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 collecting 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 being provided to Appalachian Power Company’s Mountaineer 

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

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

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

mercury and cyanide at the carbon capture wastewater treatment effluent sampling point, 

if the plant treats the carbon capture wastewater on site. 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 carbon capture wastewater and provide a description of 

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

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

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

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

hours). 

Samples must be collected Monday through Thursday 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 suitable 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 through 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 carbon capture wastewater generated from the carbon 

capture process prior to any 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 carbon capture wastewater treatment system, 

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

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

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

located on site and the treatment system is treating only the carbon capture 

wastewater. 

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

carbon capture wastewater generation, the carbon capture wastewater 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 Analytical Methods Included in the Sampling Program 

Parameter Method Number 

Classicals

Biochemical oxygen demand (BOD5) SM 5210 B 

Chemical oxygen demand (COD) EPA 410.4 

Total suspended solids (TSS) SM 2540 D 

Total dissolved solids (TDS) SM 2540 C 

Sulfate EPA 300.0 

Chloride EPA 300.0 

Ammonia as nitrogen EPA 350.1 

Nitrate/nitrate as nitrogen EPA 353.2 

Total Kjeldahl nitrogen (TKN) EPA 351.2 

Total phosphorus EPA 365.1 

Total cyanide SM 4500 CN E 

Total Metals

Total mercury EPA 1631E 

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

selenium, silver, thallium, 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 are 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 preserve the samples with sulfuric acid after 

sample collection, or the plant can order 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 presence of chlorine). If sulfide is present, 

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

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

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

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

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

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

cyanide. 
Table 2. Summary of Sample Container and Planned Preservation 

Parameter 

Sample Container 

and Volume On-Site Preservation 

BOD5 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 

H2SO4 to pH <2, ≤6°C 

Total cyanide One 1-L HDPE 

bottle 

Dilution until sulfide is not detected, 

NaAsO2 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, TDS, sulfate, and chloride. 

(b) Group II includes ammonia as nitrogen, COD, nitrate/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 completed in indelible ink and must contain the 

following information: 

• Sample number (see Table 3); 

• Sampling episode number (see Table 3); 

• Sampling point/description (see Table 3); 

• Date of sample collection; 

• Analysis to be performed; 

• Sample bottle type; and 

• Required on-site preservation. 

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

Once applied to the sample container, the plant must 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 outer plastic bag of the sample bottle. To 
ensure that the sample label does not become separated from the bottle, the doublebagged sample bottle should be placed in an additional 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 descriptions, 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 should be provided on the sample bottle labels for 

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

the 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 capture wastewater treatment effluent 

laboratory composite samples. The bottles 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 Wastewater - Set 1 72491 6575 

Untreated Carbon Capture Wastewater - Set 2 72492 6575 

Untreated Carbon Capture Wastewater - Set 3 72493 6575 

Untreated Carbon Capture Wastewater - 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) Classicals1 

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 sets2 

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 sample sets, but the plant must use the sample number 

and sampling point description associated with the correct 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 team should follow the clean hands/dirty hands 

sampling techniques outlined in EPA Method 1669. Additionally, the plant must try to 
avoid significant contamination during sample collection, especially from sources such as 

airborne particles, dirt, and corrosion particulates from piping, railing, etc. 

The plant must collect grab samples for all 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 mercury 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 mercury grab collected every six 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 samples 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 treatment 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 cyanide grab samples at the carbon capture 

wastewater treatment effluent sampling point. Please note that the 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 the grab sample collection of the cyanide and 

mercury samples. Additionally, the description 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 effluent 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 Tyvek® 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 cleanbox open with the clips located 

inside the box. 

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

tubing, a “T” splitter, and two additional 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 threaded 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 directly 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 the metals field blank water and the 

field blank composite container. Clean 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 mouth 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 purging of the tubing and collection of 

the field blank sample volume, dirty 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 silicone tubing, replaces the lid on the 

field blank composite container, places the silicone tubing back in the 

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

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

7. 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. Dirty 

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

the sample tap valve to allow the wastewater to flow through the tubing. 

Dirty hands operates the pump to purge the pump portion of the tubing for 

a minimum of 2 minutes. 

8. Dirty hands programs the automatic compositor 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 hands calibrates the compositor to ensure 

that 830 mL is being collected for each individual grab. 

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

hands opens the inner bag and connects the silicone tubing to the port on 

the composite container, securing the 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 composite container and covers the port 

with a closed lid or small plastic bag. The samplers transport each of the 
composite containers, including the field 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 through 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 supplies and bottles for the 

sample collection. 

13. Clean hands and dirty hands put on Tyvek® 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 cleanbox open with the clips located 

inside the box. 

15. Dirty hands opens the opening on the peristaltic 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 tubing into the peristaltic pump head. 

17. Dirty hands shakes the field blank composite 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 composite container. Clean hands places 

the end of the silicone tubing in the 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 inner bag and bottle in the outer bag 

and dirty hands closes the outer bag. 

