Sampling Episode Report 

We Energies’ 

Pleasant Prairie Power Plant 

Pleasant Prairie, WI 

Sampling Episode 6559 

Prepared for:

U.S. Environmental Protection Agency

Engineering and Analysis Division 

Office of Water 

1200 Pennsylvania Avenue, NW 

Washington, D.C. 20460 

Prepared by: 

Eastern Research Group, Inc.

14555 Avion Parkway 

Suite 200 

Chantilly, VA 20151 

 13 December 2011 

EPA Contract No. 68-C-02-095 

Work Assignment 9-29
i 

CONTENTS 

Page 

1. INTRODUCTION ................................................................................................................. 1-1

1.1 Background of Detailed Study ............................................................................. 1-1

1.2 Power Plant Site Selection ................................................................................... 1-1

1.3 Sampling Episode Overview................................................................................ 1-2

2. FACILITY OVERVIEW ........................................................................................................ 2-1

2.1 FGD Scrubber System ......................................................................................... 2-2

2.2 FGD Wastewater Treatment System ................................................................... 2-3

2.2.1 Physical/Chemical Separation ................................................................. 2-3

2.2.2 Sampling Points ....................................................................................... 2-5

3. SAMPLE COLLECTION ....................................................................................................... 3-1

3.1 Sampling Points, Sample Collection Methods, and Field Measurements ........... 3-1

3.1.1 Influent to FGD Wastewater Treatment System ...................................... 3-2

3.1.2 Effluent from FGD Wastewater Treatment ............................................. 3-4

3.2 List of Analytes and Sample Preservation ........................................................... 3-7

3.3 Plant Operational Data ......................................................................................... 3-8

3.4 Deviations from the Sampling and Analysis Plan ............................................... 3-8

4. LABORATORY ANALYTICAL RESULTS AND DISCUSSION ................................................... 4-1

5. DATA QUALITY ................................................................................................................. 5-1

5.1 Analytical Quality Control ................................................................................... 5-1

5.2 Field Quality Control ........................................................................................... 5-1

5.2.1 Bottle Blanks ............................................................................................ 5-1

5.2.2 Equipment Blanks .................................................................................... 5-2

5.2.3 Field Blanks ............................................................................................. 5-2

5.2.4 Field Duplicates ....................................................................................... 5-4

6. REFERENCES ..................................................................................................................... 6-1

Appendix A: ANALYTICAL RESULTS

Appendix B: DATA REVIEW NARRATIVES

Appendix C: PICTURES FROM THE SAMPLING EPISODE
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LIST OF TABLES 

Page 

Table 3-1. Sample Collection Information, Pleasant Prairie ....................................................... 3-9

Table 3-2. Sample Collection at Pleasant Prairie ....................................................................... 3-11

Table 3-3. Field Measurements, Pleasant Prairie ....................................................................... 3-12

Table 3-4. Crosswalk of Sample Number to Sampling Point and Day, Pleasant Prairie .......... 3-14

Table 3-5. Analytical Methods, Pleasant Prairie ....................................................................... 3-15

Table 3-6. Summary of Sample Container and Planned Preservation, Pleasant Prairie ............ 3-16

Table 3-7. Sample Preservation Summary, Pleasant Prairie ...................................................... 3-17

Table 3-8. Generating Unit Operating Characteristics during Sample Collection, Pleasant 

Prairie ............................................................................................................................. 3-19

Table 3-9. FGD Scrubber System Operating Characteristics, Pleasant Prairie ......................... 3-20

Table 3-10. Coal Usage during Sample Collection, Pleasant Prairie ........................................ 3-21

Table 3-11. Scrubber Slurry Information during Sample Collection, Pleasant Prairie ............. 3-21

Table 3-12. FGD Wastewater Treatment System Operation Information, Pleasant Prairie ...... 3-22

Table 4-1. Influent to FGD Wastewater Treatment System, Pleasant Prairie ............................ 4-3

Table 4-2. Effluent From FGD Wastewater Treatment System, Pleasant Prairie ...................... 4-6

Table 4-3. Classical Pollutants 4-Day Average Data Summary for FGD Wastewater 

Treatment System, Pleasant Prairie ................................................................................. 4-9

Table 4-4. Metal Pollutants 4-Day Average Data Summary for FGD Wastewater 

Treatment System, Pleasant Prairie ............................................................................... 4-10

Table 5-1. Field Blank Analytical Results, Pleasant Prairie ....................................................... 5-5

Table 5-2. Field Duplicate Results – Effluent from FGD Wastewater Treatment System, 

Pleasant Prairie ................................................................................................................. 5-6

Table A-1. Influent to FGD Wastewater Treatment System, Day 1 Analytical Results, 

Pleasant Prairie ................................................................................................................ A-1

Table A-2. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, 

Pleasant Prairie ................................................................................................................ A-4
LIST OF TABLES (Continued) 

Page 

iii

Table A-3. Influent to FGD Wastewater Treatment System, Day 3 Analytical Results, 

Pleasant Prairie ................................................................................................................ A-7

Table A-4. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, 

Pleasant Prairie .............................................................................................................. A-10

Table A-5. Effluent from FGD Wastewater Treatment System, Day 1 Analytical Results, 

Pleasant Prairie .............................................................................................................. A-13

Table A-6. Effluent from FGD Wastewater Treatment System, Day 2 Analytical Results, 

Pleasant Prairie .............................................................................................................. A-16

Table A-7. Effluent from FGD Wastewater Treatment System, Day 3 Analytical Results, 

Pleasant Prairie .............................................................................................................. A-19

Table A-8. Effluent from FGD Wastewater Treatment System, Day 4 Analytical Results, 

Pleasant Prairie .............................................................................................................. A-22

Table A-9. Duplicate of Effluent from FGD Wastewater Treatment System, Analytical 

Results, Pleasant Prairie ................................................................................................ A-25

Table A-10. Bottle Blank and Equipment Blank Analytical Data, Pleasant Prairie ................. A-28

Table A-11. Influent to FGD Wastewater Treatment System Field Blank, Day 1 

Analytical Results, Pleasant Prairie .............................................................................. A-33

Table A-12. Effluent from FGD Wastewater Treatment System Field Blank, Day 1 

Analytical Results, Pleasant Prairie .............................................................................. A-35

Table A-13. Effluent from FGD Wastewater Treatment System Field Blank, Day 2 

Analytical Results, Pleasant Prairie .............................................................................. A-37

Table A-14. Effluent from FGD Wastewater Treatment System Field Blank, Day 3 

Analytical Results, Pleasant Prairie .............................................................................. A-38

Table A-15. Effluent from FGD Wastewater Treatment System Field Blank, Day 4 

Analytical Results, Pleasant Prairie .............................................................................. A-39
iv

LIST OF FIGURES 

Page 

Figure 2.1. FGD Wastewater Treatment System, Pleasant Prairie Power Plant .......................... 2-6

Figure C-1. Sampler Working Inside a “Cleanbox” ....................................................................C-1

Figure C-2. Sample Tap and Tubing at the Influent to the FGD Wastewater Treatment 

System ..............................................................................................................................C-2

Figure C-3. Sample Collection Set-Up at the Pump-Off Station .................................................C-3

Figure C-4. Sample Tap and Tubing at the Effluent from the FGD Wastewater Treatment 

System ..............................................................................................................................C-4
1-1 

1. INTRODUCTION

The Engineering and Analysis Division (EAD) of the U.S. Environmental Protection 

Agency (EPA) is conducting a sampling program at steam electric power plants. The sampling 

program will characterize raw wastewaters generated by coal-fired steam electric power plants 

and evaluate treatment technologies and best management practices used to reduce pollutant 

discharges. This Sampling Episode Report (SER) describes the sampling activities that took 

place June 20 - 25, 2010, at We Energies’ Pleasant Prairie Power Plant (Pleasant Prairie), located 

in Pleasant Prairie, Wisconsin (Sampling Episode 6559). The focus of Episode 6559 was to 

characterize the purge stream entering the flue gas desulfurization (FGD) wastewater treatment 

system and the effluent from the chemical precipitation system. 

1.1 Background of Detailed Study

 During EPA’s recently completed detailed study of the steam electric industry, EPA 

identified metals and certain other constituents present in the wastewater discharges from steam 

electric power plants that substantially contribute to the toxic loadings for the industry. 

Additionally, EPA determined that one of the waste streams contributing most of these toxic 

loadings are associated with wet flue gas desulfurization (FGD) systems present at coal-fired 

power plants. Based on these findings, EPA has focused the sampling program on characterizing 

the untreated FGD wastewaters and effluent quality from technologies designed to treat the 

wastewater. 

1.2 Power Plant Site Selection

EPA selected steam electric plants for FGD wastewater sampling based on the process 

configurations and characteristics of the plants. 

Pleasant Prairie was selected by EPA for sampling based on the following site 

characteristics: 

 The plant is a coal-fired power plant that burns Powder River Basin (PRB) coal in 

each of its two generating units; 

 The plant operates limestone forced oxidation wet FGD systems on both units; 

 The plant operates a segregated FGD wastewater treatment system, which 

includes the following steps: 

— Equalization, 

— pH adjustment (lime addition), 

— Primary clarification, 

— Organosulfide addition, 

— Ferric chloride addition, 

— Polymer addition, 

— Secondary clarification; 
1-2 

 The plant operates selective catalytic reduction (SCR) systems on both generating 

units; and 

 The plant produces a commercial-grade gypsum by-product. 

1.3 Sampling Episode Overview

EPA and its technical contractor, Eastern Research Group, Inc. (ERG) conducted a oneday pre-sampling site visit at Pleasant Prairie on March 2, 2010 as part of the rulemaking. The 

information collected during the pre-sampling site was used to create Sampling Plan, We 

Energies’ Pleasant Prairie Power Station (Sampling Plan) [1], which describes the sample 

collection procedures used during the sampling episode. 

On Sunday, June 20, 2010, EPA arrived at Pleasant Prairie to meet with plant personnel, 

receive on-site safety training, review the sampling points, and determine the set-up for the 

sample collection. EPA and ERG collected the samples specified in the Sampling Plan on 

Monday through Friday (June 21 – 25, 2010). The following personnel participated in EPA’s 

sample collection activities: 

 Ron Jordan, EPA/EAD; 

 TJ Finseth, ERG; 

 Kavya Kasturi, ERG; 

 Elizabeth Sabol, ERG; 

 Becky Schwantes, ERG; and 

 Kim Wagoner, ERG. 

In addition, during the sample collection, EPA collected split samples with the Utility 

Water Act Group (UWAG). UWAG is a trade association for the electric power generating 

industry. During the sampling episode, UWAG acted as Pleasant Prairie’s representative and 

collected samples on behalf of the plant. 
2-1 

2. FACILITY OVERVIEW

Pleasant Prairie operates two steam electric generating units and each has a coal-fired 

boiler. Units 1 and 2 each have a capacity of 615 megawatts (MW), and came online in 1980 and 

1985, respectively. The plant is located in Pleasant Prairie, Wisconsin, about 5 miles from Lake 

Michigan. 

Pleasant Prairie burns approximately 5.5 million tons of PRB coal each year. The plant 

also burns bottom and fly ash from older power plants to reclaim some of the carbon in the ash. 

The old ash is burned at approximately one to two percent weight of the total fuel burned. 

Approximately three years ago, Pleasant Prairie retrofitted both units with FGD scrubber 

systems to control the sulfur dioxide (SO2) releases from the plant. The Unit 1 FGD system was 

installed in November 2006, and the Unit 2 FGD system was installed in March 2007. The wet 

FGD scrubbers remove approximately 97 to 98 percent of the SO2 from the flue gas. In addition 

to the FGD scrubber systems, Pleasant Prairie installed an FGD wastewater treatment system to 

control the discharges of the wastewater generated during the operation of the FGD scrubbers. 

Sections 2.1 and 2.2 further discuss the FGD scrubber systems and the FGD wastewater 

treatment system, respectively. 

Pleasant Prairie retrofitted Units 1 and 2 with SCR systems in 2006 and 2003, 

respectively. The plant operates the SCR systems, which are used to control nitrogen oxide 

(NOX) emissions, year round. 

The electrostatic precipitators (ESPs) at Pleasant Prairie are particulate control devices 

that are designed to remove 99.7 percent of the fly ash and other particulates from the flue gas. 

Pleasant Prairie utilizes ESPs to remove the fly ash from both units. The fly ash and other 

particulates are collected in hoppers and pneumatically conveyed to storage silos. Pleasant 

Prairie markets the fly ash produced. There is no wastewater discharge associated with the ESPs. 

Pleasant Prairie installed a calcium bromide injection system in November 2009 and 

began continuous calcium bromide injection in January 2010. The system injects a solution of 

calcium bromide on to the coal prior to it being pulverized. Adding the calcium bromide to the 

coal enhances the oxidation of the mercury in the boiler and, therefore, results in better removals 

of mercury in the downstream FGD system. Since the addition of the injection system, Pleasant 

Prairie has noticed an increase in the mercury concentrations present in the gypsum, as well as 

the sludge generated from the FGD wastewater treatment system. 

Units 1 and 2 each have the following configuration: 

 Boiler; 

 SCR system; 

 ESP; and 

 FGD scrubber system. 
2-2 

2.1 FGD Scrubber System

Pleasant Prairie operates two identical wet FGD scrubber systems that treat the flue gas 

from Units 1 and 2. The plant uses limestone slurry as the sorbent for SO2 absorption. Limestone 

and service water are fed to on-site ball mills, which pulverize the limestone to create the slurry. 

From the ball mills, the slurry is transferred to hydrocyclones to collect limestone particles that 

are too large to use in the FGD scrubber system. The underflow from the hydrocyclones is 

returned to the ball mill for additional processing. The overflow from the hydrocyclones, which 

is approximately 40 to 50 percent solids (by weight), is transferred to a limestone slurry storage 

tank and used as fresh limestone slurry in the absorber. 

The fresh limestone slurry is fed to the reaction tank of the FGD scrubber system and the 

recycle pumps send the slurry to the various levels of the FGD scrubber (typically two of the 

three spray levels are operating at one time). The slurry is pressurized and sprayed downward 

into the scrubber vessel through the spray nozzles. As the slurry falls downward and the flue gas 

flows countercurrent to the slurry, the spray droplets of the limestone slurry contact the flue gas 

and absorb the SO2, which reacts with the limestone particles and produces calcium sulfite. The 

spray droplets flow downward until they reach the dual flow tray, which forms a layer of slurry 

that the flue gas must pass through to exit the FGD scrubber system. The tray has small holes in 

it that allow the flue gas to bubble through the limestone slurry layered on the tray, which 

provides additional contact between the limestone slurry and the flue gas. The spray droplets 

continue to flow downward in the scrubber until they reach the reaction tank. Pleasant Prairie 

bubbles air through the reaction tank to oxidize the calcium sulfite to calcium sulfate (i.e., 

gypsum). 

The SO2 removal in the FGD systems is optimized at a pH of 5.9; however the plant 

operates the FGD systems at a pH of 5.6 to 5.7 to reduce the scaling potential in the system. The 

limestone slurry feed rate is adjusted to maintain the pH in the system at 5.6 to 5.7. In addition, 

the plant operates the FGD systems to maintain a solids concentration in the scrubber of 15 to 18 

percent solids. When the solids concentration exceeds 18 percent, the plant blows down from the 

FGD system. The blowdown from each FGD system lasts for about eight to ten hours each day 

and is transferred to the gypsum dewatering operations. The plant staggers the blowdown from 

the two units. 

Pleasant Prairie also maintains the chloride concentration in the FGD scrubber systems 

between 3,000 and 10,000 ppm. The maximum design chlorides concentration is 15,000 ppm, 

but the plant tries to keep the chlorides concentration around 6,000 ppm. 

