Appendix B

We Energies’ Pleasant Prairie Power 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 We Energies’ Pleasant Prairie Power Plant to aid 

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

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

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

and cyanide at the effluent from the FGD wastewater treatment sampling point. At the 

FGD wastewater treatment effluent, the plant must collect cyanide as a single grab 

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

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

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

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

letter of this request. If the plant has any questions 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 once per month for four months, based on the schedule 

specified in the letter. Samples are to be collected from each of the two sampling points 

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

for this sampling program. The following is a description of the two sampling points: 

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

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

transferred to the FGD wastewater treatment system prior to any commingling 

with other wastewaters or treatment system recycle streams. This sample should 

be collected from the sample tap located on the secondary hydroclone. 

• FGD wastewater treatment effluent (SP-2): This sampling point shall represent 

the effluent from the FGD wastewater treatment system, prior to mixing with 

dilution water or other streams. This sampling point should be collected from the 

sample tap that is located on the wastewater piping downstream of the effluent 

storage tanks; where the plant collects its samples associated with its NPDES 

internal monitoring point. 

Analytes

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

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

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

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

Table 1. Analytes and Analytical Methods Included in the Monitoring 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, vanadium, and zinc 

EPA 200.8 with collision 

cell 

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

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

EPA 200.7 
Secondary 

Hydrocyclone 

Overflow

Lime

Organosulfide

Ferric 

Chloride Polymer Hydrochloric 

Acid

Treated 

Effluent to Discharge

To Sludge Disposal

Equalization 

Tank Reaction Tank 1

Primary Clarifier

Reaction 

Tank 2

Reaction 

Tank 3

Flash 

Mix Tank

Flocculation 

Tank

Secondary 

Clarifier

Treated 

Wastewater 

Storage 

Tanks

Sludge Holding 

Tank

Filter Press

Filtrate 

Sump

SP-1

SP-2

Indicates a Sampling Point

Treated 

Effluent 

Recycle

Polymer Hydrochloric 

Acid

Figure 1. Pleasant Prairie FGD Wastewater Treatment System Monitoring Program Sampling Points
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 FGD 

wastewater treatment effluent 

Four 125-mL glass 

bottles 

Influent samples and field blank samples Two 250-mL glass 

bottles 

None 

(acid preserve at laboratory) 

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

(b) Group II includes ammonia as nitrogen, COD, nitrate/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 metal 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. 

Table 3 provides the sampling point descriptions, sample numbers, and sampling episode 

number for the plant for this monitoring program. 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 influent and field blank samples); 

• Total Mercury – Grab 1 (for FGD 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 Monitoring 

Program 

 

Sampling Point Description Sample Number Sampling Episode Number 

FGD Wastewater Treatment Influent – Set 1 72041 6566 

FGD Wastewater Treatment Influent – Set 2 72042 6566 

FGD Wastewater Treatment Influent – Set 3 72043 6566 

FGD Wastewater Treatment Influent – Set 4 72044 6566 

FGD Wastewater Treatment Effluent – Set 1 72045 6566 

FGD Wastewater Treatment Effluent – Set 2 72046 6566 

FGD Wastewater Treatment Effluent – Set 3 72047 6566 

FGD Wastewater Treatment Effluent – Set 4 72048 6566 

FGD Wastewater Treatment Influent Field Blank 72049 6566 

FGD Wastewater Treatment Effluent Field Blank – Set 1 72050 6566 

FGD Wastewater Treatment Effluent Field Blank – Set 2 72051 6566 

FGD Wastewater Treatment Effluent Field Blank – Set 3 72052 6566 

FGD Wastewater Treatment Effluent Field Blank – Set 4 72053 6566 

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 

FGD Wastewater 

Treatment Influent 

Collected during one 

of the four sets 

Collected during one 

of the four sets 

No field blanks 

required 

FGD Wastewater 

Treatment Effluent 

Collected during all 

four sets 

Collected during all 

four sets 

No field blanks 

required 

1

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

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

analyses; however, no additional sample volume is 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 influent to the FGD wastewater 

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

except cyanide and mercury at the FGD 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 FGD 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 FGD wastewater treatment 

effluent sampling point, the plant must collect a single grab sample after the one of the 

mercury grab samples. 

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

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

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

up the composite containers, and perform the composite pump-off procedures for the FGD 

wastewater treatment effluent sampling point. The following instructions can be used to 

collect the grab samples at the influent to the FGD wastewater treatment system sampling 

point and for the mercury and cyanide grab samples at the FGD wastewater treatment 

effluent sampling point: (NOTE: If a sample tap or valve is not available to collect these 

samples or if the FGD wastewater treatment effluent sampling point has intermittent flows 

which may interfere with the automatic composite collection, please contact TJ Finseth, 

(703) 633-1698 to discuss possible alternatives.) 

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

the sample collection. 

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

gloves. 

3. Dirty hands gets a clear plastic bag and opens it 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 bag. 

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 

Bottle 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 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

The plant must provide engineering data regarding the operation of the plant and FGD 

systems 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,” which will be provided by ERG. 

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

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

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

Certification Statement 

The individual responsible for directing and supervising the 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 1Set 2Set 3Set 4

Plant Name

Sample 

Collection 

Number

Unit Overflow 

Sampled at 

Influent 

(7 or 8)

Influent Samples 

Collected as Grabs

(Yes or No)

Mercury and Cyanide 

Samples Collected as 

Grabs

(Yes or No)

Effluent Samples 

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 Sample 

Collection Technique (if 

different than 

instructions)

Description of Abnormal 

Conditions in FGD System 

or FGD Wastewater 

Treatment System that May 

Impact Concentrations

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

Set 1Set 2Set 3Set 4

Flow Rate (gpm) Duration

Set 1Set 2Set 3Set 4

Lime Usage 

(tons)

Ferric Chloride 

Usage 

(Liters/day)

Organosulfide Usage 

(Liters/day)

Polymer Usage 

(Liters/day)

Acid Usage 

(Liters/day)

Chemical 

Precipitation 

System Effluent Flow Rate (gpd)

Set 1Set 2Set 3Set 4

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Plant Operation During Sample Collection

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Plant Operation During Sample Collection

Scrubber Slurry Blowdown Flow 

Rate Scrubber Slurry 

Percent Solids

Percent Hydroclone 

Overflow Recycled 

Back to Scrubber

FGD Wastewater Treatment Operation During Sample Collection

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Scrubber Purge 

Flow Rate During 

Influent Sample 

Collection

(gpm)
Unit 1 Unit 2

Daily Power Generation (MW-hrs)

Plant Name Date

Provide the daily power generation for each scrubbed unit starting two weeks prior to the first 

set of samples through the last set of samples
FGD Wastewater Treatment System Flow 

Rates

(gpd)

Plant Name Date Chemical Precipitation Effluent

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

table starting two weeks prior to the first set of samples through the last set of samples
Enclosure 2 

Authority

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

Water Pollution Control Act, as amended, 33 USC 1318. 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 the 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 follow-on 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
MEMORANDUM 

TO: Ron Jordan, EPA 

Jezebele Alicea, EPA 

FROM: TJ Finseth, ERG 

 

DATE: 12 November 2010 

SUBJECT: Notes from On-Site Review of Industry Self-Monitoring Sampling at We 

Energies’ Pleasant Prairie Power Plant on November 2-3, 2010 

 ERG conducted an on-site review of the self-monitoring sampling conducted at the We 

Energies’ Pleasant Prairie Power Plant (Pleasant Prairie) located in Pleasant Prairie, WI. ERG 

was on site for all sample collection activities that Pleasant Prairie conducted for the second set 

of the industry self-monitoring sampling on November 2 and 3, 2010. These notes summarize 

the sample collection techniques used by Pleasant Prairie at each of the sampling points and 

EPA’s observations/findings from the on-site review. An overall process water diagram for the 

Pleasant Prairie plant is provided as Attachment 1. The checklists that EPA completed as part of 

the on-site review are provided as Attachment 2. 

 During this set of the industry self-monitoring, Unit 1 was shut down to replace a layer of 

catalyst in its selective catalytic reduction system. The unit was shut down on October 8, 2010, 

and was expected to commence operation on Friday, November 5, 2010. Therefore, for this set 

of samples, only Unit 2 was operating. 

 

The following sections describe the sample collection at each of the sampling points and 

the observations/findings from each sampling point. 

FGD Wastewater Treatment Influent (SP-1) 

 The FGD wastewater treatment influent consists of the secondary hydrocyclone overflow 

that is transferred to the equalization tank at the beginning of the FGD wastewater treatment 

system; therefore, the samples from this sampling point were collected as grab samples. For this 

sampling point, Pleasant Prairie used a sample tap off of the drain of the secondary hydrocyclone 

overflow piping that transfers the secondary hydrocyclone overflow to the equalization tank. 

This is the same sampling point that EPA used during its sample collection. 

Sample Collection 

 To collect the samples of the FGD wastewater treatment influent, Pleasant Prairie 

personnel followed EPA Method 1669 protocols and the EPA-provided instructions. Pleasant 
Memorandum 

November 9, 2010 

Page 2 

Prairie personnel shrouded the tap with a clean plastic bag and let the sample flow from the tap 

for two minutes prior to collecting any samples. The samplers then collected the samples 

underneath the shroud. At this sampling point, Pleasant Prairie only collected samples for the 

EPA program and did not collect their own split samples. All samples were filled from the tap 

while the samplers held the bottles under the shrouding. 

Preservation 

 Pleasant Prairie personnel followed all method specifications when preserving the 

classical samples. The Group II samples were preserved using H2SO4 and the pH was confirmed 

to be below 2 S.U. The cyanide samples were checked for sulfides and chlorine using lead 

acetate paper and potassium iodide starch paper, respectively. The samplers did not detect 

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

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

were all placed on ice after collection or preservation. 

Field Measurements 

 Pleasant Prairie personnel used a pH probe and a temperature probe to measure the pH 

and temperature of the FGD wastewater influent samples. Pleasant Prairie personnel filled a 

small bottle with sample after collecting the metals samples and prior to collecting the classicals 

samples. After completing the classicals sample collection, Pleasant Prairie personnel 

transported the field test bottle to the laboratory area, poured some of the sample into a small 

beaker, and inserted temperature and pH probes into the beaker with sample. Pleasant Prairie 

personnel stated that they had already calibrated the temperature and pH probes; however, ERG 

did not observe the calibration of the probes. Pleasant Prairie personnel allowed the temperature 

and pH stabilize and then recorded the values. 

Observations/Findings 

 ERG observed the Pleasant Prairie personnel collecting the Set 2 samples of the FGD 

wastewater treatment influent stream. Pleasant Prairie did not collect the field blanks during the 

sample collection activities because they were collected during Set 1. Pleasant Prairie personnel 

followed all applicable procedures during the sample collection. Pleasant Prairie personnel used 

the correct techniques to preserve the classicals samples. The Group II samples were preserved 

18 minutes after collection. 

FGD Wastewater Treatment Effluent (SP-2) 

 The FGD wastewater treatment effluent stream is the effluent from a chemical 

precipitation system used to treat the Pleasant Prairie FGD wastewater; therefore, the samples for 

this sampling point were collected as composite samples, except for the mercury and cyanide 

samples. For the composite samples at this sampling point, Pleasant Prairie collected the 

samples using the plant’s existing compliance monitoring point and the existing ISCO auto 

sampler, which is not the same sampling point that EPA used during its sample collection; 
Memorandum 

November 9, 2010 

Page 3 

however, the two sampling points are both on the same wastewater piping and there are no 

chemical additions or process operations that occur between the two sampling points. The 

Pleasant Prairie auto sampler is configured with a piece of tubing that connects a tap on the 

wastewater piping to a three-way control valve. The valve is controlled by the ISCO auto 

sampler to either pull sample to the compositor or purge sample to the drain. When the ISCO 

sampler is preparing to collect a sample, the valve opens the line to the drain to let fresh sample 

enter the tubing and once the line is flushed, the valve switches to allow the sample to be pulled 

to the compositor. For the mercury and cyanide grab samples at this sampling point, Pleasant 

Prairie collected the samples from one of the effluent samples taps, which are the same taps that 

were used by EPA during its sample collection. 

Sample Collection 

 To collect the samples of the FGD wastewater treatment effluent, Pleasant Prairie 

personnel followed EPA Method 1669 protocols and the EPA-provided instructions. To collect 

the composite samples, Pleasant Prairie personnel replaced the tubing that connects the threeway control valve to the ISCO auto sampler with specially-cleaned silicone tubing. Pleasant 

Prairie personnel attached one end of the specially-cleaned silicone tubing to the outlet from the 

three-way control valve and the other end was threaded through the ISCO 6712 auto sampler and 

attached to a vented cap on a 20-liter carboy. The samplers programmed the compositor to 

collect 830 mL of sample every hour for a 24-hour period. After the 24-hour period, the 

samplers removed the composite tubing from the ISCO auto sampler and replaced it with a short 

piece of Teflon® tubing connected to a length of silicone tubing to transfer the samples to 

individual sample bottles. The samplers first shook the 20-liter container to homogenize the 

sample and then they attached a pump-off cap onto the carboy. The Teflon® end of the tubing 

was then inserted into the carboy and the tubing was purged with two liters of sample. Pleasant 

Prairie personnel then collected the metals samples using a cleanbox. Additionally, the plant 

collected multi-fill splits in the cleanbox. After all the metals samples were collected, the 

samplers filled the classical samples outside the cleanbox. Pleasant Prairie collected multi-fill 

split samples for the Group I and Group II samples; however, for the BOD and cyanide samples, 

the samplers only collected samples for the EPA program. 

 Pleasant Prairie personnel also collected grab samples for mercury every six hours during 

the sampling. The samplers collected the mercury samples at this sampling point by shrouding 

one of their effluent sample taps with a clean plastic bag and letting sample flow through the 

sample tap for two minutes prior to collecting any samples. Pleasant Prairie personnel filled the 

mercury bottles directly from the tap, underneath the shroud. The samplers collected the 

mercury samples as multi-fill splits. Pleasant Prairie personnel also collected the cyanide 

samples as a grab sample immediately after the first of the four mercury grab samples at the 

sampling point. Pleasant Prairie personnel did not collect a cyanide split sample. 

Preservation 

 Pleasant Prairie personnel followed all method specifications when preserving the 

classicals samples, which are the same as those described in the Preservation section for the FGD 
Memorandum 

November 9, 2010 

Page 4 

wastewater treatment influent stream. Additionally, the plant kept the composite container on 

ice during the sample collection time period. 

Field Measurements 

 Pleasant Prairie personnel did not collect a field test sample to test for the temperature 

and pH. Instead, the samplers calibrated the inline temperature and pH probes at the effluent 

sampling location prior to the sampling episode and recorded the temperature and pH at the time 

each mercury grab was collected, which was every six hours. ERG was not present at the time 

the temperature and pH probes were calibrated. 

Observations/Findings 

ERG/EPA observed the Pleasant Prairie personnel collecting the composite set up, composite 

breakdown, and composite pump off for the Set 2 samples. Pleasant Prairie personnel collected 

field blank samples for the total metals samples during this set. ERG also observed the Grab 1 

and 2 mercury grab samples and the cyanide grab sample. Pleasant Prairie personnel collected 

the mercury field blank sample during the Grab 1 sample. Pleasant Prairie personnel followed 

all applicable procedures during the sample collection and preservation, except the samplers did 

not test the temperature of the composite carboy after the completion of the compositing period. 

ERG communicated this issue to the samplers to allow them to fix this for the remaining 

samples. 

 ERG noted that the Pleasant Prairie personnel replaced the tubing that connected the 

three-way control valve to the ISCO auto sampler; however, the Pleasant Prairie personnel did 

not replace the tubing that connected the wastewater piping to the three-way control valve. 

Therefore, ERG cannot be certain that there was not contamination from that tubing. ERG 

communicated this issue to the samplers to allow them to fix this for the remaining samples. 

 ERG also noted that the ISCO 6712 auto sampler required the samplers to thread the 

tubing (including the end of the tubing) through the pump to set up the composite tubing; 

however, when the samplers were threading the tubing through the ISCO, the end of the tubing 

was covered with a Ziploc bag to prevent potential contamination. 

 

 

 
Attachment 1 

Overall Process Water Diagram 

Attachment 2 

Checklists 














Section 3

Signed Certification Statement
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 

 

David M. Lee

March 3, 2011

Manager - Water Quality

Wisconsin Electric Power Company

414 221-2158

, d/b/a We Energies

Digitally signed by David M. Lee 

DN: cn=David M. Lee, o=We Energies, ou=Environmental Department, email=David.

Lee@we-energies.com, c=US 

Date: 2011.03.03 10:11:57 -06'00'
Section 4

Engineering Data
Table B4-1. Field Measurements for Sample Collection at the Influent to FGD Wastewater Treatment System, Pleasant Prairie

Episode Number

Sample Collection 

Number

Date of Sample 

Collection

Sample Collection 

Time

Temperature

(°C)

pH

(S.U.)

6566 Set 1 - Grab 1 09/30/10 0808 53.0 6.40

6566 Set 2 - Grab 1 11/03/10 0757 46.1 6.89

6566 Set 3 - Grab 1 12/08/10 0806 50.5 6.70

6566 Set 4 - Grab 1 01/26/11 0756 51.0 6.27
Table B4-2. Field Measurements for Sample Collection at the Effluent from the FGD Wastewater Treatment System, Pleasant 

Prairie

Episode Number

Sample Collection 

Number

Date of Sample 

Collection

Sample Collection 

Time

Temperature

(°C)

pH

(S.U.)

6566 Set 1 - Grab 1 09/29/2010 1019 40.1 6.78

6566 Set 1 - Grab 2 09/29/2010 1617 40.6 6.89

6566 Set 1 - Grab 3 09/29/2010 2210 40.5 6.97

6566 Set 1 - Grab 4 09/30/2010 0410 40.1 6.89

6566 Set 2 - Grab 1 11/02/2010 1034 33.9 7.10

6566 Set 2 - Grab 2 11/02/2010 1630 34.9 7.09

6566 Set 2 - Grab 3 11/02/2010 2228 35.1 7.05

6566 Set 2 - Grab 4 11/03/2010 0423 35.2 7.07

6566 Set 3 - Grab 1 12/07/2010 1010 34.9 7.02

6566 Set 3 - Grab 2 12/07/2010 1604 34.6 6.97

6566 Set 3 - Grab 3 12/07/2010 2206 35.0 7.03

6566 Set 3 - Grab 4 12/08/2010 0402 35.2 7.03

6566 Set 4 - Grab 1 01/25/2011 1008 36.8 7.07

6566 Set 4 - Grab 2 01/25/2011 1558 36.9 7.05

6566 Set 4 - Grab 3 01/25/2011 2155 37.9 6.99

6566 Set 4 - Grab 4 01/26/2011 0357 38.2 7.70
Table B4-3. Sample Collection Procedures Used during the Sampling Episode

Episode 

Number

Sample 

Collection 

Number

Influent 

Samples 

Collected as 

Grabs

(Yes or No)

Mercury 

and Cyanide 

Samples 

Collected as 

Grabs

(Yes or No)

Bioreactor Influent 

and Bioreactor 

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)

Description of Abnormal 

Conditions in FGD 

System or FGD 

Wastewater Treatment 

System that May Impact 

Concentrations

6566 Set 1 Yes Yes Yes Yes None None

6566 Set 2 Yes Yes Yes Yes None None

6566 Set 3 Yes Yes Yes Yes None None

6566 Set 4 Yes Yes Yes Yes None None

* Includes the use of tyveks suits during all sampling events and dust masks during the collection of mercury samples.
Table B4-4. Generating Unit Operation at Time of Sampling, Pleasant Prairie

Episode Number

Sample Collection 

Number

Date of Sample 

Collection

Plant Operation During Sample Collection

Units Operating 

During Sampling 

Day

Units Off-line Entire 

Sampling Day

SCRs/SNCRs 

Operating on 

Units

6566 Set 1 09/30/10 Unit 1/2 None SCR

6566 Set 2 11/03/10 Unit 1/2* None SCR

6566 Set 3 12/08/10 Unit 1/2 None SCR

6566 Set 4 01/26/11 Unit 1/2 None SCR

* Unit 1 was in start up mode on November 3, 2010. The FGD system was in service, but the unit had not yet reached high enough steam pressure 

to generate power.
Table B4-5. FGD Scrubber Slurry Information at Time of Sampling, Pleasant Prairie

Episode 

Number

Sample 

Collection 

Number

Date of Sample 

Collection

Plant Operation During Sample Collection

Scrubber Slurry Blowdown 

Flow Rate

Scrubber 

Slurry 

Percent 

Solids

Percent Hydroclone 

Overflow Recycled 

Back to Scrubber**

Flow Rate 

(gpm) Duration*

6566 Set 1 09/30/10 500 continuous 20% 75%

6566 Set 2 11/03/10 500 continuous 20% 75%

6566 Set 3 12/08/10 500 continuous 20% 75%

6566 Set 4 01/26/11 530 continuous 20% 75%

* Primary hydroclone flow on both scrubbers was 24 hr/day on sampling days, with minor flow rate variation.

