Final 

Sampling Episode Report 

Tampa Electric Company’s 

Big Bend Station 

Apollo Beach, FL 

Episode 6547 

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 

27 August 2008 

EPA Contract No. 68-C02-095 

Work Assignment 5-22
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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. PLANT OVERVIEW.............................................................................................................2-1 

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

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

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 ..................................................3-2 

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

3.2 List of Analytes and Sample Preservation...........................................................3-6 

3.3 Plant Operational Data.........................................................................................3-7 

3.4 Deviations from the Sampling and Analysis Plan ...............................................3-7 

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

4.1 Measured and Calculated Results for FGD Influent Samples .............................4-1 

4.2 FGD Wastewater Treatment System ...................................................................4-4 

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 .......................................................................................5-3 

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

Appendix A: ANALYTICAL RESULTS

Appendix B: ANALYTICAL DATA FOR METALS, FGD WASTEWATER

Appendix C: DATA REVIEW NARRATIVES

Appendix D: FGD WASTEWATER TREATMENT SYSTEM FLOW RATE DATA

Appendix E: PICTURES FROM THE SAMPLING EPISODE
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LIST OF TABLES 

Page 

2-1 Big Bend NPDES Monitoring Requirements for the FGD Effluent (I-130) ................... 2-6 

3-1 Sample Collection Information, Big Bend....................................................................... 3-9 

3-2 Number of Samples Collected by Sampling Point, Big Bend ....................................... 3-10 

3-3 Field Measurements, Big Bend...................................................................................... 3-11 

3-4 Analytical Methods and Procedures for Samples Collected at Big Bend...................... 3-12 

3-5 Summary of Sample Container and Planned Preservation ............................................ 3-13 

3-6 Sample Preservation Summary, Big Bend..................................................................... 3-14 

3-7 Generating Unit Operating Characteristics during Sample Collection, Big Bend......... 3-15 

3-8 FGD Scrubber System Operating Characteristics, Big Bend ........................................ 3-16 

3-9 FGD Wastewater Treatment System Operating Characteristics, Big Bend .................. 3-17 

4-1 Biphasic Sample Results for Low-Level Total Metals and Routine Total Metals 

Measured Above the Report Limit, FGD Influent, Big Bend.......................................... 4-5 

4-2 Biphasic Sample Results for Routine Total Mercury, FGD Influent, Big Bend ............. 4-6 

4-3 Biphasic Sample Results for Classical Analytes Measured Above the Report Limit, 

FGD Influent, Big Bend................................................................................................... 4-6 

4-4 Classical Pollutants Measured Above the Report Limit for the FGD Wastewater 

Treatment System, Big Bend ........................................................................................... 4-6 

4-5 Metals Measured Above the Report Limit for the FGD Wastewater Treatment 

System, Big Bend............................................................................................................. 4-7 

5-1 Field Blank Results Measured Above the Report Limit, Big Bend................................. 5-4 

5-2 Field Duplicate Results, Big Bend................................................................................... 5-5 

A-1 FGD Influent Analytical Data, Big Bend ....................................................................... A-1 

A-2 ProChem Biphasic Filtration Blank Analytical Results, Big Bend ................................ A-9 

A-3 FGD Effluent Analytical Data, Big Bend..................................................................... A-10 

A-4 Duplicate of FGD Effluent Analytical Data, Big Bend ................................................ A-15 

A-5 Bottle Blank and Equipment Blank Analytical Data, Big Bend................................... A-19 
LIST OF TABLES (Continued) 

Page 

iii

A-6 FGD Influent Field Blank Analytical Data, Big Bend.................................................. A-24 

A-7 FGD Effluent Field Blank Analytical Data, Big Bend ................................................. A-25 

B-1 Analytical Results for Metals in the FGD Wastewater Treatment System, Big Bend ....B-1 

D-1 Flow Data during FGD Wastewater Treatment Effluent Sample Collection, Big 

Bend ................................................................................................................................ D-1 

D-2 Flow Data during FGD Wastewater Treatment Influent Sample Collection, Big 

Bend ................................................................................................................................ D-5 
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LIST OF FIGURES 

Page 

2-1 FGD Wastewater Treatment System, Big Bend Power Plant.......................................... 2-7 

E-1 Sampler Working Inside a “Cleanbox”............................................................................E-1 

E-2 Three-Way Splitter at the Influent to FGD Wastewater Treatment System....................E-2 