The gypsum slurry for each scrubber is pumped to its primary hydrocyclone, where the 

solid gypsum is separated from the water by centrifugal force. The solid gypsum is forced 

outward to the walls of the hydrocyclones and falls downward, while the water exits the top of 

the hydrocyclones. The gypsum from the primary hydrocyclones, which is approximately 50 

percent solids, is transferred to the vacuum belt filters for final dewatering. The overflow from 

both the Unit 1 and Unit 2 primary hydrocyclones are commingled in the secondary 

hydrocyclone feed tank and transferred to a common secondary hydrocyclone. The overflow 

from the secondary hydrocyclone is transferred to the FGD wastewater treatment system. 
2-3 

Pleasant Prairie washes the gypsum sent to the vacuum filter belts with service water, as 

the gypsum slurry is poured onto the belts. The vacuum filter belts dry the gypsum to a moisture 

content less than 10 percent. Pleasant Prairie sells the gypsum for use in wallboard 

manufacturing or for agricultural purposes. Pleasant Prairie generates approximately 45,000 tons 

of gypsum per hour, when the plant is dewatering the gypsum. 

The filtrate from the vacuum belt filters is collected and transferred back to the FGD 

scrubber systems. Typically, the filtrate is transferred back to the Unit 1 FGD scrubber system; 

however, the plant has the capability to send the filtrate to the Unit 2 FGD scrubber system.

2.2 FGD Wastewater Treatment System

The Pleasant Prairie FGD wastewater treatment system is designed to receive intermittent 

transfers of wastewater from the FGD scrubber system, which consists of secondary 

hydrocyclone overflow, at a flow rate of approximately 40 gallons per minute (gpm). The 

intermittent transfers typically occur twice per day. According to plant personnel, the secondary 

hydrocyclone typically operates for ten hours and is then off for six hours and then operates for 

ten hours again. The FGD wastewater treatment system is a chemical precipitation system and 

contains the following treatment operations: 

 Equalization tank; 

 pH adjustment (lime addition); 

 Primary clarification and polymer addition; 

 Organosulfide and hydrochloric acid addition; 

 Ferric chloride addition; 

 Mixing tank; 

 Flocculation tank; 

 Secondary clarification; and 

 pH adjustment (hydrochloric acid addition). 

Figure 2-1, located at the end of this section, presents the process flow diagram of the 

FGD wastewater treatment system, as well as the sampling locations for EPA’s sampling 

episode. Pleasant Prairie estimates that the total residence time of the FGD wastewater treatment 

system is approximately 55 hours. 

The secondary hydrocyclone overflow from the scrubbers is transferred directly to the 

equalization tank at the start of the wastewater treatment system. During the sampling episode, 

the FGD influent wastewater was found to contain 0.3 to 0.7 percent solids, had a pH between 

5.8 and 6.8 S.U., and a temperature between 54 and 55 °C. The equalization tank also receives 

water from the filtrate sump, which includes the filtrate from the treatment system sludge filter 

presses. 

2.2.1 Physical/Chemical Separation 

From the equalization tank, the wastewater enters reaction tank 1, where hydrated lime is 

added to raise the pH of the wastewater from 5.6 to 8.5 S.U. to precipitate the soluble metals as 

insoluble hydroxides and oxyhydroxides. The reaction tank also desaturates the gypsum in the 
2-4 

wastewater, which prevents gypsum scale formation in the downstream wastewater treatment 

equipment. To desaturate the gypsum, some of the sludge from the downstream primary clarifier 

is recycled back to reaction tank 1 to provide seed crystals for gypsum nucleation. 

From reaction tank 1, the wastewater flows to the primary clarifier, where polymer is 

added to aid in the settling of the solids. Pleasant Prairie stated that 96 percent of the solids settle 

out of the wastewater in the primary clarifier. The overflow from the primary clarifier flows to 

reaction tank 2, where the plant adds organosulfide and hydrochloric acid. When the plant first 

began operating the treatment system, they used TMT 15® as the organosulfide. Since that time, 

the plant has switched to using Nalmet 1689®, which is an organosulfide that has a longer 

polymer chain, and therefore, a higher molecular weight, which helps aid in the settling of 

precipitates. Pleasant Prairie also began adding hydrochloric acid to reaction tank 2, which was 

not in the initial design of the system, because the plant determined that they achieve better 

removals of mercury when the system is operated at a lower pH. 

From reaction tank 2, the wastewater flows to reaction tank 3, where ferric chloride is 

added to the wastewater. The pH in reaction tank 3 is targeted at 7.0 to 7.2 S.U. The effluent 

from reaction tank 3 flows to the flash mix tank, where polymer is added to the wastewater. 

From the flash mix tank, the wastewater flows to the flocculation tank. Gentle mixing in the 

flocculation tank allows denser floc to form. 

The wastewater from the flocculation tank flows to the secondary clarifier. The 

secondary clarifier settles the solids that were formed during the chemical conditioning steps. 

Pleasant Prairie operates an inclined-plate lamella separator type clarifier. Hydrochloric acid may 

be added to the overflow from the secondary clarifier to readjust the pH value, if needed, to meet 

effluent limits. From the secondary clarifier, water flows to the effluent tank and is then 

commingled with other waste streams (e.g., cooling tower blowdown) prior to discharging to 

Lake Michigan. Pleasant Prairie commingles the effluent from the FGD wastewater treatment 

plant with other plant wastewater to meet the final outfall mercury and chloride limits. To meet 

the effluent mercury limit, Pleasant Prairie must dilute the FGD wastewater at a 30:1 ratio. 

Because Pleasant Prairie does not discharge cooling tower blowdown when the plant is 

chlorinating the cooling system, the plant continuously operated the effluent pumps and 

transferred the flow to the Metal Cleaning Basin so that ERG could collect the effluent sample 

for the entire 24-hour period, even during chlorination. Pleasant Prairie directed the treated 

effluent collected in the Metal Cleaning Basin to the scrubber as make-up water so it would not 

impact the FGD wastewater treatment system performance. 

The sludge from the primary and secondary clarifiers is transferred to sludge holding 

tanks using sludge transfer pumps. A portion of the clarifier sludge is recycled from the sludge 

holding tank to reaction tank 1, while the majority is pumped to a filter press for dewatering. The 

solids are then stacked on-site prior to being transferred to an off-site landfill. The filtrate is 

transferred to the filtrate sump, the contents of which are recycled back to the equalization tank. 

Pleasant Prairie typically operates the FGD wastewater treatment system Monday 

through Saturday. The system is shut down Sunday to perform weekly cleaning and 

maintenance. This weekly maintenance includes draining and flushing of the secondary clarifier 

to avoid buildup from flocculation. Pleasant Prairie personnel stated that the weekly maintenance 
2-5 

was performed on the Thursday prior to the EPA sampling episode (June 17, 2010) so the plant 

could verify the system performance on Friday and have it available for the sampling episode on 

Monday. 

Pleasant Prairie has made the following modifications to the FGD wastewater treatment 

system since the system first began operating in early 2007: 

 Changed the type of organosulfide used in the system from TMT 15® to Nalmet® 

1689 (described previously); 

 Added a hydrochloric acid addition point to reaction tank 2 because the system 

removes more mercury at a lower pH (described previously); 

 Bypassed a set of sand filters that were located after the secondary clarifiers 

because of scaling issues (the sand filters are not shown in Figure 2-1); and 

 Added the capability to use cartridge filtration to remove colloidal particles from 

the wastewater after the secondary clarifier, which may build up in the system if 

the plant recirculates the wastewater without discharging for several weeks; 

however the cartridge filtration is not used regularly (the cartridge filters are not 

shown in Figure 2-1). 

2.2.2 Sampling Points 

Figure 2-1 shows the sampling points for the Pleasant Prairie sampling episode; they are 

summarized below: 

 A sample of the purge stream entering the FGD wastewater treatment system 

downstream of the purge tank and upstream of the equalization tank (i.e., the 

sample was collected prior to any chemical addition or mixing with recycle 

streams); and 

 A sample of the effluent from the FGD wastewater treatment system downstream 

of the two effluent tanks prior to commingling with other streams for discharge. 
2-6 

Figure 2.1. FGD Wastewater Treatment System, Pleasant Prairie Power Plant 
3-1 

3. SAMPLE COLLECTION

During the Pleasant Prairie sampling episode, the sampling team followed the collection 

protocols specified in the Sampling Plan. Section 3.1 describes the sampling points, sample 

collection methods, and field measurements. Section 3.2 describes the list of analytes and the 

sample preservation procedures. Section 3.3 discusses the plant operational data collected during 

the sampling episode. Finally, Section 3.4 discusses any deviations from the planned sampling 

activities. 

3.1 Sampling Points, Sample Collection Methods, and Field Measurements

This section describes the sampling points, sample collection methods, and field 

measurements. Additional details are available in Section 3 of the Sampling Plan. Figure 2-1 of 

this report presents a flow diagram of the plant’s wastewater treatment system, including 

sampling point locations. 

Table 3-1 lists the sampling points, sampling point descriptions, type of sample 

collection, and sample collection dates and times. Table 3-2 lists the sampling point numbers and 

descriptions, the number of samples collected, and the pollutant parameters for which the 

samples were analyzed. Table 3-3 presents the field measurement data collected from each 

sampling point. Table 3-4 presents a crosswalk between the sample numbers used for laboratory 

sample identification and the sample points for each day. 

The sampling points for this episode were: 

 SP-1 Influent to FGD Wastewater Treatment System; 

 SP-2 Effluent from FGD Wastewater Treatment System; 

 SP-3 Duplicate of Effluent from FGD Wastewater Treatment System (SP-2); 

 SP-4 Influent to FGD Wastewater Treatment System (SP-1) Field Blank; and 

 SP-5 Effluent from FGD Wastewater Treatment System (SP-2) Field Blank. 

For all the sampling points, EPA collected split samples with Pleasant Prairie’s 

representative by inserting a “Y” splitter into the sample tubing configuration at each sampling 

point to allow for split sample collection. EPA collected all samples (other than mercury and 

cyanide) at all sampling points as “true” splits (i.e., samples for the same analyte were collected 

simultaneously). The mercury and cyanide samples were collected directly from a sample tap; 

therefore, for these samples, EPA and Pleasant Prairie’s representative collected duplicate 

samples, with one filling the bottle immediately after the other. 

At each of the sampling points, EPA collected metals sample fractions following EPA 

Method 1669 collection protocols. To collect these samples, EPA samplers donned Tyvek® 

coveralls and dust masks (dust masks were worn until all mercury samples had been collected). 

In addition, EPA set up a “cleanbox,” which consists of a portable plastic rectangular box with a 

shallow lip and a flip-top lid that secures itself open with clips. The “cleanbox” is double-bagged 

with a clear inner bag, enclosed in a translucent outer bag. The “cleanbox” is handled using 

“clean hands / dirty hands” techniques, whereby the inner bag is handled only by the “clean 

hands” sampler. When the “cleanbox” is opened, the sampler is able to position his/her hands in 
3-2 

the box and pull the bag over the opening of the box, but is still able to see the sample bottles and 

tubing. The “cleanbox” minimizes potential atmospheric contamination during sample 

collection. Figure C-1, in Appendix C, is a picture of a sampler working inside a “cleanbox.” 

The metals sample bottles were also double-bagged. To collect the metals samples, EPA 

placed the sample bottles (while still in its sealed inner bag) into the “cleanbox” following the 

protocols specified in Method 1669, also referred to as “clean hands / dirty hands” protocols. 

Sampling staff filled the sample container, then closed the sample bottle lid and sealed the inner 

bag as quickly as possible within the “cleanbox.” The bagged sample bottles were then removed 

from the “cleanbox” and placed into the outer bag following the “clean hands / dirty hands” 

protocols. 

3.1.1 Influent to FGD Wastewater Treatment System 

The influent to FGD wastewater treatment system (SP-1) was collected from a sample tap 

located on the secondary hydrocyclone and upstream of the equalization tank. Figure 2-1 

identifies the sampling location for SP-1. This sample was collected as a grab sample because, 

according to plant representatives, the wastewater characteristics of the purge to the wastewater 

treatment system are fairly consistent during the purge. In addition, due to the relatively high 

concentration of suspended solids, the FGD purge was not amenable to collecting representative 

split samples using composite sampling techniques. The sample tap was located inside the FGD 

building (see Figure 2-1 for the sampling location for SP-1). Because the sampling point was 

located inside, there were no wind or rain concerns during the sample collection. 

On Day 1 only, prior to collecting the samples at the influent to the FGD wastewater 

treatment system (SP-1), the sampling team collected field blanks (SP-4) for total mercury, total 

and dissolved metals, and dissolved hexavalent chromium. See Section 5.2.3 for a description of 

the field blank sample collection procedures at the influent to the FGD wastewater treatment 

system. 

To collect the wastewater samples at the influent to the FGD wastewater treatment 

system, the samplers attached a 10-foot length of silicone tubing to the sample tap on the 

wastewater piping. The end of the silicone tubing was fitted with a “Y” splitter, with two 

additional lengths of silicone tubing attached to the “Y” splitter. Figure C-2, in Appendix C, is a 

picture of the tubing attached to the sample tap at the influent to the FGD wastewater treatment 

system. The samplers attached the silicone tubing to the sample tap, opened the valve, and 

allowed sample to flow through the tubing for two minutes before beginning to fill sample 

containers. The samplers did not close the valve until all samples were collected (except the 

dissolved metals samples). 

The samplers collected the following samples using a “cleanbox,” as described in Section 

3.1: 

 Total and dissolved mercury; 

 Total metals by 200.8; and 

 Total metals by 200.7. 
3-3 

Samplers then filled a 10-liter container with sample to be pumped off later for collection 

of dissolved metals sample fractions. After all samples were collected at the sampling point for 

the day, the filled 10-liter container was transported to the staging area, put on ice, and then left 

untouched to allow the solids in the wastewater to settle. 

The sampling team collected an aliquot of sample for field testing. Sample pH and 

temperature were measured immediately at the sampling point using four-color pH paper, a pH 

meter, and a thermometer. Table 3-3 presents the field measurement data for the influent to the 

FGD wastewater treatment system. 

The samplers then filled containers for biochemical oxygen demand (BOD5), Group I, 

Group II, and total cyanide samples directly from the tubing without using a “cleanbox.” See 

Table 3-6 for a list of Group I and Group II analytes. BOD5, Group I, Group II, and total cyanide 

samples were immediately placed on ice after sample collection. 

The total cyanide sample was immediately preserved. Lead acetate test strips and 

potassium-iodide starch test strips were used to measure for sulfides and oxidants, respectively. 

No sulfides or oxidants were detected during the sampling episode. The samplers then preserved 

the total cyanide sample with sodium hydroxide to a pH >10 S.U. and placed it on ice. 

Samples for the dissolved metals analyses were pumped from the previously filled 10-

liter container. The pump-off station consisted of a length of Teflon® tubing attached to a length 

of silicone tubing, which was threaded through an ISCO peristaltic pump. The sampling team 

attached a capsule filter to the silicone tubing, which was a short distance downstream of the 

pump. They then attached another short length of silicone tubing to the capsule filter effluent, 

which was attached to a “Y” splitter and two lengths of silicone tubing. This set-up allowed EPA 

to collect “true” split samples with Pleasant Prairie’s representatives. Figure C-3, in Appendix C, 

is a picture of the set-up at the pump-off station. 

The sampling team placed the end of the Teflon® tubing into the 10-liter container filled 

with wastewater from the influent to the FGD wastewater treatment system. By this time, the 

solids in the wastewater had been settling for approximately 90 minutes. Approximately 0.5 - 1 

liters1

 of sample were pumped through the tubing/filter to purge the line before collecting 

samples. 

Samplers collected the following dissolved samples using a “cleanbox,” as described in 

Section 3.1: 

 Dissolved metals by 200.8; 

 Dissolved metals by 200.7; and 

 Dissolved hexavalent chromium. 

Hexavalent chromium samples were immediately placed on ice after sample collection. 