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

then opens the outer bag of the large composite container for the metals 

samples and clean hands opens the inner bag. Clean hands transfers the 

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

sample composite container. 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 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 the 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 inner 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 BOD5, 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 Tyvek® 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 sample 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 the 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 unscrews the lid. Clean hands then opens 

the inner bag of the total mercury and 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 closes 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 the sample tap and purges the tap for at 

least two minutes, then keeps the valve 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 inner 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 total 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 the information provided in the “Sample 

Bottles and Preservation” section of these instruction for the preservation 

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

should be placed on ice immediately after 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 bottle threads are dirty to where the lid is impeded 

from closing, clean the threads on the 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 sample bottle. Enclose each “bubblewrapped” container and plastic container in an individual sealable plastic 

freezer bag. 

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

ship samples to the laboratories. 

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

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

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

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

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

ice inside two one-gallon sealable freezer bags. Put at 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 garbage 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 the 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 cooler between the interior and outer 

garbage bags to keep the samples cold. 

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

coolers with additional cushioning material. Sufficient 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 secured to the inside of the top of the 

cooler(s). NOTE: the top page of the traffic 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 label on the lid of the cooler(s). The 

classicals and metals samples should 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 garbage bag by tying, or with a twist-tie. 

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

by tying, or with a twist-tie. 

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

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

containers will not shift during shipment. 

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

electronically by ERG). Seal the last two pages of the traffic report form 
in a plastic envelope secured to the inside of the top 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 label 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 arrive at the laboratories the following morning. Ship 

the coolers to the laboratories. 

23. After the coolers have been dropped off (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 engineering data regarding the operation of the plant, the carbon 

capture system, and the carbon capture wastewater treatment system during the sample 

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

samples are collected, including pH, temperature, and visual observations, and provide 

the data to EPA after the sample collection period. The engineering data and field 

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

Engineering Data Tables.” The tables are also included at the end of this enclosure. The 
plant must also submit a detailed process flow diagram for the carbon capture process and 

the carbon capture wastewater treatment system, annotated to indicate 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 the generation and treatment of carbon capture 

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

sheets in the Excel® file and e-mail the completed 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 and supervising the sample collection and the 

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

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

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

the same time the engineering data is submitted. 
Complete the following tables for each sampling point

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Sample Collection 

Time 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 4

NOTE: For influent samples, only the grab 1 row needs to be completed.

Plant Name

Sample 

Collection 

Number

Untreated Carbon 

Capture 

Wastewater 

Samples 

Collected as 

Grabs

(Yes or No)

Mercury and Cyanide 

Samples Collected as 

Grabs

(Yes or No)

Carbon Capture WWT 

Effluent Samples 

(Except Mercury & 

Cyanide) Collected as 

24-Hour Composites

(Yes or No)

Tyvek Suits used

(Yes or No)

Dust Masks 

Used for 

Mercury 

(Yes or No)

Clean 

Hands/Dirty 

Hands Sampling 

Techniques Used

(Yes or No)

Description of Sam

Collection Techniq

(if different than 

instructions)

Set 1Set 2Set 3Set 4
Complete the following tables based on the plant operating characteristics during each set of samples collected

Units Operating 

During Sampling 

Day

Units Off-line 

Entire 

Sampling Day

SCRs/SNCRs 

Operating on 

Units FGD Operating

Set 1Set 2Set 3Set 4

(Liters/day) (Liters/day) (Liters/day) (Liters/day) (Liters/day)

Set 1Set 2Set 3Set 4

NOTE: 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, a

well 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 Amou

Used During Each Set of Sampling and Usage

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Carbon 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)

Plant Name Date Unit 1 Unit 1

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 

Plant Name Date Effluent

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 authority provided by Section 308 of the Federal 

Water Pollution Control Act, as amended, 33 USC 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 limitation . . . 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 effluent . . . and provide such other information as 

he may reasonably require." 

Confidentiality

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

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

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

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

Subpart B. The manner of asserting such a claim 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 the 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 decides to make a determination as to whether or 

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

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

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

satisfy the criteria for confidentiality. 

Note that effluent data are not eligible for confidential 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 identified below access to all data (including 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 contractors to assist EPA in performing technical, 

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

guidelines and standards for the Steam Electric Power Generating industry. 

The contractors and subcontractors that will be providing support to EPA during the development 

of these regulations are listed below: 

EPA Office 

Receiving 

Support 

Contractor Name EPA Contract 

No. Type of Support 

Eastern Research Group, 

Inc. 68-C-02-095 Engineering 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 transfer the information described above to the 

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

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

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

In accordance with these confidentiality regulations, you are entitled to provide comments to EPA 

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

in writing within 10 days of your receipt of this 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 directing or supervising the sample collection and engineering data 

preparation for the sampling program must read and 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 supervision, that qualified personnel collected the samples following the 

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

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

data required, and that the sampling and engineering data provided are complete and reflect 

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

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

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

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

B. We understand that we may be required at a later time to justify our claim in detail with 

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

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

Section 308 of the Clean Water Act.

