.U.)6575FGC Set 1 - Grab 1 1/31/2011 0828 21.9 6.36575FGC Set 2 - Grab 1 2/1/2011 0835 17.7 3.446575FGC Set 3 - Grab 1 2/2/2011 0920 24.6 8.386575FGC Set 4 - Grab 1 2/3/2011 0938 23.1 4.99Table K4-3. Sample Collection Procedures Used during the Sampling EpisodeEpisodeNumberSampleCollectionNumberUntreatedCarbonCaptureWastewaterSamplesCollected asGrabs(Yes or No)MercuryandCyanideSamplesCollectedas Grabs(Yes or No)Carbon CaptureWWT EffluentSamplesCollected as 24-Hour Composites(Yes or No)CleanHands/DirtyHandsSamplingTechniquesUsed(Yes or No)*Description ofSampleCollectionTechnique (ifdifferent thaninstructions)Description ofAbnormal Conditionsin FGD System or FGDWastewater TreatmentSystem that MayImpact Concentrations6575Set 1 Yes Yes None Yes None Note 16575Set 2 Yes Yes NoneYes NoneNone6575Set 3 Yes Yes NoneYes NoneNone6575Set 4 Yes Yes NoneYes NoneNone* Includes the use of tyveks suits during all sampling events and dust masks during the collection of mercury samples.Note 1: Facility temporarily shutdown following sampling.Table K4-4. Generating Unit Operationat Time of Sampling, MountaineerEpisodeNumberSampleCollectionNumberDate of SampleCollectionPlant Operation During Sample CollectionUnits OperatingDuring SamplingDayUnits Off-lineEntire SamplingDaySCRs/SNCRsOperating onUnitsFGDOperating6575 Set 11/31/2011Unit 1 None SCR Yes6575 Set 22/1/2011Unit 1 None SCR Yes6575 Set 32/2/2011Unit 1 None SCR Yes6575 Set 42/3/2011Unit 1 None SCR YesTable K4-5. Daily Average Flue Gas Flow and MW-Equivalent Power Generation for the CarbonCapture System DuringSampling Period, MountaineerEpisodeNumberDateDaily Average FlueGas Flow to CarbonCapture System(lbs/hr)MW-EquivalentPower GenerationTreated by theCarbon CaptureSystem (MWn)CommentsUnit 1Unit 165751/17/2011 0 0.00 Main unit out of service.65751/18/2011 46,697 4.79Main Unit returned to service at 12:50 AM andCAP process began start-up at 1:20 PM.65751/19/2011 47,544 5.91Cap process out of service from 6:40 AM to 7:50PM for CAP process repairs.65751/20/2011 131,019 12.91Main Unit load reduced to 700 MWN and CAPprocess reduced flue gas flow to 100K indicated at4:30 PM due LP expansion joint problems on mainunit.65751/21/2011 69,174 6.27CAP process out of service at 4:45 PM due to mainunit reducing load below 200 MWN.65751/22/2011 0 0.00Cap process outage continued for this reportingperiod.65751/23/2011 109,606 11.07 CAP process began restart at 5:30 AM.65751/24/2011 159,994 15.40 CAP processin service for 24 hour period.65751/25/2011 160,014 15.74 CAP processin service for 24 hour period.65751/26/2011 159,997 15.87CAP process tripped out of service to loss of main34.5KV feed from switchyard at 11:30 PM.65751/27/2011 9,107 0.00Process remained out of service due to failed VFDdrives on the chiller condenser cooling fans afterpower was restored at 11:30 AM on 1/27/2011.Table K4-5. Daily Average Flue Gas Flow and MW-Equivalent Power Generation for the CarbonCapture System DuringSampling Period, MountaineerEpisodeNumberDateDaily Average FlueGas Flow to CarbonCapture System(lbs/hr)MW-EquivalentPower GenerationTreated by theCarbon CaptureSystem (MWn)CommentsUnit 1Unit 165751/28/2011 3,441 0.00Cap process outage continued for this reportingperiod.65751/29/2011 3,415 0.00Cap process outage continued for this reportingperiod.65751/30/2011 145,083 14.81 CAP process began restart at 1:15 AM.65751/31/2011 137,665 13.78CAP process removed from service at 9:00 AM to10:45 AM to clean flue gas cooling coils thatindicated signs of pluggage.65752/1/2011 153,124 15.09CAP process removed from service at 11:00 PM to11:45 PM to clean flue gas cooling coils thatindicated signs of pluggage.65752/2/2011 137,595 13.87 CAP processin service for 24 hour period.65752/3/2011 134,355 13.34CAP process removed from service at 5:15 PM to6:45 PM to clean flue gas cooling coils thatindicated signs of pluggage.Table K4-6. Carbon Capture Wastewater Generation andTreatment System Flow Rates during Sampling Period,MountaineerEpisodeNumberDateCarbon Capture Wastewater Generation and Treatment System Flow Rates(gpd)Untreated CarbonCaptureWastewater –PVF BleedUntreated CarbonCapture Wastewater- FGCCDilution WaterFlow RateCarbon CaptureWastewaterTreatment Effluent65751/17/2011 0 0 N/A N/A65751/18/2011 812 2,851 N/A N/A65751/19/2011 1,620 2,675 N/A N/A65751/20/2011 4,058 7,513 N/A N/A65751/21/2011 2,651 5,508 N/A N/A65751/22/2011 0 0 N/A N/A65751/23/2011 1,174 4,620 N/A N/A65751/24/2011 1,213 6,138 N/A N/A65751/25/2011 0 7,527 N/A N/A65751/26/2011 4,429 9,911 N/A N/A65751/27/2011 0 0 N/A N/A65751/28/2011 0 0 N/A N/A65751/29/2011 3,884 0 N/A N/A65751/30/2011 0 7,148 N/A N/A65751/31/2011 967 6,813 N/A N/A65752/1/2011 5,136 9,249 N/A N/A65752/2/2011 2,763 6,904 N/A N/A65752/3/2011 3,317 6,103 N/A N/AN/A – Not Applicable

# Carbon Capture Wastewater Treatment

Does the plant ship the carbon capture wastew ater off site for treatment or disposal?