** Based on system design.
Table B4-6. FGD Wastewater Treatment System Operation Information, Pleasant Prairie

Episode 

Number

Sample 

Collection 

Number

Date of Sample 

Collection

Scrubber Purge 

Flow Rate During 

Influent Sample 

Collection

(gpm)

FGD Wastewater Treatment Operation During Sample Collection

Lime 

Usage 

(tons)*

Ferric 

Chloride 

Usage 

(Liters/day)

Organosulfide 

Usage 

(Liters/day)

Polymer Usage 

(Liters/day)*

Acid Usage 

(Liters/day)

6566 Set 1 09/30/10 46 0.26 40 12 4 20

6566 Set 2 11/03/10 50 0.26 40 7 4 20

6566 Set 3 12/08/10 40 0.26 37 7 4 10

6566 Set 4 01/26/11 46 0.26 36 9 4 20

* Based on longer-term averages.
Table B4-7. Daily Power Generation During Sampling Period, Pleasant Prairie

Episode Number Date

Daily Power Generation

(MW-hrs)

Unit 1 Unit 2

6566 09/15/10 12,936 13,098

6566 09/16/10 12,706 11,819

6566 09/17/10 13,104 12,332

6566 09/18/10 8,875 9,315

6566 09/19/10 7,944 7,969

6566 09/20/10 12,097 12,013

6566 09/21/10 12,205 12,653

6566 09/22/10 12,716 11,551

6566 09/23/10 12,679 12,378

6566 09/24/10 11,106 11,870

6566 09/25/10 9,575 10,867

6566 09/26/10 9,743 9,506

6566 09/27/10 11,049 11,837

6566 09/28/10 10,076 12,660

6566 09/29/10 9,907 12,814

6566 09/30/10 7,573 11,345

6566 10/01/10 13,324 13,968

6566 10/02/10 11,830 10,509

6566 10/03/10 10,912 11,253

6566 10/04/10 13,808 12,960

6566 10/05/10 12,882 13,331

6566 10/06/10 13,443 13,067

6566 10/07/10 12,649 12,761

6566 10/08/10 13,325 13,146

6566 10/09/10 12,823 13,034

6566 10/10/10 12,624 12,533

6566 10/11/10 13,043 13,177

6566 10/12/10 13,517 13,862

6566 10/13/10 12,949 13,179

6566 10/14/10 12,316 12,052

6566 10/15/10 11,037 12,810

6566 10/16/10 337 12,714

6566 10/17/10 0 11,630

6566 10/18/10 0 13,871

6566 10/19/10 0 13,541

6566 10/20/10 0 13,256

6566 10/21/10 0 13,706

6566 10/22/10 0 13,250

6566 10/23/10 0 13,518

6566 10/24/10 0 12,306

6566 10/25/10 0 13,349
Table B4-7. Daily Power Generation During Sampling Period, Pleasant Prairie

Episode Number Date

Daily Power Generation

(MW-hrs)

Unit 1 Unit 2

6566 10/26/10 0 12,446

6566 10/27/10 0 12,984

6566 10/28/10 0 13,035

6566 10/29/10 0 13,477

6566 10/30/10 0 14,693

6566 10/31/10 0 13,936

6566 11/01/10 0 14,105

6566 11/02/10 0 14,039

6566 11/03/10 0 13,711

6566 11/04/10 14 14,341

6566 11/05/10 9,017 14,539

6566 11/06/10 11,168 11,655

6566 11/07/10 9,547 10,492

6566 11/08/10 12,537 10,077

6566 11/09/10 12,624 10,891

6566 11/10/10 11,942 12,044

6566 11/11/10 11,077 11,165

6566 11/12/10 12,094 12,165

6566 11/13/10 11,534 12,032

6566 11/14/10 11,107 11,110

6566 11/15/10 13,562 13,311

6566 11/16/10 13,228 12,871

6566 11/17/10 13,472 11,778

6566 11/18/10 14,827 327

6566 11/19/10 13,532 0

6566 11/20/10 12,397 0

6566 11/21/10 12,213 0

6566 11/22/10 12,762 0

6566 11/23/10 13,129 0

6566 11/24/10 12,924 0

6566 11/25/10 9,641 0

6566 11/26/10 10,874 0

6566 11/27/10 13,309 0

6566 11/28/10 8,695 981

6566 11/29/10 10,675 10,424

6566 11/30/10 10,997 10,902

6566 12/01/10 12,729 12,752

6566 12/02/10 12,519 12,366

6566 12/03/10 13,429 12,869

6566 12/04/10 9,903 10,388

6566 12/05/10 10,614 10,656

6566 12/06/10 12,564 12,433

6566 12/07/10 12,583 12,910
Table B4-7. Daily Power Generation During Sampling Period, Pleasant Prairie

Episode Number Date

Daily Power Generation

(MW-hrs)

Unit 1 Unit 2

6566 12/08/10 12,023 12,472

6566 12/09/10 11,050 11,248

6566 12/10/10 12,274 12,137

6566 12/11/10 9,536 9,610

6566 12/12/10 10,193 10,036

6566 12/13/10 13,350 13,785

6566 12/14/10 12,281 11,699

6566 12/15/10 10,525 10,476

6566 12/16/10 10,944 12,950

6566 12/17/10 12,545 12,750

6566 12/18/10 13,306 11,192

6566 12/19/10 14,780 11,925

6566 12/20/10 13,528 11,878

6566 12/21/10 13,883 11,090

6566 12/22/10 13,652 11,642

6566 12/23/10 12,953 10,966

6566 12/24/10 11,680 9,750

6566 12/25/10 8,506 8,428

6566 12/26/10 8,773 8,600

6566 12/27/10 11,568 10,752

6566 12/28/10 11,927 12,074

6566 12/29/10 8,687 9,463

6566 12/30/10 9,077 8,153

6566 12/31/10 9,461 9,259

6566 01/01/11 8,179 8,674

6566 01/02/11 10,569 9,834

6566 01/03/11 12,519 11,894

6566 01/04/11 12,510 12,174

6566 01/05/11 13,534 12,950

6566 01/06/11 12,605 12,643

6566 01/07/11 10,131 9,895

6566 01/08/11 12,158 11,522

6566 01/09/11 10,544 12,371

6566 01/10/11 12,844 12,669

6566 01/11/11 12,309 12,034

6566 01/12/11 9,949 9,759

6566 01/13/11 11,856 11,852

6566 01/14/11 12,389 10,630

6566 01/15/11 11,932 10,122

6566 01/16/11 9,617 9,585

6566 01/17/11 10,131 9,583

6566 01/18/11 10,627 11,009

6566 01/19/11 11,297 10,893
Table B4-7. Daily Power Generation During Sampling Period, Pleasant Prairie

Episode Number Date

Daily Power Generation

(MW-hrs)

Unit 1 Unit 2

6566 01/20/11 11,869 10,645

6566 01/21/11 11,624 10,516

6566 01/22/11 12,454 10,686

6566 01/23/11 8,778 9,953

6566 01/24/11 12,357 12,182

6566 01/25/11 13,042 13,041

6566 01/26/11 13,381 12,695

Note: Unit 1 was shut down from October 17 – November 4, 2010 to replace SCR catalyst. Unit 2 was 

shut down from November 19 – 28, 2010 to repair a superheater tube leak. The plant does not expect that 

these shut downs had any major impact on the wastewater samples collected during or near these outages.
Table B4-8. FGD Wastewater Treatment System Flow Rate during Sampling Period, 

Pleasant Prairie

Episode Number Date

FGD Wastewater Treatment System Flow Rates

(gpd)

Chemical Precipitation Effluent

6566 09/15/10 66,519

6566 09/16/10 46,657

6566 09/17/10 65,405

6566 09/18/10 49,088

6566 09/19/10 7,462

6566 09/20/10 27,287

6566 09/21/10 55,058

6566 09/22/10 51,324

6566 09/23/10 68,913

6566 09/24/10 57,490

6566 09/25/10 59,318

6566 09/26/10 11,389

6566 09/27/10 28,910

6566 09/28/10 50,103

6566 09/29/10 57,805

6566 09/30/10 57,705

6566 10/01/10 64,702

6566 10/02/10 58,417

6566 10/03/10 0

6566 10/04/10 26,776

6566 10/05/10 57,176

6566 10/06/10 62,193

6566 10/07/10 52,653

6566 10/08/10 65,033

6566 10/09/10 53,279

6566 10/10/10 0

6566 10/11/10 28,732

6566 10/12/10 41,366

6566 10/13/10 15,276

6566 10/14/10 57,590

6566 10/15/10 48,246

6566 10/16/10 38,595

6566 10/17/10 42,249

6566 10/18/10 67,006

6566 10/19/10 47,189

6566 10/20/10 52,341

6566 10/21/10 66,490

6566 10/22/10 58,215

6566 10/23/10 41,733
Table B4-8. FGD Wastewater Treatment System Flow Rate during Sampling Period, 

Pleasant Prairie

Episode Number Date

FGD Wastewater Treatment System Flow Rates

(gpd)

Chemical Precipitation Effluent

6566 10/24/10 0

6566 10/25/10 33,651

6566 10/26/10 11,023

6566 10/27/10 39,026

6566 10/28/10 65,718

6566 10/29/10 38,183

6566 10/30/10 42,073

6566 10/31/10 12,071

6566 11/01/10 25,020

6566 11/02/10 54,967

6566 11/03/10 57,603

6566 11/04/10 66,572

6566 11/05/10 25,674

6566 11/06/10 0

6566 11/07/10 0

6566 11/08/10 153

6566 11/09/10 22,710

6566 11/10/10 59,203

6566 11/11/10 36,795

6566 11/12/10 64,266

6566 11/13/10 57,444

6566 11/14/10 0

6566 11/15/10 21,620

6566 11/16/10 48,053

6566 11/17/10 57,285

6566 11/18/10 63,463

6566 11/19/10 47,348

6566 11/20/10 54,652

6566 11/21/10 15,375

6566 11/22/10 32,175

6566 11/23/10 49,798

6566 11/24/10 57,785

6566 11/25/10 55,649

6566 11/26/10 56,615

6566 11/27/10 52,735

6566 11/28/10 15,436

6566 11/29/10 25,575

6566 11/30/10 58,290

6566 12/01/10 58,104

6566 12/02/10 38,057

6566 12/03/10 59,997
Table B4-8. FGD Wastewater Treatment System Flow Rate during Sampling Period, 

Pleasant Prairie

Episode Number Date

FGD Wastewater Treatment System Flow Rates

(gpd)

Chemical Precipitation Effluent

6566 12/04/10 56,449

6566 12/05/10 8,148

6566 12/06/10 21,975

6566 12/07/10 60,070

6566 12/08/10 55,510

6566 12/09/10 47,693

6566 12/10/10 62,496

6566 12/11/10 59,826

6566 12/12/10 2,430

6566 12/13/10 24,737

6566 12/14/10 42,010

6566 12/15/10 69,009

6566 12/16/10 49,713

6566 12/17/10 60,752

6566 12/18/10 58,909

6566 12/19/10 0

6566 12/20/10 0

6566 12/21/10 34,848

6566 12/22/10 51,044

6566 12/23/10 62,279

6566 12/24/10 53,463

6566 12/25/10 60,912

6566 12/26/10 306

6566 12/27/10 29,573

6566 12/28/10 63,829

6566 12/29/10 52,017

6566 12/30/10 63,769

6566 12/31/10 59,315

6566 01/01/11 53,767

6566 01/02/11 0

6566 01/03/11 27,029

6566 01/04/11 45,561

6566 01/05/11 63,453

6566 01/06/11 63,374

6566 01/07/11 60,008

6566 01/08/11 55,355

6566 01/09/11 0

6566 01/10/11 0

6566 01/11/11 0

6566 01/12/11 0

6566 01/13/11 0
Table B4-8. FGD Wastewater Treatment System Flow Rate during Sampling Period, 

Pleasant Prairie

Episode Number Date

FGD Wastewater Treatment System Flow Rates

(gpd)

Chemical Precipitation Effluent

6566 01/14/11 0

6566 01/15/11 0

6566 01/16/11 0

6566 01/17/11 0

6566 01/18/11 27,094

6566 01/19/11 56,829

6566 01/20/11 43,440

6566 01/21/11 14,766

6566 01/22/11 4,858

6566 01/23/11 11,504

6566 01/24/11 14,662

6566 01/25/11 53,096

6566 01/26/11 43,622

NOTE 1: The FGD wastewater secondary clarifier (a lamella type clarifier) is typically removed from service 

every Saturday to clean scale from the incline section and baffles. Without weekly cleaning, the secondary clarifier 

performance deteriorates to unacceptable levels. Sometimes the system is not returned to service during a 24-hour 

period, so a zero flow for the day will be indicated. Since this is a routine practice, there would be no impact to the 

wastewater samples from one week compared to another. 

NOTE 2: The January flow data had zero flow for a number of consecutive days due to Lake intake warming with 

the wastewater discharge line. (Some or all of the cooling tower blowdown and other wastewaters flowing through 

the common discharge line can be recirculated to the intake structure in Lake Michigan to keep it free from icing.)

During intake warming, the plant does not discharge FGD wastewater effluent to avoid potential cooling tower 

chemistry problems that could arise from mixing the treated FGD wastewater with the cooling tower makeup 

water from the lake. The plant expects that higher concentrations of various constituents could be present in samples 

taken after this period compared to periods of more continuous effluent discharge.
Section 5

Analytical Data
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 limitpresented in Tables B5-6 through B5-18 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitaresult is a J-value. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. 

Table B5-1. Influent to FGD Wastewater Treatment System, Pleasant Prairie 

Analyte Units Method 

Influent to FGD Wastewater Treatment System (

Set 1 Set 2 Set 3 S

ClassicalsAmmonia mg/L 350.1 1.90 2.10 2.30 3.2Nitrate Nitrite as N mg/L 353.2 190 160 160 23Nitrogen, Total Kjeldahl 

mg/L 351.2 64.0 B, Min 34.0 73.0 29

Biochemical Oxygen Demand 

mg/L 5210B ND (2.00) ND (2.00) ND (2.00) ND (2

Chemical Oxygen Demand 

mg/L 410.4 480 450 F 420 52

Chloride mg/L 300.0 2,300 1,800 2,000 3,1Sulfate mg/L 300.0 14,000 14,000 11,000 13,0Cyanide, Total mg/L 4500 CN E 0.290 Est 0.160 0.290 0.3Total Dissolved Solids 

mg/L 2540C 27,000 19,000 23,000 21,0

Total Suspended Solids 

mg/L 2540D 4,200 4,900 4,700 6,4

Phosphorus, Total mg/L 365.1 5.00 8.00 B 0.0560 B 8.8Total MetalsAluminum ug/L 200.7 140,000 170,000 B 87,000 95,0Antimony ug/L 200.8 56.0 57.0 42.0 25Arsenic ug/L 200.8 150 170 110 72
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 limitpresented in Tables B5-6 through B5-18 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitaresult is a J-value. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. 

Table B5-1. Influent to FGD Wastewater Treatment System, Pleasant Prairie 

Analyte Units Method 

Influent to FGD Wastewater Treatment System (

Set 1 Set 2 Set 3 S

Barium ug/L 200.7 840 1,000 B 790 67Beryllium ug/L 200.7 4.60 4.70 3.70 3.3Boron ug/L 200.7 18,000 B 17,000 B 17,000 B 19,0Cadmium ug/L 200.8 12.0 11.0 7.70 8.8Calcium ug/L 200.7 660,000 710,000 B 780,000 610,Chromium ug/L 200.8 1,100 1,100 ^ 690 37Cobalt ug/L 200.7 140 140 130 16Copper ug/L 200.8 900 1,000 680 40Iron ug/L 200.7 390,000 410,000 B 250,000 180,Lead ug/L 200.8 210 270 170 11Magnesium ug/L 200.7 4,600,000 B 4,100,000 B 3,500,000 B 4,300Manganese ug/L 200.7 96,000 B 90,000 B 75,000 86,0Mercury ng/L 1631E 1,320,000 973,000 1,420,000 1,830Molybdenum ug/L 200.7 250 220 190 14Nickel ug/L 200.8 1,400 1,400 1,500 1,2Selenium ug/L 200.8 16,000 18,000 11,000 9,1Silver ug/L 200.8 NQ (2.00) NQ (2.00) NQ (2.00) NQ (2Sodium ug/L 200.7 490,000 B 390,000 B 360,000 540,Thallium ug/L 200.8 10.0 12.0 10.0 8.9Tin ug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (Titanium ug/L 200.7 3,300 3,600 B 2,400 2,6
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 limitpresented in Tables B5-6 through B5-18 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitaresult is a J-value. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. 

Table B5-1. Influent to FGD Wastewater Treatment System, Pleasant Prairie 

Analyte Units Method 

Influent to FGD Wastewater Treatment System (

Set 1 Set 2 Set 3 S

Vanadium ug/L 200.8 930 1,000 620 40Zinc ug/L 200.7 1,500 1,600 ^ 1,100 93

[QUESTION FOR PLEASANT PRAIRIE: Please provide the split sampling mercury results associated with Se

Influent to FGD Wastewater Treatment System.]
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 limitpresented in Tables B5-6 through B5-18 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitaresult is a J-value. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. 

Table B5-2. Effluent from FGD Wastewater Treatment System, Pleasant Prairie 

Analyte Units Method 

Effluent from FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 

ClassicalsAmmonia mg/L 350.1 2.40 2.00 1.10 Nitrate Nitrite as N mg/L 353.2 210 170 150 Nitrogen, Total Kjeldahl 

mg/L 351.2 46.0 B,4, Min 31.0 25.0 

Biochemical Oxygen Demand 

mg/L 5210B NQ (2.50) ND (2.00) NQ (2.50) N

Chemical Oxygen Demand 

mg/L 410.4 330 F 290 B,*, F 320 

Chloride mg/L 300.0 2,400 2,000 1,900 Sulfate mg/L 300.0 13,000 12,000 9,600 Cyanide, Total mg/L 4500 CN E 0.170 F, Est 0.240 0.230 Total Dissolved Solids 

mg/L 2540C 25,000 21,000 14,000 

Total Suspended Solids 

mg/L 2540D NQ (4.00) NQ (4.00) ND (4.00) N

Phosphorus, Total 

mg/L 365.1 0.0570 F, Min 0.130 B NQ 

(0.0500) 

B 

Total MetalsAluminum ug/L 200.7 ND (200) ND (200) ND (200) N
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 limitpresented in Tables B5-6 through B5-18 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitaresult is a J-value. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. 

Table B5-2. Effluent from FGD Wastewater Treatment System, Pleasant Prairie 

Analyte Units Method 

Effluent from FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 

Antimony ug/L 200.8 2.70 2.80 2.40 Arsenic ug/L 200.8 8.00 6.20 6.10 Barium ug/L 200.7 76.0 51.0 B 63.0 Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) NBoron ug/L 200.7 14,000 B,4 14,000 B 11,000 B Cadmium ug/L 200.8 ND (4.00) ND (4.00) ND (4.00) NCalcium ug/L 200.7 670,000 4 650,000 B 720,000 7Chromium ug/L 200.8 ND (8.00) ND (8.00) ^ ND (8.00) NCobalt ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) NCopper ug/L 200.8 12.0 NQ (4.00) NQ (4.00) NIron ug/L 200.7 NQ (200) NQ (200) B NQ (200) NLead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) NMagnesium ug/L 200.7 4,200,000 B,4 3,400,000 B 2,600,000 B 3,Manganese ug/L 200.7 15,000 B,4 12,000 B 5,200 Mercury ng/L 1631E 175 108 34.2 Molybdenum ug/L 200.7 47.0 44.0 52.0 Nickel ug/L 200.8 NQ (4.00) 5.50 NQ (4.00) Selenium ug/L 200.8 2,900 4 2,800 1,800 Silver ug/L 200.8 ND (2.00) F ND (2.00) ND (2.00) NSodium ug/L 200.7 600,000 B,4 450,000 B 380,000 5Thallium ug/L 200.8 2.10 NQ (2.00) ND (2.00) N
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 limitpresented in Tables B5-6 through B5-18 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitaresult is a J-value. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. 

Table B5-2. Effluent from FGD Wastewater Treatment System, Pleasant Prairie 

Analyte Units Method 

Effluent from FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 

Tin ug/L 200.7 ND (200) ND (200) ND (200) NTitanium ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) NVanadium ug/L 200.8 ND (10.0) NQ (10.0) ND (10.0) NZinc ug/L 200.7 NQ (40.0) NQ (40.0) ^ NQ (40.0) N

[QUESTION FOR PLEASANT PRAIRIE: Please provide the split sampling mercury results associated with Se

Effluent from FGD Wastewater Treatment System.]
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).