 

Signature of Certifying Official Date 

( ) 

Printed Name of Certifying Official Telephone 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 Data
Table K4-1. Field Measurements for Sample Collection at the PVF Bleed Stream, Mountaineer 

Episode Number 

Sample Collection 

Number 

Date of Sample 

Collection 

Sample Collection 

Time 

Temperature 

(°C) 

6575 PVF Set 1 - Grab 1 1/31/2011 0904 16.4 6575 PVF Set 2 - Grab 1 2/1/2011 0825 35.7 6575 PVF Set 3 - Grab 1 2/2/2011 0915 30.5 6575 PVF Set 4 - Grab 1 2/3/2011 0933 32.1 
Table K4-2. Field Measurements for Sample Collection at the Flue Gas Condensate Stream, Mountai

Episode Number 

Sample Collection 

Number 

Date of Sample 

Collection 

Sample Collection 

Time 

Temperature 

(°C) 

6575 FGC Set 1 - Grab 1 1/31/2011 0828 21.9 6575 FGC Set 2 - Grab 1 2/1/2011 0835 17.7 6575 FGC Set 3 - Grab 1 2/2/2011 0920 24.6 6575 FGC Set 4 - Grab 1 2/3/2011 0938 23.1 
Table K4-3. Sample Collection Procedures Used during the Sampling Episode 

Episode 

Number 

Sample 

Collection 

Number 

Untreated 

Carbon 

Capture 

Wastewater 

Samples 

Collected as 

Grabs 

(Yes or No) 

Mercury 

and 

Cyanide 

Samples 

Collected 

as Grabs 

(Yes or No) 

Carbon Capture 

WWT Effluent 

Samples 

Collected as 24-

Hour Composites

(Yes or No) 

Clean 

Hands/Dirty 

Hands 

Sampling 

Techniques 

Used 

(Yes or No)* 

Description of 

Sample 

Collection 

Technique (if 

different than 

instructions) 

6575 Set 1 Yes Yes None Yes None 6575 Set 2 Yes Yes None Yes None 6575 Set 3 Yes Yes None Yes None 6575 Set 4 Yes Yes None Yes None 

* 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 Operation at Time of Sampling, Mountaineer 

Episode 

Number 

Sample 

Collection 

Number 

Date of Sample 

Collection 

Plant Operation During Sample Collectio

Units Operating 

During Sampling 

Day 

Units Off-line 

Entire Sampling 

Day 

SCRs/SNCRs 

Operating on 

Units 

6575 Set 1 1/31/2011 Unit 1 None SCR 6575 Set 2 2/1/2011 Unit 1 None SCR 6575 Set 3 2/2/2011 Unit 1 None SCR 6575 Set 4 2/3/2011 Unit 1 None SCR 
Table K4-5. Daily Average Flue Gas Flow and MW-Equivalent Power Generation for the Carbon Capture S

Sampling Period, Mountaineer 

Episode 

Number Date 

Daily Average Flue 

Gas Flow to Carbon 

Capture System 

(lbs/hr) 

MW-Equivalent 

Power Generation 

Treated by the 

Carbon Capture 

System (MWn) 

Unit 1 Unit 1 Comments 

6575 1/17/2011 0 0.00 Main unit out of service. 6575 1/18/2011 46,697 4.79 Main Unit returned to service at 

CAP process began start-up at 1

6575 1/19/2011 47,544 5.91 Cap process out of service from 

PM for CAP process repairs. 

6575 1/20/2011 131,019 12.91 

Main Unit load reduced to 700 Mprocess reduced flue gas flow to 4:30 PM due LP expansion joint unit. 

6575 1/21/2011 69,174 6.27 CAP process out of service at 4:

unit reducing load below 200 M

6575 1/22/2011 0 0.00 Cap process outage continued fo

period. 

6575 1/23/2011 109,606 11.07 CAP process began restart at 5:36575 1/24/2011 159,994 15.40 CAP process in service for 24 ho6575 1/25/2011 160,014 15.74 CAP process in service for 24 ho6575 1/26/2011 159,997 15.87 CAP process tripped out of serv

34.5KV feed from switchyard at 

6575 1/27/2011 9,107 0.00 

Process remained out of service drives on the chiller condenser cpower was restored at 11:30 AM 
Table K4-5. Daily Average Flue Gas Flow and MW-Equivalent Power Generation for the Carbon Capture S

Sampling Period, Mountaineer 

Episode 

Number Date 

Daily Average Flue 

Gas Flow to Carbon 

Capture System 

(lbs/hr) 

MW-Equivalent 

Power Generation 

Treated by the 

Carbon Capture 

System (MWn) 

Unit 1 Unit 1 Comments 

6575 1/28/2011 3,441 0.00 Cap process outage continued fo

period. 

6575 1/29/2011 3,415 0.00 Cap process outage continued fo

period. 

6575 1/30/2011 145,083 14.81 CAP process began restart at 1:16575 1/31/2011 137,665 13.78 

CAP process removed from serv10:45 AM to clean flue gas coolindicated signs of pluggage. 

6575 2/1/2011 153,124 15.09 

CAP process removed from serv11:45 PM to clean flue gas cooliindicated signs of pluggage. 