Yes

If the plant answered yes to the question ab ove, please answer the following questions:

Provide the name of the company and facility wh ere the carbon capture wastewater is transferred.

Company Vickery Environmental

Facility A waste management company

Address 3956 State Route 412

City Vickery

State OH

Zip 43464

Provide a description of the wastewater treatment or disposal system used for the carbon capture

wastewater.

The PVF bleed stream is hauled off-site for disposal into deep injection wells. The broker or “middle

man” is Aquilex/HydroChem, who “manages” the disposal of the wastewater and contacts Vickery when

disposal services are needed. Vickery Transportation transports the waste water to Vickery

Environmental for disposal by deep well injection.

# Section 5

Analytical DataNA – Not analyzed.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 K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day averageresult indicates that all results were below the quantitation limit, but at least oneresult is a J-value.1 – Sample arrived at lab outside criteria holding time.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.MI – Matrix interferences present.Table K5-1. PVF Bleed Stream, MountaineerPVF Bleed Stream (SP-1)AnalyteUnitsMethodDay 1Day 2Day 3Day 44-DayAverageClassicalsAmmonia mg/L 350.1 3,000 38,000 B 35,000 B,4 31,000 B 26,800Nitrate Nitrite as N mg/L 353.2 8.70 9.20 8.30 9.70 8.98Nitrogen, Total Kjeldahl mg/L 351.2 6,300 56,000 48,000 4 61,000 42,800Biochemical OxygenDemandmg/L 5210B ND (2.00) NA1ND (2.00) ND (40.0) ND (14.7)Chemical OxygenDemandmg/L 410.4 80.0 100 82.0 F 93.0 88.8Chloridemg/L 300.0 NQ (300) NQ (300) NQ (300) NQ (300) NQ (300)Sulfatemg/L 300.0 180,000 150,000 130,000 F 190,000 163,000Cyanide, Total mg/L 4500 CN E 1.00 0.910 1.20 F 1.70 1.20Total Dissolved Solids mg/L 2540C 190,000 160,000 130,000 170,000 163,000Total Suspended Solids mg/L 2540D 21.0 27.0 24.0 37.0 27.3Phosphorus, Total mg/L 365.1 0.110 0.280 0.110 F 0.120 0.155Total MetalsAluminum ug/L 200.7 270 600 390 540 450Antimony ug/L 200.8 3.00 2.70 2.10 2.80 2.65Arsenic ug/L 200.8 41.0 52.0 30.0 F, MI 37.0 40.0Bariumug/L 200.7 53.0 61.0 54.0 F 62.0 57.5Berylliumug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.00) ND (2.00)Boronug/L 200.7 15,000 B 13,000 B 11,000 B,4 13,000 B 13,000Cadmiumug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.00)NA – Not analyzed.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 K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day averageresult indicates that all results were below the quantitation limit, but at least oneresult is a J-value.1 – Sample arrived at lab outside criteria holding time.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.MI – Matrix interferences present.Table K5-1. PVF Bleed Stream, MountaineerPVF Bleed Stream (SP-1)AnalyteUnitsMethodDay 1Day 2Day 3Day 44-DayAverageCalciumug/L 200.7 27,000 22,000 20,000 27,000 24,000Chromium ug/L 200.8 690 1,200 970 4, MI 3,300 1,540Cobaltug/L 200.7 57.0 66.0 60.0 110 73.3Copperug/L 200.8 440 410 300 4 450 400Ironug/L 200.7 2,200 4,600 2,900 7,800 4,380Leadug/L 200.8 6.10 13.0 3.60 8.40 7.78Magnesium ug/L 200.7 13,000 13,000 14,000 23,000 15,800Manganese ug/L 200.7 880 870 810 1,300 965Mercury ng/L 1631E 2,000 5,080 3,070 3,960 3,530Molybdenum ug/L 200.7 2,900 2,200 2,700 2,700 2,630Nickelug/L 200.8 4,400 B 4,300 B 3,800 B,4 5,600 B 4,530Selenium ug/L 200.8 4,000 5,600 5,100 4 4,900 4,900Silverug/L 200.8 ND (2.00) ND (2.00) ND (2.00) F, MI ND (2.00) ND (2.00)Sodiumug/L 200.7 15,000 15,000 14,000 20,000 16,000Thallium ug/L 200.8 2.30 2.30 2.00 2.60 2.30Tinug/L 200.7 ND (200) ND (200) ND (200) ND (200) ND (200)Titaniumug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.0)Vanadium ug/L 200.8 16.0 26.0 13.0 21.0 19.0Zincug/L 200.7 330 B 260 B 250 B 330 B 293NA – Not analyzed.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 K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day averageresult indicates that all results were below the quantitation limit, but at least oneresult is a J-value.1 – Sample arrived at lab outside criteria holding time.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.MI – Matrix interferences present.Table K5-2. Flue Gas Condensate, MountaineerFlue Gas Condensate (SP-2)AnalyteUnitsMethodDay 1Day 2Day 3Day 44-DayAverageClassicalsAmmonia mg/L 350.1 210 NQ (1.00) B 1,200 B 120 B < 383Nitrate Nitrite as N mg/L 353.2 5.60 0.320 1.10 0.170 1.80Nitrogen, TotalKjeldahl mg/L 351.2 430 150 1,600 780 740Biochemical OxygenDemand mg/L 5210B 2.50 NA17.20 NQ (2.50) < 3.65Chemical OxygenDemandmg/L 410.4 ND (20.0) NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.0)Chloridemg/L 300.0 NQ (6.00) NQ (3.00) NQ (15.0) NQ (3.00) NQ (6.75)Sulfate mg/L 300.0 1,200 330 2,300 360 1,050Cyanide, Total mg/L 4500 CN E ND (0.100) ND (0.100) ND (0.100) ND (0.100) ND (0.100)Total Dissolved Solids mg/L 2540C 1,300 340 2,200 360 1,050Total Suspended Solids mg/L 2540D 11.0 ND (4.00) 10.0 4.00 < 6.75Phosphorus, Total mg/L 365.1 NQ (0.0500) NQ (0.0500) NQ (0.0500) NQ (0.0500) NQ (0.0500)Total MetalsAluminumug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (200) NQ (200)Antimonyug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.00) ND (2.00)Arsenicug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.00)Bariumug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.0)Berylliumug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.00) ND (2.00)Boronug/L 200.7 1,600 B 850 B 2,100 B 1,600 B 1,540NA – Not analyzed.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 K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day averageresult indicates that all results were below the quantitation limit, but at least oneresult is a J-value.1 – Sample arrived at lab outside criteria holding time.