ND – Not detected (number in parentheses is the quantitation limit).

NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result is 

presented in Tables B5-6 through B5-18 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least one 

result is a J-value.

Table B5-3. Classical Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment System, 

Pleasant Prairie

Analyte Unit Method

Influent to FGD 

Wastewater Treatment 

System (SP-1)

4-Set Average

Effluent from FGD 

Wastewater Treatment 

System (SP-2)

4-Set Average

Classicals

Ammonia mg/L 350.1 2.38 2.08

Nitrate Nitrite as N mg/L 353.2 185 188

Nitrogen, Total Kjeldahl mg/L 351.2 50.0 34.5

Biochemical Oxygen Demand mg/L 5210B ND (2.00) NQ (2.25)

Chemical Oxygen Demand mg/L 410.4 468 350

Chloride mg/L 300.0 2,300 2,400

Sulfate mg/L 300.0 13,000 11,900

Cyanide, Total mg/L 4500 CN E 0.278 0.250

Total Dissolved Solids mg/L 2540C 22,500 20,000

Total Suspended Solids mg/L 2540D 5,050 NQ (4.00)

Phosphorus, Total mg/L 365.1 5.46 < 0.0758
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).

ND – Not detected (number in parentheses is the quantitation limit).

NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result is 

presented in Tables B5-6 through B5-18 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least one 

result is a J-value.

Table B5-4. Metals Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment System, 

Pleasant Prairie

Analyte Units Method

Influent to FGD 

Wastewater Treatment 

System (SP-1)

4-Set Average

Effluent from FGD 

Wastewater Treatment 

System (SP-2)

4-Set Average

Total Metals

Aluminum ug/L 200.7 123,000 ND (200)

Antimony ug/L 200.8 45.0 2.90

Arsenic ug/L 200.8 126 6.95

Barium ug/L 200.7 825 64.8

Beryllium ug/L 200.7 4.08 ND (2.00)

Boron ug/L 200.7 17,800 13,800

Cadmium ug/L 200.8 9.88 ND (4.00)

Calcium ug/L 200.7 690,000 695,000

Chromium ug/L 200.8 815 ND (8.00)

Cobalt ug/L 200.7 143 ND (20.0)

Copper ug/L 200.8 745 < 4.50

Iron ug/L 200.7 308,000 NQ (200)

Lead ug/L 200.8 190 ND (2.00)

Magnesium ug/L 200.7 4,130,000 3,530,000

Manganese ug/L 200.7 86,800 11,300

Mercury ng/L 1631E 1,390,000 112

Molybdenum ug/L 200.7 200 53.8

Nickel ug/L 200.8 1,380 < 3.73

Selenium ug/L 200.8 13,500 2,730
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).

ND – Not detected (number in parentheses is the quantitation limit).

NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result is 

presented in Tables B5-6 through B5-18 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantitation limit, but at least one 

result is a J-value.

Table B5-4. Metals Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment System, 

Pleasant Prairie

Analyte Units Method

Influent to FGD 

Wastewater Treatment 

System (SP-1)

4-Set Average

Effluent from FGD 

Wastewater Treatment 

System (SP-2)

4-Set Average

Silver ug/L 200.8 NQ (2.00) ND (2.00)

Sodium ug/L 200.7 445,000 505,000

Thallium ug/L 200.8 10.2 < 1.28

Tin ug/L 200.7 NQ (200) ND (200)

Titanium ug/L 200.7 2,980 ND (20.0)

Vanadium ug/L 200.8 738 NQ (10.0)

Zinc ug/L 200.7 1,280 NQ (40.0)
Table B5-5. Field Blank Analytical Results, Pleasant Prairie

Analyte Sample Point Method Unit Concentration

Total Metals

Mercury

Effluent from FGD Wastewater Treatment System Field 

Blank - Day 2 1631E ng/L 1.20
ND – Not detected (number in parentheses is the quantitation limit).

B – Analyte was found in the blank and sample.

Est – Estimated value.

J – Result measured above the MDL, but less than the quantitation limit.

Min – Minimum value.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-6. Influent to FGD Wastewater Treatment System, Set 1 Analytical Results, Pleasant Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentration

Classicals

Ammonia 350.1 mg/L 1 0.055 1 1.9

Nitrate Nitrite as N 353.2 mg/L 50 0.95 5 190

Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.77 10 64 B, Min

Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) U

Chemical Oxygen Demand 410.4 mg/L 5 20 100 480

Chloride 300.0 mg/L 50 13 150 2,300

Sulfate 300.0 mg/L 500 120 2,500 14,000

Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.29 Est

Total Dissolved Solids 2540C mg/L 1 47 100 27,000

Total Suspended Solids 2540D mg/L 1 55 200 4,200

Phosphorus, Total 365.1 mg/L 10 0.05 0.5 5

Total Metals

Aluminum 200.7 ug/L 2 9.4 200 140,000

Antimony 200.8 ug/L 2 0.72 2 56

Arsenic 200.8 ug/L 2 1.2 4 150

Barium 200.7 ug/L 2 2.5 20 840

Beryllium 200.7 ug/L 2 0.71 2 4.6

Boron 200.7 ug/L 50 170 5,000 18,000 B

Cadmium 200.8 ug/L 5 2.9 10 12

Calcium 200.7 ug/L 2 69 400 660,000

Chromium 200.8 ug/L 2 3.3 8 1,100
ND – Not detected (number in parentheses is the quantitation limit).

B – Analyte was found in the blank and sample.

Est – Estimated value.

J – Result measured above the MDL, but less than the quantitation limit.

Min – Minimum value.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-6. Influent to FGD Wastewater Treatment System, Set 1 Analytical Results, Pleasant Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentration

Cobalt 200.7 ug/L 2 1.1 20 140

Copper 200.8 ug/L 5 2.4 10 900

Iron 200.7 ug/L 2 32 200 390,000

Lead 200.8 ug/L 2 0.73 2 210

Magnesium 200.7 ug/L 50 540 10,000 4,600,000 B

Manganese 200.7 ug/L 50 13 500 96,000 B

Mercury 1631E ng/L 400,000 104,000 218,000 1,320,000

Molybdenum 200.7 ug/L 2 1.6 40 250

Nickel 200.8 ug/L 5 2.2 10 1,400

Selenium 200.8 ug/L 50 16 100 16,000

Silver 200.8 ug/L 2 0.59 2 0.8 J

Sodium 200.7 ug/L 2 180 10,000 490,000 B

Thallium 200.8 ug/L 2 0.47 2 10

Tin 200.7 ug/L 2 4.8 200 24 J

Titanium 200.7 ug/L 2 1.6 20 3,300

Vanadium 200.8 ug/L 2 1.7 10 930

Zinc 200.7 ug/L 2 9.1 40 1,500
ND – Not detected (number in parentheses is the quantitation limit).

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.

B – Analyte was found in the blank and sample.

F – MS and/or MSD not within laboratory control limits.

J – Result measured above the MDL, but less than the quantitation limit.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-7. Influent to FGD Wastewater Treatment System, Set 2 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentration

Classicals

Ammonia 350.1 mg/L 1 0.055 1 2.1

Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 160

Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 34

Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) U

Chemical Oxygen Demand 410.4 mg/L 5 20 100 450 F

Chloride 300.0 mg/L 100 25 300 1,800

Sulfate 300.0 mg/L 500 120 2,500 14,000

Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.16

Total Dissolved Solids 2540C mg/L 1 94 200 19,000

Total Suspended Solids 2540D mg/L 1 46 170 4,900

Phosphorus, Total 365.1 mg/L 10 0.05 0.5 8 B

Total Metals

Aluminum 200.7 ug/L 2 9.4 200 170,000 B

Antimony 200.8 ug/L 2 0.72 2 57

Arsenic 200.8 ug/L 2 1.2 4 170

Barium 200.7 ug/L 2 2.5 20 1,000 B

Beryllium 200.7 ug/L 2 0.71 2 4.7

Boron 200.7 ug/L 50 170 5,000 17,000 B

Cadmium 200.8 ug/L 2 1.2 4 11

Calcium 200.7 ug/L 2 69 400 710,000 B
ND – Not detected (number in parentheses is the quantitation limit).

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.

B – Analyte was found in the blank and sample.

F – MS and/or MSD not within laboratory control limits.

J – Result measured above the MDL, but less than the quantitation limit.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-7. Influent to FGD Wastewater Treatment System, Set 2 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentration

Chromium 200.8 ug/L 2 3.3 8 1,100 ^

Cobalt 200.7 ug/L 2 1.1 20 140

Copper 200.8 ug/L 2 0.96 4 1,000

Iron 200.7 ug/L 2 32 200 410,000 B

Lead 200.8 ug/L 2 0.73 2 270

Magnesium 200.7 ug/L 50 540 10,000 4,100,000 B

Manganese 200.7 ug/L 50 13 500 90,000 B

Mercury 1631E ng/L 50,000 12,400 26,000 973,000

Molybdenum 200.7 ug/L 2 1.6 40 220

Nickel 200.8 ug/L 2 0.89 4 1,400

Selenium 200.8 ug/L 50 16 100 18,000

Silver 200.8 ug/L 2 0.59 2 1.1 J

Sodium 200.7 ug/L 2 180 10,000 390,000 B

Thallium 200.8 ug/L 2 0.47 2 12

Tin 200.7 ug/L 2 4.8 200 24 J

Titanium 200.7 ug/L 2 1.6 20 3,600 B

Vanadium 200.8 ug/L 2 1.7 10 1,000

Zinc 200.7 ug/L 2 9.1 40 1,600 ^
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 B5-8. Influent to FGD Wastewater Treatment System, Set 3 Analytical Results, Pleasant Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentration

Classicals

Ammonia 350.1 mg/L 1 0.055 1 2.3

Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 160

Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.77 10 73

Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) U

Chemical Oxygen Demand 410.4 mg/L 5 20 100 420

Chloride 300.0 mg/L 100 25 300 2,000

Sulfate 300.0 mg/L 500 120 2,500 11,000

Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.29

Total Dissolved Solids 2540C mg/L 1 240 500 23,000

Total Suspended Solids 2540D mg/L 1 55 200 4,700

Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.056 B

Total Metals

Aluminum 200.7 ug/L 2 9.4 200 87,000

Antimony 200.8 ug/L 2 0.72 2 42

Arsenic 200.8 ug/L 2 1.2 4 110

Barium 200.7 ug/L 2 2.5 20 790

Beryllium 200.7 ug/L 2 0.71 2 3.7

Boron 200.7 ug/L 50 170 5,000 17,000 B

Cadmium 200.8 ug/L 2 1.2 4 7.7

Calcium 200.7 ug/L 50 1,700 10,000 780,000

Chromium 200.8 ug/L 2 3.3 8 690

Cobalt 200.7 ug/L 2 1.1 20 130

Copper 200.8 ug/L 2 0.96 4 680
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 B5-8. Influent to FGD Wastewater Treatment System, Set 3 Analytical Results, Pleasant Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentration

Iron 200.7 ug/L 2 32 200 250,000

Lead 200.8 ug/L 2 0.73 2 170

Magnesium 200.7 ug/L 50 540 10,000 3,500,000 B

Manganese 200.7 ug/L 50 13 500 75,000

Mercury 1631E ng/L 400,000 99,400 208,000 1,420,000

Molybdenum 200.7 ug/L 2 1.6 40 190

Nickel 200.8 ug/L 2 0.89 4 1,500

Selenium 200.8 ug/L 10 3.1 20 11,000

Silver 200.8 ug/L 2 0.59 2 0.94 J

Sodium 200.7 ug/L 2 180 10,000 360,000

Thallium 200.8 ug/L 2 0.47 2 10

Tin 200.7 ug/L 2 4.8 200 8.2 J

Titanium 200.7 ug/L 2 1.6 20 2,400

Vanadium 200.8 ug/L 2 1.7 10 620

Zinc 200.7 ug/L 2 9.1 40 1,100
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 B5-9. Influent to FGD Wastewater Treatment System, Set 4 Analytical Results, Pleasant Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentration

Classicals

Ammonia 350.1 mg/L 1 0.055 1 3.2

Nitrate Nitrite as N 353.2 mg/L 50 0.95 5 230

Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 29

Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) U

Chemical Oxygen Demand 410.4 mg/L 5 20 100 520

Chloride 300.0 mg/L 100 25 300 3,100

Sulfate 300.0 mg/L 500 120 2,500 13,000

Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.37

Total Dissolved Solids 2540C mg/L 1 94 200 21,000

Total Suspended Solids 2540D mg/L 1 140 500 6,400

Phosphorus, Total 365.1 mg/L 10 0.05 0.5 8.8 B

Total Metals

Aluminum 200.7 ug/L 2 9.4 200 95,000

Antimony 200.8 ug/L 2 0.72 2 25

Arsenic 200.8 ug/L 2 1.2 4 72

Barium 200.7 ug/L 2 2.5 20 670

Beryllium 200.7 ug/L 2 0.71 2 3.3

Boron 200.7 ug/L 50 170 5,000 19,000 B

Cadmium 200.8 ug/L 2 1.2 4 8.8

Calcium 200.7 ug/L 2 69 400 610,000

Chromium 200.8 ug/L 2 3.3 8 370

Cobalt 200.7 ug/L 2 1.1 20 160

Copper 200.8 ug/L 2 0.96 4 400
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 B5-9. Influent to FGD Wastewater Treatment System, Set 4 Analytical Results, Pleasant Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentration

Iron 200.7 ug/L 2 32 200 180,000

Lead 200.8 ug/L 2 0.73 2 110

Magnesium 200.7 ug/L 50 540 10,000 4,300,000

Manganese 200.7 ug/L 50 13 500 86,000 B

Mercury 1631E ng/L 400,000 99,400 208,000 1,830,000

Molybdenum 200.7 ug/L 2 1.6 40 140

Nickel 200.8 ug/L 5 2.2 10 1,200

Selenium 200.8 ug/L 10 3.1 20 9,100

Silver 200.8 ug/L 2 0.59 2 0.84 J

Sodium 200.7 ug/L 2 180 10,000 540,000

Thallium 200.8 ug/L 2 0.47 2 8.9

Tin 200.7 ug/L 2 4.8 200 7.4 J

Titanium 200.7 ug/L 2 1.6 20 2,600

Vanadium 200.8 ug/L 2 1.7 10 400

Zinc 200.7 ug/L 2 9.1 40 930
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 not applicable.

B – Analyte was found in the blank and sample.

Est – Estimated value.

F – MS and/or MSD not within laboratory control limits.

J – Result measured above the MDL, but less than the quantitation limit.

Min – Minimum value.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-10. Effluent from FGD Wastewater Treatment System, Set 1 Analytical Results, Pleasant Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentration

Classicals

Ammonia 350.1 mg/L 1 0.055 1 2.4

Nitrate Nitrite as N 353.2 mg/L 50 0.95 5 210

Nitrogen, Total Kjeldahl 351.2 mg/L 10 0.77 10 46 B,4, Min

Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 1.7 J

Chemical Oxygen Demand 410.4 mg/L 5 20 100 330 F

Chloride 300.0 mg/L 50 13 150 2,400

Sulfate 300.0 mg/L 500 120 2,500 13,000

Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.17 F, Est

Total Dissolved Solids 2540C mg/L 1 47 100 25,000

Total Suspended Solids 2540D mg/L 1 1.1 4 2.8 J

Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.057 F, Min

Total Metals

Aluminum 200.7 ug/L 2 9.4 200 ND (200) U

Antimony 200.8 ug/L 2 0.72 2 2.7

Arsenic 200.8 ug/L 2 1.2 4 8

Barium 200.7 ug/L 2 2.5 20 76

Beryllium 200.7 ug/L 2 0.71 2 ND (2) U

Boron 200.7 ug/L 50 170 5,000 14,000 B,4

Cadmium 200.8 ug/L 2 1.2 4 ND (4) U

Calcium 200.7 ug/L 2 69 400 670,000 4

Chromium 200.8 ug/L 2 3.3 8 ND (8) U
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 not applicable.

B – Analyte was found in the blank and sample.

Est – Estimated value.

F – MS and/or MSD not within laboratory control limits.

J – Result measured above the MDL, but less than the quantitation limit.

Min – Minimum value.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-10. Effluent from FGD Wastewater Treatment System, Set 1 Analytical Results, Pleasant Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentration

Cobalt 200.7 ug/L 2 1.1 20 ND (20) U

Copper 200.8 ug/L 2 0.96 4 12

Iron 200.7 ug/L 2 32 200 150 J

Lead 200.8 ug/L 2 0.73 2 ND (2) U

Magnesium 200.7 ug/L 50 540 10,000 4,200,000 B,4

Manganese 200.7 ug/L 2 0.51 20 15,000 B,4

Mercury 1631E ng/L 10 2.48 5.2 175

Molybdenum 200.7 ug/L 2 1.6 40 47

Nickel 200.8 ug/L 2 0.89 4 2.4 J

Selenium 200.8 ug/L 5 1.6 10 2,900 4

Silver 200.8 ug/L 2 0.59 2 ND (2) U,F

Sodium 200.7 ug/L 2 180 10,000 600,000 B,4

Thallium 200.8 ug/L 2 0.47 2 2.1

Tin 200.7 ug/L 2 4.8 200 ND (200) U

Titanium 200.7 ug/L 2 1.6 20 ND (20) U

Vanadium 200.8 ug/L 2 1.7 10 ND (10) U

Zinc 200.7 ug/L 2 9.1 40 22 J
ND – Not detected (number in parentheses is the quantitation limit).

* - LCS or LCSD is outside the laboratory control limits.

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.

B – Analyte was found in the blank and sample.

F – MS and/or MSD not within laboratory control limits.

J – Result measured above the MDL, but less than the quantitation limit.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-11. Effluent from FGD Wastewater Treatment System, Set 2 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentration

Classicals

Ammonia 350.1 mg/L 1 0.055 1 2

Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 170

Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 31

Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) U

Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 290 B,*, F

Chloride 300.0 mg/L 100 25 300 2,000

Sulfate 300.0 mg/L 500 120 2,500 12,000

Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.24

Total Dissolved Solids 2540C mg/L 1 47 100 21,000

Total Suspended Solids 2540D mg/L 1 1.1 4 2 J

Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.13 B

Total Metals

Aluminum 200.7 ug/L 2 9.4 200 ND (200) U

Antimony 200.8 ug/L 2 0.72 2 2.8

Arsenic 200.8 ug/L 2 1.2 4 6.2

Barium 200.7 ug/L 2 2.5 20 51 B

Beryllium 200.7 ug/L 2 0.71 2 ND (2) U

Boron 200.7 ug/L 50 170 5,000 14,000 B

Cadmium 200.8 ug/L 2 1.2 4 ND (4) U

Calcium 200.7 ug/L 2 69 400 650,000 B
ND – Not detected (number in parentheses is the quantitation limit).

* - LCS or LCSD is outside the laboratory control limits.

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.

B – Analyte was found in the blank and sample.

F – MS and/or MSD not within laboratory control limits.