E-3 Sampling Set Up at the Influent to FGD Wastewater Treatment System (SP-1) ............E-3 

E-4 Pump-Off Station for Dissolved Metals Sample Collection............................................E-4 

E-5 Collection of Dissolved Metals Samples at Pump-Off Station........................................E-5 

E-6 Three-Way Splitter at the Effluent from FGD Wastewater Treatment System...............E-6 

E-7 Sampling Set Up at Effluent from FGD Wastewater Treatment System (SP-2).............E-7 

E-8 Field Blank Collection at Effluent from FGD Wastewater Treatment (SP-5).................E-8 
1-1

1. INTRODUCTION

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

Agency (EPA) has been conducting a program that consists of site visits and sampling at steam 

electric power plants. The purpose of this program is to characterize raw wastewaters generated 

by coal-fired steam electric power plants, as well as to evaluate treatment technologies and best 

management practices used to reduce pollutant discharges. This Sampling Episode Report (SER) 

describes the sampling activities that took place on July 24 through July 26, 2007 at Tampa 

Electric Company’s Big Bend Station (Big Bend), located in Apollo Beach, Florida (Sampling 

Episode 6547). The focus of Episode 6547 was to characterize the influent to and effluent from 

the flue gas desulfurization (FGD) wastewater treatment system at Big Bend. 

1.1 Background of Detailed Study

 Section 304(m) of the Clean Water Act (CWA) requires EPA to develop and publish a 

biennial plan that establishes a schedule for the annual review and revision of national effluent 

limitations guidelines and standards (ELGs) required by CWA section 304(b). During EPA’s 

2005/2006 review of ELGs, EPA determined that the steam electric power generating point 

source category (40 CFR Part 423) was the second-largest discharger of toxic-weighted 

pollutants. EPA’s analyses indicated that the toxic-weighted loadings were predominantly driven 

by metals present in wastewater discharges, and that the waste streams contributing the majority 

of the metals are associated with air pollution controls. Other potential sources of metals include 

coal pile runoff, metal/chemical cleaning wastes, coal washing, and certain low-volume wastes. 

 In the 2005/2006 study, EPA noted certain data limitations that affected the Agency’s 

estimate of the potential hazards posed by discharges from this category. Therefore, EPA 

determined that further review of these discharges during the 2007/2008 ELG planning cycle 

was warranted. EPA has concentrated its efforts for the 2007/2008 study on better characterizing 

the sources generating the pollutants responsible for the majority of the toxic-weighted pollutant 

loadings and available pollution control technologies/practices for steam electric plants. 

1.2 Power Plant Site Selection

 EPA selected six coal-fired steam electric plants for wastewater sampling. EPA based the 

plant selection on the process configurations and characteristics of the plants, as well as the site 

visits conducted for the study. The following characteristics (not listed in any priority order) 

were used to select plants for sampling: 

• Coal-fired boilers; 

• Wet FGD scrubber system, including: 

— Type of scrubber, 

— Sorbent used, 

— Year operation began, 

— Chemical additives used, 

— Forced oxidation process, 

— Water cycling, and 

— Solids removal process; 
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• FGD wastewater treatment system; 

• Type of coal; 

• NOx controls; 

• Ash handling systems; 

• Ash treatment system; and 

• Mercury air controls. 

 EPA selected Big Bend for sampling based on the following site characteristics: 

• The plant is a coal-fired power plant that burns eastern bituminous coal in all four 

units; 

• The plant operates two wet FGD systems (each system services two units), which 

are both limestone forced oxidation systems; 

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

includes the following steps: 

— pH adjustment, 

— Ferric chloride addition, 

— Polymer addition, 

— Clarification, and 

— Filtration; 

• The plant recently began the operation of a selective catalytic reduction (SCR) 

system on one of its units; and 

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

1.3 Sampling Episode Overview

 On April 27, 2007, EPA and its technical contractor, Eastern Research Group, Inc. 

(ERG), conducted a site visit at Big Bend. The purpose of the site visit was to learn about the 

wastewater treatment operations, regarding the FGD scrubber purge, and to gather information in 

order to collect wastewater samples at Big Bend. Information collected during the site visit was 

used to create Sampling Plan, Tampa Electric Company’s Big Bend Station (Sampling Plan) [1], 

which describes the sample collection procedures used during the sampling episode. 