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.MI – Matrix interferences present.Table K5-2. Flue Gas Condensate, MountaineerFlue Gas Condensate (SP-2)AnalyteUnitsMethodDay 1Day 2Day 3Day 44-DayAverageCadmiumug/L 200.8 ND (4.00) ND (4.00) ND (4.00) ND (4.00) ND (4.00)Calcium ug/L 200.7 670 NQ (400) 8,000 690 < 2,390Chromium ug/L 200.8 20.0 NQ (8.00) 23.0 23.0 < 17.5Cobaltug/L 200.7 ND (20.0) ND (20.0) NQ (20.0) ND (20.0) NQ (20.0)Copperug/L 200.8 8.30 10.0 35.0 6.20 14.9Ironug/L 200.7 1,400 1,300 4,400 960 2,020Leadug/L 200.8 NQ (2.00) ND (2.00) NQ (2.00) ND (2.00) NQ (2.00)Magnesium ug/L 200.7 1,300 450 4,600 1,600 1,990Manganese ug/L 200.7 42.0 55.0 240 65.0 101Mercury ng/L 1631E 2,970 279 702 277 1,060Molybdenumug/L 200.7 NQ (40.0) ND (40.0) NQ (40.0) ND (40.0) NQ (40.0)Nickelug/L 200.8 30.0 B 15.0 B 49.0 B 16.0 B 27.5Selenium ug/L 200.8 150 85.0 180 96.0 128Silverug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.00) ND (2.00)Sodiumug/L 200.7 NQ (10,000) ND (10,000) NQ (10,000) ND (10,000) NQ (10,000)Thalliumug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.00) ND (2.00)Tinug/L 200.7 ND (200) ND (200) ND (200) ND (200) ND (200)Titaniumug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.0)Vanadiumug/L 200.8 NQ (10.0) ND (10.0) NQ (10.0) ND (10.0) NQ (10.0)Zincug/L 200.7 NQ (40.0) B ND (40.0) NQ (40.0) B NQ (40.0) B 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 K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day averageresult indicates that all results were below the quantitation limit, but at least oneresult is a J-value.Table K5-3. Classical Pollutants 4-Day Average DataSummary for Carbon Capture Wastewater, MountaineerAnalyteUnitMethodPVF Bleed Stream (SP-1)4-Day AverageFlue Gas Condensate (SP-2)4-Day AverageClassicalsAmmonia mg/L350.1 26,800 <383Nitrate Nitrite as Nmg/L 353.28.981.80Nitrogen, Total Kjeldahl mg/L 351.242,800740Biochemical Oxygen Demand mg/L 5210BND (14.7)< 3.65Chemical Oxygen Demand mg/L 410.488.8NQ (20.0)Chloridemg/L 300.0NQ (300)NQ (6.75)Sulfate mg/L300.0 163,000 1,050Cyanide, Totalmg/L 4500 CN E1.20ND (0.100)Total Dissolved Solids mg/L 2540C163,0001,050Total Suspended Solids mg/L 2540D27.3< 6.75Phosphorus, Totalmg/L 365.10.155NQ (0.0500)< - 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 K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day averageresult indicates that all results were below the quantitation limit, but at least oneresult is a J-value.Table K5-4. Metal Pollutants 4-Day Average DataSummary for Carbon Capture Wastewater, MountaineerAnalyteUnitMethodPVF Bleed Stream (SP-1)4-Set AverageFlue Gas Condensate (SP-2)4-Set AverageTotal MetalsAluminum ug/L 200.7450NQ (200)Antimony ug/L 200.82.65ND (2.00)Arsenic ug/L 200.840.0NQ (4.00)Barium ug/L 200.757.5NQ (20.0)Beryllium ug/L 200.7ND (2.00)ND (2.00)Boron ug/L 200.713,0001,540Cadmium ug/L 200.8NQ (4.00)ND (4.00)Calcium ug/L 200.724,000< 2,390Chromium ug/L 200.81,540< 17.5Cobalt ug/L 200.773.3NQ (20.0)Copper ug/L 200.840014.9Iron ug/L 200.74,3802,020Lead ug/L 200.87.78NQ (2.00)Magnesium ug/L 200.715,8001,990Manganese ug/L 200.7965101Mercury ng/L 1631E3,5301,060Molybdenum ug/L 200.72,630NQ (0.0)Nickel ug/L 200.84,53027.5Selenium ug/L 200.84,900128Silver ug/L 200.8ND (2.00)ND (2.00)Sodium ug/L 200.716,000NQ (10,000)Thallium ug/L 200.82.30ND (2.00)Tin ug/L 200.7ND (200)ND (200)< - 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 K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day averageresult indicates that all results were below the quantitation limit, but at least oneresult is a J-value.Table K5-4. Metal Pollutants 4-Day Average DataSummary for Carbon Capture Wastewater, MountaineerAnalyteUnitMethodPVF Bleed Stream (SP-1)4-Set AverageFlue Gas Condensate (SP-2)4-Set AverageTitanium ug/L 200.7NQ (20.0)NQ (20.0)Vanadium ug/L 200.819.0NQ (10.0)Zinc ug/L 200.7293NQ (40.0)ND – Not detected (number in parentheses is the quantitation limit).B – Analyte was found in the blank and sample.J – Result measured above the MDL, but less than the quantitation limit.U – Result below the MDL. (Number shown in parentheses is the quantitation limit).Table K5-5. PVF Bleed Steam, Day1 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L80044 8003,000Nitrate Nitrite as N353.2 mg/L 5 0.0950.5 8.7Nitrogen, Total Kjeldahl 351.2 mg/L 20 771,000 6,300Biochemical Oxygen Demand 5210B mg/L 1 0.242 ND (2) UChemical Oxygen Demand 410.4 mg/L 1 4.120 80Chloride 300.0mg/L1002530062JSulfate 300.0mg/L5,0001,20025,000180,000Cyanide, Total4500 CN E mg/L 1 0.020.1 1Total Dissolved Solids2540C mg/L 1 4701,000 190,000Total Suspended Solids 2540D mg/L 1 1.14 21Phosphorus, Total365.1 mg/L 1 0.005 0.05 0.11Total MetalsAluminum 200.7ug/L29.4 200270Antimony 200.8ug/L20.72 23Arsenic 200.8ug/L21.2441Barium 200.7ug/L22.52053Beryllium 200.7ug/L20.71 2ND(2)UBoron 200.7ug/L26.720015,000BCadmium 200.8ug/L21.2 41.5JCalcium 200.7ug/L26940027,000Chromium 200.8ug/L23.3 8690Cobalt 200.7ug/L21.12057ND – 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 K5-5. PVF Bleed Steam, Day1 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCopper 200.8ug/L20.964440Iron 200.7ug/L2322002,200Lead 200.8ug/L20.7326.1Magnesium 200.7ug/L2 21 40013,000Manganese 200.7ug/L20.51 20880Mercury 1631Eng/L5001222552,000Molybdenum 200.7ug/L2 1.6 402,900Nickel 200.8ug/L50221004,400BSelenium 200.8ug/L50161004,000Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00015,000Thallium 200.8ug/L20.4722.3Tin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.6206JVanadium 200.8ug/L21.7 1016Zinc 200.7ug/L29.140330BND – 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 K5-6. PVF Bleed Steam, Day2 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L40 440 8,00038,000BNitrate Nitrite as N353.2 mg/L 5 0.095 0.5 9.2Nitrogen, Total Kjeldahl 351.2 mg/L 10770 10,000 56,000Chemical Oxygen Demand 410.4 mg/L 28.140 100Chloride 300.0mg/L100 25 