 

1 On day 1, the filter/tubing was purged for 1.5 liters for the field blank and 0.5 liters for the remaining samples. On 

days 2, 3, and 4, the filter/tubing was purged for 1 liter. There was no need to change the filters on any of the 

sampling days. 
3-4 

3.1.2 Effluent from FGD Wastewater Treatment 

The effluent from FGD wastewater treatment system (SP-2) was collected downstream of 

the two effluent tanks prior to the effluent commingling with other wastewaters for discharge. 

Pleasant Prairie installed a three-way splitter on the sample tap that had three separate taps to 

collect samples from the sampling point. The sample tap was located inside the FGD wastewater 

treatment building (see Figure 2-1 for the sampling location for SP-2). Because the sampling 

point was located inside, there were no wind or rain concerns during the sample collection. 

However, the sampling team did observe that the close proximity of the coal pile resulted in a 

significant amount of coal dust settling around and inside the building during coal loading 

operations. The rate of coal dust accumulation was such that visible amounts of dust would 

collect in less than 10 minutes. To minimize the amount of dust entering open tanks in the 

treatment system building, the building doors were generally kept closed. Nevertheless, it is 

possible that some amount of coal dust settled in the treatment system tanks and the pollutants 

present in the coal dust may have affected the measured concentrations in the treatment system 

effluent. 

ERG collected the effluent from the FGD wastewater treatment system composite 

samples using two automatic compositors which were programmed to collect individual sample 

volumes into two 20-liter containers. The compositors were programmed to collect 830 mL 

every hour during the 24-hour composite period. Following the composite period, ERG pumped 

off the specific sample volumes into the individual sample containers. 

ERG used one automatic compositor to collect sample volume for the metals analyses 

(excluding mercury) and another automatic compositor to collect sample volume for all classical 

analytes (i.e., BOD5, Group I, and Group II, excluding cyanide). In addition to collecting 

automatic composite samples for the analytes listed above, ERG collected total and dissolved 

mercury grab samples every six hours during each compositing period. ERG also collected one 

grab sample for cyanide during each compositing period. 

On day 1 only, ERG collected field blank samples (SP-5) for hexavalent chromium, total 

and dissolved metals by 200.7, and total and dissolved metals by 200.8. See Section 5.2.3 for a 

description of the field blank sample collection procedures at the effluent from the FGD 

wastewater treatment system. 

Samplers set up the compositors by attaching two T-splitter tubing sets to two of the taps 

on the three-way splitter. The T-splitter tubing set consisted of three silicone tubes attached to a 

T-splitter. The tubing configuration was set up such that one end was connected to the sample 

tap, one end was threaded through the automatic compositor and connected to the large 

composite container, and one end was placed next to a sump/drain near the sampling point. The 

samplers attached the silicone tubing to the sample tap, opened the valve, and allowed sample to 

flow through both sets of tubing before calibrating either of the automatic compositors. This 

ensured that the flow through the tubing during calibration would be the expected flow through 

the tubing during sample collection. The automatic compositors were calibrated such that they 

collected 830 mL every hour, so that the projected complete volume would be 20 liters. After 

calibration, the tubing was attached to a vented cap on a 20-liter composite container. The 

sample tap was left open during the entire sample collection time period and flowed directly to 
3-5 

the sump/drain. The automatic compositor pulled sample from the flowing stream as dictated by 

the sampling program and was capable of purging the line back to the flowing stream between 

each individual sample aliquot. 

Both 20-liter composite containers were placed into plastic trash cans, and maintained on 

ice for the entire 24-hour compositing period. A plastic bag was placed on top of the trash cans 

to minimize contamination. Figure C-4, in Appendix C, is a picture of the composite sampling 

set-up at the effluent from the FGD wastewater treatment system. 

Immediately after setting up the compositors, ERG collected the first set of the total and 

dissolved mercury grab samples. At the first grab sample every day, ERG collected field blanks 

for total mercury samples. See Section 5.2.3 for a description of the field blank sample collection 

procedures at the effluent from the FGD wastewater treatment system. 

For mercury collection, samplers shrouded one of the three taps on the three-way splitter 

(the other two taps were being used by the two compositors) with a clean plastic bag by 

puncturing a hole in the bottom of the bag with the end of the tap and then securing it to the tap 

with a ziptie. After purging the tap for two minutes, the samples were collected directly from the 

tap into the sample bottles. Because total mercury and dissolved mercury samples were collected 

directly from the tap, ERG was not able to collect split samples with Pleasant Prairie’s 

representatives; therefore, duplicate samples were collected. ERG collected another set of total 

and dissolved mercury samples every six hours thereafter over the 24-hour period. The plastic 

shroud was replaced for each set of mercury grab samples. After collecting each set of mercury 

grabs, ERG filled a field test bottle and tested for pH and temperature using four-colored pH 

paper, a pH meter, and a thermometer. Table 3-3 presents the field measurement data for the 

effluent from the FGD wastewater treatment. 

After the collection of the third set of mercury grabs, ERG collected a total cyanide grab 

sample from the same tap on the three-way splitter that was used for mercury sample collection. 

Because total cyanide samples were collected directly from the tap, ERG was not able to collect 

split samples with Pleasant Prairie’s representatives; therefore, duplicate samples were collected. 

The total cyanide sample was immediately preserved. Lead acetate test strips and potassiumiodide starch test strips were used to measure for sulfides and oxidants, respectively. No sulfides 

or oxidants were detected during this sampling episode at the effluent from the FGD wastewater 

treatment system. ERG samplers then preserved the total cyanide samples with sodium 

hydroxide to a pH >10 S.U. and placed the samples on ice. 

After the twenty-fourth aliquots were collected in the two composite containers, ERG 

followed “clean hands / dirty hands” sampling techniques to disassemble the compositors from 

the sampling set up. Closed caps were placed on the two composite containers and the 

composite containers were moved to the pump-off area where they remained on ice until 

individual sample bottles were filled. The samplers then began setting up the compositors for the 

next day of samples using new tubing sets and composite containers. The automatic compositor 

was programmed to collect the same volume on each day of sample collection. 

After completing the set up for the next day of composite samples, the sampling team 

transferred the wastewater collected in the 20-liter containers into the individual sample 
3-6 

containers at the pump-off area. For this sampling point, ERG used a sample pump-off approach 

to transfer the composite samples to the individual sample bottles. For this sample pump-off 

procedure, the dissolved metals samples were collected before the total metals and classical 

samples to prevent cross-contamination within the tubing, which could lead to greater 

concentrations in the dissolved metals fractions. 

Samples for the dissolved and total metals analyses were pumped from one of the 

previously filled 20-liter containers. The pump-off station consisted of a length of Teflon® 

tubing attached to a length of silicone tubing, which was threaded through an ISCO peristaltic 

pump. The sampling team attached a capsule filter to the silicone tubing, which was a short 

distance downstream of the pump. They then attached another short length of silicone tubing to 

the capsule filter effluent, which was attached to a “Y” splitter and two lengths of silicone 

tubing. This set-up allowed EPA to collect “true” split samples with Pleasant Prairie’s 

representatives. Figure C-3, in Appendix C, is a picture of the set-up at the pump-off station. 

On Day 1 only, prior to collecting any samples of the effluent from the FGD wastewater 

treatment system, the samplers collected a field blank sample (SP-5) for dissolved and total 

metals. See Section 5.2.3 for a description of the dissolved and total metals field blank sample 

collection at the effluent from the FGD wastewater treatment system. 

After collecting the field blank samples, the sampling team placed the end of the Teflon® 

tubing into one of the 20-liter composite containers filled with wastewater from the effluent from 

the FGD wastewater treatment system. After the tubing and filter were purged with 1-2 liters of 

sample, samplers collected the following samples using a “cleanbox,” as described in Section 

3.1: 

 Dissolved metals by 200.8; 

 Dissolved metals by 200.7; and 

 Dissolved hexavalent chromium. 

Hexavalent chromium samples were immediately placed on ice after sample collection. 

After the dissolved metals had been collected, the filter was removed. Once the tubing was 

purged with 1-2 liters of sample, samplers collected the following samples using a “cleanbox,” as 

described in Section 3.1: 

 Total metals by 200.8; and 

 Total metals by 200.7. 

 

After the metal samples had been collected, the sampling team placed the end of the 

Teflon® tubing into the other previously filled 20-liter container. After the tubing was purged 

with 1-2 liters of sample, samplers filled containers for biochemical oxygen demand (BOD5), 

Group I, and Group II samples directly from the tubing without using a “cleanbox.” See Table 3-

5 for a list of Group I and Group II analytes. BOD5, Group I, and Group II samples were 

immediately placed on ice after sample collection. 

For all analytes, ERG collected QC samples at the effluent from the FGD wastewater 

treatment system (SP-2) on Day 3 of the sampling episode. In addition, for all analytes, ERG 
3-7 

collected a duplicate sample of the FGD wastewater treatment system (SP-3) on Day 2 of the 

sampling episode. 

3.2 List of Analytes and Sample Preservation

Samples collected at Pleasant Prairie were analyzed for the following pollutants: 

 Classicals: 

Biochemical oxygen demand, 5-day (BOD5), 

Chemical oxygen demand (COD), 

Total suspended solids (TSS), 

Total dissolved solids (TDS), 

Sulfate, 

Chloride, 

Total Kjeldahl nitrogen (TKN), 

Ammonia as nitrogen, 

Nitrate/nitrite as nitrogen, 

Total phosphorus, 

Total cyanide; 

 Total Metals: 

— Aluminum, antimony, arsenic, barium, beryllium, boron, cadmium, 

calcium, chromium, cobalt, copper, iron, lead, magnesium, manganese, 

mercury, molybdenum, nickel, selenium, silver, sodium, thallium, tin, 

titanium, vanadium, and zinc. 

 Dissolved Metals: 

— Same parameters as listed for total metals, plus hexavalent chromium. 

The analytes selected reflect the current understanding of coal-fired power plant air 

pollution control wastewaters, including contributions from coal, scrubber sorbents, treatment 

chemicals, and other sources. Table 3-5 lists the analytical methods used to determine pollutant 

concentrations. 

Table 3-6 lists the containers used for sample collection as well as the preservation 

requirements for each sample. Table 3-7 summarizes the chemical preservation for each of the 

samples that were preserved on site. The sampling team preserved samples in accordance with 

procedures described in Section 3.4 of the Sampling Plan. Immediately following sample 

collection, the samplers placed the BOD5, Group I, Group II, dissolved hexavalent chromium, 

and total cyanide samples on ice to cool the samples to <6°C. The sampling team did not place 

the total and dissolved metals or the total and dissolved mercury samples on ice, which comports 

with the requirements of Methods 200.7, 200.8 and 1631E. All dissolved metals samples, except 

for mercury, were filtered in the field. The hexavalent chromium samples were preserved in the 

field, but all other metals samples were acid-preserved prior to extraction at the laboratory. The 

hexavalent chromium samples were preserved with ammonium sulfate buffer solution and 

ammonium hydroxide to a pH between 9.3 and 9.5 S.U. The Group II samples were preserved 

with sulfuric acid to a pH of <2 S.U. in the staging area, and the pH was confirmed with four-
3-8 

color pH strips. Each total cyanide sample was tested for sulfides and oxidants immediately after 

sample collection. Because sulfides and oxidants were not detected at any of the sampling points 

during the sampling episode, the samplers did not need to dilute the samples or add sodium 

arsenite to the samples. After testing for sulfides and oxidants, the total cyanide samples were 

preserved with sodium hydroxide to a pH >10 S.U. and placed on ice. 

3.3 Plant Operational Data

During the EPA sampling episode, Pleasant Prairie plant personnel provided the sampling 

team with operational data for each of the generating units and the FGD scrubber system, as well 

as operational and flow data for the FGD wastewater treatment system. Table 3-8 presents the 

unit operating characteristics, Table 3-9 presents the FGD scrubber system operating 

characteristics, Table 3-10 presents information on the coal burned during the sampling episode, 

Table 3-11 presents information on the FGD scrubber slurry generation during the sampling 

episode, and Table 3-12 presents the FGD wastewater treatment system operating characteristics. 

3.4 Deviations from the Sampling and Analysis Plan

The sampling episode proceeded as specified in the Sampling Plan with the exceptions 

described below: 

 Influent sample tap set up at SP-1 (Day 1): Before the sample line was purged 

prior to sample collection, the secondary hydrocyclone became clogged. A plant 

operator cleaned the blockage in the plugged hydrocyclone. Once the 

hydrocyclone was operating, the line was purged for approximately 1 minute. 

 Preservation of hexavalent chromium: ERG planned to preserve the hexavalent 

chromium samples to a pH between 9.3 and 9.7 S.U. using an ammonium sulfate 

buffer solution; however, since the ammonium sulfate buffer solution was not 

achieving the desired pH, the samplers added only 100 drops of ammonium 

sulfate buffer solution, followed by as much ammonium hydroxide as necessary 

to reach the desired pH. 

 pH field test measurements: The sampling team was unable to locate the pH 

measurement strips during the following samples: the effluent from the FGD 

wastewater treatment system mercury grab samples 3 and 4 on day 1 and the 

influent to the FGD wastewater treatment system grab sample on day 2. 

Therefore, the team only took a pH reading using the pH meter, not the pH strips 

for these samples. 

 Total mercury grab sample at SP-2 (Days 1 and 2): On days 1 and 2 of sample 

collection at the effluent from the FGD wastewater treatment system (SP-2), the 

inner bag for grab three of the four total mercury grab sample bottles was leaking. 

The inner bag was removed from the outer bag, dried, and re-labeled. The 

samplers placed the inner bag back in the outer bag. 
3-9 

Table 3-1. Sample Collection Information, Pleasant Prairie

Sampling 

Point 

Number Sampling Point Description 

Type of 

Sample 

Sample 

Collection Date 

Sample Collection 

Time 

SP-1 Influent to FGD Wastewater Treatment 

System – Day 1 

Grab 6/21/10 1013a and 1220b

Influent to FGD Wastewater Treatment 

System – Day 2 

Grab 6/22/10 0939a and 1132b

Influent to FGD Wastewater Treatment 

System – Day 3 

Grab 6/23/10 0917a and 1112b

Influent to FGD Wastewater Treatment 

System – Day 4 

Grab 6/24/10 0924a and 1108b

SP-2 Effluent from FGD Wastewater Treatment 

System – Day 1 

Composite 6/21/10 

6/22/10

0730c

0827d

Grab 6/21/10 

6/22/10 

0748e, 1348f , and 1946 g

0147 h 

Effluent from FGD Wastewater Treatment 

System – Day 2 

Composite 6/22/10 

 6/23/10 

0728c

0806d 

Grab 6/22/10 

6/23/10 

0745e, 1348f , and 1947 g

0145 h 

Effluent from FGD Wastewater Treatment 

System – Day 3 

Composite 6/23/10 

6/24/10 

0730c

0810d 

Grab 6/23/10 

 6/24/10 

0743e, 1347f , and 1950 g

0147 h 

Effluent from FGD Wastewater Treatment 

System – Day 4 

Composite 6/24/10 

6/25/10 

0729c

0651d 

Grab 6/24/10 

6/25/10 

0749e, 1348f , and 1947 g

0147 h 

SP-3 Duplicate of Effluent from FGD 

Wastewater Treatment System – Day 2 

Composite 6/22/10 

 6/23/10 

0728c

0806d 

Grab 6/22/10 

6/23/10 

0747e, 1349f , and 1948 g

0146 h 

SP-4 Influent to FGD Wastewater Treatment 

System Field Blank 

Grab 6/21/10 0958 i and 1212j

SP-5 Effluent from FGD Wastewater Treatment 

System Field Blank – Day 1 

Composite 6/21/10 

6/22/10

0653k

0813l

Grab 6/21/10 0742m

Effluent from FGD Wastewater Treatment 

System Field Blank – Day 2 

Grab 6/22/10 0740m

Effluent from FGD Wastewater Treatment 

System Field Blank – Day 3 

Grab 6/23/10 0738m

Effluent from FGD Wastewater Treatment 

System Field Blank – Day 4 

Grab 6/24/10 0744m

a

 Start time for the collection of the total metals samples (total metals by 200.7, total metals by 200.8, total mercury, 

and dissolved mercury) and classicals (BOD5, Group I, Group II, and total cyanide). 
3-10 

b

 Start time for the collection of the dissolved metals samples (dissolved metals by 200.7, dissolved metals by 200.8, 

and dissolved hexavalent chromium). Does not include dissolved mercury. 