6575 2/2/2011 137,595 13.87 CAP process in service for 24 ho6575 2/3/2011 134,355 13.34 

CAP process removed from serv6:45 PM to clean flue gas coolinindicated signs of pluggage. 
Table K4-6. Carbon Capture Wastewater Generation and Treatment System Flow Rates during Sampling Perio

Mountaineer 

Episode 

Number Date 

Carbon Capture Wastewater Generation and Treatment System Flow Rates 

(gpd) 

Untreated Carbon 

Capture 

Wastewater – 

PVF Bleed 

Untreated Carbon 

Capture Wastewater 

- FGCC 

Dilution Water 

Flow Rate 

Carbon Captu

Wastewater 

Treatment Effl

6575 1/17/2011 0 0 N/A N/A 6575 1/18/2011 812 2,851 N/A N/A 6575 1/19/2011 1,620 2,675 N/A N/A 6575 1/20/2011 4,058 7,513 N/A N/A 6575 1/21/2011 2,651 5,508 N/A N/A 6575 1/22/2011 0 0 N/A N/A 6575 1/23/2011 1,174 4,620 N/A N/A 6575 1/24/2011 1,213 6,138 N/A N/A 6575 1/25/2011 0 7,527 N/A N/A 6575 1/26/2011 4,429 9,911 N/A N/A 6575 1/27/2011 0 0 N/A N/A 6575 1/28/2011 0 0 N/A N/A 6575 1/29/2011 3,884 0 N/A N/A 6575 1/30/2011 0 7,148 N/A N/A 6575 1/31/2011 967 6,813 N/A N/A 6575 2/1/2011 5,136 9,249 N/A N/A 6575 2/2/2011 2,763 6,904 N/A N/A 6575 2/3/2011 3,317 6,103 N/A N/A 

N/A – Not Applicable 
Carbon Capture Wastewater Treatment 

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

Yes 

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 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 Data
NA – Not analyzed. 

ND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

presented in Tables K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quanti

result is a J-value. 1 – Sample arrived at lab outside criteria holding time. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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, Mountaineer 

PVF Bleed Stream (SP-1) 

Analyte Units Method Day 1 Day 2 Day 3 D

ClassicalsAmmonia mg/L 350.1 3,000 38,000 B 35,000 B,4 31,0Nitrate Nitrite as N mg/L 353.2 8.70 9.20 8.30 9.7Nitrogen, Total Kjeldahl mg/L 351.2 6,300 56,000 48,000 4 61,0Biochemical Oxygen Demand mg/L 5210B ND (2.00) NA1 ND (2.00) ND (4Chemical Oxygen Demand mg/L 410.4 80.0 100 82.0 F 93.Chloride mg/L 300.0 NQ (300) NQ (300) NQ (300) NQ (3Sulfate mg/L 300.0 180,000 150,000 130,000 F 190,0Cyanide, Total mg/L 4500 CN E 1.00 0.910 1.20 F 1.7Total Dissolved Solids mg/L 2540C 190,000 160,000 130,000 170,0Total Suspended Solids mg/L 2540D 21.0 27.0 24.0 37.Phosphorus, Total mg/L 365.1 0.110 0.280 0.110 F 0.12Total MetalsAluminum ug/L 200.7 270 600 390 540 Antimony ug/L 200.8 3.00 2.70 2.10 2.8Arsenic ug/L 200.8 41.0 52.0 30.0 F, MI 37.Barium ug/L 200.7 53.0 61.0 54.0 F 62.Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2Boron ug/L 200.7 15,000 B 13,000 B 11,000 B,4 13,0Cadmium ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4
NA – Not analyzed. 

ND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

presented in Tables K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quanti

result is a J-value. 1 – Sample arrived at lab outside criteria holding time. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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, Mountaineer 

PVF Bleed Stream (SP-1) 

Analyte Units Method Day 1 Day 2 Day 3 D

Calcium ug/L 200.7 27,000 22,000 20,000 27,0Chromium ug/L 200.8 690 1,200 970 4, MI 3,30Cobalt ug/L 200.7 57.0 66.0 60.0 110 Copper ug/L 200.8 440 410 300 4 450 Iron ug/L 200.7 2,200 4,600 2,900 7,80Lead ug/L 200.8 6.10 13.0 3.60 8.4Magnesium ug/L 200.7 13,000 13,000 14,000 23,0Manganese ug/L 200.7 880 870 810 1,30Mercury ng/L 1631E 2,000 5,080 3,070 3,96Molybdenum ug/L 200.7 2,900 2,200 2,700 2,70Nickel ug/L 200.8 4,400 B 4,300 B 3,800 B,4 5,60Selenium ug/L 200.8 4,000 5,600 5,100 4 4,90Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) F, MI ND (2Sodium ug/L 200.7 15,000 15,000 14,000 20,0Thallium ug/L 200.8 2.30 2.30 2.00 2.6Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (2Titanium ug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (2Vanadium ug/L 200.8 16.0 26.0 13.0 21.Zinc ug/L 200.7 330 B 260 B 250 B 330 
NA – Not analyzed. 