30062JSulfate300.0 mg/L 5,000 1,200 25,000 150,000Cyanide, Total4500 CN E mg/L 10.020.1 0.91Total Dissolved Solids 2540C mg/L 1470 1,000 160,000Total Suspended Solids 2540D mg/L 11.14 27Phosphorus, Total365.1 mg/L 1 0.005 0.05 0.28Total MetalsAluminum 200.7ug/L2 9.4 200600Antimony 200.8ug/L2 0.72 2 2.7Arsenic 200.8ug/L2 1.2 452Barium 200.7ug/L22.52061Beryllium 200.7ug/L2 0.71 2ND(2)UBoron 200.7ug/L26.720013,000BCadmium 200.8ug/L2 1.2 4 1.3JCalcium 200.7ug/L2 69 40022,000Chromium 200.8ug/L2 3.3 81,200Cobalt 200.7ug/L21.12066Copper 200.8ug/L20.964410ND – 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 K5-6. PVF Bleed Steam, Day2 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationIron 200.7ug/L2322004,600Lead 200.8ug/L20.73213Magnesium 200.7ug/L2 21 40013,000Manganese 200.7ug/L2 0.51 20 870Mercury 1631Eng/L500122 2555,080Molybdenum 200.7ug/L 2 1.6 40 2,200Nickel 200.8ug/L50221004,300BSelenium 200.8ug/L50 16 1005,600Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00015,000Thallium 200.8ug/L2 0.47 22.3Tin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L2 1.6 2011JVanadium 200.8ug/L2 1.7 10 26Zinc 200.7ug/L29.140260BND – 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 K5-7. PVF Bleed Steam, Day3 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L 202204,00035,000B,4Nitrate Nitrite as N353.2 mg/L 5 0.095 0.5 8.3Nitrogen, Total Kjeldahl 351.2 mg/L 10 770 10,000 48,000 4Biochemical Oxygen Demand 5210B mg/L 1 0.242 ND (2) UChemical Oxygen Demand 410.4 mg/L 2 8.140 82 FChloride 300.0mg/L 1002530058JSulfate 300.0mg/L 5,0001,20025,000130,000FCyanide, Total4500 CN E mg/L 1 0.02 0.1 1.2 FTotal Dissolved Solids 2540C mg/L 1 470 1,000 130,000Total Suspended Solids 2540D mg/L 1 1.1424Phosphorus, Total365.1 mg/L 1 0.005 0.05 0.11 FTotal MetalsAluminum 200.7ug/L29.4 200390Antimony 200.8ug/L20.72 22.1Arsenic 200.8ug/L21.2430F,MIBarium 200.7ug/L22.52054FBeryllium 200.7ug/L20.71 2ND(2)UBoron 200.7ug/L26.720011,000B,4Cadmium 200.8ug/L21.2 41.3JCalcium 200.7ug/L26940020,000ND – 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 K5-7. PVF Bleed Steam, Day3 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationChromium 200.8ug/L23.3 89704,MICobalt 200.7ug/L21.12060Copper 200.8ug/L20.9643004Iron 200.7ug/L2322002,900Lead 200.8ug/L20.7323.6Magnesium 200.7ug/L2 21 40014,000Manganese 200.7ug/L20.51 20810Mercury 1631Eng/L5001212523,070Molybdenum 200.7ug/L2 1.6 40 2,700Nickel 200.8ug/L50221003,800B,4Selenium 200.8ug/L50161005,1004Silver200.8 ug/L 2 0.592 ND (2) U,F, MISodium 200.7ug/L218010,00014,000Thallium 200.8ug/L20.4722Tin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.62013JVanadium 200.8ug/L21.7 1013Zinc 200.7ug/L29.140250BND – 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 K5-8. PVF Bleed Steam, Day4 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L 202204,00031,000BNitrate Nitrite as N353.2 mg/L 5 0.095 0.5 9.7Nitrogen, Total Kjeldahl 351.2 mg/L 10770 10,000 61,000Biochemical Oxygen Demand 5210B mg/L 204.740 ND (40) UChemical Oxygen Demand 410.4 mg/L 28.140 93Chloride 300.0mg/L 1002530083JSulfate 300.0mg/L 5,0001,20025,000190,000Cyanide, Total4500 CN E mg/L 10.020.1 1.7Total Dissolved Solids2540C mg/L 1470 1,000 170,000Total Suspended Solids 2540D mg/L 11.14 37Phosphorus, Total365.1 mg/L 1 0.005 0.05 0.12Total MetalsAluminum 200.7ug/L2 9.4 200540Antimony 200.8ug/L20.72 22.8Arsenic 200.8ug/L21.2437Barium 200.7ug/L22.52062Beryllium 200.7ug/L20.71 2ND(2)UBoron 200.7ug/L26.720013,000BCadmium 200.8ug/L21.2 41.4JCalcium 200.7ug/L26940027,000Chromium 200.8ug/L2 3.3 83,300Cobalt 200.7ug/L21.120110ND – 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 K5-8. PVF Bleed Steam, Day4 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCopper 200.8ug/L20.964450Iron 200.7ug/L2322007,800Lead 200.8ug/L20.7328.4Magnesium 200.7ug/L2 21 40023,000Manganese 200.7ug/L2 0.51 201,300Mercury 1631Eng/L5001222553,960Molybdenum 200.7ug/L2 1.6 402,700Nickel 200.8ug/L50221005,600BSelenium 200.8ug/L50161004,900Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,00020,000Thallium 200.8ug/L20.4722.6Tin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.6208.9JVanadium 200.8ug/L2 1.7 1021Zinc 200.7ug/L29.140330BND – 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 K5-9. Flue Gas Condensate, Day 1 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L 1005.5100210Nitrate Nitrite as N353.2 mg/L 1 0.019 0.1 5.6Nitrogen, Total Kjeldahl351.2 mg/L 50 3.850 430Biochemical Oxygen Demand 5210B mg/L 10.32.5 2.5Chemical Oxygen Demand410.4 mg/L 14.120 ND (20) UChloride 300.0mg/L 20.5161.8JSulfate 300.0mg/L 50122501,200Cyanide, Total4500 CN E mg/L 1 0.02 0.1 ND (0.1) UTotal Dissolved Solids2540C mg/L 19.420 1,300Total Suspended Solids2540D mg/L 11.14 11Phosphorus, Total365.1 mg/L 1 0.005 0.05 0.011 JTotal MetalsAluminum 200.7ug/L29.420090JAntimony 200.8ug/L20.722ND(2)UArsenic 200.8ug/L21.243.7JBarium 200.7ug/L22.5206.2JBeryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L26.72001,600BCadmium 200.8ug/L21.24ND(4)UCalcium 200.7ug/L269400670Chromium 200.8ug/L23.3820Cobalt 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 K5-9. Flue Gas Condensate, Day 1 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCopper 200.8ug/L20.9648.3Iron 200.7ug/L2322001,400Lead 200.8ug/L20.7320.76JMagnesium 200.7ug/L2214001,300Manganese 200.7ug/L20.512042Mercury 1631Eng/L5001212522,970Molybdenum 200.7ug/L21.64012JNickel 200.8ug/L20.89430BSelenium 200.8ug/L20.624150Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,000250JThallium 200.8ug/L20.472ND(2)UTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.6206.4JVanadium 200.8ug/L21.7101.7JZinc 200.7ug/L29.14013J,BND – 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 K5-10. Flue Gas Condensate, Day 2 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L 10.05510.4J,BNitrate Nitrite as N353.2 mg/L 1 0.019 0.1 0.32Nitrogen, Total