c Started compositor. 

d

 Start time for the collection of dissolved metals samples (dissolved metals by 200.7, dissolved metals by 200.8, 

and dissolved hexavalent chromium), total metals samples (total metals by 200.7 and total metals by 200.8), and 

classicals (BOD5, Group I, and Group II). e Start time for the collection of the total and dissolved mercury Grab 1 samples. 

f

 Start time for the collection of the total and dissolved mercury Grab 2 samples. 

g

 Start time for the collection of the total and dissolved mercury Grab 3 and total cyanide samples. 

h

 Start time for the collection of the total and dissolved mercury Grab 4 samples. 

i

 Start time for the collection of total and dissolved mercury and total metals by 200.7 and total metals by 200.8 field 

blank samples. 

j

 Start time for the collection of dissolved metals by 200.7 and dissolved metals by 200.8, and hexavalent chromium 

field blank samples. 

k

 Filled 20L field blank carboy 

l Start time for the collection of total metals by 200.7 and total metals by 200.8 field blank samples and collection of 

dissolved hexavalent chromium, dissolved metals by 200.7, and dissolved metals by 200.8 field blank samples. 

m Start time for the collection of total mercury field blank samples. 
3-11 

Table 3-2. Sample Collection at Pleasant Prairie

Sampling 

Point 

Number Sampling Point Name 

Total Metals 

(EPA Method 200.8 with 

collision cell

Total Metals 

(EPA Method 200.7 

Dissolved Metals 

(EPA Method 200.8 with 

collision cell 

Dissolved Metals 

(EPA Method 200.7 

Total Mercury 

Dissolved Mercury 

Hexavalent Chromium 

BOD

5

GI 

a

SP-1 Influent to the FGD Wastewater 

Treatment System 

4 4 4 4 4 4 4 4 

SP-2 Effluent from the FGD 

Wastewater Treatment System 

4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1

SP-3 Duplicate of the Effluent from 

FGD Wastewater Treatment System 

1 1 1 1 1 1 1 1 

SP-4 Influent to the FGD Wastewater 

Treatment System Field Blank 

1 1 1 1 1 1 

SP-5 Effluent from the FGD 

Wastewater Treatment System Field Blank 

1 1 1 1 4 1 

Total Number of Samples 11+1QC 11+1QC 11+1QC 11+1QC 14+1QC 9+1QC 11+1QC 9+1QC 9+1

a – Group I includes total suspended solids (TSS), total dissolved solids (TDS), sulfate, and chloride. b – Group II includes ammonia as nitrogen, nitrate/nitrite as nitrogen, total Kjeldahl nitrogen (TKN), chemical oxygen demand (COD), and total phosp
3-12 

Table 3-3. Field Measurements, Pleasant Prairie

Sampling 

Point 

Number 

Sampling Point 

Description Date Time 

Temperature 

(°C) 

pH 

(S.U.) 

Waste 

Stream Flow 

Rate 

Meter (GPM) 

a Strips 

SP-1 Influent to FGD 

Wastewater Treatment System – Day 1

6/21/2010 1029 55 5.8 6 XX Sample

had a dappearedetectetotal cy

Influent to FGD Wastewater Treatment System – Day 2 

6/22/2010 0953 55 6.4 NC XX 

Influent to FGD Wastewater Treatment System – Day 3 

6/23/2010 0928 55 6.34 7 XX 

Influent to FGD Wastewater Treatment System – Day 4 

6/24/2010 0935 54 6.77 7 XX 

SP-2 Effluent from FGD 

Wastewater Treatment System – Day 1

6/21/10 0750 43 6.6 6.5 40.3 Sample

and did particulor oxid

6/21/10 1348 43 6.9 6.5 XX6/21/10 1946 42.4 6.8 NC 38.1 6/22/10 0147 42.4 6.9 NC 38.1 

Effluent from FGD Wastewater Treatment System – Day 2 

6/22/10 0750 43 6.9 6.5 35 

6/22/10 1352 43 6.9 7 32.7 6/22/10 1947 41.5 6.9 7 35.0 6/23/10 0145 43.3 6.9 6.5 34.9 

Effluent from FGD Wastewater Treatment System – Day 3 

6/23/10 0745 44 6.87 7 35 

6/23/10 1350 44 6.85 7 35 6/23/10 1950 44.4 6.1 6.5 34.9 6/24/10 0155 44.2 6.9 6.5 34.4 

Effluent from FGD Wastewater Treatment System – Day 4 

6/24/10 0752 44 6.86 7 35 

6/24/10 1350 43 6.86 7 35 6/24/10 1947 43.8 6.9 6.5 35 
3-13 

Table 3-3. Field Measurements, Pleasant Prairie

Sampling 

Point 

Number 

Sampling Point 

Description Date Time 

Temperature 

(°C) 

pH 

(S.U.) 

Waste 

Stream Flow 

Rate 

Meter (GPM) 

a Strips 

6/25/10 0147 43.6 7.0 7 34.9 

a The pH meter was calibrated prior to the sampling episode and once every day during the sampling episode using prepackaged buffer 

and 10.0. NC – Not collected. The sampling team was unable to locate the pH strips during the collection of these samples; therefore, the pH mea

with the pH meter. 

[NOTE TO PLEASANT PRAIRIE: Provide the flow rate (gpm) for the influent to the FGD wastewater treatment system from the secoeach minute from start to end times: 06/21/2010, 1000 to1032; 06/22/2010, 0935 to 0957; 06/23/2010, 0915 to 0931; AND 06/24/2010complete set of the flow rates for the effluent from the FGD wastewater treatment system as an hourly average for each hour of the sam(if not available as an hourly average, please provide flow rate in 10 minute increments): 6/21/2010 at 0700 through 6/25/2010 at 0700
3-14

Table 3-4. Crosswalk of Sample Number to Sampling Point and Day, Pleasant Prairie

Sample Number Sample Point Sample Description 

71691 SP-1, Day 1 Influent to FGD Wastewater Treatment System - Day 1 

71692 SP-1, Day 2 Influent to FGD Wastewater Treatment System - Day 2 

71693 SP-1, Day 3 Influent to FGD Wastewater Treatment System - Day 3 

71694 SP-1, Day 4 Influent to FGD Wastewater Treatment System - Day 4 

71695 SP-2, Day 1 Effluent to FGD Wastewater Treatment System - Day 1 

71696 SP-2, Day 2 Effluent to FGD Wastewater Treatment System - Day 2 

71697 SP-2, Day 3 Effluent to FGD Wastewater Treatment System - Day 3 

71698 SP-2, Day 4 Effluent to FGD Wastewater Treatment System - Day 4 

71699 SP-3, Day 2 Duplicate of Effluent to FGD Wastewater Treatment System - Day 2 

71700 SP-4, Day 1 Influent to FGD Wastewater Treatment System Field Blank - Day 1 

71701 SP-5, Day 1 Effluent to FGD Wastewater Treatment System Field Blank - Day 1 

71702 SP-5, Day 2 Effluent to FGD Wastewater Treatment System Field Blank - Day 2 

71703 SP-5, Day 3 Effluent to FGD Wastewater Treatment System Field Blank - Day 3 

71704 SP-5, Day 4 Effluent to FGD Wastewater Treatment System Field Blank - Day 4 
3-15

Table 3-5. Analytical Methods, Pleasant Prairie 

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 and Dissolved Metals

Mercury EPA 1631E 

Hexavalent chromium (dissolved only) EPA 218.6 

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

selenium, silver, thallium, vanadium, and zinc 

EPA 200.8 with collision cell 

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

molybdenum, sodium, tin, and titanium 

EPA 200.7 
3-16

Table 3-6. Summary of Sample Container and Planned Preservation, Pleasant Prairie 

Parameter 

Sample 

Container and 

Volume 

QC Sample 

Container and 

Volume On-Site Preservation 

Classicals 

BOD5 One 1-L plastic 

bottle 

One 1-L plastic 

bottle 

≤6C 

Group I a One 1-L plastic 

bottles 

One 1-L plastic 

bottles 

≤6C 

Group II b Two 1-L plastic 

bottles 

Two 1-L plastic 

bottles 

H2SO4 to pH <2 S.U., ≤6C 

Total cyanide One 1-L plastic 

bottle 

One 1-L plastic 

bottles 

Dilution until sulfide is not detected, 

NaAsO2 until total chlorine is not 

present, NaOH to pH >10 S.U., 

≤6C 

Metals 

Total metals (EPA Method 200.8 with 

collision cell) 

One 500-mL 

plastic bottle 

No additional 

volume needed 

None 

(acid preserve at laboratory) 

Total metals (EPA Method 200.7) One 500-mL 

plastic bottle 

No additional 

volume needed 

None 

(acid preserve at laboratory) 

Dissolved metals (EPA Method 200.8 

with collision cell) 

One 500-mL 

plastic bottle 

No additional 

volume needed 

0.45-μm filter (performed in field) 

(acid preserve at laboratory) 

Dissolved metals (EPA Method 200.7) One 500-mL 

plastic bottle 

No additional 

volume needed 

0.45-μm filter (performed in field) 

(acid preserve at laboratory) 

Total mercury: None 

Manual composite grab samples Four 125-mL (acid preserve at laboratory) 

glass bottle 

No additional 

volume needed 

Influent samples and field blank 

samples 

Two 250-mL 

glass bottle 

No additional 

volume needed 

Dissolved mercury: None 

(filter and acid preserve at 

laboratory) Manual composite grab samples Four 125-mL 

glass bottle 

No additional 

volume needed 

Influent samples One 250-mL 

glass bottle 

No additional 

volume needed 

Hexavalent chromium One 250-mL 

plastic bottle 

No additional 

volume needed 

0.45-μm filter (performed in field) 

Ammonium sulfate buffer to 

pH 9.3 – 9.7 S.U., ≤6C 

(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.
3-17 

Table 3-7. Sample Preservation Summary, Pleasant Prairie

Sampling Point 

Number Analysis Date 

Chemical 

Added Initial pH Final pH 

Amount 

Added 

(drops) 

71691 Group II Volume 1 6/21/10 H2SO4 6.0 2 55 

71691 Group II Volume 2 6/21/10 H2SO4 6.0 2 55 

71691 Hexavalent Chromium 6/21/10 (NH4)2SO4

Buffer 

6.0 9.4 100 

NH4OH 5 

71700 Hexavalent Chromium Field 

Blank 

6/21/10 (NH4)2SO4

Buffer 

5.5 9.5 100 

NH4OH 3 

71691 Total Cyanide 6/21/10 NaOH 6.0 10 35 

71692 Total Cyanide 6/22/10 NaOH 6.5 10 35 

71695 Total Cyanide 6/21/10 NaOH 7.0 10 55 

71692 Group II Volume 1 6/22/10 H2SO4 6.5 2 65 

71692 Group II Volume 2 6/22/10 H2SO4 6.5 2 65 

71695 Group II Volume 1 6/22/10 H2SO4 6.0 2 50 

71695 Group II Volume 2 6/22/10 H2SO4 6.0 2 50 

71692 Hexavalent Chromium 6/22/10 (NH4)2SO4

Buffer 

6.5 9.5 100 

NH4OH 3 

71695 Hexavalent Chromium 6/22/10 (NH4)2SO4

Buffer 

6.5 9.5 100 

NH4OH 5 

71701 Hexavalent Chromium Field 

Blank 

6/22/10 (NH4)2SO4

Buffer 

5.5 9.5 100 

NH4OH 3 

71696 Total Cyanide 6/22/10 NaOH 6.9 10 45 

71699 Total Cyanide 6/22/10 NaOH 6.9 10 45 

71693 Group II Volume 1 6/23/10 H2SO4 6.5 2 55 

71693 Group II Volume 2 6/23/10 H2SO4 6.5 2 55 

71696 Group II Volume 1 6/23/10 H2SO4 6.5 2 65 

71696 Group II Volume 2 6/23/10 H2SO4 6.5 2 65 

71699 Group II Volume 1-Duplicate 6/23/10 H2SO4 6.5 2 65 

71697 Group II Volume 2-Duplicate 6/23/10 H2SO4 6.5 2 65 

71693 Hexavalent Chromium 6/23/10 (NH4)2SO4

Buffer 

6.5 9.5 100 

NH4OH 5 

71696 Hexavalent Chromium 6/23/10 (NH4)2SO4

Buffer 

6.5 9.5 100 

NH4OH 4 
3-18 

Table 3-7. Sample Preservation Summary, Pleasant Prairie

Sampling Point 

Number Analysis Date 

Chemical 

Added Initial pH Final pH 

Amount 

Added 

(drops) 

71699 Hexavalent Chromium - 

Duplicate 

6/23/10 (NH4)2SO4

Buffer 

6.5 9.5 34 

NH4OH 5 

71693 Total Cyanide 6/23/10 NaOH 6.5 10 40 

71697 Total Cyanide 6/23/10 NaOH 6.1 10 50 

71697 Total Cyanide - QC 6/23/10 NaOH 6.1 10 50 

71694 Group II Volume 1 6/24/10 H2SO4 6.5 2 65 

71694 Group II Volume 2 6/24/10 H2SO4 6.5 2 65 

71697 Group II Volume 1 6/24/10 H2SO4 6.5 2 55 

71697 Group II Volume 2 6/24/10 H2SO4 6.5 2 55 

71697 Group II Volume 1 - QC 6/24/10 H2SO4 6.5 2 55 

71697 Group II Volume 2 - QC 6/24/10 H2SO4 6.5 2 55 

71698 Group II Volume 1 6/25/10 H2SO4 6.5 2 55 

71698 Group II Volume 2 6/25/10 H2SO4 6.5 2 55 

71694 Hexavalent Chromium 6/24/10 (NH4)2SO4

Buffer 

6.7 9.5 100 

NH4OH 5 

71697 Hexavalent Chromium - QC 6/24/10 (NH4)2SO4

Buffer 

6.5 9.5 100 

NH4OH 4 

71698 Hexavalent Chromium 6/25/10 (NH4)2SO4

Buffer 

6.5 9.5 100 

NH4OH 5 

71694 Total Cyanide 6/24/10 NaOH 6.5 10 40 

71698 Total Cyanide 6/24/10 NaOH 6.5 10 40 
3-19 

Table 3-8. Generating Unit Operating Characteristics during Sample Collection, Pleasant 

Prairie

Unit ID Boiler Type 

Capacity 

(MW) 

Electricity Production 

(MW) 

(or Percent Capacity %)

SCR 

(No, On, Off)

Particulate Control System 

(HS/CS ESP, or BH) 

1 Riley Turbo Opposed 

Wall - Fired 594 49,997 MWHr On CS ESP 

2 Riley Turbo Opposed 

Wall - Fired 594 50,540 MWhr On CS ESP 

CS ESP – Cold-side electrostatic precipitator. 
3-20 

Table 3-9. FGD Scrubber System Operating Characteristics, Pleasant Prairie 

Unit ID 

Wet FGD 

System (Yes/No) 

Type of 

Scrubber 

Forced 

Oxidation 

(Yes/No) Sorbent 

Additives (DBA, 

formic acid, 

etc.) 