ND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

presented in Tables K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quanti

result is a J-value. 1 – Sample arrived at lab outside criteria holding time. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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, Mountaineer 

Flue Gas Condensate (SP-2) 

Analyte Units Method Day 1 Day 2 Day 3 Day 

ClassicalsAmmonia mg/L 350.1 210 NQ (1.00) B 1,200 B 120 Nitrate Nitrite as N mg/L 353.2 5.60 0.320 1.10 0.170 Nitrogen, Total Kjeldahl mg/L 351.2 430 150 1,600 780 Biochemical Oxygen Demand mg/L 5210B 2.50 NA1 7.20 NQ (2.5Chemical Oxygen Demand mg/L 410.4 ND (20.0) NQ (20.0) NQ (20.0) NQ (20.Chloride mg/L 300.0 NQ (6.00) NQ (3.00) NQ (15.0) NQ (3.0Sulfate mg/L 300.0 1,200 330 2,300 360 Cyanide, Total mg/L 4500 CN E ND (0.100) ND (0.100) ND (0.100) ND (0.10Total Dissolved Solids mg/L 2540C 1,300 340 2,200 360 Total Suspended Solids mg/L 2540D 11.0 ND (4.00) 10.0 4.00 Phosphorus, Total mg/L 365.1 NQ (0.0500) NQ (0.0500) NQ (0.0500) NQ (0.05Total MetalsAluminum ug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (20Antimony ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.0Arsenic ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.0Barium ug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.0Boron ug/L 200.7 1,600 B 850 B 2,100 B 1,600 
NA – Not analyzed. 

ND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

presented in Tables K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quanti

result is a J-value. 1 – Sample arrived at lab outside criteria holding time. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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, Mountaineer 

Flue Gas Condensate (SP-2) 

Analyte Units Method Day 1 Day 2 Day 3 Day 

Cadmium ug/L 200.8 ND (4.00) ND (4.00) ND (4.00) ND (4.0Calcium ug/L 200.7 670 NQ (400) 8,000 690 Chromium ug/L 200.8 20.0 NQ (8.00) 23.0 23.0 Cobalt ug/L 200.7 ND (20.0) ND (20.0) NQ (20.0) ND (20.Copper ug/L 200.8 8.30 10.0 35.0 6.20 Iron ug/L 200.7 1,400 1,300 4,400 960 Lead ug/L 200.8 NQ (2.00) ND (2.00) NQ (2.00) ND (2.0Magnesium ug/L 200.7 1,300 450 4,600 1,600 Manganese ug/L 200.7 42.0 55.0 240 65.0 Mercury ng/L 1631E 2,970 279 702 277 Molybdenum ug/L 200.7 NQ (40.0) ND (40.0) NQ (40.0) ND (40.Nickel ug/L 200.8 30.0 B 15.0 B 49.0 B 16.0 Selenium ug/L 200.8 150 85.0 180 96.0 Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.0Sodium ug/L 200.7 NQ (10,000) ND (10,000) NQ (10,000) ND (10,0Thallium ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.0Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (20Titanium ug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.Vanadium ug/L 200.8 NQ (10.0) ND (10.0) NQ (10.0) ND (10.Zinc ug/L 200.7 NQ (40.0) B ND (40.0) NQ (40.0) B NQ (40.
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

ND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

presented in Tables K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quanti

result is a J-value. 

Table K5-3. Classical Pollutants 4-Day Average Data Summary for Carbon Capture Wastewater, 

Analyte Unit Method

PVF Bleed Stream (SP-1) 

4-Day Average 

Flue Gas C

4-D

ClassicalsAmmonia mg/L 350.1 26,800 Nitrate Nitrite as N mg/L 353.2 8.98 Nitrogen, Total Kjeldahl mg/L 351.2 42,800 Biochemical Oxygen Demand mg/L 5210B ND (14.7) Chemical Oxygen Demand mg/L 410.4 88.8 NChloride mg/L 300.0 NQ (300) NSulfate mg/L 300.0 163,000 Cyanide, Total mg/L 4500 CN E 1.20 NTotal Dissolved Solids mg/L 2540C 163,000 Total Suspended Solids mg/L 2540D 27.3 Phosphorus, Total mg/L 365.1 0.155 NQ 
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

ND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

presented in Tables K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quanti

result is a J-value. 

Table K5-4. Metal Pollutants 4-Day Average Data Summary for Carbon Capture Wastewater, M

Analyte Unit Method

PVF Bleed Stream (SP-1) 

4-Set Average 

Flue Gas Conde

4-Set Av

Total MetalsAluminum ug/L 200.7 450 NQ (2Antimony ug/L 200.8 2.65 ND (2.Arsenic ug/L 200.8 40.0 NQ (4.Barium ug/L 200.7 57.5 NQ (20Beryllium ug/L 200.7 ND (2.00) ND (2.Boron ug/L 200.7 13,000 1,54Cadmium ug/L 200.8 NQ (4.00) ND (4.Calcium ug/L 200.7 24,000 < 2,39Chromium ug/L 200.8 1,540 < 17Cobalt ug/L 200.7 73.3 NQ (20Copper ug/L 200.8 400 14.9 Iron ug/L 200.7 4,380 2,02Lead ug/L 200.8 7.78 NQ (2.Magnesium ug/L 200.7 15,800 1,99Manganese ug/L 200.7 965 101 Mercury ng/L 1631E 3,530 1,06Molybdenum ug/L 200.7 2,630 NQ (0Nickel ug/L 200.8 4,530 27.5 Selenium ug/L 200.8 4,900 128 Silver ug/L 200.8 ND (2.00) ND (2.Sodium ug/L 200.7 16,000 NQ (10,Thallium ug/L 200.8 2.30 ND (2.Tin ug/L 200.7 ND (200) ND (2
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

ND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

presented in Tables K5-5 through K5-14 with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quanti

result is a J-value. 