Kjeldahl 351.2 mg/L 20 1.520 150Chemical Oxygen Demand 410.4 mg/L 1 4.120 4.9 JChloride 300.0mg/L 10.2530.63JSulfate 300.0mg/L 102.350330Cyanide, Total4500 CN E mg/L 1 0.02 0.1 ND (0.1) UTotal Dissolved Solids2540C mg/L 1 4.710 340Total Suspended Solids 2540D mg/L 1 1.14 ND (4) UPhosphorus, Total365.1 mg/L 1 0.005 0.05 0.0086 JTotal MetalsAluminum 200.7ug/L29.420062JAntimony 200.8ug/L20.722ND(2)UArsenic 200.8ug/L21.242.9JBarium 200.7ug/L22.5205.3JBeryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L26.7200850BCadmium 200.8ug/L21.2 4ND(4)UCalcium 200.7ug/L269400250JChromium 200.8ug/L23.3 87.8JCobalt 200.7ug/L21.120ND(20)UCopper 200.8ug/L20.96410ND – 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 K5-10. Flue Gas Condensate, Day 2 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationIron 200.7ug/L2322001,300Lead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L2 21 400450Manganese 200.7ug/L20.51 2055Mercury 1631Eng/L500121252279Molybdenum 200.7ug/L2 1.6 40ND(40)UNickel 200.8ug/L20.89415BSelenium 200.8ug/L20.62485Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,000ND(10,000) UThallium 200.8ug/L20.472ND(2)UTin 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).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 K5-11. Flue Gas Condensate, Day 3 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia350.1 mg/L 5 11 200 1,200 BNitrate Nitrite as N353.2 mg/L 1 0.019 0.1 1.1Nitrogen, Total Kjeldahl351.2 mg/L 215200 1,600Biochemical Oxygen Demand 5210B mg/L 1 0.595 7.2Chemical Oxygen Demand410.4 mg/L 14.120 17 JChloride 300.0mg/L51.3159.6JSulfate 300.0mg/L50122502,300Cyanide, Total4500 CN E mg/L 1 0.020.1 ND (0.1) UTotal Dissolved Solids2540C mg/L 147100 2,200Total Suspended Solids2540D mg/L 11.1410Phosphorus, Total365.1 mg/L 1 0.005 0.05 0.03 JTotal MetalsAluminum 200.7ug/L29.4200150JAntimony 200.8ug/L20.722ND(2)UArsenic 200.8ug/L21.243.7JBarium 200.7ug/L22.52013JBeryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L26.72002,100BCadmium 200.8ug/L21.24ND(4)UCalcium 200.7ug/L2694008,000Chromium 200.8ug/L23.3823Cobalt 200.7ug/L21.1201.2JND – 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 K5-11. Flue Gas Condensate, Day 3 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCopper 200.8ug/L20.96435Iron 200.7ug/L2322004,400Lead 200.8ug/L20.7320.93JMagnesium 200.7ug/L2214004,600Manganese 200.7ug/L20.5120240Mercury 1631Eng/L10024.150.5702Molybdenum 200.7ug/L21.6409.3JNickel 200.8ug/L20.89449BSelenium 200.8ug/L20.624180Silver 200.8ug/L20.592ND(2)USodium200.7 ug/L 2 180 10,000 1,500 JThallium 200.8ug/L20.472ND(2)UTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.6208.4JVanadium 200.8ug/L21.7102.8JZinc 200.7ug/L29.14017J,BND – 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 K5-12. Flue Gas Condensate, Day 4 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1mg/L 201.120120BNitrate Nitrite as N353.2 mg/L 1 0.019 0.1 0.17Nitrogen, Total Kjeldahl 351.2 mg/L 10 15200 780Biochemical Oxygen Demand 5210B mg/L 1 0.32.5 2.4 JChemical Oxygen Demand 410.4 mg/L 1 4.120 6.3 JChloride 300.0mg/L 10.2531.7JSulfate 300.0mg/L 102.350360Cyanide, Total4500 CN E mg/L 1 0.02 0.1 ND (0.1) UTotal Dissolved Solids 2540C mg/L 1 4.710 360Total Suspended Solids 2540D mg/L 1 1.144Phosphorus, Total365.1 mg/L 1 0.005 0.05 0.013 JTotal MetalsAluminum 200.7ug/L29.4 20095JAntimony 200.8ug/L20.722ND(2)UArsenic 200.8ug/L21.242.4JBarium 200.7ug/L22.5204JBeryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L26.72001,600BCadmium 200.8ug/L21.2 4ND(4)UCalcium 200.7ug/L269400690Chromium 200.8ug/L23.3 8 23Cobalt 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 K5-12. Flue Gas Condensate, Day 4 Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCopper 200.8ug/L20.9646.2Iron 200.7ug/L232200960Lead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L2 21 4001,600Manganese 200.7ug/L20.51 20 65Mercury 1631Eng/L204.8310.1277Molybdenum 200.7ug/L2 1.6 40ND(40)UNickel 200.8ug/L20.89416BSelenium 200.8ug/L20.62496Silver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,000ND(10,000) UThallium 200.8ug/L20.472ND(2)UTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.6203.9JVanadium 200.8ug/L21.7 10ND(10)UZinc 200.7ug/L29.14011J,BZinc 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 K5-13. PVF Bleed Stream Field Blank Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific 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 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) 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 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) 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 K5-13. PVF Bleed Stream Field Blank Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific 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 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 K5-14. Flue Gas Condensate FieldBlank Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7ug/L29.4200ND(200)UAntimony 200.8ug/L20.722ND(2)UArsenic 200.8ug/L21.24ND(4)UBarium 200.7ug/L22.520ND(20)UBeryllium 200.7ug/L20.712ND(2)UBoron 200.7ug/L26.720016J,BCadmium 200.8ug/L21.24ND(4)UCalcium 200.7ug/L269400ND(400)UChromium 200.8ug/L23.38ND(8)UCobalt 200.7ug/L21.120ND(20)UCopper 200.8ug/L20.964ND(4)UIron 200.7ug/L232200ND(200)ULead 200.8ug/L20.732ND(2)UMagnesium 200.7ug/L221400ND(400)UManganese 200.7ug/L20.5120ND(20)UMercury 1631Eng/L10.240.5ND(0.5)UMolybdenum 200.7ug/L21.640ND(40)UNickel 200.8ug/L20.894ND(4)USelenium 200.8ug/L20.624ND(4)USilver 200.8ug/L20.592ND(2)USodium 200.7ug/L218010,000ND(10,000)UThallium 200.8ug/L20.472ND(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 K5-14. Flue Gas Condensate FieldBlank Analytical Results, MountaineerAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTin 200.7ug/L24.8200ND(200)UTitanium 200.7ug/L21.620ND(20)UVanadium 200.8ug/L21.710ND(10)UZinc 200.7ug/L29.140ND(40)U