FGD Make-up 

Water Source 

SO2 Rem

Percen

1 Yes Spray / Tray Yes Limestone Silicon antifoam 17 gpd/unit Lake Michigan 97% 2 Yes Spray / Tray Yes Limestone Silicon antifoam 17 gpd/unit Lake Michigan 96% 
3-21

Table 3-10. Coal Usage during Sample Collection, Pleasant Prairie 

Day of 

Sampling Unit ID Coal Type 

Amount of Coal 

Used During Day 

of Sampling 

(tpd) 

Source of Coal 

(Coal Region 

and/or State) 

Percent 

Sulfur in 

Coal 

(%) 

Chlorine Content of 

Coal 

(ppm) 

1 1 Sub Bit 8205.66 PRB/WY 0.5 % Est 42 ppm Est 

2 Sub Bit 8059.82 PRB/WY 0.5 % Est 42 ppm Est 

2 1 Sub Bit 8550.83 PRB/WY 0.5 % Est 42 ppm Est 

2 Sub Bit 8365.23 PRB/WY 0.5 % Est 42 ppm Est 

3 1 Sub Bit 8530.58 PRB/WY 0.5 % Est 42 ppm Est 

2 Sub Bit 8276.14 PRB/WY 0.5 % Est 42 ppm Est 

4 1 Sub Bit 8119.66 PRB/WY 0.5 % Est 42 ppm Est 

2 Sub Bit 8371.29 PRB/WY 0.5 % Est 42 ppm Est 

Table 3-11. Scrubber Slurry Information during Sample Collection, Pleasant Prairie

Day of 

Sampling 

FGD 

System ID 

Associated 

Unit IDs 

Scrubber Slurry 

Blowdown Flow Rate Scrubber 

Slurry 

Percent 

Solids 

Time of 

Dewatering 

During 

Sampling Day 

Percent 

Filtrate 

Recycled 

Back to 

Scrubber 

Flow Rate 

(gpm) Duration 

1 

1 1 280 9.25 hr ~15% 0413 – 0900 EST, 

1400 – 1830 EST 100% 

2 2 280 9.0 hr ~15% 0830 – 1400 EST, 

1600 – 1930 EST 100% 

2 

1 1 280 12.0 hr ~15% 0130 – 0800 EST 

1300 – 1822 EST 100% 

2 2 280 10.5 hr ~15% 0500 – 1100 EST, 

1600 – 2030 EST 100% 

3 

1 1 280 8.5 hr ~15% 0125 – 0620 EST 

1125 – 1500 EST 100% 

2 2 280 10.0 hr ~15% 

0620 – 1130 EST 

1345 – 1500 EST 

2230 – 2400 EST 

100% 

4 

1 1 280 13.5 hr ~15% 0018 – 0710 EST 

1725 – 2400 EST 100% 

2 2 280 9.0 hr ~15% 0000 – 0312 EST 

1400 – 1945 EST 100% 
3-22 

Table 3-12. FGD Wastewater Treatment System Operation Information, Pleasant Prair

Day of 

Sampling 

Scrubber Purge Chemical Usage 

Flow Rate 

(GPM)a 

Duration 

ACT 

Lime 

(added to adjust 

pH 5.6 to 8.5)b

Ferric Chloride 

ACT 

Organosulfide 

Nalmet 1689 

50 ppm 

 ACT 

Polymer

GE AE17

20 ppm prim

3.5 ppm sec 

1 60 18.0 hr 670 lb/day 40 mL/min 6 mL/min 4 mL/min 2 60 16.25 hr 670 lb/day 40 mL/min 6 mL/min 4 mL/min 3 60 17.5 hr 670 lb/day 40 mL/min 6 mL/min 4 mL/min 4 60 20.25 hr 670 lb/day 40 mL/min 6 mL/min 4 mL/min 

a - Purge rate estimated from tank level changes. Similar to Secondary Hydrocyclone design data of 60 gpm to overflow/purge b - Lime feeder operates 4 times per day for 10 minutes; feeder rate is 1000 lb/hr, 670 lbs/day. Checks against lime deliveries. 

ACT – Actual value during sampling episode.
4-1 

4. LABORATORY ANALYTICAL RESULTS AND DISCUSSION

This section summarizes the laboratory results of analyses of samples for the influent to 

the FGD wastewater treatment system and the effluent from the FGD wastewater treatment 

system. 

Appendix A provides all analytical results for all samples collected at Pleasant Prairie, 

including all qualified results and all results that were measured above the method detection 

limit, but below the quantitation limit (i.e., J-values). 

Table 4-1 presents the analytical results for all classical and metal analytes for the four 

days of sampling at the influent to the FGD wastewater treatment system (SP-1), as well as the 

calculated 4-day average result for each analyte for the sampling point. Table 4-2 presents the 

analytical results for all classical and metal analytes for the four days of sampling at the effluent 

from the FGD wastewater treatment system (SP-2). 

Tables 4-1 and 4-2 include the analytical results for all analytes for which EPA conducted 

analyses. Results are rounded to three significant digits. If an analyte was not detected in a 

sample above the method detection limit, the result is reported as “ND” followed by the samplespecific quantitation limit in parentheses. If an analyte was measured above the method 

detection limit, but below the quantitation limit, the result is reported as “NQ” followed by the 

sample-specific quantitation limit in parentheses. 

For Table 4-2 (effluent from the FGD wastewater treatment system), a duplicate sample 

was collected on Day 2 of the sampling episode. The Day 2 results presented in Table 4-2 

represent the average of the original and the duplicate sample results. Table 5-2 presents the 

analytical results for the original and duplicate results and the calculated relative percent 

difference (RPD). 

When calculating the average concentrations for the duplicate samples or for the 4-day 

averages, ERG used the following methodology: 

 If all results were above the quantitation limit, then all results were averaged 

together; 

 If at least one result was above the quantitation limit, then 1⁄2 the quantitation limit 

was used in the average calculation for all results that were less than the 

quantitation limit and the result is reported with a less than sign (“<”); 

 If all results were below the quantitation limit, but at least one result was above 

the method detection limit (i.e., J-value), then the sample-specific quantitation 

limits for all results were averaged and the result is reported as “NQ” followed by 

the average of the sample-specific quantitation limits; and 

 If all results were below the method detection limit, then the sample-specific 

quantitation limits for all results were averaged and the result is reported as “ND” 

followed by the average of the sample-specific quantitation limits. 

Table 4-3 presents the 4-day average results for all classical analytes for the influent to 

the FGD wastewater treatment system (SP-1) and the effluent from the FGD wastewater 
4-2 

treatment system (SP-2). Table 4-4 presents the 4-day average results for all metal analytes, 

including total and dissolved analyses, for the influent to the FGD wastewater treatment system 

(SP-1) and the effluent from the FGD wastewater treatment system (SP-2). The results presented 

in this report are not paired results, meaning that the sample collection across the treatment 

system was not timed to reflect the amount of time it takes the wastewater to pass through the 

system. 

Appendix Tables A-1 through A-9 present all the analytical results from the influent to 

the FGD wastewater treatment system (SP-1), the effluent from the FGD wastewater treatment 

system (SP-2), and the duplicate of the effluent from the FGD wastewater treatment system (SP3) sample analyses, including J-values. 
4-3 

< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

presented in Appendix A with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quantitation limit, but 

value. 

+ - The accuracy of the Day 1 dissolved mercury analytical result seems questionable based on the results from the other sampling days. If the Day 1 d

excluded from the calculated average, the 4-day average would be 2,940 ng/L. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. 

Table 4-1. Influent to FGD Wastewater Treatment System, Pleasant Prairie 

Analyte Units Method

Influent to FGD Wastewater Treatment Syste

Day 1 Day 2 Day 3 Day 4 

ClassicalsAmmonia mg/L 350.1 19.0 13.0 12.0 14.0 Nitrate Nitrite as N mg/L 353.2 150 160 160 160 Nitrogen, Total Kjeldahl mg/L 351.2 86.0 4 72.0 B 16.0 B 76.0 Biochemical Oxygen Demand mg/L 5210B ND (2.00) ND (2.00) ND (2.00) ND (2.00) Chemical Oxygen Demand mg/L 410.4 420 F 460 410 400 Chloride mg/L 300.0 1,800 1,800 1,800 1,800 Sulfate mg/L 300.0 14,000 16,000 17,000 17,000 Cyanide, Total mg/L 4500 CN E 0.250 B 0.280 B 0.180 B 0.230 Total Dissolved Solids mg/L 2540C 23,000 24,000 24,000 26,000 Total Suspended Solids mg/L 2540D 3,800 7,100 3,300 3,500 Phosphorus, Total mg/L 365.1 0.950 B 0.250 B NQ (0.250) B 0.0630 Total MetalsAluminum ug/L 200.7 110,000 B,4 130,000 120,000 140,000 Antimony ug/L 200.8 65.0 63.0 63.0 60.0 Arsenic ug/L 200.8 150 160 140 150 Barium ug/L 200.7 680 F 770 750 510 Beryllium ug/L 200.7 4.80 5.10 5.00 5.10 Boron ug/L 200.7 11,000 B,4 12,000 B 12,000 B 13,000 Cadmium ug/L 200.8 9.20 11.0 11.0 13.0 Calcium ug/L 200.7 670,000 B,4 690,000 690,000 700,000 Chromium ug/L 200.8 1,400 4,^ 1,000 ^ 960 980 Cobalt ug/L 200.7 140 140 140 140 
4-4 

< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

presented in Appendix A with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quantitation limit, but 

value. 

+ - The accuracy of the Day 1 dissolved mercury analytical result seems questionable based on the results from the other sampling days. If the Day 1 d

excluded from the calculated average, the 4-day average would be 2,940 ng/L. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. 

Table 4-1. Influent to FGD Wastewater Treatment System, Pleasant Prairie 

Analyte Units Method

Influent to FGD Wastewater Treatment Syste

Day 1 Day 2 Day 3 Day 4 

Copper ug/L 200.8 1,300 4 1,100 1,000 1,100 Iron ug/L 200.7 400,000 B,4 420,000 420,000 410,000 Lead ug/L 200.8 280 4 280 280 280 Magnesium ug/L 200.7 4,200,000 B,4 4,200,000 B 4,000,000 4,200,000 Manganese ug/L 200.7 72,000 B,4 76,000 B 73,000 74,000 Mercury ng/L 1631E 2,020,000 2,080,000 2,060,000 1,730,000 Molybdenum ug/L 200.7 240 240 240 240 Nickel ug/L 200.8 1,600 4 1,400 1,400 1,400 Selenium ug/L 200.8 20,000 4 15,000 15,000 B 15,000 Silver ug/L 200.8 NQ (2.00) F NQ (2.00) NQ (2.00) NQ (2.00) Sodium ug/L 200.7 470,000 4 510,000 500,000 520,000 Thallium ug/L 200.8 11.0 12.0 11.0 10.0 Tin ug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (200) Titanium ug/L 200.7 4,500 4 4,400 4,300 4,900 Vanadium ug/L 200.8 1,400 4 1,100 B 910 970 Zinc ug/L 200.8 2,500 4 1,300 B 1,400 1,500 Dissolved MetalsAluminum ug/L 200.7 NQ (200) NQ (200) B 210 NQ (200) Antimony ug/L 200.8 3.80 3.40 3.70 4.10 Arsenic ug/L 200.8 7.20 6.90 7.70 7.00 Barium ug/L 200.7 90.0 F 96.0 97.0 85.0 Beryllium ug/L 200.7 NQ (2.00) NQ (2.00) NQ (2.00) ND (2.00) Boron ug/L 200.7 13,000 4 13,000 B 13,000 B 13,000 
4-5 

< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

presented in Appendix A with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quantitation limit, but 

value. 

+ - The accuracy of the Day 1 dissolved mercury analytical result seems questionable based on the results from the other sampling days. If the Day 1 d

excluded from the calculated average, the 4-day average would be 2,940 ng/L. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. 

Table 4-1. Influent to FGD Wastewater Treatment System, Pleasant Prairie 

Analyte Units Method

Influent to FGD Wastewater Treatment Syste

Day 1 Day 2 Day 3 Day 4 

Cadmium ug/L 200.8 4.50 4.40 6.90 NQ (4.00) Calcium ug/L 200.7 550,000 4 550,000 550,000 560,000 Chromium ug/L 200.8 ND (8.00) ^ ND (8.00) ^ ND (8.00) ^ ND (8.00) Chromium (VI) ug/L 218.6 ND (10.0) ND (10.0) ND (10.0) ND (10.0) Cobalt ug/L 200.7 110 120 120 110 Copper ug/L 200.8 28.0 31.0 34.0 23.0 Iron ug/L 200.7 NQ (200) ND (200) NQ (200) NQ (200) Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.00) Magnesium ug/L 200.7 4,100,000 4 4,000,000 B 3,800,000 B 3,800,000 Manganese ug/L 200.7 70,000 4 72,000 B 70,000 67,000 Mercury ng/L 1631E 1.96+ 3,860 2,370 2,600 Molybdenum ug/L 200.7 49.0 40.0 47.0 50.0 Nickel ug/L 200.8 930 4 940 1,000 870 Selenium ug/L 200.8 3,600 4 3,500 B 3,800 3,900 Silver ug/L 200.8 ND (2.00) F ND (2.00) ND (2.00) ND (2.00) Sodium ug/L 200.7 510,000 4 470,000 490,000 490,000 Thallium ug/L 200.8 9.30 9.80 9.70 9.50 Tin ug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (200) Titanium ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND (20.0) Vanadium ug/L 200.8 NQ (10.0) B NQ (10.0) B NQ (10.0) NQ (10.0) Zinc ug/L 200.8 93.0 100 110 43.0 
4-6 

Note: The Day 2 results represent the average of the original sample and the field duplicate (SP-3). See Section 5.2.4 for the analytical results for the < - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

presented in Appendix A with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quantitation limit, but 

value. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. 

Table 4-2. Effluent From FGD Wastewater Treatment System, Pleasant Prairie

Analyte Units Method

Effluent from the FGD Wastewater Treatment S

Day 1 Day 2 Day 3 D

ClassicalsAmmonia mg/L 350.1 23.0 20.0 18.0 16.0 Nitrate Nitrite as N mg/L 353.2 160 160 160 160 Nitrogen, Total Kjeldahl mg/L 351.2 72.0 B 68.0 64.0 B,4 52.0 Biochemical Oxygen Demand mg/L 5210B ND (2.00) NQ (2.50) NQ (2.50) NQ (2.Chemical Oxygen Demand mg/L 410.4 390 * 455 410 F,* 420 Chloride mg/L 300.0 2,000 2,000 1,900 1,90Sulfate mg/L 300.0 16,000 16,000 15,000 15,00Cyanide, Total mg/L 4500 CN E 0.190 B 0.185 0.240 B,F 0.18Total Dissolved Solids mg/L 2540C 21,000 23,500 23,000 22,00Total Suspended Solids mg/L 2540D NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.Phosphorus, Total mg/L 365.1 0.0700 B < 0.0825 NQ (0.0500) B,F NQ (0.0Total MetalsAluminum ug/L 200.7 680 F < 410 ND (200) NQ (20Antimony ug/L 200.8 2.50 2.35 2.20 2.40 Arsenic ug/L 200.8 6.40 4.80 5.00 5.30 Barium ug/L 200.7 68.0 69.0 74.0 73.0 Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.Boron ug/L 200.7 10,000 B,4 10,000 9,300 4 10,00Cadmium ug/L 200.8 ND (4.00) ND (4.00) ND (4.00) ND (4.Calcium ug/L 200.7 650,000 4 655,000 660,000 4 660,0Chromium ug/L 200.8 ND (8.00) ^ ND (8.00) ND (8.00) ND (8.Cobalt ug/L 200.7 ND (20.0) NQ (20.0) ND (20.0) NQ (20
4-7 

Note: The Day 2 results represent the average of the original sample and the field duplicate (SP-3). See Section 5.2.4 for the analytical results for the < - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

presented in Appendix A with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quantitation limit, but 

value. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. 