Table K5-4. Metal Pollutants 4-Day Average Data Summary for Carbon Capture Wastewater, M

Analyte Unit Method

PVF Bleed Stream (SP-1) 

4-Set Average 

Flue Gas Conde

4-Set Av

Titanium ug/L 200.7 NQ (20.0) NQ (20Vanadium ug/L 200.8 19.0 NQ (10Zinc ug/L 200.7 293 NQ (40
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, Day 1 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL C

Classicals Ammonia 350.1 mg/L 800 44 800 Nitrate Nitrite as N 353.2 mg/L 5 0.095 0.5 Nitrogen, Total Kjeldahl 351.2 mg/L 20 77 1,000 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 Chemical Oxygen Demand 410.4 mg/L 1 4.1 20 Chloride 300.0 mg/L 100 25 300 Sulfate 300.0 mg/L 5,000 1,200 25,000 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 470 1,000 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 
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, Day 1 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL C

Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 500 122 255 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 50 22 100 Selenium 200.8 ug/L 50 16 100 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 NTitanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 
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 K5-6. PVF Bleed Steam, Day 2 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL C

Classicals Ammonia 350.1 mg/L 40 440 8,000 Nitrate Nitrite as N 353.2 mg/L 5 0.095 0.5 Nitrogen, Total Kjeldahl 351.2 mg/L 10 770 10,000 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 100 25 300 Sulfate 300.0 mg/L 5,000 1,200 25,000 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 470 1,000 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 
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 K5-6. PVF Bleed Steam, Day 2 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL C

Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 500 122 255 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 50 22 100 Selenium 200.8 ug/L 50 16 100 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 NTitanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 
ND – Not detected (number in parentheses is the quantitation limit). 

4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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, Day 3 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Con

Classicals Ammonia 350.1 mg/L 20 220 4,000 35,0Nitrate Nitrite as N 353.2 mg/L 5 0.095 0.5 8.3 Nitrogen, Total Kjeldahl 351.2 mg/L 10 770 10,000 48,0Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 82 Chloride 300.0 mg/L 100 25 300 58 Sulfate 300.0 mg/L 5,000 1,200 25,000 130,0Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 1.2 Total Dissolved Solids 2540C mg/L 1 470 1,000 130,0Total Suspended Solids 2540D mg/L 1 1.1 4 24 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.1Total MetalsAluminum 200.7 ug/L 2 9.4 200 390 Antimony 200.8 ug/L 2 0.72 2 2.1 Arsenic 200.8 ug/L 2 1.2 4 30 Barium 200.7 ug/L 2 2.5 20 54 Beryllium 200.7 ug/L 2 0.71 2 ND (Boron 200.7 ug/L 2 6.7 200 11,0Cadmium 200.8 ug/L 2 1.2 4 1.3 Calcium 200.7 ug/L 2 69 400 20,0
ND – Not detected (number in parentheses is the quantitation limit). 

4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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, Day 3 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Con

Chromium 200.8 ug/L 2 3.3 8 970 Cobalt 200.7 ug/L 2 1.1 20 60 Copper 200.8 ug/L 2 0.96 4 300 Iron 200.7 ug/L 2 32 200 2,90Lead 200.8 ug/L 2 0.73 2 3.6 Magnesium 200.7 ug/L 2 21 400 14,0Manganese 200.7 ug/L 2 0.51 20 810 Mercury 1631E ng/L 500 121 252 3,07Molybdenum 200.7 ug/L 2 1.6 40 2,70Nickel 200.8 ug/L 50 22 100 3,80Selenium 200.8 ug/L 50 16 100 5,10Silver 200.8 ug/L 2 0.59 2 ND (Sodium 200.7 ug/L 2 180 10,000 14,0Thallium 200.8 ug/L 2 0.47 2 2 Tin 200.7 ug/L 2 4.8 200 ND (2Titanium 200.7 ug/L 2 1.6 20 13 Vanadium 200.8 ug/L 2 1.7 10 13 Zinc 200.7 ug/L 2 9.1 40 250 
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 K5-8. PVF Bleed Steam, Day 4 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Classicals Ammonia 350.1 mg/L 20 220 4,000 Nitrate Nitrite as N 353.2 mg/L 5 0.095 0.5 Nitrogen, Total Kjeldahl 351.2 mg/L 10 770 10,000 Biochemical Oxygen Demand 5210B mg/L 20 4.7 40 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 100 25 300 Sulfate 300.0 mg/L 5,000 1,200 25,000 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 470 1,000 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 
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 K5-8. PVF Bleed Steam, Day 4 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 500 122 255 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 50 22 100 Selenium 200.8 ug/L 50 16 100 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 
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 K5-9. Flue Gas Condensate, Day 1 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Classicals Ammonia 350.1 mg/L 100 5.5 100 Nitrate Nitrite as N 353.2 mg/L 1 0.019 0.1 Nitrogen, Total Kjeldahl 351.2 mg/L 50 3.8 50 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 1 4.1 20 Chloride 300.0 mg/L 2 0.51 6 Sulfate 300.0 mg/L 50 12 250 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 9.4 20 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 
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 K5-9. Flue Gas Condensate, Day 1 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 500 121 252 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 
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 K5-10. Flue Gas Condensate, Day 2 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Co