# Section 6

Data Review Narratives

# 1



# MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

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

Deb Bartram, ERG

TJ Finseth, ERG

From: Donna Tedder, ERG

Date: 2/9/2012

Subject: FGS Data Review Narrative for Total Mercury – Episodes 6572 an d 6575

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 23 samples (excluding laboratory pre p blanks) FGS extracted

and analyzed for total mercury.

Table 1. 

# EPA Episode 6572, 6575 Mercury– Sample Identification

EPA

Sample # Lab Sample

ID # Sample

Matrix Sample Description Sampling

Date

72341 1101348-22 Aqueous FGD Scrubber Purge, Set 1 1/24/2011

72342 1101348-15 Aqueous FGD Scrubber Purge, Set 2 1/25/2011

72343 1101348-01 Aqueous FGD Scrubber Purge, Set 3 1/26/2011

72344 1101348-08 Aqueous FGD Scrubber Purge, Set 4 1/27/2011

72345 1101348-27 Aqueous FGD Concentrator Distillate, Set 1 1/25/2011

72346 1101348-20 Aqueous FGD Concentrator Distillate, Set 2 1/26/2011

72347 1101348-06 Aqueous FGD Concentrator Distillate, Set 3 1/27/2011

72348 1101348-13 Aqueous FGD Concentrator Distillate, Set 4 1/28/2011

72349 1101348-28 Aqueous Scrubber Purge Field Blank 1/24/2011

72350 1101348-29 Aqueous FGD Concentrator Distillate Field Blank, Set 1 1/24/2011

72351 1101348-21 Aqueous FGD Concentrator Distillate Field Blank, Set 2 1/25/2011

72352 1101348-07 Aqueous FGD Concentrator Distillate Field Blank, Set 3 1/26/2011

72353 1101348-14 Aqueous FGD Concentrator Distillate Field Blank, Set 4 1/27/2011