Table 4-2. Effluent From FGD Wastewater Treatment System, Pleasant Prairie

Analyte Units Method

Effluent from the FGD Wastewater Treatment S

Day 1 Day 2 Day 3 D

Copper ug/L 200.8 ND (4.00) NQ (4.00) ND (4.00) ND (4.Iron ug/L 200.7 NQ (200) NQ (200) 210 390 Lead ug/L 200.8 ND (2.00) NQ (2.00) ND (2.00) ND (2.Magnesium ug/L 200.7 3,700,000 B,4 3,550,000 3,700,000 4 3,500,0Manganese ug/L 200.7 11,000 B,4 11,000 11,000 4 11,00Mercury ng/L 1631E 78.4 86.4 72.9 74.9 Molybdenum ug/L 200.7 NQ (40.0) NQ (40.0) NQ (40.0) 41.0 Nickel ug/L 200.8 NQ (4.00) < 11.0 NQ (4.00) 7.30 Selenium ug/L 200.8 2,100 4 2,150 2,000 B,4 2,00Silver ug/L 200.8 ND (2.00) F ND (2.00) ND (2.00) F ND (2.Sodium ug/L 200.7 510,000 4 510,000 530,000 4 500,0Thallium ug/L 200.8 2.90 2.95 2.80 2.30 Tin ug/L 200.7 ND (200) NQ (200) ND (200) NQ (20Titanium ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND (20Vanadium ug/L 200.8 ND (10.0) ND (10.0) ND (10.0) ND (10Zinc ug/L 200.8 ND (10.0) < 9.50 ND (10.0) NQ (10Dissolved MetalsAluminum ug/L 200.7 ND (200) ND (200) NQ (200) ^ NQ (20Antimony ug/L 200.8 2.80 < 1.75 2.60 2.70 Arsenic ug/L 200.8 4.90 5.40 4.20 4.90 Barium ug/L 200.7 67.0 69.0 72.0 69.0 Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.Boron ug/L 200.7 10,000 B,4 10,000 9,900 B,4 9,80
4-8 

Note: The Day 2 results represent the average of the original sample and the field duplicate (SP-3). See Section 5.2.4 for the analytical results for the < - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

presented in Appendix A with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quantitation limit, but 

value. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. 

Table 4-2. Effluent From FGD Wastewater Treatment System, Pleasant Prairie

Analyte Units Method

Effluent from the FGD Wastewater Treatment S

Day 1 Day 2 Day 3 D

Cadmium ug/L 200.8 ND (4.00) ND (4.00) ND (4.00) ND (4.Calcium ug/L 200.7 640,000 4 645,000 660,000 4 610,0Chromium ug/L 200.8 ND (8.00) ^ ND (8.00) ND (8.00) ^ ND (8.Chromium (VI) ug/L 218.6 ND (10.0) ND (10.0) ND (10.0) ND (10Cobalt ug/L 200.7 ND (20.0) NQ (20.0) ND (20.0) NQ (20Copper ug/L 200.8 ND (4.00) ND (4.00) ND (4.00) ND (4.Iron ug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (20Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.Magnesium ug/L 200.7 3,700,000 B,4 3,550,000 3,500,000 B,4 3,500,0Manganese ug/L 200.7 11,000 B,4 11,000 10,000 B,4 11,00Mercury ng/L 1631E 22.8 27.0 20.5 19.0 Molybdenum ug/L 200.7 NQ (40.0) NQ (40.0) NQ (40.0) NQ (40Nickel ug/L 200.8 NQ (4.00) NQ (4.00) 6.10 NQ (4.Selenium ug/L 200.8 2,100 B,4 2,100 2,000 B,4 2,10Silver ug/L 200.8 ND (2.00) F ND (2.00) ND (2.00) F ND (2.Sodium ug/L 200.7 530,000 4 530,000 520,000 4 490,0Thallium ug/L 200.8 2.50 2.65 2.30 2.90 Tin ug/L 200.7 ND (200) NQ (200) ND (200) NQ (20Titanium ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND (20Vanadium ug/L 200.8 NQ (10.0) B ND (10.0) ND (10.0) ND (10Zinc ug/L 200.8 19.0 F ND (10.0) ND (10.0) ND (10
4-9 

< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

presented in Appendix A with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quantitation limit, but 

value. 

Table 4-3. Classical Pollutants 4-Day Average Data Summary for FGD Wastewater Treatment System

Analyte Units Method SP-1 

ClassicalsAmmonia mg/L 350.1 14.5 Nitrate Nitrite as N mg/L 353.2 158 Nitrogen, Total Kjeldahl mg/L 351.2 62.5 Biochemical Oxygen Demand mg/L 5210B ND (2.00) Chemical Oxygen Demand mg/L 410.4 423 Chloride mg/L 300.0 1,800 Sulfate mg/L 300.0 16,000 Cyanide, Total mg/L 4500 CN E 0.235 Total Dissolved Solids mg/L 2540C 24,300 Total Suspended Solids mg/L 2540D 4,430 Phosphorus, Total mg/L 365.1 < 0.347 
4-10 

< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu* - The 4-day average result includes an analytical result where the accuracy is questionable. If the questionable result was excluded from the calculataverage would be 2,940 ng/L. ND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

presented in Appendix A with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quantitation limit, but 

value. 

Table 4-4. Metal Pollutants 4-Day Average Data Summary for FGD Wastewater Treatment System, Ple

Analyte Units Method 

Influent to FGD 

Wastewater Treatment

System (SP-1)

4-Day Average 

Effluent 

FGD Wastewat

System 

4-Day A

Total Dissolved Total 

MetalsAluminum ug/L 200.7 125,000 < 128 < 323 Antimony ug/L 200.8 62.8 3.75 2.36 Arsenic ug/L 200.8 150 7.20 5.38 Barium ug/L 200.7 678 92.0 71.0 Beryllium ug/L 200.7 5.00 NQ (2.00) ND (2.00) Boron ug/L 200.7 12,000 13,000 9,830 Cadmium ug/L 200.8 11.1 < 4.45 ND (4.00) Calcium ug/L 200.7 688,000 553,000 656,000 Chromium ug/L 200.8 1,090 ND (8.00) ND (8.00) Chromium (VI) ug/L 218.6 NA ND (10.0) NA Cobalt ug/L 200.7 140 115 NQ (20.0) Copper ug/L 200.8 1,130 29.0 NQ (4.00) Iron ug/L 200.7 413,000 NQ (200) < 200 Lead ug/L 200.8 280 ND (2.00) NQ (2.00) Magnesium ug/L 200.7 4,150,000 3,930,000 3,610,000 Manganese ug/L 200.7 73,800 69,800 11,000 Mercury ng/L 1631E 1,970,000 2,210* 78.1 Molybdenum ug/L 200.7 240 46.5 < 25.3 Nickel ug/L 200.8 1,450 935 < 5.58 Selenium ug/L 200.8 16,300 3,700 2,060 Silver ug/L 200.8 NQ (2.00) ND (2.00) ND (2.00) Sodium ug/L 200.7 500,000 490,000 513,000 Thallium ug/L 200.8 11.0 9.58 2.74 
4-11 

< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu* - The 4-day average result includes an analytical result where the accuracy is questionable. If the questionable result was excluded from the calculataverage would be 2,940 ng/L. ND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

presented in Appendix A with a J flag designation. A “NQ” for the 4-day average result indicates that all results were below the quantitation limit, but 

value. 

Table 4-4. Metal Pollutants 4-Day Average Data Summary for FGD Wastewater Treatment System, Ple

Analyte Units Method 

Influent to FGD 

Wastewater Treatment

System (SP-1)

4-Day Average 

Effluent 

FGD Wastewat

System 

4-Day A

Total Dissolved Total 

Tin ug/L 200.7 NQ (200) NQ (200) NQ (200) Titanium ug/L 200.7 4,530 ND (20.0) ND (20.0) Vanadium ug/L 200.8 1,100 NQ (10.0) ND (10.0) Zinc ug/L 200.8 1,680 86.5 < 6.13 
5-1 

5. DATA QUALITY

Quality assurance/quality control (QA/QC) procedures applicable to the Pleasant Prairie 

sampling episode are outlined in the Quality Assurance Project Plan for the Steam Electric 

Rulemaking (QAPP) [2]. This section describes the QC procedures used to assess the precision 

and accuracy of the analytical data presented in Section 4 and Appendix A. QC practices used 

for this sampling episode include the analysis of matrix spikes, blanks, duplicate samples, and 

QC standard checks. 

5.1 Analytical Quality Control

ERG contracted directly with analytical laboratories for the analysis of samples collected 

during this episode. ERG verified that the performance of the laboratories selected were 

acceptable by conducting QC checks of the analytical data. Data review chemists at ERG 

prepared written data review narratives describing any qualifications of the analytical data from 

this episode. The data review narratives are included in Appendix B. 

5.2 Field Quality Control

This subsection discusses the bottle blanks, equipment blanks, field blanks, and field 

duplicate sample results. Section 3.8 of the Sampling Plan discusses field QC specifications. 

5.2.1 Bottle Blanks 

ERG collects bottle blanks to evaluate possible contamination from the sample collection 

bottles. Bottle blanks were collected and analyzed for metals (EPA Method 200.8, 200.7, and 

1631E) by the supplier of the precleaned bottles, Frontier Global Sciences. 

Frontier Global Sciences collected the bottle blanks for the metals sample bottles by 

filling the precleaned bottle with reagent water, preserving the sample with nitric acid to a pH <2 

S.U. Frontier Global Sciences then analyzed the samples using EPA Method 1638. 

Frontier Global Sciences collected the bottle blanks for the mercury sample bottles by 

filling the precleaned bottle with reagent water, preserving the sample with bromine 

monochloride. Frontier Global Sciences then analyzed the samples using EPA Method 1631E. 

Albion Environmental collected the bottle blanks for the 10- and 20-liter composite 

containers by filling the container with approximately two liters of ASTM Type 1 water and 

allowing it to soak for approximately 24 hours. During this period, the laboratory shook the 

container periodically and changed its orientation to expose all surfaces of the container to the 

ASTM Type 1 water. Albion Environmental then shook the 10- and 20-liter containers and 

poured a representative sample into a precleaned LDPE sample bottle. The blank samples were 

then preserved and analyzed according to the analytical methods (i.e., EPA Method 1638). 

No metals were detected in the bottle blanks, except for aluminum in the 10-liter 

composite containers. Aluminum was detected in the 10-L container at a concentration of 4.71 

ug/L, which is well below the quantitation limit used for the sample analyses (i.e., 200 ug/L); 

therefore, this contamination did not affect the results of the sampling episode. Appendix Table 
5-2 

A-10 presents all of the analytical results from the bottle blank analyses for the bottles used to 

collect the metals and mercury samples. 

5.2.2 Equipment Blanks 

EPA collects equipment blanks to evaluate possible contamination from the equipment 

used for sample collection. The techniques used to collect field blanks (as described in Section 

5.2.3) include the sampling equipment and therefore would identify whether the sampling 

equipment was introducing contamination. In addition, Frontier Global Sciences collected and 

analyzed equipment blanks for metals (EPA Method 1638 and 1631E) for each type of 

precleaned equipment supplied for the episode. 

Frontier Global Sciences collected the equipment blanks for the capsule filters and 

fabricated tubing sets by pumping reagent water through the cleaned and fully assembled 

equipment sets (with the filter attached) into a cleaned bottle (an HDPE bottle for metals and a 

glass bottle for mercury). The blank samples were then preserved and analyzed according to the 

analytical methods (EPA Method 1638 and 1631E), as described in Section 5.2.1 for the bottle 

blank samples. 

No other metals were detected in the equipment blanks, indicating that there was no 

contamination from the sampling equipment. Appendix Table A-10 presents all of the analytical 

results from the bottle blank and equipment blank analyses for all of the equipment used for the 

collection of metals and mercury samples. 

5.2.3 Field Blanks 

The sampling team collected field blanks (SP-4 and SP-5) to evaluate possible 

contamination from sampling equipment, sampling equipment decontamination procedures, 

sample collection procedures, or atmospheric contamination. EPA analyzed the field blank 

samples for the total and dissolved metals and total and dissolved mercury samples2

. 

The total mercury, total metals by 200.8, and total metals by 200.7 field blank samples 

for the influent to the FGD wastewater treatment system (SP-4) were collected by pouring 

ASTM Type 1 water through a precleaned funnel attached to the silicone tubing used for sample 

collection. To prevent potential atmospheric deposition, the sampling team shrouded the blank 

water and funnel with a plastic bag while pouring the blank water into the funnel and placed the 

sample bottles in a “cleanbox.” Prior to filling the sample bottles, the tubing was purged with 

approximately 1 liter of blank water. The ASTM Type 1 water flowed through the funnel, tubing, 

and “Y” splitter, and was poured into the sample bottles. EPA collected the field blank samples 

as “true” split samples with Pleasant Prairie’s representative, using the same procedure discussed 

in the sample collection description (Section 3.1). 

 

2 EPA did not collect a dissolved mercury field blank sample because the sample filtration was performed at the 

laboratory to minimize potential mercury contamination. The laboratory performed a filtration blank prior to 

filtering the sample, which is assessed as the field blank for the dissolved mercury sample. Mercury was not 

detected above the method detection limit (0.24 ng/L) in the filtration blanks performed for any of the days of 

samples.
5-3 

The dissolved metals by 200.8, dissolved metals by 200.7, and dissolved hexavalant 

chromium field blank samples for the influent to the FGD wastewater treatment system (SP-4) 

were collected by pouring ASTM Type 1 water through the funnel and tubing and into a 10-liter 

composite container. After around 120 minutes, the sampling team began pumping off the 

ASTM Type 1 water from the 10-liter composite container. Prior to filling the sample bottles, the 

tubing was purged for around 40 seconds. The sample bottles were placed in a “cleanbox” and 

the ASTM Type 1 water was pumped through the tubing, capsule filter, and “Y” splitter, and into 

the sample bottles. EPA collected the field blank samples as “true” split samples with Pleasant 

Prairie’s representative, using the same procedure discussed in the sample collection description 

(Section 3.1). 

The total mercury field blank sample for the effluent from the FGD wastewater treatment 

system (SP-5) was collected by shrouding one of the three taps on the sample tap splitter with a 

clear plastic bag. Before purging the sample tap, ASTM Type 1 water was poured directly into 

the sample bottles under the clear plastic bag. 

The total and dissolved metals by 200.7 and metals by 200.8 field blank samples for the 

effluent from the FGD wastewater treatment system (SP-5) were collected by filling a 20-liter 

composite container with ASTM Type 1 water. The same T-splitter tubing used to fill the metals 

composite container was used with a pump to fill the 20-liter field blank composite container. 

Prior to attaching one end of the tubing to the sample tap, it was placed directly into the 

container holding ASTM Type 1 water. The other end of the tubing was attached to the vented 

cap on top of the 20-liter field blank composite container. After enough volume was pumped into 

the 20-liter field blank composite container, the vented cap was replaced with a closed cap and 

the container was placed on ice in a covered plastic trash can. The vented cap used for the field 

blank collection was the same cap that was later used for the metals composite container. 

After 24 hours, the ASTM Type 1 water in the 20-liter field blank composite container 

was pumped off into the individual sample bottles. The sample bottles were placed in a 

“cleanbox” and the ASTM Type 1 water was pumped through the tubing and “Y” splitter, and 

into the sample bottles. EPA collected the field blank samples as “true” split samples with 

Pleasant Prairie’s representative, using the same procedure discussed in the sample collection 

description (Section 3.1). Prior to filling the sample bottles, the tubing was purged with 

approximately one liter of ASTM Type 1 water. First the samplers collected the total metals by 

200.8 and total metals by 200.7 field blank samples. Then the sampling team attached a filter to 

the tubing set and purged the tubing with approximately one liter of ASTM Type 1 water. The 

samplers then collected the dissolved metals by 200.8, dissolved metals by 200.7, and dissolved 

hexavalent chromium field blank samples. 

Table 5-1 presents the field blank analytical results for SP-4 and SP-5. Only those 

analytes that were detected in the field blank samples at levels above the quantitation limit are 

included in the table. Results are rounded to three significant digits. Appendix Tables A-11 

through A-15 present all the analytical results for the field blanks from each of the sampling 

points, including all qualified results and all results that were measured above the method 

detection limit, but below the quantitation limit (i.e., J-values). 
5-4 

5.2.4 Field Duplicates 

The sampling team collected field duplicate samples to assess the sampling measurement 

precision for the episode. Field duplicate samples are separate samples collected from the same 

location as the original sample. The duplicate is filled immediately after the original sample and 

is stored and analyzed independently. The RPD between the two sample results is examined to 

determine the precision of the data. EPA used the following equation to calculate the RPD for 

the duplicate sample results. 