Classicals Ammonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 1 0.019 0.1 0Nitrogen, Total Kjeldahl 351.2 mg/L 20 1.5 20 Chemical Oxygen Demand 410.4 mg/L 1 4.1 20 Chloride 300.0 mg/L 1 0.25 3 0Sulfate 300.0 mg/L 10 2.3 50 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 ND Total Dissolved Solids 2540C mg/L 1 4.7 10 Total Suspended Solids 2540D mg/L 1 1.1 4 NPhosphorus, Total 365.1 mg/L 1 0.005 0.05 0.Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 NArsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 NBoron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 NCalcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 ND Copper 200.8 ug/L 2 0.96 4 
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 K5-10. Flue Gas Condensate, Day 2 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Co

Iron 200.7 ug/L 2 32 200 1Lead 200.8 ug/L 2 0.73 2 N

Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 500 121 252 Molybdenum 200.7 ug/L 2 1.6 40 ND Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 NSodium 200.7 ug/L 2 180 10,000 ND (Thallium 200.8 ug/L 2 0.47 2 NTin 200.7 ug/L 2 4.8 200 ND Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 ND Zinc 200.7 ug/L 2 9.1 40 ND 
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 K5-11. Flue Gas Condensate, Day 3 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Classicals Ammonia 350.1 mg/L 5 11 200 Nitrate Nitrite as N 353.2 mg/L 1 0.019 0.1 Nitrogen, Total Kjeldahl 351.2 mg/L 2 15 200 Biochemical Oxygen Demand 5210B mg/L 1 0.59 5 Chemical Oxygen Demand 410.4 mg/L 1 4.1 20 Chloride 300.0 mg/L 5 1.3 15 Sulfate 300.0 mg/L 50 12 250 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 
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 K5-11. Flue Gas Condensate, Day 3 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 100 24.1 50.5 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 
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 K5-12. Flue Gas Condensate, Day 4 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Co

Classicals Ammonia 350.1 mg/L 20 1.1 20 Nitrate Nitrite as N 353.2 mg/L 1 0.019 0.1 Nitrogen, Total Kjeldahl 351.2 mg/L 10 15 200 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 1 4.1 20 Chloride 300.0 mg/L 1 0.25 3 Sulfate 300.0 mg/L 10 2.3 50 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 ND Total Dissolved Solids 2540C mg/L 1 4.7 10 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 NArsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 NBoron 200.7 ug/L 2 6.7 200 1Cadmium 200.8 ug/L 2 1.2 4 NCalcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 N
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 K5-12. Flue Gas Condensate, Day 4 Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Co

Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 NMagnesium 200.7 ug/L 2 21 400 1Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 20 4.83 10.1 Molybdenum 200.7 ug/L 2 1.6 40 NNickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 NSodium 200.7 ug/L 2 180 10,000 ND Thallium 200.8 ug/L 2 0.47 2 NTin 200.7 ug/L 2 4.8 200 ND Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 NZinc 200.7 ug/L 2 9.1 40 Zinc 200.7 ug/L 2 9.1 40 N
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 K5-13. PVF Bleed Stream Field Blank Analytical Results, Mountaineer 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Concentr

Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) Antimony 200.8 ug/L 2 0.72 2 ND (2) Arsenic 200.8 ug/L 2 1.2 4 ND (4) Barium 200.7 ug/L 2 2.5 20 ND (20) Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 2 6.7 200 18 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 ND (400) Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 ND (4) Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 2 21 400 ND (400) Manganese 200.7 ug/L 2 0.51 20 ND (20) Mercury 1631E ng/L 1 0.24 0.5 ND (0.5) Molybdenum 200.7 ug/L 2 1.6 40 ND (40) Nickel 200.8 ug/L 2 0.89 4 ND (4) Selenium 200.8 ug/L 2 0.62 4 ND (4) Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 ND (10,000Thallium 200.8 ug/L 2 0.47 2 ND (2) 
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 K5-13. PVF Bleed Stream Field Blank Analytical Results, Mountaineer 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Concentr

Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 ND (10) Zinc 200.7 ug/L 2 9.1 40 ND (40) 
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 K5-14. Flue Gas Condensate Field Blank Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 NThallium 200.8 ug/L 2 0.47 2 
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 K5-14. Flue Gas Condensate Field Blank Analytical Results, Mountaineer 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 
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 and 6575

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

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

Atomic Fluorescence Spectrometry (CVAFS) analysis. 

Table 1 summarizes the 23 samples (excluding laboratory prep 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 additional 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 analysis day. The initial calibration for 

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

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

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS 

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

criteria. 

BLANKS 

All the preparation blanks or laboratory reagent blanks (LRBs) 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 than 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 qualified based on these preparation blank 

results. 

DUPLICATES 

No field duplicate samples were collected with these sampling episodes. Two samples 

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

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

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

based on these analytical duplicate results. 
3

LABORATORY CONTROL SAMPLES 

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

and 24% RPD. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

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

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

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

DETECTION LIMITS 

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

were reported as not detected (ND). 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

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

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Randy Mercurio, ERG 

Date: 2/9/2012 

Subject: TestAmerica Data Review Narrative for Total Metals by 200.8 – 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 Method 200.8. 