72491 1102006-01 Aqueous PVF Bleed Stream, Set 1 1/31/2011

72492 1102020-01 Aqueous PVF Bleed Stream, Set 2 2/1/2011

72493 1102020-03 Aqueous PVF Bleed Stream, Set 3 2/2/2011

72494 1102045-01 Aqueous PVF Bleed Stream, Set 4 2/3/2011

72495 1102006-02 Aqueous Flue Gas Condensate, Set 1 1/31/2011

72496 1102020-02 Aqueous Flue Gas Condensate, Set 2 2/1/2011

72497 1102020-04 Aqueous Flue Gas Condensate, Set 3 2/2/2011

# 2 Table 1. 

# EPA Episode 6572, 6575 Mercury– Sample Identification

EPA

Sample # Lab Sample

ID # Sample

Matrix Sample Description Sampling

Date

72498 1102045-02 Aqueous Flue Gas Condensate, Set 4 2/3/2011

72499 1102006-03 Aqueous PVF Bleed Stream Field Blank 1/31/2011

72500 1102006-04 Aqueous Flue Gas Condensate Field Blank 1/31/2011



# 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.

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. Two samples

were analyzed in duplicate at the laboratory, sample 72347 an d 72493. The relative

percent difference (RPD) was 22.4% and 8.08%, respectively. The laboratory’s RPD

criteria between analytical duplicates is 24%. No samp le qualifications were needed

based on these analytical duplicate results.

# 3

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

72347, 72348, 72493, and 72497. All aqueous MS/MSD recoveries were within me thod

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

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 – Episode 6575

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

chromium, copper, lead, nickel, selenium, silver, thallium and vanadium) for Sample

Episode 6575. The samples were analyzed according to EPA Met hod 200.8.

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

EPA Method 200.8.

Table 1. 

# EPA Episode 6575 – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

72491 PVF Bleed Stream, Set 1 280

- 12104

- 1 Aqueous 1/31/2011 2/1/2011

72492 PVF Bleed Stream, Set 2 280

- 12147

- 1 Aqueous 2/1/2011 2/3/2011

72493 PVF Bleed Stream, Set 3 280

- 12147

- 3 Aqueous 2/2/2011 2/3/2011

72494 PVF Bleed Stream, Set 4 280

- 12203

- 1 Aqueous 2/3/2011 2/4/2011

72495 Flue Gas Condensate, Set 1 280

- 12104

- 2 Aqueous 1/31/2011 2/1/2011

72496 Flue Gas Condensate, Set 2 280

- 12147

- 2 Aqueous 2/1/2011 2/3/2011

72497 Flue Gas Condensate, Set 3 280

- 12147

- 4 Aqueous 2/2/2011 2/3/2011

72498 Flue Gas Condensate, Set 4 280

- 12203

- 2 Aqueous 2/3/2011 2/4/2011

72499 PVF Bleed Stream Field Blank 280

- 12104

- 3 Aqueous 1/31/2011 2/1/2011

72500 Flue Gas Condensate Field

Blank 280

- 12104

- 4 Aqueous 1/31/2011 2/1/2011



# 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.

# 2

Any significant findings are summarized below. Additiona l data qualifiers were required

and are found in Table 2.

• The serial dilution for chromium for sample 72493 failed TestAmerica’s control

limits of percent differences less than 10 percent.

• The matrix spike (MS) and matrix spike duplicate (MSD) recoveries for arsenic

and silver for sample 72493 failed the EPA Method 200.8 control limits of 70-

130%.

• The post digestion spike (PDS) recoveries for arsenic, chromium, copper,

selenium, and silver for sample 72493 failed TestAmerica’s control limits of 85–

115%.

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). 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. 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.

# 3

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 72493 passed TestAmer ica’s criteria of ±10%

difference for all analytes except chromium, which was flagged with a “V” qualifier. No

further data qualifiers were needed for the serial dilutio ns.

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 sample 72493. The MS/MSD of sa mple 72493 failed

the method control limits of 70–130% recovery for arsenic, chromium, copper, nickel,

selenium and silver. Chromium, copper, nickel, and selenium were flagged with a “4”

qualifier indicating the concentrations in the parent samp les were greater than four times

the spike and could not be reliably calculated. These data were considered acceptable

based on the LCS passing the method control limits. Arse nic and silver were flagged with

an “F” qualifier. The relative percent difference (RPD) for the MS/MSDs were within the

FGD ICP/MS SOP control limits of ±20% for all analytes . No additional data qualifiers

were required for the MS/MSD samples.

POST DIGESTION SPIKES (PDS)

The PDS performed on sample 72493 passed TestAmerica’s cont rol limits of 85–115%

recovery for all analytes, except for arsenic, chromiu m, copper, selenium, and silver,

which were flagged with a “W” qualifier. Chromium also fai led the MS/MSD and the

serial dilution recovery criteria. Arsenic and silver also failed the MS/MSD recovery

criteria. These additional data qualifiers appear in Tabl e 2 below.

# 4

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

72493 Arsenic

(total) Matrix

Interference PDS, MS/MSD

Failed Recovery 30 μg/L

72493 Chromium

(total) Matrix

Interference PDS, SRD,

MS/MSD Failed

Recovery 970 μg/L

72493 Silver

(total) Matrix

Interference PDS, MS/MSD

Failed Recovery 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 200.7 – Episode 6575

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

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

titanium and zinc) for Sample Episode 6575. The samples wer e 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. 

# EPA Episode 6575 Total Metals – Sample Identification

EPA

Sample # EPA Sample Description Lab Sample

ID # Sample

Matrix Sampling

Date Receipt

Date

7 2 491 PVF Bleed Stream, Set 1 280

- 12104

- 1 Aqueous 1 / 31 /2011 2 / 1 /201 1

7 2492 PVF Bleed Stream, Set 2 280

- 12147

- 1 Aqueous 2/1 /2011 2/3 /2011

7 2493 PVF Bleed Stream, Set 3 280

- 12147

- 3 Aqueous 2/2 /2011 2/3 /2011

7 2494 PVF Bleed Stream, Set 4 280

- 12203

- 1 Aqueous 2/3 /2011 2/4 /2011

7 2495 Flue Gas Condensate, Set 1 280

- 12104

- 2 Aqueous 1 / 31 /2011 2/1 /201 1

7 2496 Flue Gas Condensate, Set 2 280

- 12147

- 2 Aqueous 2/1 /2011 2/3 /2011

7 2497 Flue Gas Condensate, Set 3 280

- 12147

- 4 Aqueous 2/2 /2011 2/3 /2011

7 2498 Flue Gas Condensate, Set 4 280

- 12203

- 2 Aqueous 2/3 /2011 2/4 /2011

7 2499 PVF Bleed Stream Field Blank 280

- 12104

- 3 Aqueous 1 / 31 /2011 2/1 /201 1

7 2500 Flue Gas Condensate Field Blank 280

- 12104

- 4 Aqueous 1 / 31 /2011 2/1 /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 data set.