100

2

S D

S D

RPD (%) 





 



 

  (5-1) 

where: 

S = concentration of the analyte from original sample analysis; 

D = concentration of the analyte from the duplicate sample analysis; and 

RPD = relative percent difference between the original and duplicate sample 

result. 

During this sampling episode, EPA collected duplicate samples for the effluent from the 

FGD wastewater treatment system (SP-3) during day 2 of the sampling episode. The duplicate 

samples were analyzed for all analytes. Table 5-2 presents analytical results and the RPD for SP3. Results are rounded to three significant digits. Appendix Tables A-6 and A-9 present all the 

analytical results for the effluent from the FGD wastewater treatment system (SP-2) Day 2 and 

the duplicate of the effluent from the FGD wastewater treatment system (SP-3) sample analyses, 

including all qualified results and all results that were measured above the method detection 

limit, but below the quantitation limit (i.e., J-values). 
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

presented in Appendix A with a J flag designation. A “NQ” for the average result indicates that all results were below the quantitation limit, but at leas^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. 

5-5 

Table 5-1. Field Blank Analytical Results, Pleasant Prairie 

Analyte Sample Description Method Units 

Total MetalsNickel Effluent from FGD Wastewater Treatment System Field Blank - Day 1 200.8 ug/L Selenium Influent to FGD Wastewater Treatment System Field Blank - Day 1 200.8 ug/L 
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

presented in Appendix A with a J flag designation. A “NQ” for the average result indicates that all results were below the quantitation limit, but at leas^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. 

5-6 

Table 5-2. Field Duplicate Results – Effluent from FGD Wastewater Treatment System, Pleasa

Analyte Method Units

Original 

Effluent from FGD 

Wastewater Treatment 

System, Day 2 

Concentration 

(SP-2)

Duplicate

Effluent from FGD 

Wastewater Treatment 

System Concentration 

(SP-4)

A

R

ClassicalsAmmonia 350.1 mg/L 20.0 20.0 Nitrate Nitrite as N 353.2 mg/L 160 160 Nitrogen, Total Kjeldahl 351.2 mg/L 66.0 B 70.0 B Biochemical Oxygen Demand 5210B mg/L NQ (2.50) NQ (2.50) NChemical Oxygen Demand 410.4 mg/L 440 470 Chloride 300.0 mg/L 2,000 2,000 Sulfate 300.0 mg/L 16,000 16,000 Cyanide, Total

4500 CN 

E mg/L 0.210 B 0.160 B 

Total Dissolved Solids 2540C mg/L 24,000 23,000 2Total Suspended Solids 2540D mg/L NQ (4.00) NQ (4.00) NPhosphorus, Total 365.1 mg/L 0.140 B NQ (0.0500) B < Total MetalsAluminum 200.7 ug/L 720 F ND (200) Antimony 200.8 ug/L 2.40 2.30 Arsenic 200.8 ug/L 4.70 4.90 Barium 200.7 ug/L 69.0 69.0 Beryllium 200.7 ug/L ND (2.00) ND (2.00) ND Boron 200.7 ug/L 10,000 B,4 10,000 B Cadmium 200.8 ug/L ND (4.00) ND (4.00) ND 
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

presented in Appendix A with a J flag designation. A “NQ” for the average result indicates that all results were below the quantitation limit, but at leas^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. 

5-7 

Table 5-2. Field Duplicate Results – Effluent from FGD Wastewater Treatment System, Pleasa

Analyte Method Units

Original 

Effluent from FGD 

Wastewater Treatment 

System, Day 2 

Concentration 

(SP-2)

Duplicate

Effluent from FGD 

Wastewater Treatment 

System Concentration 

(SP-4)

A

R

Calcium 200.7 ug/L 650,000 4 660,000 6Chromium 200.8 ug/L ND (8.00) ND (8.00) ND Cobalt 200.7 ug/L NQ (20.0) NQ (20.0) NCopper 200.8 ug/L NQ (4.00) ND (4.00) NIron 200.7 ug/L NQ (200) NQ (200) NLead 200.8 ug/L NQ (2.00) ND (2.00) NMagnesium 200.7 ug/L 3,600,000 4 3,500,000 3,Manganese 200.7 ug/L 11,000 4 11,000 Mercury 1631E ng/L 88.3 84.4 Molybdenum 200.7 ug/L NQ (40.0) NQ (40.0) NNickel 200.8 ug/L 20.0 F NQ (4.00) Selenium 200.8 ug/L 2,200 B,4 2,100 B Silver 200.8 ug/L ND (2.00) F ND (2.00) ND Sodium 200.7 ug/L 510,000 4 510,000 5Thallium 200.8 ug/L 3.10 2.80 Tin 200.7 ug/L ND (200) NQ (200) NTitanium 200.7 ug/L ND (20.0) ND (20.0) ND Vanadium 200.8 ug/L ND (10.0) ND (10.0) ND Zinc 200.8 ug/L 14.0 F ND (10.0) Dissolved MetalsAluminum 200.7 ug/L ND (200) ND (200) N
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

presented in Appendix A with a J flag designation. A “NQ” for the average result indicates that all results were below the quantitation limit, but at leas^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. 

5-8 

Table 5-2. Field Duplicate Results – Effluent from FGD Wastewater Treatment System, Pleasa

Analyte Method Units

Original 

Effluent from FGD 

Wastewater Treatment 

System, Day 2 

Concentration 

(SP-2)

Duplicate

Effluent from FGD 

Wastewater Treatment 

System Concentration 

(SP-4)

A

R

Antimony 200.8 ug/L NQ (2.00) 2.50 Arsenic 200.8 ug/L 5.50 5.30 Barium 200.7 ug/L 68.0 70.0 Beryllium 200.7 ug/L ND (2.00) ND (2.00) ND Boron 200.7 ug/L 10,000 B,4 10,000 B Cadmium 200.8 ug/L ND (4.00) ND (4.00) ND Calcium 200.7 ug/L 640,000 4 650,000 6Chromium 200.8 ug/L ND (8.00) ^ ND (8.00) ^ ND Chromium (VI) 218.6 ug/L ND (10.0) ND (10.0) ND Cobalt 200.7 ug/L ND (20.0) NQ (20.0) NCopper 200.8 ug/L ND (4.00) ND (4.00) ND Iron 200.7 ug/L NQ (200) NQ (200) NLead 200.8 ug/L ND (2.00) ND (2.00) ND Magnesium 200.7 ug/L 3,500,000 B,4 3,600,000 B 3,Manganese 200.7 ug/L 11,000 4 11,000 Mercury 1631E ng/L 27.4 26.5 Molybdenum 200.7 ug/L NQ (40.0) NQ (40.0) NNickel 200.8 ug/L NQ (4.00) NQ (4.00) NSelenium 200.8 ug/L 2,000 4 2,200 Silver 200.8 ug/L ND (2.00) F ND (2.00) ND Sodium 200.7 ug/L 520,000 4 540,000 5
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

presented in Appendix A with a J flag designation. A “NQ” for the average result indicates that all results were below the quantitation limit, but at leas^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. 

5-9 

Table 5-2. Field Duplicate Results – Effluent from FGD Wastewater Treatment System, Pleasa

Analyte Method Units

Original 

Effluent from FGD 

Wastewater Treatment 

System, Day 2 

Concentration 

(SP-2)

Duplicate

Effluent from FGD 

Wastewater Treatment 

System Concentration 

(SP-4)

A

R

Thallium 200.8 ug/L 2.70 2.60 Tin 200.7 ug/L ND (200) NQ (200) NTitanium 200.7 ug/L ND (20.0) ND (20.0) ND Vanadium 200.8 ug/L ND (10.0) ND (10.0) ND Zinc 200.8 ug/L ND (10.0) ND (10.0) ND 
6-1

6. REFERENCES

1. Eastern Research Group, Inc., 2010. Sampling Plan, We Energies’ Pleasant Prairie 

Power Station. June 3. DCN SE00506. 

2. Eastern Research Group, Inc., 2010. Quality Assurance Project Plan for the Steam 

Electric Effluent Guidelines Rulemaking. (October). DCN SE00058. 
Appendix A 

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

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-1 

Table A-1. Influent to FGD Wastewater Treatment System, Day 1 Analytical Results, Pleasan

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 4 1.9 4 Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 Nitrogen, Total Kjeldahl 351.2 mg/L 4 1.5 20 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 Chemical Oxygen Demand 410.4 mg/L 5 20 100 Chloride 300.0 mg/L 50 13 150 Sulfate 300.0 mg/L 500 120 2,500 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 11 40 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 50 82 200 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 50 24 100 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 50 18 50 Magnesium 200.7 ug/L 50 540 10,000 
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. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-2 

Table A-1. Influent to FGD Wastewater Treatment System, Day 1 Analytical Results, Pleasan

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 200,000 49,700 104,000 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 50 22 100 Selenium 200.8 ug/L 50 16 100 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 50 42 250 Zinc 200.8 ug/L 50 100 250 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 
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. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-3 

Table A-1. Influent to FGD Wastewater Treatment System, Day 1 Analytical Results, Pleasan

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 1 0.24 0.5 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 50 22 100 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
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). 

A-4 

Table A-2. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, Pleasan

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 2 0.94 2 Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 Nitrogen, Total Kjeldahl 351.2 mg/L 4 1.5 20 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 Chemical Oxygen Demand 410.4 mg/L 5 20 100 Chloride 300.0 mg/L 50 13 150 Sulfate 300.0 mg/L 500 120 2,500 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 28 100 Phosphorus, Total 365.1 mg/L 5 0.025 0.25 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 50 82 200 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 50 24 100 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 50 18 50 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 200,000 48,300 101,000 
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). 

A-5 

Table A-2. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, Pleasan

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 50 22 100 Selenium 200.8 ug/L 50 16 100 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 50 42 250 Zinc 200.8 ug/L 50 100 250 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 4,000 975 2,040 Molybdenum 200.7 ug/L 2 1.6 40 
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). 

A-6 

Table A-2. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, Pleasan

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Nickel 200.8 ug/L 10 4.5 20 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
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). 

A-7 

Table A-3. Influent to FGD Wastewater Treatment System, Day 3 Analytical Results, Pleasan

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 2 0.94 2 Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.38 5 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 Chemical Oxygen Demand 410.4 mg/L 5 20 100 Chloride 300.0 mg/L 50 13 150 Sulfate 300.0 mg/L 500 120 2,500 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 28 100 Phosphorus, Total 365.1 mg/L 5 0.025 0.25 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 10 16 40 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 50 24 100 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 10 3.6 10 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 200,000 48,300 101,000 
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). 

A-8 

Table A-3. Influent to FGD Wastewater Treatment System, Day 3 Analytical Results, Pleasan

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 50 22 100 Selenium 200.8 ug/L 10 3.1 20 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 10 8.4 50 Zinc 200.8 ug/L 50 100 250 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 100 24.1 50.5 Molybdenum 200.7 ug/L 2 1.6 40 
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). 

A-9 

Table A-3. Influent to FGD Wastewater Treatment System, Day 3 Analytical Results, Pleasan

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Nickel 200.8 ug/L 50 22 100 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
ND – Not detected (number in parentheses is the quantitation limit). 

* - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-10 

Table A-4. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, Pleasan

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 2 0.94 2 Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 Nitrogen, Total Kjeldahl 351.2 mg/L 4 1.5 20 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 Chemical Oxygen Demand 410.4 mg/L 5 20 100 Chloride 300.0 mg/L 50 13 150 Sulfate 300.0 mg/L 500 120 2,500 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 28 100 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 50 240 5,000 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 10 16 40 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 50 24 100 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 10 3.6 10 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 
ND – Not detected (number in parentheses is the quantitation limit). 

* - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-11 

Table A-4. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, Pleasan

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Mercury 1631E ng/L 200,000 48,300 101,000 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 50 22 100 Selenium 200.8 ug/L 10 3.1 20 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 10 8.4 50 Zinc 200.8 ug/L 50 100 250 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 
ND – Not detected (number in parentheses is the quantitation limit). 

* - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-12 

Table A-4. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, Pleasan

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 2,000 487 1,020 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 10 4.5 20 Selenium 200.8 ug/L 10 3.1 20 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
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. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-13 

Table A-5. Effluent from FGD Wastewater Treatment System, Day 1 Analytical Results, Pleasa

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 4 1.9 4 Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 Nitrogen, Total Kjeldahl 351.2 mg/L 10 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 Chemical Oxygen Demand 410.4 mg/L 5 20 100 Chloride 300.0 mg/L 50 13 150 Sulfate 300.0 mg/L 500 120 2,500 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 
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. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-14 

Table A-5. Effluent from FGD Wastewater Treatment System, Day 1 Analytical Results, Pleasa

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 10 2.41 5.05 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 
ND – Not detected (number in parentheses is the quantitation limit). 

* - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-15 

Table A-5. Effluent from FGD Wastewater Treatment System, Day 1 Analytical Results, Pleasa

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 10 2.41 5.05 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
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. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-16 

Table A-6. Effluent from FGD Wastewater Treatment System, Day 2 Analytical Results, Pleasa

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 4 1.9 4 Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 Nitrogen, Total Kjeldahl 351.2 mg/L 10 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 5 20 100 Chloride 300.0 mg/L 50 13 150 Sulfate 300.0 mg/L 500 120 2,500 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 
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. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-17 

Table A-6. Effluent from FGD Wastewater Treatment System, Day 2 Analytical Results, Pleasa

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 20 4.83 10.1 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 
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. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-18 

Table A-6. Effluent from FGD Wastewater Treatment System, Day 2 Analytical Results, Pleasa

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 50 12.1 25.2 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
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. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-19 

Table A-7. Effluent from FGD Wastewater Treatment System, Day 3 Analytical Results, Pleasa

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 2 0.94 2 Nitrate Nitrite as N 353.2 mg/L 50 0.95 5 Nitrogen, Total Kjeldahl 351.2 mg/L 10 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 5 20 100 Chloride 300.0 mg/L 50 13 150 Sulfate 300.0 mg/L 500 120 2,500 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 19 40 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 
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. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-20 

Table A-7. Effluent from FGD Wastewater Treatment System, Day 3 Analytical Results, Pleasa

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 10 2.41 5.05 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 
ND – Not detected (number in parentheses is the quantitation limit). 

* - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-21 

Table A-7. Effluent from FGD Wastewater Treatment System, Day 3 Analytical Results, Pleasa

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 10 2.41 5.05 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
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. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-22 

Table A-8. Effluent from FGD Wastewater Treatment System, Day 4 Analytical Results, Pleasa

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.94 2 Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 Nitrogen, Total Kjeldahl 351.2 mg/L 10 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 5 20 100 Chloride 300.0 mg/L 50 13 150 Sulfate 300.0 mg/L 500 120 2,500 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 
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. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-23 

Table A-8. Effluent from FGD Wastewater Treatment System, Day 4 Analytical Results, Pleasa

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 100 24.1 50.5 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 
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. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

A-24 

Table A-8. Effluent from FGD Wastewater Treatment System, Day 4 Analytical Results, Pleasa

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 10 2.41 5.05 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
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). 

A-25 

Table A-9. Duplicate of Effluent from FGD Wastewater Treatment System, Analytical Results, Ple

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 4 1.9 4 Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 Nitrogen, Total Kjeldahl 351.2 mg/L 10 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 5 20 100 Chloride 300.0 mg/L 50 13 150 Sulfate 300.0 mg/L 500 120 2,500 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 50 12.1 25.2 
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). 

A-26 

Table A-9. Duplicate of Effluent from FGD Wastewater Treatment System, Analytical Results, Ple

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 50 12.1 25.2 Molybdenum 200.7 ug/L 2 1.6 40 
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). 

A-27 

Table A-9. Duplicate of Effluent from FGD Wastewater Treatment System, Analytical Results, Ple

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

ND – Not detected (number in parenthesis is the report limit). 