J – Result measured above the MDL, but less than the quantitation limit.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-11. Effluent from FGD Wastewater Treatment System, Set 2 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentration

Chromium 200.8 ug/L 2 3.3 8 ND (8) U,^

Cobalt 200.7 ug/L 2 1.1 20 ND (20) U

Copper 200.8 ug/L 2 0.96 4 3.8 J

Iron 200.7 ug/L 2 32 200 110 J,B

Lead 200.8 ug/L 2 0.73 2 ND (2) U

Magnesium 200.7 ug/L 50 540 10,000 3,400,000 B

Manganese 200.7 ug/L 2 0.51 20 12,000 B

Mercury 1631E ng/L 20 4.87 10.2 108

Molybdenum 200.7 ug/L 2 1.6 40 44

Nickel 200.8 ug/L 2 0.89 4 5.5

Selenium 200.8 ug/L 2 0.62 4 2,800

Silver 200.8 ug/L 2 0.59 2 ND (2) U

Sodium 200.7 ug/L 2 180 10,000 450,000 B

Thallium 200.8 ug/L 2 0.47 2 0.49 J

Tin 200.7 ug/L 2 4.8 200 ND (200) U

Titanium 200.7 ug/L 2 1.6 20 ND (20) U

Vanadium 200.8 ug/L 2 1.7 10 2.1 J

Zinc 200.7 ug/L 2 9.1 40 20 J,^
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 B5-12. Effluent from FGD Wastewater Treatment System, Set 3 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific

MDL

SampleSpecific 

QL Concentration

Classicals

Ammonia 350.1 mg/L 1 0.055 1 1.1

Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 150

Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 25

Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 1.7 J

Chemical Oxygen Demand 410.4 mg/L 5 20 100 320

Chloride 300.0 mg/L 100 25 300 1,900

Sulfate 300.0 mg/L 500 120 2,500 9,600

Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.23

Total Dissolved Solids 2540C mg/L 1 47 100 14,000

Total Suspended Solids 2540D mg/L 1 1.1 4 ND (4) U

Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.025 J,B

Total Metals

Aluminum 200.7 ug/L 2 9.4 200 ND (200) U

Antimony 200.8 ug/L 2 0.72 2 2.4

Arsenic 200.8 ug/L 2 1.2 4 6.1

Barium 200.7 ug/L 2 2.5 20 63

Beryllium 200.7 ug/L 2 0.71 2 ND (2) U

Boron 200.7 ug/L 50 170 5,000 11,000 B

Cadmium 200.8 ug/L 2 1.2 4 ND (4) U

Calcium 200.7 ug/L 50 1,700 10,000 720,000

Chromium 200.8 ug/L 2 3.3 8 ND (8) U

Cobalt 200.7 ug/L 2 1.1 20 ND (20) U
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 B5-12. Effluent from FGD Wastewater Treatment System, Set 3 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific

MDL

SampleSpecific 

QL Concentration

Copper 200.8 ug/L 2 0.96 4 3.2 J

Iron 200.7 ug/L 2 32 200 51 J

Lead 200.8 ug/L 2 0.73 2 ND (2) U

Magnesium 200.7 ug/L 50 540 10,000 2,600,000 B

Manganese 200.7 ug/L 2 0.51 20 5,200

Mercury 1631E ng/L 20 4.97 10.4 34.2

Molybdenum 200.7 ug/L 2 1.6 40 52

Nickel 200.8 ug/L 2 0.89 4 3.4 J

Selenium 200.8 ug/L 10 3.1 20 1,800

Silver 200.8 ug/L 2 0.59 2 ND (2) U

Sodium 200.7 ug/L 2 180 10,000 380,000

Thallium 200.8 ug/L 2 0.47 2 ND (2) U

Tin 200.7 ug/L 2 4.8 200 ND (200) U

Titanium 200.7 ug/L 2 1.6 20 ND (20) U

Vanadium 200.8 ug/L 2 1.7 10 ND (10) U

Zinc 200.7 ug/L 2 9.1 40 15 J
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 B5-13. Effluent from FGD Wastewater Treatment System, Set 4 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific

MDL

SampleSpecific 

QL Concentration

Classicals

Ammonia 350.1 mg/L 1 0.055 1 2.8

Nitrate Nitrite as N 353.2 mg/L 50 0.95 5 220

Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 36

Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) U

Chemical Oxygen Demand 410.4 mg/L 5 20 100 460

Chloride 300.0 mg/L 100 25 300 3,300

Sulfate 300.0 mg/L 500 120 2,500 13,000

Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.36

Total Dissolved Solids 2540C mg/L 1 94 200 20,000

Total Suspended Solids 2540D mg/L 1 1.1 4 1.2 J

Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.091 B

Total Metals

Aluminum 200.7 ug/L 2 9.4 200 ND (200) U

Antimony 200.8 ug/L 2 0.72 2 3.7

Arsenic 200.8 ug/L 2 1.2 4 7.5

Barium 200.7 ug/L 2 2.5 20 69

Beryllium 200.7 ug/L 2 0.71 2 ND (2) U

Boron 200.7 ug/L 50 170 5,000 16,000 B

Cadmium 200.8 ug/L 2 1.2 4 ND (4) U

Calcium 200.7 ug/L 2 69 400 740,000

Chromium 200.8 ug/L 2 3.3 8 ND (8) U

Cobalt 200.7 ug/L 2 1.1 20 ND (20) U
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 B5-13. Effluent from FGD Wastewater Treatment System, Set 4 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

SampleSpecific

MDL

SampleSpecific 

QL Concentration

Copper 200.8 ug/L 2 0.96 4 1.6 J

Iron 200.7 ug/L 2 32 200 57 J

Lead 200.8 ug/L 2 0.73 2 ND (2) U

Magnesium 200.7 ug/L 50 540 10,000 3,900,000

Manganese 200.7 ug/L 2 0.51 20 13,000 B

Mercury 1631E ng/L 100 24.8 52 132

Molybdenum 200.7 ug/L 2 1.6 40 72

Nickel 200.8 ug/L 2 0.89 4 5.4

Selenium 200.8 ug/L 2 0.62 4 3,400

Silver 200.8 ug/L 2 0.59 2 ND (2) U

Sodium 200.7 ug/L 2 180 10,000 590,000

Thallium 200.8 ug/L 2 0.47 2 1.3 J

Tin 200.7 ug/L 2 4.8 200 ND (200) U

Titanium 200.7 ug/L 2 1.6 20 ND (20) U

Vanadium 200.8 ug/L 2 1.7 10 2 J

Zinc 200.7 ug/L 2 9.1 40 14 J
ND – Not detected (number in parentheses is the quantitation limit).

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.

B – Analyte was found in the blank and sample.

J – Result measured above the MDL, but less than the quantitation limit.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-14. Influent to FGD Wastewater Treatment System Field Blank, Set 1 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

Sample-Specific 

MDL

SampleSpecific QL Concentration

Total Metals

Aluminum 200.7 ug/L 2 9.4 200 ND (200) U,^

Antimony 200.8 ug/L 2 0.72 2 ND (2) U

Arsenic 200.8 ug/L 2 1.2 4 ND (4) U

Barium 200.7 ug/L 2 2.5 20 ND (20) U

Beryllium 200.7 ug/L 2 0.71 2 ND (2) U

Boron 200.7 ug/L 2 6.7 200 14 J,B

Cadmium 200.8 ug/L 2 1.2 4 ND (4) U

Calcium 200.7 ug/L 2 69 400 ND (400) U

Chromium 200.8 ug/L 2 3.3 8 ND (8) U

Cobalt 200.7 ug/L 2 1.1 20 ND (20) U

Copper 200.8 ug/L 2 0.96 4 ND (4) U

Iron 200.7 ug/L 2 32 200 ND (200) U

Lead 200.8 ug/L 2 0.73 2 ND (2) U

Magnesium 200.7 ug/L 2 21 400 60 J,B

Manganese 200.7 ug/L 2 0.51 20 ND (20) U

Mercury 1631E ng/L 1 0.24 0.5 ND (0.5) U

Molybdenum 200.7 ug/L 2 1.6 40 ND (40) U

Nickel 200.8 ug/L 2 0.89 4 ND (4) U

Selenium 200.8 ug/L 2 0.62 4 0.78 J

Silver 200.8 ug/L 2 0.59 2 ND (2) U

Sodium 200.7 ug/L 2 180 10,000 180 J,B

Thallium 200.8 ug/L 2 0.47 2 ND (2) U
ND – Not detected (number in parentheses is the quantitation limit).

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.

B – Analyte was found in the blank and sample.

J – Result measured above the MDL, but less than the quantitation limit.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-14. Influent to FGD Wastewater Treatment System Field Blank, Set 1 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

Sample-Specific 

MDL

SampleSpecific QL Concentration

Tin 200.7 ug/L 2 4.8 200 ND (200) U

Titanium 200.7 ug/L 2 1.6 20 ND (20) U

Vanadium 200.8 ug/L 2 1.7 10 1.8 J

Zinc 200.7 ug/L 2 9.1 40 ND (40) U
ND – Not detected (number in parentheses is the quantitation limit).

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.

B – Analyte was found in the blank and sample.

J – Result measured above the MDL, but less than the quantitation limit.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-15. Effluent from FGD Wastewater Treatment System Field Blank, Set 1 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

Sample-Specific 

MDL

SampleSpecific QL Concentration

Total Metals

Aluminum 200.7 ug/L 2 9.4 200 ND (200) U,^

Antimony 200.8 ug/L 2 0.72 2 ND (2) U

Arsenic 200.8 ug/L 2 1.2 4 ND (4) U

Barium 200.7 ug/L 2 2.5 20 ND (20) U

Beryllium 200.7 ug/L 2 0.71 2 ND (2) U

Boron 200.7 ug/L 2 6.7 200 14 J,B

Cadmium 200.8 ug/L 2 1.2 4 ND (4) U

Calcium 200.7 ug/L 2 69 400 ND (400) U

Chromium 200.8 ug/L 2 3.3 8 ND (8) U

Cobalt 200.7 ug/L 2 1.1 20 ND (20) U

Copper 200.8 ug/L 2 0.96 4 ND (4) U

Iron 200.7 ug/L 2 32 200 ND (200) U

Lead 200.8 ug/L 2 0.73 2 ND (2) U

Magnesium 200.7 ug/L 2 21 400 23 J,B

Manganese 200.7 ug/L 2 0.51 20 2.4 J,B

Mercury 1631E ng/L 1 0.24 0.5 ND (0.5) U

Molybdenum 200.7 ug/L 2 1.6 40 2 J

Nickel 200.8 ug/L 2 0.89 4 ND (4) U

Selenium 200.8 ug/L 2 0.62 4 1.1 J

Silver 200.8 ug/L 2 0.59 2 1 J

Sodium 200.7 ug/L 2 180 10,000 320 J,B

Thallium 200.8 ug/L 2 0.47 2 ND (2) U
ND – Not detected (number in parentheses is the quantitation limit).

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.

B – Analyte was found in the blank and sample.

J – Result measured above the MDL, but less than the quantitation limit.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-15. Effluent from FGD Wastewater Treatment System Field Blank, Set 1 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

Sample-Specific 

MDL

SampleSpecific QL Concentration

Tin 200.7 ug/L 2 4.8 200 ND (200) U

Titanium 200.7 ug/L 2 1.6 20 ND (20) U

Vanadium 200.8 ug/L 2 1.7 10 2.1 J

Zinc 200.7 ug/L 2 9.1 40 ND (40) U
ND – Not detected (number in parentheses is the quantitation limit).

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.

B – Analyte was found in the blank and sample.

J – Result measured above the MDL, but less than the quantitation limit.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-16. Effluent from FGD Wastewater Treatment System Field Blank, Set 2 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

Sample-Specific 

MDL

SampleSpecific QL Concentration

Total Metals

Aluminum 200.7 ug/L 2 9.4 200 ND (200) U

Antimony 200.8 ug/L 2 0.72 2 ND (2) U

Arsenic 200.8 ug/L 2 1.2 4 ND (4) U

Barium 200.7 ug/L 2 2.5 20 4.4 J,B

Beryllium 200.7 ug/L 2 0.71 2 ND (2) U

Boron 200.7 ug/L 2 6.7 200 17 J,B

Cadmium 200.8 ug/L 2 1.2 4 ND (4) U

Calcium 200.7 ug/L 2 69 400 ND (400) U

Chromium 200.8 ug/L 2 3.3 8 ND (8) U,^

Cobalt 200.7 ug/L 2 1.1 20 ND (20) U

Copper 200.8 ug/L 2 0.96 4 ND (4) U

Iron 200.7 ug/L 2 32 200 ND (200) U

Lead 200.8 ug/L 2 0.73 2 ND (2) U

Magnesium 200.7 ug/L 2 21 400 24 J,B

Manganese 200.7 ug/L 2 0.51 20 ND (20) U

Mercury 1631E ng/L 1 0.24 0.5 1.2

Molybdenum 200.7 ug/L 2 1.6 40 ND (40) U

Nickel 200.8 ug/L 2 0.89 4 ND (4) U

Selenium 200.8 ug/L 2 0.62 4 1.2 J

Silver 200.8 ug/L 2 0.59 2 ND (2) U

Sodium 200.7 ug/L 2 180 10,000 ND (10,000) U

Thallium 200.8 ug/L 2 0.47 2 ND (2) U
ND – Not detected (number in parentheses is the quantitation limit).

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.

B – Analyte was found in the blank and sample.

J – Result measured above the MDL, but less than the quantitation limit.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-16. Effluent from FGD Wastewater Treatment System Field Blank, Set 2 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

Sample-Specific 

MDL

SampleSpecific QL Concentration

Tin 200.7 ug/L 2 4.8 200 ND (200) U

Titanium 200.7 ug/L 2 1.6 20 ND (20) U

Vanadium 200.8 ug/L 2 1.7 10 2.6 J

Zinc 200.7 ug/L 2 9.1 40 25 J,^
ND – Not detected (number in parentheses is the quantitation limit).

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.

B – Analyte was found in the blank and sample.

J – Result measured above the MDL, but less than the quantitation limit.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-17. Effluent from FGD Wastewater Treatment System Field Blank, Set 3 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

Sample-Specific 

MDL

SampleSpecific QL Concentration

Total Metals

Aluminum 200.7 ug/L 2 9.4 200 ND (200) U

Antimony 200.8 ug/L 2 0.72 2 ND (2) U

Arsenic 200.8 ug/L 2 1.2 4 ND (4) U

Barium 200.7 ug/L 2 2.5 20 ND (20) U

Beryllium 200.7 ug/L 2 0.71 2 ND (2) U

Boron 200.7 ug/L 2 6.7 200 75 J,B

Cadmium 200.8 ug/L 2 1.2 4 ND (4) U

Calcium 200.7 ug/L 2 69 400 96 J

Chromium 200.8 ug/L 2 3.3 8 ND (8) U

Cobalt 200.7 ug/L 2 1.1 20 ND (20) U

Copper 200.8 ug/L 2 0.96 4 ND (4) U

Iron 200.7 ug/L 2 32 200 ND (200) U

Lead 200.8 ug/L 2 0.73 2 ND (2) U

Magnesium 200.7 ug/L 2 21 400 98 J,B

Manganese 200.7 ug/L 2 0.51 20 ND (20) U

Mercury 1631E ng/L 1 0.24 0.5 ND (0.5) U

Molybdenum 200.7 ug/L 2 1.6 40 ND (40) U

Nickel 200.8 ug/L 2 0.89 4 ND (4) U

Selenium 200.8 ug/L 2 0.62 4 0.83 J,^

Silver 200.8 ug/L 2 0.59 2 ND (2) U

Sodium 200.7 ug/L 2 180 10,000 370 J

Thallium 200.8 ug/L 2 0.47 2 ND (2) U
ND – Not detected (number in parentheses is the quantitation limit).

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits.

B – Analyte was found in the blank and sample.

J – Result measured above the MDL, but less than the quantitation limit.

U – Result below the MDL. (Number shown in parentheses is the quantitation limit).

Table B5-17. Effluent from FGD Wastewater Treatment System Field Blank, Set 3 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

Sample-Specific 

MDL

SampleSpecific QL Concentration

Tin 200.7 ug/L 2 4.8 200 ND (200) U

Titanium 200.7 ug/L 2 1.6 20 ND (20) U

Vanadium 200.8 ug/L 2 1.7 10 1.9 J

Zinc 200.7 ug/L 2 9.1 40 ND (40) U
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 B5-18. Effluent from FGD Wastewater Treatment System Field Blank, Set 4 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

Sample-Specific 

MDL

SampleSpecific QL Concentration

Total Metals

Aluminum 200.7 ug/L 2 9.4 200 ND (200) U

Antimony 200.8 ug/L 2 0.72 2 ND (2) U

Arsenic 200.8 ug/L 2 1.2 4 ND (4) U

Barium 200.7 ug/L 2 2.5 20 ND (20) U

Beryllium 200.7 ug/L 2 0.71 2 ND (2) U

Boron 200.7 ug/L 2 6.7 200 19 J,B

Cadmium 200.8 ug/L 2 1.2 4 ND (4) U

Calcium 200.7 ug/L 2 69 400 ND (400) U

Chromium 200.8 ug/L 2 3.3 8 ND (8) U

Cobalt 200.7 ug/L 2 1.1 20 ND (20) U

Copper 200.8 ug/L 2 0.96 4 ND (4) U

Iron 200.7 ug/L 2 32 200 ND (200) U

Lead 200.8 ug/L 2 0.73 2 ND (2) U

Magnesium 200.7 ug/L 2 21 400 34 J

Manganese 200.7 ug/L 2 0.51 20 ND (20) U

Mercury 1631E ng/L 1 0.24 0.5 ND (0.5) U

Molybdenum 200.7 ug/L 2 1.6 40 ND (40) U

Nickel 200.8 ug/L 2 0.89 4 ND (4) U

Selenium 200.8 ug/L 2 0.62 4 1.2 J

Silver 200.8 ug/L 2 0.59 2 ND (2) U

Sodium 200.7 ug/L 2 180 10,000 180 J

Thallium 200.8 ug/L 2 0.47 2 ND (2) U

Tin 200.7 ug/L 2 4.8 200 ND (200) U
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 B5-18. Effluent from FGD Wastewater Treatment System Field Blank, Set 4 Analytical Results, Pleasant 

Prairie

Analyte Method Unit

Dilution 

Factor

Sample-Specific 

MDL

SampleSpecific QL Concentration

Titanium 200.7 ug/L 2 1.6 20 ND (20) U

Vanadium 200.8 ug/L 2 1.7 10 2 J

Zinc 200.7 ug/L 2 9.1 40 ND (40) U
Section 6 

Data Review Narratives 

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

removed.] 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

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

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Donna Tedder, ERG 

Date: 2/9/2012

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

Month 1 (Part 1)

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 14 samples (excluding laboratory prep blanks) FGS extracted 

and analyzed for total mercury. 

Table 1. Long-Term Monitoring Month 1 (Part 1) Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72041 1010010-01 Aqueous FGD Influent, Set 1 9/30/2010 

72045 1010010-02 Aqueous FGD Effluent, Set 1 9/30/2010

72049 1010010-04 Aqueous FGD Influent Field Blank 9/30/2010

72050 1010010-03 Aqueous FGD Effluent Field Blank, Set 1 9/30/2010 

72091 1009237-07 Aqueous FGD Influent, Set 1 9/28/2010

72095 1009237-08 Aqueous FGD Effluent, Set 1 9/28/2010

72099 1009237-10 Aqueous FGD Influent Field Blank 9/28/2010

72100 1009237-09 Aqueous FGD Effluent Field Blank, Set 1 9/27/2010

72191 1009237-01 Aqueous FGD Influent Set 1 9/29/2010 

72195 1009237-02 Aqueous FGD SBR Influent, Set 1 9/29/2010

72199 1009237-03 Aqueous FGD SBR Effluent, Set 1 9/29/2010

72203 1009237-06 Aqueous FGD Influent Field Blank 9/29/2010

72204 1009237-04 Aqueous FGD SBR Influent Field Blank, Set 1 9/28/2010

72208 1009237-05 Aqueous FGD SBR Effluent Field Blank, Set 1 9/28/2010

SUMMARY 

The samples were prepared according to EPA Method 1631E to be analyzed by CVAFS. 
2

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, samples 72095 and 72195. The relative 

percent difference (RPD) for samples 72095 and 72195 were 2.45% and 3.32%, 

respectively. The laboratory’s RPD criteria between analytical duplicates is 24%. 

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 

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

72095, 72199, and 72195 for the total mercury analyses. All aqueous MS/MSD 

recoveries were within method specifications of 71-125%. All RPDs met methodspecified criteria. 
3

DETECTION LIMITS 

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

were reported as not detected (ND). 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

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

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Randy Mercurio, ERG 

Date: 2/9/2012

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

Monitoring: Month 1 (Part 1)

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

chromium, copper, lead, nickel, selenium, silver, thallium, and vanadium) for these longterm monitoring samples. The samples were analyzed according to EPA Method 200.8. 

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

EPA Method 200.8. 

Table 1. Long-Term Monitoring Month 1 (Part 1) Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72041 FGD Influent, Set 1 280-7918-1 Aqueous 9/30/2010 10/1/2010

72045 FGD Effluent, Set 1 280-7918-2 Aqueous 9/30/2010 10/1/2010

72049 FGD Influent Field Blank 280-7918-4 Aqueous 9/30/2010 10/1/2010

72050 FGD Effluent Field Blank, Set 1 280-7918-3 Aqueous 9/30/2010 10/1/2010

72091 FGD Influent, Set 1 280-7817-1 Aqueous 9/28/2010 9/29/2010

72095 FGD Effluent, Set 1 280-7817-2 Aqueous 9/28/2010 9/29/2010

72099 FGD Influent Field Blank, Set 1 280-7817-4 Aqueous 9/28/2010 9/29/2010

72100 FGD Effluent Field Blank, Set 1 280-7817-3 Aqueous 9/28/2010 9/29/2010

72191 FGD Influent, Set 1 280-7870-1 Aqueous 9/29/2010 9/30/2010

72195 FGD SBR Influent, Set 1 280-7870-2 Aqueous 9/29/2010 9/30/2010

72199 FGD SBR Effluent, Set 1 280-7870-3 Aqueous 9/29/2010 9/30/2010

72203 FGD Influent Field Blank 280-7870-6 Aqueous 9/29/2010 9/30/2010

72204 FGD SBR Influent Field Blank, 

Set 1 

280-7870-4 Aqueous 9/29/2010 9/30/2010

72208 FGD SBR Effluent Field Blank, 

Set 2 

280-7870-5 Aqueous 9/29/2010 9/30/2010
2

SUMMARY 

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

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

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

EPA Method 200.8, by ICP/MS analysis. 