• The serial dilution for boron for sample 72493 failed Test America’s requirements

of percent difference less than 10%.

# 2

• The matrix spike (MS) and matrix spike duplicate (MSD) rec overies for total

barium for sample 72493 failed the EPA method 200.7 control li mits of 70-130%.

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 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)

The LCS 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.

# 3

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 boron,

which was flagged with a “V” qualifier. No additional data qualifiers were required.

FIELD DUPLICATES

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

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

A MS and MSD was performed on the total sample of 72493. Al l MS/MSD spike

recoveries were within the method control criteria of 70 -130%, except for barium, which

was qualified with an “F”. This result was considered ac ceptable based on the LCS,

serial dilution, and post digestion spike (PDS) passing the method control limits. The

relative percent difference (RPD) for the MS/MSDs we re within TestAmerica’s ± 20%

requirement.

POST DIGESTION SPIKE (PDS)

The PDS performed on sample 72493 passed TestAmerica’s contr ol limits of 85-115%

recovery for all analytes. No additional data qualifier s 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: Donna Tedder, ERG

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Classicals Ana lyses – Episode 6575

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry

analyses for Sample Episode 6575. All samples were test ed 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 8 samples that TestAmerica anal yzed for the above analytes.

Table 1. EPA Episode 6575 Classical Analytes – Sample Identifi cation

EPA

Sample # Sample

Matrix Sample Description Sampling

Date

72491 Water PVF Bleed Stream, Set 1 1/31/11

72492 Water PVF Bleed Stream, Set 2 2/1/11

72493 Water PVF Bleed Stream, Set 3 2/2/11

72494 Water PVF Bleed Stream, Set 4 2/3/11

72495 Water Flue Gas Condensate, Set 1 1/31/11

72496 Water Flue Gas Condensate, Set 2 2/1/11

72497 Water Flue Gas Condensate, Set 3 2/2/11

72498 Water Flue Gas Condensate, Set 4 2/3/11

# 2

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.

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) sample wa s analyzed on samples 72493

and 72494 for each analyte to check for matrix interferences . For some analytes,

TestAmerica spiked more samples than required. All MS s amples analyzed met the

criteria specified in the method unless described below.

DATA NOTES/ISSUES

Ammonia

One method blank detected ammonia at 0.106 mg/L, which is great er than the MDL, but

less than the RL and therefore, was flagged with a “J” qualifier. The associated samples

were flagged with “B” qualifiers. No further qualificatio n was required.

MS and matrix spike duplicates (MSD) were performed on sa mple 72493. The MS/MSD

recoveries for sample 72493 were 116% and 29%, respectively; ho wever, the sample

concentration was greater than 4 times the spike amoun t in the MS and MSD samples and

therefore, the recoveries and RPD could not be reliabl y calculated and the results were

flagged with a “4” qualifier.

BOD 5



# BOD was not performed on samples 72492 and 72496 because they w ere received at the

laboratory after hold time expired due to adverse weather during shipping. BOD could

not be performed on sample 72494 because the sample had been pr eserved with sulfuric

acid.

# 3

All glucose-glutamic acid standards were analyzed appropri ately and met the criteria

specified in SM 5210B.

Laboratory duplicate analyses were performed on sample s 72491, 72493, and 72498.

Samples 72491 and 72493 and their duplicates had no BOD detected and could not be

used to calculate RPD. Sample 72498 had an RPD of 2%.

Chloride and Sulfate

MS and MSD were performed on sample 72493. The MS/MSD sulf ate recoveries for

sample 72493 were below the EPA method 300.0 control limits a nd flagged with an “F”

qualifier. The LFB associated with this sample met the method criteria. No further

qualification was necessary.

COD

MS and MSD were performed on sample 72493. The MS/MSD reco veries for sample

72493 were 122% and 112%, respectively, which are below the contr ol limits of 90-

110% required by EPA Method 410.4 and flagged with an “F” qualifier. Additionally,

the RPD was 11%, which is greater than the method requirem ent of 10%. The LFB

percent recoveries associated with this sample met the method criteria. No further

qualification was necessary.

Cyanide

MS and MSD were performed on samples 72493 and 72494. The MS/MS D recoveries

for sample 72494 passed the method criteria. The MS/MSD r ecoveries for sample 72493

were both 41%, which is less than the method criteria o f 90-100%. However, because

there are no criteria for MS/MSD analyses specified i n SM 4500 CN

- 

# E, no further

qualification was necessary.

Nitrate/Nitrite

No issues were identified by the data reviewer.

Phosphorus

MS and MSD were performed on sample 72493. The MS/MSD reco veries were above

the method specified control limits. Additionally, the MS percent recovery was above

the laboratory control criteria and was flagged with an “F” qualifier. However, the MSD

was within the laboratory control criteria and was not flagged. If reported, the MSD

should be flagged with an “F” qualifier.

Samples 72495, 72496, and 72498 had results below the lowest calibration standard.

These results were above the MDL, but below the RL an d therefore, were flagged with

“J” qualifiers. No further qualification was necessary.

# 4

TDS

No issues were identified by the data reviewer.

TKN

MS and MSD were performed on sample 72493. The MS/MSD reco veries were 136%

and 108%, respectively. The concentration in the original sample was greater than four

times the spike amount; therefore, the percent recove ries could not be reliably calculated

and the results were flagged with a “4” qualifier.

TSS

No issues were identified by the data reviewer.