A-28 

Table A-10. Bottle Blank and Equipment Blank Analytical Data, Pleasant Prairie

Analyte Method Process Units Concentration 

HDPE 250 ml Plastic Bottles – Bottle Blank (for metals and hexavalent chromium samples) 

Aluminum EPA 1638 Total Recoverable ug/L ND (4.0) 

Antimony EPA 1638 Total Recoverable ug/L ND (0.020) 

Arsenic EPA 1638 Total Recoverable ug/L ND (0.15) 

Barium EPA 1638 Total Recoverable ug/L ND (0.20) 

Beryllium EPA 1638 Total Recoverable ug/L ND (0.060) 

Boron EPA 1638 Total Recoverable ug/L ND (3.0) 

Cadmium EPA 1638 Total Recoverable ug/L ND (0.020) 

Calcium EPA 1638 Total Recoverable ug/L ND (40) 

Chromium EPA 1638 Total Recoverable ug/L ND (0.10) 

Cobalt EPA 1638 Total Recoverable ug/L ND (0.10) 

Copper EPA 1638 Total Recoverable ug/L ND (0.10) 

Iron EPA 1638 Total Recoverable ug/L ND (10) 

Lead EPA 1638 Total Recoverable ug/L ND (0.040) 

Magnesium EPA 1638 Total Recoverable ug/L ND (2.5) 

Manganese EPA 1638 Total Recoverable ug/L ND (0.10) 

Molybdenum EPA 1638 Total Recoverable ug/L ND (0.060) 

Nickel EPA 1638 Total Recoverable ug/L ND (0.10) 

Selenium EPA 1638 Total Recoverable ug/L ND (0.60) 

Silver EPA 1638 Total Recoverable ug/L ND (0.020) 

Sodium EPA 1638 Total Recoverable ug/L ND (20) 

Thallium EPA 1638 Total Recoverable ug/L ND (0.0050) 

Tin EPA 1638 Total Recoverable ug/L ND (0.10) 

Titanium EPA 1638 Total Recoverable ug/L ND (0.50) 

Vanadium EPA 1638 Total Recoverable ug/L ND (0.10) 

Zinc EPA 1638 Total Recoverable ug/L ND (0.20) 

HDPE 500 ml Plastic Bottles – Bottle Blank (for metals samples) 

Aluminum EPA 1638 Total Recoverable ug/L ND (4.0) 

Antimony EPA 1638 Total Recoverable ug/L ND (0.020) 

Arsenic EPA 1638 Total Recoverable ug/L ND (0.15) 

Barium EPA 1638 Total Recoverable ug/L ND (0.20) 

Beryllium EPA 1638 Total Recoverable ug/L ND (0.060) 

Boron EPA 1638 Total Recoverable ug/L ND (3.0) 

Cadmium EPA 1638 Total Recoverable ug/L ND (0.020) 

Calcium EPA 1638 Total Recoverable ug/L ND (40) 

Chromium EPA 1638 Total Recoverable ug/L ND (0.10) 

Cobalt EPA 1638 Total Recoverable ug/L ND (0.10) 

Copper EPA 1638 Total Recoverable ug/L ND (0.10) 

Iron EPA 1638 Total Recoverable ug/L ND (10) 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

ND – Not detected (number in parenthesis is the report limit). 

A-29 

Table A-10. Bottle Blank and Equipment Blank Analytical Data, Pleasant Prairie

Analyte Method Process Units Concentration 

Lead EPA 1638 Total Recoverable ug/L ND (0.040) 

Magnesium EPA 1638 Total Recoverable ug/L ND (2.5) 

Manganese EPA 1638 Total Recoverable ug/L ND (0.10) 

Molybdenum EPA 1638 Total Recoverable ug/L ND (0.060) 

Nickel EPA 1638 Total Recoverable ug/L ND (0.10) 

Selenium EPA 1638 Total Recoverable ug/L ND (0.60) 

Silver EPA 1638 Total Recoverable ug/L ND (0.020) 

Sodium EPA 1638 Total Recoverable ug/L ND (20) 

Thallium EPA 1638 Total Recoverable ug/L ND (0.0050) 

Tin EPA 1638 Total Recoverable ug/L ND (0.10) 

Titanium EPA 1638 Total Recoverable ug/L ND (0.50) 

Vanadium EPA 1638 Total Recoverable ug/L ND (0.10) 

Zinc EPA 1638 Total Recoverable ug/L ND (0.20) 

125 ml Glass Bottles – Bottle Blank (for mercury composite samples)

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

250 ml Glass Bottles – Bottle Blank (for mercury grab samples)

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

LDPE 10 L Composite Bottles – Bottle Blank (sample composite bottle for dissolved/filtration pump-off)

Aluminuma EPA 1638 Dissolved ug/L 4.71 

Antimony EPA 1638 Dissolved ug/L ND (0.50) 

Arsenic EPA 1638 Dissolved ug/L ND (0.50) 

Barium EPA 1638 Dissolved ug/L ND (0.10) 

Beryllium EPA 1638 Dissolved ug/L ND (0.10) 

Cadmium EPA 1638 Dissolved ug/L ND (0.10) 

Chromium EPA 1638 Dissolved ug/L ND (1.0) 

Cobalt EPA 1638 Dissolved ug/L ND (0.10) 

Copper EPA 1638 Dissolved ug/L ND (0.30) 

Lead EPA 1638 Dissolved ug/L ND (0.050) 

Manganese EPA 1638 Dissolved ug/L ND (0.50) 

Molybdenum EPA 1638 Dissolved ug/L ND (0.50) 

Nickel EPA 1638 Dissolved ug/L ND (0.50) 

Selenium EPA 1638 Dissolved ug/L ND (2.0) 

Silver EPA 1638 Dissolved ug/L ND (0.10) 

Thallium EPA 1638 Dissolved ug/L ND (0.050) 

Vanadium EPA 1638 Dissolved ug/L ND (1.0) 

Zinc EPA 1638 Dissolved ug/L ND (0.50) 

LDPE 20 L Composite Bottles – Bottle Blank (sample composite bottle for dissolved/filtration pump-off)

Aluminum EPA 1638 Dissolved ug/L ND (2.0) 

Antimony EPA 1638 Dissolved ug/L ND (0.50) 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

ND – Not detected (number in parenthesis is the report limit). 

A-30 

Table A-10. Bottle Blank and Equipment Blank Analytical Data, Pleasant Prairie

Analyte Method Process Units Concentration 

Arsenic EPA 1638 Dissolved ug/L ND (0.50) 

Barium EPA 1638 Dissolved ug/L ND (0.10) 

Beryllium EPA 1638 Dissolved ug/L ND (0.10) 

Cadmium EPA 1638 Dissolved ug/L ND (0.10) 

Chromium EPA 1638 Dissolved ug/L ND (1.0) 

Cobalt EPA 1638 Dissolved ug/L ND (0.10) 

Copper EPA 1638 Dissolved ug/L ND (0.30) 

Lead EPA 1638 Dissolved ug/L ND (0.050) 

Manganese EPA 1638 Dissolved ug/L ND (0.50) 

Molybdenum EPA 1638 Dissolved ug/L ND (0.50) 

Nickel EPA 1638 Dissolved ug/L ND (0.50) 

Selenium EPA 1638 Dissolved ug/L ND (2.0) 

Silver EPA 1638 Dissolved ug/L ND (0.10) 

Thallium EPA 1638 Dissolved ug/L ND (0.050) 

Vanadium EPA 1638 Dissolved ug/L ND (1.0) 

Zinc EPA 1638 Dissolved ug/L ND (0.50) 

Sample Tap Tubing Set – Equipment Blank (seven feet of #73 silicone tubing, Y-splitter, and two pieces of 5 

feet of #24 silicone tubing for sample collection for mercury and metals from sample taps) 

Aluminum EPA 1638 Total Recoverable ug/L ND (4.0) 

Antimony EPA 1638 Total Recoverable ug/L ND (0.020) 

Arsenic EPA 1638 Total Recoverable ug/L ND (0.15) 

Barium EPA 1638 Total Recoverable ug/L ND (0.20) 

Beryllium EPA 1638 Total Recoverable ug/L ND (0.060) 

Boron EPA 1638 Total Recoverable ug/L ND (3.0) 

Cadmium EPA 1638 Total Recoverable ug/L ND (0.020) 

Calcium EPA 1638 Total Recoverable ug/L ND (40) 

Chromium EPA 1638 Total Recoverable ug/L ND (0.10) 

Cobalt EPA 1638 Total Recoverable ug/L ND (0.10) 

Copper EPA 1638 Total Recoverable ug/L ND (0.10) 

Iron EPA 1638 Total Recoverable ug/L ND (10) 

Lead EPA 1638 Total Recoverable ug/L ND (0.040) 

Magnesium EPA 1638 Total Recoverable ug/L ND (2.5) 

Manganese EPA 1638 Total Recoverable ug/L ND (0.10) 

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

Molybdenum EPA 1638 Total Recoverable ug/L ND (0.060) 

Nickel EPA 1638 Total Recoverable ug/L ND (0.10) 

Selenium EPA 1638 Total Recoverable ug/L ND (0.60) 

Silver EPA 1638 Total Recoverable ug/L ND (0.020) 

Sodium EPA 1638 Total Recoverable ug/L ND (20) 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

ND – Not detected (number in parenthesis is the report limit). 

A-31 

Table A-10. Bottle Blank and Equipment Blank Analytical Data, Pleasant Prairie

Analyte Method Process Units Concentration 

Thallium EPA 1638 Total Recoverable ug/L ND (0.0050) 

Tin EPA 1638 Total Recoverable ug/L ND (0.10) 

Titanium EPA 1638 Total Recoverable ug/L ND (0.50) 

Vanadium EPA 1638 Total Recoverable ug/L ND (0.10) 

Zinc EPA 1638 Total Recoverable ug/L ND (0.20) 

Pump-Off Tubing Set – Equipment Blank (Three feet of Teflon® tubing, 10 feet of #73 silicone tubing, Ysplitter, and two pieces of 5 feet of #24 silicone tubing for total and dissolved sample collection for metals)

Aluminum EPA 1638 Total Recoverable ug/L ND (4.0) 

Antimony EPA 1638 Total Recoverable ug/L ND (0.020) 

Arsenic EPA 1638 Total Recoverable ug/L ND (0.15) 

Barium EPA 1638 Total Recoverable ug/L ND (0.20) 

Beryllium EPA 1638 Total Recoverable ug/L ND (0.060) 

Boron EPA 1638 Total Recoverable ug/L ND (3.0) 

Cadmium EPA 1638 Total Recoverable ug/L ND (0.020) 

Calcium EPA 1638 Total Recoverable ug/L ND (40) 

Chromium EPA 1638 Total Recoverable ug/L ND (0.10) 

Cobalt EPA 1638 Total Recoverable ug/L ND (0.10) 

Copper EPA 1638 Total Recoverable ug/L ND (0.10) 

Iron EPA 1638 Total Recoverable ug/L ND (10) 

Lead EPA 1638 Total Recoverable ug/L ND (0.040) 

Magnesium EPA 1638 Total Recoverable ug/L ND (2.5) 

Manganese EPA 1638 Total Recoverable ug/L ND (0.10) 

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

Molybdenum EPA 1638 Total Recoverable ug/L ND (0.060) 

Nickel EPA 1638 Total Recoverable ug/L ND (0.10) 

Selenium EPA 1638 Total Recoverable ug/L ND (0.60) 

Silver EPA 1638 Total Recoverable ug/L ND (0.020) 

Sodium EPA 1638 Total Recoverable ug/L ND (20) 

Thallium EPA 1638 Total Recoverable ug/L ND (0.0050) 

Tin EPA 1638 Total Recoverable ug/L ND (0.10) 

Titanium EPA 1638 Total Recoverable ug/L ND (0.50) 

Vanadium EPA 1638 Total Recoverable ug/L ND (0.10) 

Zinc EPA 1638 Total Recoverable ug/L ND (0.20) 

T-Splitter Tubing Set – Equipment Blank (Ten feet of #73 silicone tubing, T-splitter, six feet of #73 silicone 

tubing, and 15 feet of #73 silicone tubing for total and dissolved sample collection for metal composites)

Aluminum EPA 1638 Total Recoverable ug/L ND (4.0) 

Antimony EPA 1638 Total Recoverable ug/L ND (0.020) 

Arsenic EPA 1638 Total Recoverable ug/L ND (0.15) 

Barium EPA 1638 Total Recoverable ug/L ND (0.20) 

Beryllium EPA 1638 Total Recoverable ug/L ND (0.060) 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

ND – Not detected (number in parenthesis is the report limit). 

A-32 

Table A-10. Bottle Blank and Equipment Blank Analytical Data, Pleasant Prairie

Analyte Method Process Units Concentration 

Boron EPA 1638 Total Recoverable ug/L ND (3.0) 

Cadmium EPA 1638 Total Recoverable ug/L ND (0.020) 

Calcium EPA 1638 Total Recoverable ug/L ND (40) 

Chromium EPA 1638 Total Recoverable ug/L ND (0.10) 

Cobalt EPA 1638 Total Recoverable ug/L ND (0.10) 

Copper EPA 1638 Total Recoverable ug/L ND (0.10) 

Iron EPA 1638 Total Recoverable ug/L ND (10) 

Lead EPA 1638 Total Recoverable ug/L ND (0.040) 

Magnesium EPA 1638 Total Recoverable ug/L ND (2.5) 

Manganese EPA 1638 Total Recoverable ug/L ND (0.10) 

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

Molybdenum EPA 1638 Total Recoverable ug/L ND (0.060) 

Nickel EPA 1638 Total Recoverable ug/L ND (0.10) 

Selenium EPA 1638 Total Recoverable ug/L ND (0.60) 

Silver EPA 1638 Total Recoverable ug/L ND (0.020) 

Sodium EPA 1638 Total Recoverable ug/L ND (20) 

Thallium EPA 1638 Total Recoverable ug/L ND (0.0050) 

Tin EPA 1638 Total Recoverable ug/L ND (0.10) 

Titanium EPA 1638 Total Recoverable ug/L ND (0.50) 

Vanadium EPA 1638 Total Recoverable ug/L ND (0.10) 

Zinc EPA 1638 Total Recoverable ug/L ND (0.20) 
A-33 

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 A-11. Influent to FGD Wastewater Treatment System Field Blank, Day 1 Analytical Results, P

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
A-34 

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 A-11. Influent to FGD Wastewater Treatment System Field Blank, Day 1 Analytical Results, P

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 0.39 2 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
A-35 

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 A-12. Effluent from FGD Wastewater Treatment System Field Blank, Day 1 Analytical Results

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 NThallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 
A-36 

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 A-12. Effluent from FGD Wastewater Treatment System Field Blank, Day 1 Analytical Results

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 0.39 2 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
A-37 

ND – Not detected (number in parentheses is the quantitation limit). U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-13. Effluent from FGD Wastewater Treatment System Field Blank, Day 2 Analytical Results

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Total MetalsMercury 1631E ng/L 1 0.24 0.5 
A-38 

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

Table A-14. Effluent from FGD Wastewater Treatment System Field Blank, Day 3 Analytical Results

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Total MetalsMercury 1631E ng/L 1 0.24 0.5 
A-39 

ND – Not detected (number in parentheses is the quantitation limit). U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-15. Effluent from FGD Wastewater Treatment System Field Blank, Day 4 Analytical Results

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Total MetalsMercury 1631E ng/L 1 0.24 0.5 
Appendix B 

DATA REVIEW NARRATIVES 
Appendix C 

PICTURES FROM THE SAMPLING EPISODE 
C-1 

Figure C-1. Sampler Working Inside a “Cleanbox” 
C-2 

Figure C-2. Sample Tap and Tubing at the Influent to the FGD Wastewater Treatment 

System 
C-3 

Figure C-3. Sample Collection Set-Up at the Pump-Off Station 
C-4 

Figure C-4. Sample Tap and Tubing at the Effluent from the FGD Wastewater Treatment 

System