Any significant findings are summarized below. No additional data qualifiers were 

required. 

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

silver for samples 72045 and 72095 failed the EPA Method 200.8 control limits of 

70–130%. 

• The MS/MSD relative percent difference (RPD) for total silver for sample 72095 

failed the FGD ICP/MS SOP control limits of ±20%. 

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

TestAmerica’s control limits of 85–115%: arsenic, chromium, selenium, silver, 

and vanadium. 

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); however, some elements 

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

required for method blanks. 

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

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

flagged with a “J” qualifier. No additional qualifiers were required for instrument blanks. 
3

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

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

LABORATORY CONTROL SAMPLES (LCS) 

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

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION 

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

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

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

ICS. 

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

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

SERIAL DILUTION 

The serial dilution performed on sample 72095 passed TestAmerica’s criteria of ±10% 

difference. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES 

MS and MSD were performed on samples 72045 and 72095. The total selenium results in 

the MS and MSD samples for sample 72045 and the MS sample for sample 72095 failed 

the 70-130% recovery method control limits and were flagged with a “4” qualifier 

indicating concentrations in the parent samples were greater than four times the spike 

amounts. These data were considered acceptable based on the LCS passing the method 

control limits. 

The total silver results in the MS and MSD samples for both samples 72045 and 72095 

failed the 70-130% method control limits with low recoveries and were flagged with an 

“F” qualifier. Additionally, the RPD for silver between the MS and MSD for sample 

72095 failed the ICP/MS SOP ±20% control limits. The poor recoveries and RPD of 

silver are probably due to high sulfates in this episode’s samples capable of forming 

insoluble silver sulfide and/or silver sulfate. 
4

Otherwise, all MS/MSD spike recoveries were within the method control limits of 70-

130% and the RPD for the MS/MSDs were within the FGD ICP/MS SOP control limits 

of ±20 percent. No additional data qualifiers were required. 

POST DIGESTION SPIKES 

The PDS performed on sample 72095 passed TestAmerica’s control limits of 85–115% 

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

which were all flagged with a “W” qualifier. No additional data qualifiers were required 

for PDS samples. 

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: Randy Mercurio, ERG 

Date: 2/9/2012 

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

Monitoring: Month 1 (Part 1)

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

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

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

according to EPA Method 200.7. 

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

EPA Method 200.7.

Table 1. Long-Term Monitoring Month 1 (Part 1) Total Metals – Sample 

Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72041 FGD Influent, Set 1 280-7918-1 Aqueous 9/30/2010 10/1/2010

72045 FGD Effluent, Set 1 280-7918-2 Aqueous 9/30/2010 10/1/2010

72049 FGD Influent Field Blank 280-7918-4 Aqueous 9/30/2010 10/1/2010

72050 FGD Effluent Field Blank, 

Set 1 

280-7918-3 Aqueous 9/30/2010 10/1/2010

72091 FGD Influent, Set 1 280-7817-1 Aqueous 9/28/2010 9/29/2010

72095 FGD Effluent, Set 1 280-7817-2 Aqueous 9/28/2010 9/29/2010

72099 FGD Influent Field Blank, 

Set 1 

280-7817-4 Aqueous 9/28/2010 9/29/2010

72100 FGD Effluent Field Blank, 

Set 1 

280-7817-3 Aqueous 9/28/2010 9/29/2010

72191 FGD Influent, Set 1 280-7870-1 Aqueous 9/29/2010 9/30/2010

72195 FGD SBR Influent, Set 1 280-7870-2 Aqueous 9/29/2010 9/30/2010

72199 FGD SBR Effluent, Set 1 280-7870-3 Aqueous 9/29/2010 9/30/2010

72203 FGD Influent Field Blank 280-7870-6 Aqueous 9/29/2010 9/30/2010

72204 FGD SBR Influent Field 

Blank, Set 1 

280-7870-4 Aqueous 9/29/2010 9/30/2010

72208 FGD SBR Effluent Field 

Blank, Set 2 

280-7870-5 Aqueous 9/29/2010 9/30/2010
2

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. 

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

barium for sample 72095 failed the EPA Method 200.7 control limits of 70–

130%. 

• The MS/MSD relative percent difference (RPD) for total magnesium for sample 

72095 failed TestAmerica’s SOP control limits of ±20%. 

• The post digestion spike (PDS) for titanium for sample 72095 failed 

TestAmerica’s control limits of 85–115% recovery. 

SAMPLE RECEIPT, HANDLING AND STORAGE ISSUES 

There were no sample receipt issues in this data package. 

INTERNAL STANDARDIZATION 

While the internal standard (ISTD) yttrium was used for these analyses, no checks for the 

ISTD recoveries within the ±30% criterion of the 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. 
3

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

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

LABORATORY CONTROL SAMPLES (LCS) 

All LCSs 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.

SERIAL DILUTION (SRD) 

Serial dilutions were performed for each batch of total samples. All serial dilution percent 

differences were less than 10% as required by TestAmerica’s SOP. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

MS and MSDs were performed on the total samples of 72095 and 72045. Some elements 

with high concentrations failed the EPA 200.7 Method spike recovery control limits of 

70–130% but were flagged with a “4” qualifier indicating that the concentration in the 

parent sample was greater than 4 times the spike and could not be reliably calculated. 

These data were considered acceptable based on the LCS passing the method control 

limits. Otherwise, all MS/MSD spike recoveries were within the method control criteria 

of 70-130%, except for barium for sample 72095, which had a recovery of 65% and was 

qualified with an “F”. The RPD for all MS/MSDs were within TestAmerica’s ± 20% 

requirement, except for magnesium for sample 72095. No additional data qualifiers were 

needed. 

POST DIGESTION SPIKE (PDS) 

The PDS performed on sample 72095 passed TestAmerica’s control limits of 85–115% 

recovery for all analytes except titanium, which was qualified with a “W”. 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 – Long-Term 

Monitoring: Month 1 (Part 1) 

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for these long-term monitoring samples. 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 seven samples that TestAmerica analyzed for the above analytes. 

Table 1. Long-Term Monitoring Month 1 (Part 1) Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72041 Water FGD Influent, Set 1 9/30/10 

72045 Water FGD Effluent, Set 1 9/30/10 

72091 Water FGD Influent, Set 1 9/28/10 

72095 Water FGD Effluent, Set 1 9/28/10 

72191 Water FGD Influent, Set 1 9/29/10 

72195 Water FGD SBR Influent, Set 1 9/29/10 

72199 Water FGD SBR Effluent, Set 1 9/29/10 
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. 

 

Field duplicate samples were not collected for these episodes. Depending on the method, 

a laboratory duplicate was analyzed, instead. The Relative Percent Difference (RPD) 

between the sample and its duplicate was less than 20% unless otherwise noted below. 

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

If sample results were above the highest standard used 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 sample 72045 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 

No issues were identified by the data reviewer. 

BOD5 

TestAmerica analyzed five dilutions, but no dilutions had a dissolved oxygen (DO) 

depletion greater than 2.0 mg/L for sample 72041 and 72091. Therefore, BOD5 was 

reported as not detected for these samples. The rest of the samples had at least one 

dilution with a DO depletion greater than 2.0 mg/L. As required in the method, the final 

result was calculated by taking the average of the results for all dilutions with a DO 

depletion greater than 2.0 mg/L and a final DO greater than 1.0 mg/L. 

BOD was not detected above the RL in any method blanks. However, for one batch, the 

results for the three water/unseeded blanks were 0.22 mg/L, 0.14 mg/L, and 0.16 mg/L. 
3 

One of these water blanks was above the method control criteria of 0.20 mg/L. However, 

all samples contained in this batch (samples 72041 and 72045) were either qualified with 

a “J” meaning that the sample result was an estimated value because it was below the RL 

or BOD was not detected in the sample, so no further qualification was necessary. 

One of the three batches had a seed correction factor lower than 0.6 mg/L. The seed 

correction factors were 0.6267 mg/L, 0.5776 mg/L, and 0.6384 mg/L for batches 33523, 

33769, and 33938, respectively. Unlike previous episodes, TestAmerica did not flag 

samples in batch 33769 with an “s” indicating the seed correction blank (SCB) recovery 

was low. This low seed correction factor suggests that samples 72191, 72195, and 72199 

may be biased low. Therefore, these samples were also flagged with an “s”. Sample 

72191 was already flagged by TestAmerica with a “J” meaning that the sample result was 

an estimated value because it was below the RL, so no further qualification was 

necessary. However, samples 72195 and 72199 were flagged as minimum values. Due to 

the short holding time for the analysis, the samples could not be reanalyzed. 

All glucose-glutamic acid standards and laboratory duplicates were analyzed 

appropriately and met the criteria specified in SM 5210B. 

Chloride and Sulfate 

The MS and matrix spike duplicate (MSD) results for sample 72045 for sulfate and 

chloride were above the calibration curve. TestAmerica did not reanalyze the samples 

with a higher dilution factor because the percent recoveries were within EPA method 

300.0 control limits. If reported, these MS/MSD results will be qualified as estimated 

values. The LFB associated with this sample met the method criteria. The analyzed result 

for sample 72045 was within the calibration curve, so there was no need to qualify this 

sample. 

COD 

The percent recovery for the MSD analyses for sample 72045 was below the control 

limits of 90-110% required by EPA method 410.4. The percent recoveries for the MS and 

MSD analyses for this sample were 109% and 87%, respectively. Because the MS 

percent recovery met the method criteria and an MSD is not required by the method, 

sample 72045 was not qualified. The LFB percent recoveries associated with sample 

72045 met the method criteria. 

Cyanide 

Samples 72041 and 72045 were received by the laboratory at neutral pH. The lab added 

more NaOH to increase the pH to greater than 10 S.U. These samples are qualified as 

estimated values. 

Results for the following samples were less than the lowest calibration standard (0.01 

mg/L): 72095, 72195, and 72199. Because all of these samples were already flagged by 
4 

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

below the RL, no further qualification was necessary. 

The percent recoveries for the MS and MSD analyses of sample 72045 were both 85%, 

which is outside of the laboratory control criteria of 90-110%. 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 

The percent recoveries for the MS/MSD analysis of sample 72045 were not within the 

control limits of 90-110% specified in EPA Method 365.1 or within the laboratory 

control limits of 71-128%. The percent recoveries of the MS and MSD samples were 

19% and 21%, respectively. The result for sample 72045 was only slightly above the RL. 

This low sample result could have caused the low percent recovery. Nevertheless, sample 

72045 was qualified as a minimum value. The LFB percent recovery met the method 

criteria. 

TDS 

Constant weight was not achieved after 3 drying cycles for all samples. It should be noted 

that the weight increased from the first weighing to the second weighing for all samples. 

Method 2540C warns that samples which contain high levels of calcium, magnesium, 

chloride, and sulfate may be hygroscopic meaning they absorb moisture from the air. 

FGD wastewater contains high concentrations of all of these species. This was likely the 

cause for the inconsistent weight calculations. The samples were not qualified, but results 

may be biased high. 

The RPDs for laboratory duplicates from samples 72045 and 72191 were less than 10% 

as required by SM 2540C. However, the RPD for sample 72091 was 14%. Because the 

RPD was greater than the method control limits, sample 72091 was qualified as an 

estimated value. 

TDS was detected at 6.0 mg/L in the method blank associated with samples 72191, 

72195, and 72199. The method blank result was greater than the MDL (4.7 mg/L), but 

less than the RL (10 mg/L). No qualification was necessary because the blank result was 

less than the RL. 

TKN 

The percent recovery for the LFB associated with samples 72041, 72045, 72091, 72095, 

72191, 72195, and 72199 was not within the method control limits of 90-110%, but was 
5 

within the laboratory control limits of 77-115%. The percent recoveries for the LFB and 

LFBD were 84% and 86%, respectively. Because the percent recovery of the LFB was 

below the method criteria, samples 72041, 72045, 72091, 72095, 72191, 72195, and 

72199 were qualified as minimum values. 

TestAmerica performed MS/MSD analysis on sample 72045. The percent recoveries for 

the MS and MSD samples were 77% and 93%, respectively. The MS sample did not meet 

the method control limits of 90-110%, but did meet the laboratory control limits of 54-

131%. The LFB associated with this batch was also not within the laboratory control 

limits, so this may have caused the low MS percent recovery. Also, the sample 

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

TestAmerica stated that the percent recoveries and RPDs could not be reliably calculated. 

Therefore, sample 72045 was not additionally qualified based on the MS failure because 

it is not possible to determine if the MS failure was a result of matrix interferences or the 

low spiking level. 

TKN was detected at 0.133 mg/L in the LRB associated with samples 72041, 72045, 

72091, 72095, 72191, 72195, and 72199. The blank result was greater than the MDL 

(0.077 mg/L), but less than the RL (1.0 mg/L). Because the blank result was less than the 

RL, no samples were qualified based on the LRB result. 

TSS 

The RPD for the laboratory duplicate of sample 72045 was 13%. This RPD was greater 

than the method control criteria of 10%. Sample 72045 and its duplicate were already 

qualified by TestAmerica with a “J” meaning that the result is an estimated value because 

the result is below the RL, so no further qualification was necessary. 

Table 2. Data Review Summary Table 

Sample Analyte Qualifier/Ac

tion 

Reason Level Detected

72191 BOD s SCB Recovery Low XXX mg/L 

72195 BOD s, Minimum 

Value 

SCB Recovery Low XXX mg/L 

72199 BOD s, Minimum 

Value 

SCB Recovery Low XXX mg/L 

72041 Cyanide Estimated 

Value 

Sample pH < 10 S.U. 

at receipt 

0.29 mg/L 

72045 Cyanide Estimated 

Value 

Sample pH < 10 S.U. 

at receipt 

0.17 mg/L 

72045 Phosphorus Minimum 

Value 

MS % recovery < 

method-specified 

criteria 

0.057 mg/L 
6 

Table 2. Data Review Summary Table 

Sample Analyte Qualifier/Ac

tion 

Reason Level Detected

72091 TDS Estimated 

Value 

Lab duplicate RPD > 

method-specified 

criteria 

XXX mg/L 

72041 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

64 mg/L 

72045 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

46 mg/L 

72091 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

XXX mg/L 

72095 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

XXX mg/L 

72191 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

XXX mg/L 

72195 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

XXX mg/L 

72199 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

XXX mg/L 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

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

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Donna Tedder, ERG 

Date: 2/9/2012

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

Month 2 (Part 1)

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 19 samples (excluding laboratory prep blanks) FGS extracted 

and analyzed for total mercury. 

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

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71992 1011064-01 Aqueous FGD Influent, Set 2 11/3/2010

71996 1011064-06 Aqueous FGD Bioreactor Influent, Set 2 11/3/2010

72000 1011064-11 Aqueous FGD Bioreactor Effluent, Set 2 11/3/2010

72005 1011064-12 Aqueous FGD Bioreactor Influent Field Blank, Set 2 11/3/2010

72009 1011064-13 Aqueous FGD Bioreactor Effluent Field Blank, Set 2 11/3/2010

72042 1011043-01 Aqueous FGD Influent, Set 2 11/3/2010

72046 1011043-02 Aqueous FGD Effluent, Set 2 11/2/2010

72051 1011043-03 Aqueous FGD Effluent Field Blank, Set 2 11/2/2010

72092 1011031-01 Aqueous FGD Influent, Set 2 11/2/2010 

72096 1011031-02 Aqueous FGD Effluent, Set 2 11/2/2010

72101 1011031-03 Aqueous FGD Effluent, Field Blank, Set 2 11/1/2010

72142 1011032-01 Aqueous FGD Influent, Set 2 11/1/2010

72146 1011032-02 Aqueous FGD Bioreactor Influent, Set 2 11/1/2010

72150 1011032-03 Aqueous FGD Bioreactor Effluent, Set 2 11/1/2010

72155 1011032-04 Aqueous FGD Bioreactor Influent Field Blank, Set 2 11/1/2010

72159 1011032-05 Aqueous FGD Bioreactor Effluent Field Blank, Set 2 11/1/2010

72242 1011061-01 Aqueous FGD Influent, Set 2 11/4/2010

72246 1011061-06 Aqueous FGD Effluent, Set 2 11/4/2010

72251 1011061-07 Aqueous FGD Effluent Field Blank, Set 2 11/3/2010
2

SUMMARY 

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

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

dataset. The following summarizes the findings from the data review: 

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES 

There were no sample receipt issues in this data package. 

INITIAL CALIBRATION 

FGS performed the initial calibrations on each 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 the method-specified criteria. Because all of the blank 

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

results. 

DUPLICATES 

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

were analyzed in duplicate at the laboratory, samples 72046 and 72246. The relative 

percent difference (RPD) for samples 72046 and 72246 were 4.25% and 0.84%, 

respectively. The laboratory’s RPD criteria between analytical duplicates is 24%. 

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 

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

71996, 72046, 72150, and 72246. All aqueous MS/MSD recoveries were within the 
3

method specifications of 71-125%, except for the MS samples for 72046 and 72150, 

which had recoveries of 20.1% and 54.5%, respectively. All RPDs met method-specified 

criteria of less than or equal to 24%, except for samples 72046 and 72150, which had 

RPDs of 72.2% and 24.5%, respectively. Because the MSDs and the associated LCSs 

were within the method specifications, no data qualification is required for these samples. 

DETECTION LIMITS 

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

were reported as not detected (ND). 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

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

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Randy Mercurio, ERG 

Date: 2/9/2012

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

Monitoring: Month 2 (Part 1) 

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

chromium, copper, lead, nickel, selenium, silver, thallium and vanadium) for these longterm monitoring samples. The samples were analyzed according to EPA Method 200.8. 

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

EPA Method 200.8. 

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

Identification 

EPA 

Sample # 

EPA Sample 

Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71992 FGD Influent, Set 2 280-9327-1 Aqueous 11/03/2010 11/04/2010

71996 FGD Bioreactor Influent, 

Set 2 

280-9389-1 Aqueous 11/04/2010 11/05/2010

72000 FGD Bioreactor Effluent, 

Set 2 

280-9389-2 Aqueous 11/04/2010 11/05/2010

72005 FGD Bioreactor Influent 

Field Blank, Set 2 

280-9389-3 Aqueous 11/04/2010 11/05/2010

72009 FGD Bioreactor Effluent 

Field Blank, Set 2 

280-9389-4 Aqueous 11/04/2010 11/05/2010

72042 FGD Influent, Set 2 280-9326-1 Aqueous 11/03/2010 11/04/2010

72046 FGD Effluent, Set 2 280-9326-2 Aqueous 11/03/2010 11/04/2010

72051 FGD Bioreactor Effluent 

Field Blank, Set 2 

280-9326-3 Aqueous 11/03/2010 11/04/2010

72092 FGD Influent, Set 2 280-9249-1 Aqueous 11/02/2010 11/03/2010

72096 FGD Effluent, Set 2 280-9249-2 Aqueous 11/02/2010 11/03/2010

72101 FGD Effluent Field 

Blank, Set 2 

280-9249-3 Aqueous 11/02/2010 11/03/2010

72142 FGD Influent, Set 2 280-9202-1 Aqueous 11/01/2010 11/02/2010

72146 FGD Bioreactor Influent, 

Set 2 

280-9250-1 Aqueous 11/02/2010 11/03/2010
2

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

Identification 

EPA 

Sample # 

EPA Sample 

Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72150 FGD Bioreactor Effluent, 

Set 2 

280-9250-2 Aqueous 11/02/2010 11/03/2010

72155 FGD Bioreactor Influent 

Field Blank, Set 2 

280-9250-3 Aqueous 11/02/2010 11/03/2010

72159 FGD Bioreactor Effluent 

Field Blank, Set 2 

280-9250-4 Aqueous 11/02/2010 11/03/2010

72242 FGD Influent, Set 2 280-9388-1 Aqueous 11/04/2010 11/05/2010

72246 FGD Effluent, Set 2 280-9388-2 Aqueous 11/04/2010 11/05/2010

72251 FGD Bioreactor Effluent 

Field Blank, Set 2 

280-9388-3 Aqueous 11/04/2010 11/05/2010

SUMMARY 

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

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

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

EPA Method 200.8, by ICP/MS analysis. 

Any significant findings are summarized below. No additional data qualifiers were 

required. 

• The serial dilution for selenium for sample 72096 failed TestAmerica’s criteria of 

±10% difference. 

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

sample 72096 failed the EPA Method 200.8 control limits of 70–130%. 