Table 1 summarizes the samples TestAmerica extracted and 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 according to TestAmerica’s “FGD 

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

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

EPA Method 200.8, by ICP/MS analysis. 
2

Any significant findings are summarized below. Additional 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 the method criteria. 

INITIAL CALIBRATION 

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

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

INITIAL AND CONTINUING CALIBRATION VERIFICATION (ICV/CCV) 

The initial calibration verifications (ICV) and continuing calibration verifications (CCV) 

performed by TestAmerica all had recoveries within the method criteria. 

METHOD/INSTRUMENT BLANKS 

All the method blanks were less than the reporting limit (RL). 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 limits of 50–150% recovery. 

LABORATORY CONTROL SAMPLES (LCS) 

All LCS samples passed the method QC limits of 85–115% recovery. 
3

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION 

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

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

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

ICS. 

All interference check sample B (ICSAB) synthetic spikes recovered within 

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

SERIAL DILUTION 

The serial dilution performed on sample 72493 passed TestAmerica’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 dilutions. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

MS and MSD were performed on sample 72493. The MS/MSD of sample 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 samples 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. Arsenic 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 control limits of 85–115% 

recovery for all analytes, except for arsenic, chromium, copper, selenium, and silver, 

which were flagged with a “W” qualifier. Chromium also failed 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 Table 2 below. 
4

DETECTION LIMITS 

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

of reagent water. 

Table 2. Data Review Summary 

Sample Analyte Qualifier/Action Reason Level Detected 

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, EPA EAD 

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Randy Mercurio, ERG 

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.7 – 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 were analyzed according to 

EPA Method 200.7. 

Table 1 summarizes the samples TestAmerica extracted and 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 

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 according to TestAmerica’s SOP for 

ICP Analysis for Trace Metals by Method 200.7. Any significant findings are 

summarized below. No additional data qualifiers were required for this data set. 

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

of percent difference less than 10%. 
2

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

barium for sample 72493 failed the EPA method 200.7 control limits 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 calibration 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 and one calibration standard. 

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS 

The initial calibration verifications (ICV) and continuing calibration verifications (CCV) 

performed by TestAmerica all had recoveries within the method criteria. 

METHOD/INSTRUMENT BLANKS 

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

were above the method detection limit (MDL) and were flagged with the “J” qualifier. 

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

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

flagged with the “J” qualifier. 

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

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

LABORATORY CONTROL SAMPLES (LCS) 

The LCS passed the method control limits of 85–115% recovery. 

INTERFERENCE CHECK SOLUTIONS 

Interference checks were performed using the synthetic matrix 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 TestAmerica’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 sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

A MS and MSD was performed on the total sample of 72493. All 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 acceptable 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 were within TestAmerica’s ± 20% 

requirement. 

POST DIGESTION SPIKE (PDS) 

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

recovery for all analytes. No additional data qualifiers were required. 

DETECTION LIMITS 

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

of reagent water. 
1 

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

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

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Donna Tedder, ERG 

Date: 2/9/2012 

Subject: TestAmerica Data Review Narrative for Classicals Analyses – Episode 6575 

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for Sample Episode 6575. All samples were tested for the following analytes: 

• Ammonia by EPA method 350.1, 

• Biochemical Oxygen Demand – 5 day (BOD5) 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 analyzed for the above analytes. 

Table 1. EPA Episode 6575 Classical Analytes – Sample Identification 

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 specified in 40 CFR 136 Table II. All 

samples were preserved appropriately unless otherwise specified below. 

 

If applicable, the appropriate number of standards was used to create a calibration curve. 

If sample results were above the highest standard used to create the curve, the sample was 

diluted and reanalyzed. All sample results were between the lowest and highest standards 

unless noted below. Additionally, unless otherwise noted, all calibration blanks and 

calibration verification samples met the criteria specified in the method. 

If required by the method, the quality control sample (QCS), a secondary source standard 

used to verify calibration, was always within the control limits specified by the method. 

As described below, the analyte of interest was detected above the method detection limit 

(MDL) in some laboratory reagent blanks (LRB). However, the analyte of interest was 

never detected above the reporting limit (RL) in the LRBs. If required by the method, all 

laboratory fortified blanks (LFB) met the criteria specified in the method unless specified 

below. 

If required by the method, a matrix spike (MS) sample was 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 samples 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 greater 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 qualification was required. 

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

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

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

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

flagged with a “4” qualifier. 

BOD5 

BOD was not performed on samples 72492 and 72496 because they were 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 preserved with sulfuric 

acid. 
3 

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

specified in SM 5210B. 

Laboratory duplicate analyses were performed on samples 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 sulfate recoveries for 

sample 72493 were below the EPA method 300.0 control limits and 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 recoveries for sample 

72493 were 122% and 112%, respectively, which are below the control 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 requirement 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/MSD recoveries 

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

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

there are no criteria for MS/MSD analyses specified in 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 recoveries 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 and 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 recoveries were 136% 

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

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

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

TSS 

No issues were identified by the data reviewer.