• The MS and MSD recoveries for selenium and silver for sample 72246 failed the 

EPA Method 200.8 control limits of 70–130%. 

• The MS/MSD relative percent difference (RPD) for silver for sample 72246 failed 

the FGD ICP/MS SOP control limits of ±20%. 

• The post digestion spike (PDS) recoveries for silver failed TestAmerica’s control 

limits of 85–115%. 

INTERNAL STANDARDIZATION 

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

INITIAL CALIBRATION 
3

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

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

INITIAL AND CONTINUING CALIBRATION VERIFICATION (ICV/CCV) 

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

performed by TestAmerica all had recoveries within the method criteria. 

METHOD/INSTRUMENT BLANKS 

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

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

required for method blanks. 

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

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

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

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

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

LABORATORY CONTROL SAMPLES (LCS) 

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

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION 

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

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

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

ICS. 

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

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

The ICSA solution for the method 200.8 analysis exceeded the acceptance limits for 

Chromium in analytical batch 280-40682. The lab has confirmed with the vendor that 

Chromium is a trace impurity in the ICSA solution. Therefore, corrective action was 

deemed unnecessary; the associated data have been flagged “^”. 
4

SERIAL DILUTION 

The serial dilution performed on sample 72096 passed TestAmerica’s criteria of ±10% 

difference for all analytes except selenium, which was flagged “V.” No further data 

qualifiers were needed for the serial dilution. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

MS and MSD were performed on samples 72096 and 72246. The MS/MSD for sample 

72096 failed the method control limits of 70–130% recovery for selenium and silver. 

Selenium was flagged for the MS/MSD with a “4” qualifier indicating that the 

concentration in the parent sample was greater than 4 times the spike and could not be 

reliably calculated. This result was considered acceptable based on the LCS passing the 

method control limits. Silver was flagged for the MS/MSD with an “F” qualifier and it is 

likely that silver failed due to matrix interference from the high concentration of sulfates, 

which can form insoluble silver sulfide and/or silver sulfate. The silver recoveries in the 

associated LCS/LCSD were acceptable. 

The MS/MSD for sample 72246 failed the method control limits of 70–130% recovery 

for selenium and silver, which were flagged with an “F” qualifier. The RPD failed the 

FGD ICP/MS SOP control limits of ±20% for silver for sample 72246. No additional data 

qualifiers were required for MS/MSD samples. 

Otherwise, all MS/MSD spike recoveries were within the method control limits of 70-

130% and the RPD for the MS/MSDs were within the FGD ICP/MS SOP control limits 

of ±20 percent. No additional data qualifiers were required. 

POST DIGESTION SPIKES (PDS) 

The PDS performed on sample 72096 passed TestAmerica’s control limits of 85–115% 

recovery for all analytes, except for silver, which was flagged with a “W” qualifier. It is 

likely that silver failed due to matrix interference from the high concentration of sulfates, 

which can form insoluble silver sulfide and/or silver sulfate. The silver recoveries in the 

associated LCS/LCSD were acceptable. No additional data qualifiers were required. 

DETECTION LIMITS 

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

of reagent water. 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

CC: Jezebele Alicea, Alternate Work Assignment Manager, 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 – Long-Term 

Monitoring: Month 2 (Part 1)

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

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

titanium and zinc). The samples were analyzed according to EPA Method 200.7. 

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

EPA Method 200.7. 

Table 1. Long-Term Monitoring Month 2 (Part 1) Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71992 FGD Influent, Set 2 280-9327-1 Aqueous 11/03/2010 11/04/2010

71996 FGD Bioreactor Influent, Set 2 280-9389-1 Aqueous 11/04/2010 11/05/2010

72000 FGD Bioreactor Effluent, Set 2 280-9389-2 Aqueous 11/04/2010 11/05/2010

72005 FGD Bioreactor Influent Field 

Blank, Set 2 

280-9389-3 Aqueous 11/04/2010 11/05/2010

72009 FGD Bioreactor Effluent Field 

Blank, Set 2 

280-9389-4 Aqueous 11/04/2010 11/05/2010

72042 FGD Influent, Set 2 280-9326-1 Aqueous 11/03/2010 11/04/2010

72046 FGD Effluent, Set 2 280-9326-2 Aqueous 11/03/2010 11/04/2010

72051 FGD Bioreactor Effluent Field 

Blank, Set 2 

280-9326-3 Aqueous 11/03/2010 11/04/2010

72092 FGD Influent, Set 2 280-9249-1 Aqueous 11/02/2010 11/03/2010

72101 FGD Effluent Field Blank, Set 2 280-9249-3 Aqueous 11/02/2010 11/03/2010

72142 FGD Influent, Set 2 280-9202-1 Aqueous 11/01/2010 11/02/2010

72146 FGD Bioreactor Influent, Set 2 280-9250-1 Aqueous 11/02/2010 11/03/2010

72150 FGD Bioreactor Effluent, Set 2 280-9250-2 Aqueous 11/02/2010 11/03/2010

72155 FGD Bioreactor Influent Field 

Blank, Set 2 

280-9250-3 Aqueous 11/02/2010 11/03/2010

72159 FGD Bioreactor Effluent Field 

Blank, Set 2 

280-9250-4 Aqueous 11/02/2010 11/03/2010

72242 FGD Influent, Set 2 280-9388-1 Aqueous 11/04/2010 11/05/2010
2

Table 1. Long-Term Monitoring Month 2 (Part 1) Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72251 FGD Bioreactor Effluent Field 

Blank, Set 2 

280-9388-3 Aqueous 11/04/2010 11/05/2010

SUMMARY 

The samples were prepared for total metals analysis 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. 

• Aluminum, calcium, iron, magnesium, and manganese were measured above the 

reporting limit (RL) in a method blank; however, the concentration of these 

elements in the samples associated with this method blank were at least 10 times 

the blank result or below the RL. 

• The matrix spike (MS)/matrix spike duplicate (MSD) relative percent difference 

(RPD) for boron, calcium, and magnesium for sample 72096 failed TestAmerica’s 

± 20% requirement. 

• The post digestion spike (PDS) for calcium, manganese, titanium, and zinc for 

sample 72096 failed TestAmerica’s control limits of 85-115% recovery. 

SAMPLE RECEIPT, HANDLING AND STORAGE ISSUES 

There were no sample receipt issues in this data package. 

INTERNAL STANDARDIZATION 

While the internal standard (ISTD) yttrium was used for these analyses, no checks for the 

ISTD recoveries within the ±30% criterion of the calibration blank as per Section 9.11 of 

the SOP were seen. All ISTD were within TestAmerica’s SOP control limits. 

INITIAL CALIBRATION 

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

calibration for the ICP analysis consisted of a blank 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. 
3

METHOD/INSTRUMENT BLANKS 

All the method blanks were less than the RL, except for MB 280-40683/1-A. Aluminum, 

calcium, iron, magnesium, and manganese were measured above the RL in this method 

blank; however, the concentration of these elements in the samples associated with this 

method blank were at least 10 times the blank result or below the RL. Therefore, no data 

needed qualification regarding the method blank result. In the other method blanks, some 

elements were above the method detection limit (MDL), but less than the RL; therefore, 

these blanks and were flagged with the “J” qualifier. 

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

(CCB)) were less than the RL; however, some 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) 

All LCSs 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.

SERIAL DILUTION (SRD) 

All serial dilution percent differences were less than 10% as required by TestAmerica’s 

SOP. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

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

samples of 72096 and 72246. Some elements with high concentrations failed the EPA 

200.7 Method spike recovery control limits of 70–130% but were flagged with a “4” 

qualifier indicating that the concentration in the parent sample was greater than 4 times 

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

based on the LCS passing the method criteria. Otherwise, all MS/MSD spike recoveries 

were within the method control criteria of 70-130%. The RPD for all MS/MSDs were 
4

within TestAmerica’s ± 20% requirement, except for boron, calcium, and magnesium for 

sample 72096. These elements were flagged with an “F” qualifier. 

POST DIGESTION SPIKE (PDS) 

The PDS performed on sample 72096 passed TestAmerica’s control limits of 85-115% 

recovery for all analytes except boron, calcium, manganese, sodium, titanium, and zinc. 

Calcium, manganese, titanium, and zinc were qualified with a “W;” however, Because 

the spike level in the MS/MSD analyses for these elements was less than 4 times the 

sample concentration, there is no evidence of matrix interferences. Additionally, these 

elements passed TestAmerica’s requirement of percent differences less than 10% for the 

serial dilution for sample 72096. Boron and sodium failed the PDS; however, the percent 

recoveries were not calculated by the laboratory because their concentrations were 

greater than 4 times the PDS spike level. Boron and sodium also passed the serial dilution 

for sample 72096 demonstrating no significant matrix interferences. 

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: Ariel Atkinson, ERG 

Date: 2/9/2012 

Subject: TestAmerica Data Review Narrative for Classicals Analyses – Long Term 

Monitoring: Month 2 (Part 1) 

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for these long-term monitoring samples. All 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 12 samples that TestAmerica analyzed for the above analytes. 

Table 1. Long-Term Monitoring Month 2 (Part 1) Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71992 Water FGD Influent, Set 2 11/3/10 

71996 Water FGD Bioreactor Influent, Set 2 11/3/10(CN) 

11/4/10(All other 

analytes) 

72000 Water FGD Bioreactor Effluent, Set 2 11/3/10(CN) 

11/4/10(All other 

analytes) 

72042 Water FGD Influent, Set 2 11/3/2010 

72046 Water FGD Effluent, Set 2 11/3/2010 
2 

Table 1. Long-Term Monitoring Month 2 (Part 1) Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72092 Water FGD Influent, Set 2 11/2/2010 

72096 Water FGD Effluent, Set 2 11/2/2010 

72142 Water FGD Influent, Set 2 11/1/2010 

72146 Water FGD Bioreactor Influent, Set 2 11/2/2010 

72150 Water FGD Bioreactor Effluent, Set 2 11/1/10(CN) 

11/2/10(All other 

analytes) 

72242 Water FGD Influent, Set 2 11/4/10 

72246 Water FGD Effluent, Set 2 11/4/10 

SUMMARY 

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

samples were preserved appropriately unless otherwise specified below. 

 

Field duplicate samples were not collected for these episodes. Depending on the method, 

a laboratory duplicate was analyzed, instead. The Relative Percent Difference (RPD) 

between the sample and its duplicate was less than 20% unless otherwise noted below. 

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

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

diluted and reanalyzed unless otherwise specified below. 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 

unless otherwise noted below. 

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 72042, 

72096, and/or 72246 for each analyte to check for matrix interferences. For some 

analytes, TestAmerica spiked more samples than required. MS samples analyzed met the 

criteria specified in the method unless described below. 
3 

DATA NOTES/ISSUES 

Ammonia 

The MS result failed criteria at 111% recovery and was qualified with an “F” flag. The 

MSD and LCS recoveries demonstrate that the analysis was under control. No additional 

qualifiers were required.

BOD5 

TestAmerica analyzed five dilutions, but no dilutions had a dissolved oxygen (DO) 

depletion greater than 2.0 mg/L for samples 72092, 72146, 72150 72042, 72046, 71992, 

71996, and 72246. Therefore, BOD5 was reported as not detected for these samples. The 

rest of the samples had at least one dilution with a DO depletion greater than 2.0 mg/L. 

As required in the method, the final result was calculated by taking the average of the 

results for all dilutions with a DO depletion greater than 2.0 mg/L and a final DO greater 

than 1.0 mg/L. 

One of the three batches had a seed correction factor lower than 0.6 mg/L. The seed 

correction factors were 0.632 mg/L, 0.5533 mg/L, and 0.6267 mg/L for batches 38776, 

39101, and 39326 respectively. The samples in batch 39101 should be flagged with an 

“s” indicating the seed correction blank (SCB) recovery was low. This low seed 

correction factor suggests that samples 72042, 72046, and 71992 may be biased low; 

however all these samples had a result of ND and therefore do not require qualification. 

All glucose-glutamic acid standards and laboratory duplicates were analyzed 

appropriately and met the criteria specified in SM 5210B. 

Chloride and Sulfate 

The MS/MSD results of samples 72246 for sulfate and chloride were above the 

calibration curve. TestAmerica did not reanalyze the samples with a higher dilution factor 

because the percent recoveries were within EPA method 300.0 control limits. If reported, 

these MS/MSD results will be qualified as estimated values. The LFB associated with 

this sample met the method criteria. The analyzed result for sample 72246 was within the 

calibration curve, so there was no need to qualify this sample. 

COD 

Several LRB and Calibration Blanks (CB) had results greater than the MDL; however, all 

the LRB and CB results less than the RL and were flagged with a “J” qualifier. No further 

qualifications are necessary. 

One LFB, LCSD from batch 41304, had a percent recovery greater that the 90-110% 

criteria. The LFB was flagged with a “*” qualifier indicating the LCS or LCSD exceeds 
4 

the control limits. The sample 72046, which is associated with this LFB, was also flagged 

with “*” qualifier. 

 

The percent recovery for the MS/MSD analyses for samples 72096 and 72246 were 

above the control limits of 90-110% required by EPA method 410.4. The percent 

recoveries for the MS and MSD analyses for sample 72096 were 115% and 118%, 

respectively and the recoveries for sample 72246 were 131% and 132%, respectively. 

These results were flagged with an “F” qualifier because they exceed control limits. The 

LFB percent recoveries associated with samples 72096 and 72246 met the method 

criteria. 

MS/MSDs were not performed in batches 41739 and 41304. The samples associated with 

these batches include 72042 and 72046. These sample results were qualified with an “F” 

qualifier because there were no MS/MSD results. 

Cyanide 

The calibration was performed using standards ranging from 0.00 ppb to 400.0 ppb. The 

method states that the appropriate calibration range of standard concentrations for this 

method are between 5 ppb and 20 ppb. Samples 72142, 72092, 72096, 72046, 72242, all 

had results ≥ 20 ug/L; but were not diluted because they were within the calibration range 

performed by the laboratory. 

The MS/MSD results for sample 72246 passed the recovery criteria; however, the 

MS/MSD results for sample 72096 failed recovery criteria. The MS/MSD results for 

72096 were qualified with an “F” flag. The associated LCS/LCSD recoveries were 

within control limits. 

Nitrate/Nitrite 

The RPD between the LFB and a duplicate LFB from batch 280-40320 is 10.7%. This 

does not meet the control limits, and therefore the LFB, LFB duplicate, and associated 

samples are flagged with a “*” qualifier meaning RPD of the LCS and LCSD exceeds the 

control limit. The RPD for the MS/MSD in this batch was 1 percent; therefore the system 

appears to be in control. No further qualifiers were needed. 

The MS/MSD results for samples 72042, 72096, and 72246 were above the calibration 

curve. TestAmerica did not reanalyze these MS/MSDs with a higher dilution factor, but 

the MS/MSD results for samples 72246 and 72042 were flagged with an “E” qualifier 

because the results exceeded calibration range. The MS/MSD results for sample 72096 

were not flagged with “E” qualifier because the percent recoveries for the MS/MSD 

analysis of sample 72096 were not within the method control limits of 90-110 percent; 

therefore, these MS/MSD results were flagged with an “F” qualifier. The percent 

recoveries for the MS/MSD of 72096 were 118% and 121%, respectively. Additionally, 

the MS of sample 72042, and the MSD of sample 72246 were not within the method 

control limits of 90-110%. The percent recovery of the MSD for sample 72246 was 89% 
5 

and the percent recovery of the MS of sample 72042 was 88 percent; however neither 

MS/MSDs were flagged with an “F’ qualifier because they did meet the laboratory 

control limits. If reported, the 72042 MS should be flagged with an “F” qualifier, the 

72096 MS/MSD should be qualified as estimated, and the 72246 MS should be flagged 

with an “F” qualifier. 

Phosphorus 

The LRB was greater than the MDL at 0.0141 mg/L, however the result was less than the 

RL. The LRB results were flagged with a “J” qualifier because the result was less than 

the RL but greater than the MDL. No further qualifiers are needed. All samples that 

contained the analyte were also flagged with a “B” qualifier because the compound was 

found in the blank and the sample. All calibration blank results were also above the MDL 

but less than the RL, and therefore are also flagged with a “J” qualifier. 

The percent recoveries for the MS/MSD analysis of samples 72096 and 72246 were not 

within the control limits of 90-110% specified in EPA Method 365.1. However the 

MS/MSD of sample 72096 were within the laboratory control limits of 71-128%. The 

percent recoveries of the MS and MSD for sample 72096 were 87% and 84%, 

respectively, and the MS and MSD recoveries for sample 72246 were 26% and 31%, 

respectively. Because the MS/MSD of sample 72096 met laboratory control limits it was 

not flagged by the laboratory, but if the MS/MSD results for sample 72096 are reported, 

they should be flagged with an “F” qualifier. 

Samples 72146, 72150, 72046, 72242, 71996, 72000, and the LRB had results that were 

lower than the lowest calibration standard. Each of these results was flagged with a “J” 

qualifier because each result was less than the RL but greater than or equal to the MDL, 

and therefore the concentrations are approximate values. No further qualifiers are needed. 

TDS 

Constant weight was not achieved after 3 drying cycles for all samples. It should be noted 

that the weight increased from the first weighing to the second weighing for all samples 

except 72042, 72046, 71992, 72242, 72246, 71996, and 72000. Method 2540C warns that 

samples which contain high levels of calcium, magnesium, chloride, and sulfate may be 

hygroscopic meaning they absorb moisture from the air. FGD wastewater contains high 

concentrations of all of these species. This was likely the cause for the inconsistent 

weight calculations. Samples 72142, 72092, 72096, 72146, and 72150 were not qualified, 

but results may be biased high. 

The RPD for the laboratory duplicate from sample 72096 was 12%, which is not less than 

10% as required by SM 2540C. The laboratory control limits are 20%; therefore, the 

laboratory did not qualify the sample. The sample result will be qualified as an estimated 

value as shown in Table 2. Laboratory duplicates were not performed in the other 

batches. 
6 

TKN 

TestAmerica performed MS/MSD analysis on samples 72096 and 72246. The percent 

recoveries for the MS and MSD for sample 72096 were 161% and 147%, respectively, 

and 145% and 149% for the MS and MSD for sample 72246. These samples did not meet 

the method control limits of 90-110%, nor the laboratory control limits of 54-131%. The 

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

samples, so TestAmerica stated that the percent recoveries and RPDs could not be 

reliably calculated. The associated LCS/LCSD were also acceptable, therefore, no 

additional data qualifiers are required. 

TKN was detected in the calibration blanks. The results were greater than the MDL 

(0.077 mg/L), but less than the RL (1.0 mg/L). Because the results were less than the RL, 

no samples were qualified, but the CBs were flagged with a “J” qualifier. 

TSS 

The RPDs for the laboratory duplicates performed on samples 72142, 72096, 72046, and 

72246 were greater than the method control criteria of 10%, at 11%, 18%, 22%, and 18%, 

respectively. The laboratory control criterion is 20 percent; therefore, samples 72142, 

72096, and 72246 were not qualified by the laboratory. Sample 72046 and its duplicate 

were already qualified by TestAmerica with a “J” meaning that the result is an estimated 

value because the result is below the RL, so no further qualification was necessary for 

this sample. Because the RPD was greater than the method control limits, sample 72142, 

72096, and 72246 were qualified as estimated values. 

Table 2. Data Review Summary Table 

Sample Analyte Qualifier/Ac

tion 

Reason Level Detected

72042 COD F MS/MSD not 

performed in batch 

450 mg/L

72046 COD F MS/MSD not 

performed in batch 

290 mg/L

72096 TDS Estimated 

Value 

Lab duplicate RPD > 

method-specified 

criteria 

Sample: XXX

mg/L 

Dup: XXX 

mg/L,12%RPD 

72142 TSS Estimated 

Value 

Lab duplicate RPD > 

method-specified 

criteria 

Sample: XXX

mg/L Dup: XXX 

mg/L; 11%RPD 

72096 TSS Estimated 

Value 

Lab duplicate RPD > 

method-specified 

criteria 

Sample: XXX

mg/L 

Dup: XXX 

mg/L; 18% RPD 
7 

Table 2. Data Review Summary Table 

Sample Analyte Qualifier/Ac

tion 

Reason Level Detected

72246 TSS Estimated 

Value 

Lab duplicate RPD > 

method-specified 

criteria 

Sample: XXX

mg/L 

Dup: XXX 

mg/L; 18% RPD 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

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

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Donna Tedder, ERG 

Date: 2/9/2012

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

Month 3

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 24 samples (excluding laboratory prep blanks) FGS extracted 

and analyzed for total mercury. 

Table 1. Long-Term Monitoring Month 3 Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71993 1012119-01 Aqueous FGD Influent, Set 3 12/8/2010

71997 1012119-06 Aqueous FGD Bioreactor Influent, Set 3 12/8/2010

72001 1012119-11 Aqueous FGD Bioreactor Effluent, Set 3 12/8/2010

72006 1012119-12 Aqueous FGD Bioreactor Influent Field Blank, Set 3 12/8/2010

72010 1012119-13 Aqueous FGD Bioreactor Effluent Field Blank, Set 3 12/8/2010

72043 1012094-01 Aqueous FGD Influent, Set 3 12/8/2010

72047 1012094-02 Aqueous FGD Effluent, Set 3 12/7/2010

72052 1012094-03 Aqueous FGD Effluent Field Blank, Set 3 12/7/2010

72093 1012077-01 Aqueous FGD Influent Set 3 12/7/2010 

72097 1012077-02 Aqueous FGD Effluent, Set 3 12/7/2010

72102 1012077-03 Aqueous FGD Effluent Field Blank, Set 3 12/7/2010

72143 1012080-01 Aqueous FGD Influent, Set 3 12/6/2010

72147 1012080-06 Aqueous FGD Bioreactor Influent, Set 3 12/6/2010

72151 1012080-11 Aqueous FGD Bioreactor Effluent, Set 3 12/6/2010

72156 1012080-12 Aqueous FGD Bioreactor Influent Field Blank, Set 3 12/6/2010

72160 1012080-13 Aqueous FGD Bioreactor Effluent Field Blank, Set 3 12/6/2010

72192 1012105-01 Aqueous FGD Influent, Set 1 12/8/2010

72196 1012105-02 Aqueous FGD SBR Influent, Set 1 12/8/2010

72200 1012105-03 Aqueous FGD SBR Effluent, Set 1 12/8/2010
2

Table 1. Long-Term Monitoring Month 3 Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72205 1012105-04 Aqueous FGD SBR Influent Field Blank, Set 1 12/8/2010

72209 1012105-05 Aqueous FGD SBR Effluent Field Blank, Set 1 12/8/2010

72243 1012117-01 Aqueous FGD Influent, Set 3 12/9/2010

72247 1012117-06 Aqueous FGD Effluent, Set 3 12/9/2010

72252 1012117-07 Aqueous FGD Effluent Field Blank, Set 3 12/8/2010

SUMMARY 

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

There were no findings from the data review that required 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. Three samples 

were analyzed in duplicate at the laboratory, Bioreactor Influent sample 72147, SBR 

Influent sample 72196, and Effluent sample 72247. The relative percent difference (RPD) 
3

for samples 72147, 72196, and 72247 were 9.74%, 4.36%, and 9.10%, respectively. A 

sample from another work order was analyzed in duplicate with these batches that 

resulted in an RPD of 79.7%, which is outside of the laboratory’s criteria. The 

laboratory’s RPD criteria between analytical duplicates is 24%. No sample qualifications 

were needed based on these analytical duplicate results.

LABORATORY CONTROL SAMPLES 

All laboratory control samples were within FGS’s 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 

72097, 72147, and 72196. Additionally, an MS/MSD was performed on sample 72296, 

which was a rerun from the long-term monitoring, month 2 set of samples. All aqueous 

MS/MSD recoveries were within method specifications of 71-125%. All RPDs met 

method-specified criteria. 

DETECTION LIMITS 

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

were reported as not detected (ND). 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

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

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Randy Mercurio, ERG 

Date: 2/9/2012

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

Monitoring: Month 3 

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

chromium, copper, lead, nickel, selenium, silver, thallium and vanadium) for these longterm monitoring samples. The samples were analyzed according to EPA Method 200.8. 

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

EPA method 200.8.

Table 1. Long-Term Monitoring Month 3 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71993 FGD Influent, Set 3 280-10586-1 Aqueous 12/08/2010 12/09/2010

71997 FGD Bioreactor Influent, Set 3 280-10586-2 Aqueous 12/08/2010 12/09/2010

71997 FGD Bioreactor Influent, Set 3 280-10654-1 Aqueous 12/09/2010 12/10/2010

72001 FGD Bioreactor Effluent, Set 3 280-10654-2 Aqueous 12/09/2010 12/10/2010

72006 FGD Bioreactor Influent Field 

Blank, Set 3 

280-10654-3 Aqueous 12/09/2010 12/10/2010

72010 FGD Bioreactor Effluent Field 

Blank, Set 3 

280-10654-4 Aqueous 12/09/2010 12/10/2010

72043 FGD Influent, Set 3 280-10584-1 Aqueous 12/08/2010 12/09/2010

72047 FGD Effluent, Set 3 280-10584-2 Aqueous 12/08/2010 12/09/2010

72052 FGD Bioreactor Effluent Field 

Blank, Set 3 

280-10584-3 Aqueous 12/08/2010 12/09/2010

72093 FGD Influent, Set 3 280-10515-1 Aqueous 12/07/2010 12/08/2010

72097 FGD Effluent, Set 3 280-10515-2 Aqueous 12/07/2010 12/08/2010

72102 FGD Effluent Field Blank, Set 3 280-10515-3 Aqueous 12/07/2010 12/08/2010

72143 FGD Influent, Set 3 280-10455-1 Aqueous 12/06/2010 12/07/2010

72147 FGD Bioreactor Influent, Set 3 280-10517-1 Aqueous 12/07/2010 12/08/2010

72151 FGD Bioreactor Effluent, Set 3 280-10517-2 Aqueous 12/07/2010 12/08/2010

72156 FGD Bioreactor Influent Field 

Blank, Set 3 

280-10517-3 Aqueous 12/07/2010 12/08/2010

72160 FGD Bioreactor Effluent Field 280-10517-4 Aqueous 12/07/2010 12/08/2010
2

Table 1. Long-Term Monitoring Month 3 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

Blank, Set 3

72192 FGD Influent, Set 1 280-10585-1 Aqueous 12/08/2010 12/09/2010

72196 FGD SBR Influent, Set 1 280-10585-2 Aqueous 12/08/2010 12/09/2010

72200 FGD SBR Effluent, Set 1 280-10585-3 Aqueous 12/08/2010 12/09/2010

72205 FGD SBR Influent Field Blank, 

Set 1 

280-10585-4 Aqueous 12/08/2010 12/09/2010

72209 FGD SBR Effluent Field Blank, 

Set 1 

280-10585-5 Aqueous 12/08/2010 12/09/2010

72243 FGD Influent, Set 3 280-10655-1 Aqueous 12/09/2010 12/10/2010

72247 FGD Effluent, Set 3 280-10655-2 Aqueous 12/09/2010 12/10/2010

72252 FGD Effluent Field Blank, Set 3 280-10655-3 Aqueous 12/09/2010 12/10/2010

SUMMARY 

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

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

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

EPA Method 200.8, by ICP/MS analysis. 

Any significant findings are summarized below. No additional data qualifiers were 

required. 

• One of the continuing calibration verifications (CCV) performed on 12/21/2010 

failed the method criteria for selenium. 

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

silver for sample 72196 failed the EPA Method 200.8 control limits of 70-130%. 

The MSD recovery for total silver for sample 72147 also failed the method 

control limits. 

• The MS/MSD relative percent difference (RPD) for total silver for samples 72147 

and 72196 failed the FGD ICP/MS SOP control limits of ±20%. 

• The post digestion spike (PDS) recoveries for copper, nickel, and silver for 

sample 72147 failed TestAmerica’s control limits of 85–115%. The PDS 

recovery for silver for sample 71997 also failed TestAmerica’s control limits. 

INTERNAL STANDARDIZATION 

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

INITIAL CALIBRATION 

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

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

INITIAL AND CONTINUING CALIBRATION VERIFICATION (ICV/CCV) 

The initial calibration verifications (ICV) and CCV performed by TestAmerica all had 

recoveries within the method criteria, except for selenium for one CCV on 12/21/2010. 

Samples associated with this CCV that had selenium values less than the reporting limit 

were reported. Any samples with selenium values above the reporting limit were 

reanalyzed. 

METHOD/INSTRUMENT BLANKS 

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

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

required for method blanks. 

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

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

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

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

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

LABORATORY CONTROL SAMPLES (LCS) 

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

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION 

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

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

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

ICS. 

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

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

SERIAL DILUTION 

The serial dilution performed on samples 72147 and 72196 passed TestAmerica’s criteria 

of ±10% difference. 
4

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

MS and MSD were performed on samples of 72147, 72196, and 71997. The MSD of 

sample 72147 failed the method control limits of 70–130% recovery for silver at 69%, 

which was flagged with an “F” qualifier. The MS/MSD of sample 72196 failed the 

method control limits of 70–130% recovery for silver, which was flagged with an “F” 

qualifier. These silver failures are likely due to matrix interference from the high 

concentration of sulfates, which can form insoluble silver sulfide and/or silver sulfate. 

The silver recoveries in the associated LCS/LCSDs were acceptable. The RPD for the 

MS/MSDs for samples 72147 and 72196 failed the FGD ICP/MS SOP ±20% control 

limits for silver. 

Otherwise, all MS/MSD spike recoveries were within the method control limits of 70-

130% and the RPD for the MS/MSDs were within the FGD ICP/MS SOP control limits 

of ±20 percent. No additional data qualifiers were required. 

POST DIGESTION SPIKES (PDS) 

The PDS performed on samples 72147 and 71997 passed TestAmerica’s control limits of 

85–115% recovery for all analytes, except for copper, nickel, and silver for PDS sample 

72147 and silver for PDS sample 71997, which were flagged with a “W” qualifier. No 

additional data qualifiers were required. 

DETECTION LIMITS 

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

of reagent water. 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

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

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Randy Mercurio, ERG 

Date: 2/9/2012

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

Monitoring: Month 3

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

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

titanium and zinc). The samples were analyzed according to EPA Method 200.7. 

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

EPA Method 200.7 

Table 1. Long-Term Monitoring Month 3 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71993 FGD Influent, Set 3 280-10586-1 Aqueous 12/08/2010 12/09/2010

71997 FGD Bioreactor Influent, Set 3 280-10654-1 Aqueous 12/09/2010 12/10/2010

72001 FGD Bioreactor Effluent, Set 3 280-10654-2 Aqueous 12/09/2010 12/10/2010

72006 FGD Bioreactor Influent Field 

Blank, Set 3 

280-10654-3 Aqueous 12/09/2010 12/10/2010

72010 FGD Bioreactor Effluent Field 

Blank, Set 3 

280-10654-4 Aqueous 12/09/2010 12/10/2010

72043 FGD Influent, Set 3 280-10584-1 Aqueous 12/08/2010 12/09/2010

72047 FGD Effluent, Set 3 280-10584-2 Aqueous 12/08/2010 12/09/2010

72052 FGD Bioreactor Effluent Field 

Blank, Set 3 

280-10584-3 Aqueous 12/08/2010 12/09/2010

72093 FGD Influent, Set 3 280-10515-1 Aqueous 12/07/2010 12/08/2010

72097 FGD Effluent, Set 3 280-10515-2 Aqueous 12/07/2010 12/08/2010

72102 FGD Effluent Field Blank, Set 3 280-10515-3 Aqueous 12/07/2010 12/08/2010

72143 FGD Influent, Set 3 280-10455-1 Aqueous 12/06/2010 12/07/2010

72147 FGD Bioreactor Influent, Set 3 280-10517-1 Aqueous 12/07/2010 12/08/2010

72151 FGD Bioreactor Effluent, Set 3 280-10517-2 Aqueous 12/07/2010 12/08/2010

72156 FGD Bioreactor Influent Field 

Blank, Set 3 

280-10517-3 Aqueous 12/07/2010 12/08/2010

72160 FGD Bioreactor Effluent Field 

Blank, Set 3 

280-10517-4 Aqueous 12/07/2010 12/08/2010

72192 FGD Influent, Set 1 280-10585-1 Aqueous 12/08/2010 12/09/2010
2

Table 1. Long-Term Monitoring Month 3 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72196 FGD SBR Influent, Set 1 280-10585-2 Aqueous 12/08/2010 12/09/2010

72200 FGD SBR Effluent, Set 1 280-10585-3 Aqueous 12/08/2010 12/09/2010

72205 FGD SBR Influent Field Blank, 

Set 1 

280-10585-4 Aqueous 12/08/2010 12/09/2010

72209 FGD SBR Effluent Field Blank, 

Set 1 

280-10585-5 Aqueous 12/08/2010 12/09/2010

72243 FGD Influent, Set 3 280-10655-1 Aqueous 12/09/2010 12/10/2010

72247 FGD Effluent, Set 3 280-10655-2 Aqueous 12/09/2010 12/10/2010

72252 FGD Effluent Field Blank, Set 3 280-10655-3 Aqueous 12/09/2010 12/10/2010

SUMMARY 

The samples were prepared for total metals analysis according to TestAmerica’s SOP for 

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

summarized below. Additional data qualifiers were required (see Table 2). 

• The serial dilution for cobalt, iron, and zinc for sample 72143 failed 

TestAmerica’s SOP control limit of percent differences less than 10%. 

• The post digestion spike (PDS) for calcium, iron, magnesium, and zinc for sample 

72143 failed TestAmerica’s control limits of 85–115% recovery. 

• The PDS for manganese for sample 72147 failed TestAmerica’s control limits of 

85–115% recovery. 

SAMPLE RECEIPT, HANDLING AND STORAGE ISSUES 

The samples associated with Episode 6569 (72192, 72196, 72200, 72205, and 72209) did

not have a sample date or time on the traffic report. 

INTERNAL STANDARDIZATION 

While the internal standard (ISTD) yttrium was used for these analyses, no checks for the 

ISTD recoveries within the ±30% criterion of the 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. 
3

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) 

All LCSs 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.

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 cobalt, 

iron, and zinc for sample 72143, which were flagged with a “V” qualifier. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

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

samples of 72143, 72147, and 72196. Some elements with high concentrations failed the 

EPA 200.7 Method spike recovery control limits of 70–130% but were flagged with a “4” 

qualifier indicating that the concentration in the parent sample was greater than 4 times 

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

based on the LCS passing the method control limits. Otherwise, all MS/MSD spike 

recoveries were within the method control criteria of 70-130%. The RPD for all 
4

MS/MSDs were within TestAmerica’s ± 20% requirement. No additional data qualifiers 

were needed. 

POST DIGESTION SPIKE (PDS) 

The PDS performed on sample 72143 passed TestAmerica’s control limits of 85–115% 

recovery for all analytes except aluminum, boron, calcium, iron, magnesium, titanium, 

and zinc. Calcium, magnesium, and zinc were qualified with a “W”. Calcium and 

magnesium did pass in the matrix spike for this sample. Aluminum, boron, iron and 

titanium failed the PDS; however, the percent recoveries were not calculated by the 

laboratory because their concentrations were greater than 4 times the PDS spike level. 

Aluminum, boron, and titanium passed TestAmerica’s requirement of percent differences 

less than 10% for the serial dilution for this sample demonstrating that there were no 

significant matrix interference with these elements. Iron and zinc failed TestAmerica’s 

requirements for the serial dilution; therefore, based on these cumulative results, iron and 

zinc are being qualified as suspect due to matrix interference. These additional qualifiers 

appear in Table 2. 

The PDS performed on sample 72147 passed TestAmerica’s control limits of 85–115% 

recovery for all analytes except boron and manganese. Manganese was qualified with a 

“W”. Boron failed the PDS; however, the percent recovery was not calculated by the 

laboratory because its concentration was greater the 4 times the PDS spike level. Both 

boron and manganese passed TestAmerica’s requirement of percent differences less than 

10% for the serial dilution for sample 72147 demonstrating that there were no significant 

matrix interferences. No additional qualifier is required due to this PDS. 

The PDS performed on sample 72196 passed TestAmerica’s control limits of 85–115% 

recovery for all analytes except boron and manganese; however, the percent recoveries 

were not calculated by the laboratory because their concentrations were greater than 4 

times the PDS spike level. Both boron and manganese passed TestAmerica’s requirement 

of percent differences less than 10% for the serial dilution for sample 72196 

demonstrating that there were no significant matrix interferences. No additional qualifier 

is required due to this PDS. 

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 

72143 Iron (total) Matrix 

Interference 

PDS and SD Failed XXX μg/L 

72143 Zinc (total) Matrix 

Interference 

PDS and SD Failed XXX ug/L 
1 

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

CC: Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Jennifer Colby, ERG 

Date: 2/9/2012 

Subject: TestAmerica Data Review Narrative for Classicals Analyses – Long-Term 

Monitoring: Month 3 

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for these long-term monitoring samples. 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 Kjeldakl Nitrogen (TKN) by EPA method 351.2, and 

• Total Suspended Solids (TSS) by SM 2540D. 

Table 1 summarizes the 15 samples that TestAmerica analyzed for the above analytes. 

Table 1. Long-Term Monitoring Month 3 Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71993 Water FGD Influent, Set 3 12/08/2010 

71997 Water FGD Bioreactor Influent, Set 3 12/09/2010 

72001 Water FGD Bioreactor Effluent, Set 3 12/09/2010 

72043 Water FGD Influent, Set 3 12/08/2010 

72047 Water FGD Effluent, Set 3 12/08/2010 

72093 Water FGD Influent, Set 3 12/07/2010 

72097 Water FGD Effluent, Set 3 12/07/2010 

72143 Water FGD Influent, Set 3 12/06/2010 

72147 Water FGD Bioreactor Influent, Set 3 12/07/2010 
2 

Table 1. Long-Term Monitoring Month 3 Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72151 Water FGD Bioreactor Effluent, Set 3 12/07/2010 

72192 Water FGD Influent, Set 1 12/08/2010 

72196 Water FGD SBR Influent, Set 1 12/08/2010 

72200 Water FGD SBR Effluent, Set 1 12/08/2010 

72243 Water FGD Influent, Set 3 12/09/2010 

72247 Water FGD Effluent, Set 3 12/09/2010 

SUMMARY 

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

unless otherwise noted below. All samples were preserved appropriately unless 

otherwise specified below. Samples 72192, 72196, and 72200 had no collection dates or 

times listed on the traffic report, and were given the date of relinquishment. Many of the 

traffic reports did not have receipt temperatures.

 

Field duplicate samples were not collected for this episode. Depending on the method, a 

laboratory duplicate was analyzed instead. The Relative Percent Difference (RPD) 

between the sample and its duplicate was less than 20% unless otherwise noted below. 

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

If sample results were above the highest standard used 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) analysis was run on sample 72147 and 

sample 72196 for each analyte to check for matrix interferences. All MS samples 

analyzed met the criteria specified in the method unless described below. 
3 

DATA NOTES/ISSUES 

Ammonia 

The result for the method blank associated with one of the batches was greater than the 

MDL. All associated samples were flagged with a “B” qualifier. This affects samples 

72147, 72143, 72093, 72097, and 72151. No further action is required. 

The percent recoveries for the MS and matrix spike duplicate (MSD) for sample 72147 

were 93% and 102%, respectively, which is within the method control criteria; however, 

the results exceeded the calibration range. These MS and MSD and results were flagged 

with an “E” qualifier. 

BOD5 

TestAmerica analyzed five dilutions, but no dilutions had a dissolved oxygen (DO) 

depletion greater than 2.0 mg/L for samples 72143, 72151, 72043, 71993, and 72247. 

Therefore, BOD5 was reported as not detected for these samples. Additionally, for sample 

72200, the dilutions did not have a residual DO criteria of greater than 1.0 mg/L; 

therefore, BOD5 was reported as not detected for this sample. The rest of the samples had 

at least one dilution with a DO depletion greater than 2.0 mg/L. As required in the 

method, the final result was calculated by taking the average of the results for all 

dilutions with a DO depletion greater than 2.0 mg/L and a final DO greater than 1.0 

mg/L. 

Chloride and Sulfate 

MS and MSD were performed on samples 72147 and 72196. The MS/MSD recoveries 

for both samples were within the method control for both chloride and sulfate; however, 

the MS and MSD results for chloride exceeded the calibration range. Both sets of 

MS/MSD results were flagged with “E” qualifiers. 

COD 

MS and MSD were performed on samples 72147 and 72196. The MS and MSD 

recoveries for sample 72147 were 66% and 71%, respectively, which is outside the 

method control criteria. These MS/MSD results were flagged with an “F” qualifier. The 

MS and MSD recoveries for sample 72196 were 72% and 70%, respectively, which is 

outside the method control criteria. These MS/MSD results were flagged with an “F” 

qualifier. 

Cyanide 

Because of the nature of the sample matrix, all of the samples in this sampling episode 

used a lower volume, which resulted in elevated RLs being calculated and reported by 

TestAmerica with the sample results. 
4 

MS and MSD were performed on samples 72147 and 72196. The MS and MSD 

recoveries for sample 72147 were 76% and 75%, respectively. The MS and MSD 

recoveries for sample 72196 were 59% and 57%, respectively. The LCS/LCSD 

recoveries associated with these batches were acceptable, which indicates the analytical 

system was operating within control. Additionally, there is no method requirement for the 

analysis of a MS/MSD and therefore, no corrective action is necessary. 

Nitrate/Nitrite 

No MS/MSD data was reported for batch 45200 in the sample and QC sample report 

summary. The method requires that a known amount of analyte be added to 10% of 

samples per batch. The general chemistry worksheet indicates that MS samples were 

performed on a sample outside of these episodes, but no spiking concentrations or percent 

recoveries are indicated. The MS/MSD recoveries for the other batches were within 

control limits. 

Phosphorus 

The results for the method blanks associated with two of the batches was greater than the 

MDL, but less than the RL. The blank results were flagged with a “J” qualifier. All 

associated samples were qualified with a “B” flag. No additional corrective action is 

necessary. 

MS and MSD were performed on sample 72001, 72147 and 72196. The percent 

recoveries for the MS and MSD for sample 72147 were 69% and 70%, respectively, 

which is outside the method control criteria. These MS/MSD results were flagged with 

an “F” qualifier. The LCS/LCSD recoveries for this batch were acceptable and indicate 

that the analytical system was operating within control. The percent recoveries for the 

MS and MSD for sample 72196 were 91% and 85%, respectively. The MSD recovery is 

outside the method control criteria, but within the laboratory criteria and therefore, was 

not flagged. If reported, the MSD result should be flagged with an “F” qualifier. The 

LCS/LCSD recoveries for this batch were acceptable and indicate that the analytical 

system was operating within control. Additionally, the MS/MSD performed on sample 

72001 was in the same batch as the MS/MSD for 72196 and the percent recoveries for the 

MS and MSD were 96% and 97%, respectively, with are within the method control 

criteria. 

TDS 

TA reports that constant weight was not achieved after 3 drying cycles for the following 

samples: 72097, 72143, 72147, 72151, 71993, 72196, 72200, 71997, 72004, and 72243. 

Review of the general chemistry worksheets indicates that constant weight was achieved 

for all samples. No further action was necessary. 
5 

Because of the nature of the sample matrix, some of the samples in this sampling episode 

used a lower volume, which resulted in elevated RLs being calculated and reported by 

TestAmerica with the sample results. 

The analytical duplicate associated with sample 72143 exceeded the recovery criteria. 

The duplicate result was qualified with an “F” flag. Because an analytical duplicate was 

not required by the method, no further corrective action is necessary. 

TKN 

MS and MSD were performed on samples 72147 and 72196. The MS and MSD 

recoveries for sample 72147 were 76% and 57%, respectively. The concentration in the 

original sample was greater than four times the spike amount; therefore, the recoveries 

cannot be reliably calculated and the results were flagged with a “4” qualifier. The MS 

and MSD recoveries for sample 72196 were 81% and 78%, respectively, which do not 

meet the method control criteria, but do meet the laboratory control criteria and therefore, 

these results were not flagged by the laboratory. If reported, the MS and MSD results 

should be flagged with “F” qualifiers. The LCS/LCSD recoveries associated with these 

batches were acceptable, which indicates the analytical system was operating within 

control. 

TSS 

Because of the nature of the sample matrix, some of the samples in this sampling episode 

used a lower volume, which resulted in elevated RLs being calculated and reported by 

TestAmerica with the sample results. 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

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

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Donna Tedder, ERG 

Date: 2/9/2012

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

Month 4 and 5

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 30 samples (excluding laboratory prep blanks) FGS extracted 

and analyzed for total mercury. 

Table 1. Long-Term Monitoring Month 4 and 5 Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71994 1101223-48 Aqueous FGD Influent, Set 4 1/17/2011

71998 1101223-53 Aqueous FGD Bioreactor Influent, Set 4 1/17/2011

72002 1101223-58 Aqueous FGD Bioreactor Effluent, Set 4 1/17/2011

72007 1101223-59 Aqueous FGD Bioreactor Influent Field Blank, Set 4 1/17/2011

72011 1101223-60 Aqueous FGD Bioreactor Effluent Field Blank, Set 4 1/17/2011

72044 1101308-01 Aqueous FGD Influent, Set 4 1/26/2011

72048 1101308-06 Aqueous FGD Effluent, Set 4 1/25/2011

72053 1101308-07 Aqueous FGD Effluent Field Blank, Set 4 1/25/2011

72094 1101223-41 Aqueous FGD Influent, Set 4 1/14/2011

72098 1101223-46 Aqueous FGD Effluent, Set 4 1/14/2011

72103 1101223-47 Aqueous FGD Effluent Field Blank, Set 4 1/13/2011

72144 1101223-21 Aqueous FGD Influent, Set 4 1/12/2011

72148 1101223-26 Aqueous FGD Bioreactor Influent, Set 4 1/12/2011

72152 1101223-31 Aqueous FGD Bioreactor Effluent, Set 4 1/12/2011

72157 1101223-32 Aqueous FGD Bioreactor Influent Field Blank, Set 4 1/12/2011

72161 1101223-33 Aqueous FGD Bioreactor Effluent Field Blank, Set 4 1/12/2011

72193 1101223-08 Aqueous FGD Influent, Set 3 1/12/2011

72197 1101223-13 Aqueous FGD SBR Influent, Set 3 1/12/2011

72201 1101223-18 Aqueous FGD SBR Effluent, Set 3 1/12/2011
2

Table 1. Long-Term Monitoring Month 4 and 5 Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72206 1101223-19 Aqueous FGD SBR Influent Field Blank, Set 3 1/12/2011

72210 1101223-20 Aqueous FGD SBR Effluent Field Blank, Set 3 1/12/2011

72244 1101223-34 Aqueous FGD Influent, Set 4 1/12/2011

72248 1101223-39 Aqueous FGD Effluent, Set 4 1/13/2011

72253 1101223-40 Aqueous FGD Effluent Field Blank, Set 4 1/12/2011

72293 1101223-01 Aqueous FGD Influent, Set 3 1/12/2011 

72297 1101223-06 Aqueous FGD Effluent, Set 3 1/12/2011

72302 1101223-07 Aqueous FGD Effluent, Field Blank, Set 3 1/12/2011

72294 1102108-01 Aqueous FGD Influent, Set 4 2/9/2011

72298 1102108-06 Aqueous FGD Effluent, Set 4 2/9/2011

72303 1102108-07 Aqueous FGD Effluent Field Blank, Set 4 2/9/2011

SUMMARY 

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

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

dataset. The following summarizes the findings from the data review: 

• The sample number for Sample 72157 was labeled incorrectly on the traffic 

report. 

• The sample description for Sample 72148 was entered incorrectly by FGS at the 

time of sample receipt. 

• Two laboratory duplicates were out of the method-suggested relative percent 

difference (RPD) criteria. 

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES 

Sample 72157 was labeled incorrectly as Sample 721557 in the traffic report submitted to 

the laboratory. The error was identified and corrected during the data review based on 

the sample description. FGS incorrectly labeled Sample 72148 as the FGD Bioreactor 

Effluent, Set 4, when the correct sample description is FGD Bioreactor Influent, Set 4. 

This error was identified and corrected during the data review and confirmed based on 

the traffic report. 
3

INITIAL CALIBRATION 

FGS performed the initial calibrations on each 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 the method-specified criteria. Because all of the blank 

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

results. 

DUPLICATES 

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

were analyzed in duplicate at the laboratory, Influent samples 72144 and 71994 and 

Effluent samples 72048 and 72298. The relative percent difference (RPD) for samples 

72144, 71994, 72048, and 72298 were 30.6%, 7.66%, 19.4% and 43.9%, respectively. 

Two of these RPDs were outside of laboratory criteria. The samples from another 

sampling episode were also analyzed in duplicate with RPDs of 13.3%, 22.4%, and 

3.03%. The laboratory’s RPD criteria between analytical duplicates is 24%. Analytical 

duplicates are not a method requirement; therefore, no samples were qualified based on 

analytical duplicates. 

LABORATORY CONTROL SAMPLES 

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

and 24% RPD. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

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

sample 72144 and Effluent samples 72048 and 72298. MS/MSDs were also performed 

on samples from another sampling episode. All aqueous MS/MSD recoveries were 

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

DETECTION LIMITS 

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

were reported as not detected (ND). 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

CC: Jezebele Alicea, Alternate Work Assignment Manager, 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 6572 

and Episode 6566 (Set 4) 

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

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

Episode 6572 and long-term monitoring, set 4 samples for Episode 6566. 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 6572 and 6566 (Set 4) – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72044 FGD Influent, Set 4 280-11953-1 Aqueous 1/26/2011 1/27/2011

72048 FGD Effluent, Set 4 280-11953-2 Aqueous 1/26/2011 1/27/2011

72053 FGD Effluent Field Blank, Set 4 280-11953-3 Aqueous 1/26/2011 1/27/2011

72341 FGD Scrubber Purge, Set 1 280-11853-1 Aqueous 1/24/2011 1/25/2011

72342 FGD Scrubber Purge, Set 2 280-11893-3 Aqueous 1/25/2011 1/26/2011

72343 FGD Scrubber Purge, Set 3 280-11958-1 Aqueous 1/26/2011 1/27/2011

72344 FGD Scrubber Purge, Set 4 280-12014-2 Aqueous 1/27/2011 1/28/2011

72345 FGD Concentrator Distillate, Set 1 280-11893-1 Aqueous 1/25/2011 1/26/2011

72346 FGD Concentrator Distillate, Set 2 280-11958-3 Aqueous 1/26/2011 1/27/2011

72347 FGD Concentrator Distillate, Set 3 280-12014-1 Aqueous 1/27/2011 1/28/2011

72348 FGD Concentrator Distillate, Set 4 280-12078-1 Aqueous 1/28/2011 1/31/2011

72349 FGD Scrubber Purge Field Blank 280-11853-3 Aqueous 1/24/2011 1/25/2011

72350 FGD Concentrator Distillate Field 

Blank, Set 1 

280-11893-2 Aqueous 1/25/2011 1/26/2011

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 
2

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

EPA Method 200.8, by ICP/MS analysis. 

Any significant findings are summarized below. No additional data qualifiers were 

required. 

• One of the continuing calibration verifications (CCV) performed on 2/9/2011 

failed the method criteria for chromium and vanadium. 

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 CCV performed by TestAmerica all had 

recoveries within the method criteria, except for chromium and vanadium for the last 

CCV performed on 2/9/2011. All chromium and vanadium results associated with this 

CCV were non-detects and therefore, no corrective action was taken. All chromium and 

vanadium values reported that were associated with this CCV have been flagged with a 

“^” qualifier. No additional qualifiers were required. 

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; however, some elements were above the MDL and 

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

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

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

LABORATORY CONTROL SAMPLES (LCS) 

All LCS samples passed the method QC limits of 85–115% recovery. 
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 72345 passed TestAmerica’s criteria of ±10% 

difference. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

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

72345 and 72346. All MS/MSD spike recoveries were within the method control limits 

of 70–130% for all analytes. 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 MS/MSD samples. 

POST DIGESTION SPIKES (PDS) 

The post digestion spike (PDS) performed on sample 72345 passed TestAmerica’s 

control limits of 85–115% recovery for all analytes. No additional data qualifiers were 

required for the PDS sample. 

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: Randy Mercurio, ERG 

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.7 – Episode 6572 

and Episode 6566 (Set 4)

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 6572 and long-term monitoring, set 4 samples for 

Episode 6566. 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 6572 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72044 FGD Influent, Set 4 280-11953-1 Aqueous 1/26/2011 1/27/2011

72048 FGD Effluent, Set 4 280-11953-2 Aqueous 1/26/2011 1/27/2011

72053 FGD Effluent Field Blank, Set 4 280-11953-3 Aqueous 1/26/2011 1/27/2011

72341 FGD Scrubber Purge, Set 1 280-11853-1 Aqueous 1/24/2011 1/25/2011

72342 FGD Scrubber Purge, Set 2 280-11893-3 Aqueous 1/25/2011 1/26/2011

72343 FGD Scrubber Purge, Set 3 280-11958-1 Aqueous 1/26/2011 1/27/2011

72344 FGD Scrubber Purge, Set 4 280-12014-2 Aqueous 1/27/2011 1/28/2011

72345 FGD Concentrator Distillate, Set 1 280-11893-1 Aqueous 1/25/2011 1/26/2011

72346 FGD Concentrator Distillate, Set 2 280-11958-3 Aqueous 1/26/2011 1/27/2011

72347 FGD Concentrator Distillate, Set 3 280-12014-1 Aqueous 1/27/2011 1/28/2011

72348 FGD Concentrator Distillate, Set 4 280-12078-1 Aqueous 1/28/2011 1/31/2011

72349 FGD Scrubber Purge Field Blank 280-11853-3 Aqueous 1/24/2011 1/25/2011

72350 FGD Concentrator Distillate Field 

Blank, Set 1 

280-11893-2 Aqueous 1/25/2011 1/26/2011
2

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. 

• A serial dilution for boron for sample 72345 failed TestAmerica’s requirements of 

percent difference less than 10%. 

• The post digestion spike (PDS) for barium for sample 72345 failed TestAmerica’s 

control limits of 85-115% recovery. 

SAMPLE RECEIPT, HANDLING AND STORAGE ISSUES 

There were no sample receipt issues in this data package. 

INTERNAL STANDARDIZATION 

While the internal standard (ISTD) yttrium was used for these analyses, no checks for the 

ISTD recoveries within the ±30% criterion of the 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. 
3

LABORATORY CONTROL SAMPLES (LCS) 

All LCSs 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.

SERIAL DILUTION (SRD) 

A serial dilution was performed on sample 72345 which had percent differences less than 

10% as required by TestAmerica’s SOP for all elements except boron at 11%. This 

boron result 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) 

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

samples of 72345 and 72346. All MS/MSD spike recoveries were within the method 

control criteria of 70-130% for all elements. The relative percent difference (RPD) for all 

MS/MSDs were within TestAmerica’s ± 20% requirement. 

POST DIGESTION SPIKE (PDS) 

The PDS performed on sample 72345 passed TestAmerica’s control limits of 85-115% 

recovery for all analytes except barium. A qualifier would have been required for this 

barium result; however, barium was not detected in this sample. 

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: Ariel Atkinson, ERG 

Date: 2/9/2012 

Subject: TestAmerica Data Review Narrative for Classicals Analyses – Episode 6572 

and Episode 6566 (Set 4) 

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for Sample Episode 6572 and Episode 6566 (Set 4 samples). 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 ten samples that TestAmerica analyzed for the above analytes. 

Table 1. Long Term Monitoring Iatan Episode 6572 Classical Analytes – 

Sample Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72044 Water FGD Influent, Set 4 1/26/11

72048 Water FGD Effluent, Set 4 1/26/11

72341 Water FGD Scrubber Purge Set 1 1/24/11

72342 Water FGD Scrubber Purge, Set 2 1/25/11

72343 Water FGD Scrubber Purge, Set 3 1/26/11

72344 Water FGD Scrubber Purge, Set 4 1/27/11

72345 Water FGD Concentrator Distillate, Set 1 1/24/11; 1/25/11

72346 Water FGD Concentrator Distillate, Set 2 1/25/11; 1/26/11

72347 Water FGD Concentrator Distillate, Set 3 1/26/11; 1/27/11

72348 Water FGD Concentrator Distillate, Set 4 1/27/11; 1/28/11
2 

SUMMARY 

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

samples were preserved appropriately. BOD analysis was not performed on sample 

72348 because it was received after the hold time had expired. 

Field duplicate samples were not collected for these episodes. Depending on the method, 

a laboratory duplicate was analyzed, instead. The Relative Percent Difference (RPD) 

between the sample and its duplicate was less than 20% unless otherwise noted below. 

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

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

diluted and reanalyzed, unless otherwise specified below. 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 

unless otherwise noted below. 

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. 

If required by the method, a matrix spike (MS) sample was analyzed on samples 72344, 

72346, or 72348 for each analyte to check for matrix interferences. MS samples analyzed 

met the criteria specified in the method unless described otherwise below. 

DATA NOTES/ISSUES 

Ammonia 

A MS and matrix spike duplicate (MSD) were performed on sample 72346. The percent 

recoveries were 130% and 127%, respectively, which are above the method specific 

control limit of 90-110%. These MS/MSD results were flagged with a “4” qualifier 

because the analyte present in the original sample is four times greater than the matrix 

spike concentration; therefore, the control limits are not applicable. No further 

qualification is necessary. 

A MS and MSD were also performed using sample 72348. The percent recoveries for the 

MS and MSD were 120% and 113%, respectively, which is greater than the control 

limits. Both the MS and MSD were flagged with “F” qualifiers. 
3 

BOD5 

TestAmerica analyzed five dilutions; the dilutions had dissolved oxygen (DO) depletions 

greater than 2.0 mg/L for samples 72345, 72346, and 72347. As required in the method, 

the final result was calculated by taking the average of the results for all dilutions with a 

DO depletion greater than 2.0 mg/L and a final DO greater than 1.0 mg/L. 

Chloride and Sulfate 

Samples 72345, 72346, 72347, and 72348 had results below the lowest calibration 

standard. All of these samples had results that were greater than the MDL, but less than 

the RL; therefore, the samples were flagged with a “J” qualifier. No further qualification 

is required.

COD 

A MS and MSD were performed for sample 72344. The MSD percent recover was 80%, 

which is outside the method criteria. The MSD result was flagged with an “F” qualifier. 

No further qualification is necessary. 

Sample 72348 had a result below the lowest calibration standard, but this result was 

greater than the MDL, but less than the RL and therefore, was flagged with “J” qualifier. 

No further qualification is necessary. 

 

Cyanide 

The calibration was performed using standards ranging from 0.00 ppb to 400.0 ppb. The 

method states that the appropriate range of calibration standard concentrations for this 

method is between 5 ppb and 20 ppb. All samples in which cyanide was detected had 

results ≥ 20 ppb. 

MS/MSDs were performed using samples 72344 and 72346. The percent recoveries for 

the MS and the MSD for sample 72344 were 43% and 45%, respectively. The percent 

recovery for both the MS and the MSD for sample 72346 was 88%. The percent 

recoveries for both sets of MS/MSDs are below the control limit of 90% and as a result 

the MS/MSDs were flagged with “F” qualifiers. 

Nitrate/Nitrite 

Samples 72345, 72346, 72347, and 72348 had results below the lowest calibration 

standard. These results were greater than the MDL, but less than the RL and therefore, 

the results were flagged with “J” qualifiers. No further qualification is necessary. 

The data report narrative for nitrate/nitrite indicates an incorrect sample ID (72493) as 

requiring a dilution. No such sample is included in this episode. 
4 

Phosphorus 

The LRB results for both batches of samples had phosphorus concentrations greater than 

the MDL at 0.0154 mg/L for batch 51117 and 0.0106 mg/L for batch 51477; however the 

results were below than the RL. Therefore, the LRB results were flagged with “J” 

qualifiers and all samples that contained the analyte were flagged with “B” qualifiers. All 

calibration blank results were also above the MDL but less than the RL, and therefore, 

were also flagged with “J” qualifiers. 

Samples 72345, 72346, 72347, and 72348 had results that were lower than the lowest 

calibration standard. These results were greater than the MDL, but less than the RL and 

therefore, were flagged with a “J” qualifier. No further qualifiers are needed. 

TDS 

Constant weight was not achieved after 3 drying cycles for the samples. It should be 

noted that the weight increased from the first weighing to the second weighing and/or 

second weighing to third weighing for samples 72344, 72347, 72343, 72346, 72345, and 

72342. Method 2540C warns that samples which contain high levels of calcium, 

magnesium, chloride, and sulfate may be hygroscopic meaning they absorb moisture 

from the air. The concentrations of all of these species may be high in these samples; and 

so this was likely the cause for the inconsistent weight calculations. These samples were 

not qualified, but results may be biased high. 

The RPD for the laboratory duplicate from sample 72347 was 67%, which is greater than 

the 10% control limit required by SM 2540C. The sample was not qualified, but the 

duplicate was flagged with a “J” qualifier because the duplicate result was greater than 

the MDL, but less than the RL. 

TKN 

The LRB results for batch 53496 had a TKN concentration greater than the MDL at 0.389 

mg/L; however the results were below the RL. The LRB result was flagged with a “J” 

qualifier and sample 72348 was flagged with a “B” qualifier. The initial calibration blank 

results for both batches were also above the MDL but less than the RL at 0.375 mg/L for 

batch 51337 and 0.378 mg/L for batch 53692, and therefore were also flagged with “J” 

qualifiers. 

TestAmerica performed MS/MSD analyses on sample 72346. The percent recoveries for 

the MS and MSD samples were 377% and 378%, respectively. The MS and the MSD did 

not meet the method control limits of 90-110%, so they were flagged with “F” qualifiers. 

No further qualification is necessary. 

TSS 

No issues were identified by data reviewer.