 For this sampling episode, EPA arrived at Big Bend on Tuesday, July 24, 2007, to review 

the sampling points, determine the set-up for the sample collection, label sample bottles, and 

purchase any additional supplies needed for the sampling episode. EPA then collected the 

samples specified in the Sampling Plan on Wednesday, July 25, 2007. The following personnel 

participated in EPA’s sample collection activities: 

• Ron Jordan, EPA/EAD; 

• Josh Hall, EPA/EAD; 

• Karrie-Jo Shell, EPA/Region IV; 

• TJ Finseth, ERG; 
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• Sarah Holman, ERG; and 

• Jessica Wolford, ERG. 

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

Group (UWAG), acting on behalf of the plant. 
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2. PLANT OVERVIEW

 The Big Bend Station operates four coal-fired steam electric generating units. Units 1 and 

2 are wet bottom turbo furnace boilers, each with a capacity of 445 megawatts (MW). These 

units came on line in 1970 and 1973, respectively. Unit 3 is a wet bottom turbo furnace boiler 

which has a capacity of 465 MW, and came on line in 1976. Finally, Unit 4 is a dry bottom 

tangentially-fired boiler which has a capacity of 485 MW, and came on line in 1985. The Big 

Bend Station is located in Apollo Beach, Florida, along the Tampa Bay. 

 Big Bend burns eastern bituminous coal in all four units. Historically, the coal used in 

Units 1, 2, and 3 was mined in Kentucky and the coal used in Unit 4 was Illinois Number 6. 

Currently, Units 1-4 burn all Kentucky coal. Big Bend burns approximately four to five million 

tons of coal per year, which is equivalent to about 450 to 570 tons per hour. In addition to 

burning coal in the boilers, Big Bend is permitted to burn a blend of coal and petroleum coke, up 

to 20 percent petroleum coke; however, the plant typically burns about one to two percent 

petroleum coke, with a maximum of five percent. During the sample collection period, no 

petroleum coke was being burned in the boilers. 

 Units 1 through 4 have the following configuration: 

• Boiler; 

• SCR system (Unit 4 only); 

• Ammonia injection for sulfur trioxide (SO3) control (Unit 4 only); 

• Electrostatic precipitator (ESP); and 

• FGD system. 

 Big Bend recently completed the addition of the Unit 4 SCR system, which began 

operation in May 2007, and is in the process of installing SCRs for each of the other three units. 

SCRs are used to control nitrogen oxide (NOx) emissions. The plant intends to install one new 

SCR each year until all four units have SCRs, with an estimated completion date of May 2010. 

Once the SCRs are installed on all units, Big Bend will operate the systems year round. The plant 

estimates that after all four SCRs are in operation, the plant’s NOx emissions will be reduced by 

89 percent, compared to 1998 levels. The SCR operation produces no direct industrial 

wastewater discharges but by altering the characteristics of the flue gases it can affect FGD 

wastewater pollutant characteristics. 

 During the operation of the SCR systems, some of the sulfur dioxide (SO2) in the flue gas 

is oxidized to SO3 over the SCR catalyst. The SO3 in the flue gas causes a blue plume; therefore, 

Big Bend attempts to remove the SO3 from the flue gas. Big Bend injects anhydrous ammonia 

directly into the flue gas to react with the SO3 and produces ammonium sulfate which is a solid 

particle. Most of the ammonium sulfate is expected to be removed from the flue gas by the ESPs. 

Big Bend intends to add excess ammonia to the flue gas to ensure a complete reaction of the SO3

in the flue gas. Some of the ammonia added to the flue gas is expected to adhere to the fly ash 

particulates and be removed by the ESPs. In addition, this excess ammonia may be removed 

from the flue gas in the FGD system, thereby affecting the wastewater characteristics of the FGD 

purge stream. 
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 The ESPs at Big Bend are particulate control devices that remove the fly ash and other 

particulates from the flue gas. The ESPs remove approximately 99.5 percent of the particulates in 

the flue gas. The fly ash and other particulates are collected in hoppers and pneumatically 

conveyed to storage silos. Prior to the installation of the Unit 4 SCR, Big Bend sold 

approximately 99 percent of the fly ash produced on site. Now that Big Bend is operating the 

SCR on Unit 4 and injecting ammonia into the flue gas for SO3 control, ammonia adheres to the 

fly ash produced by Unit 4; therefore, Big Bend is installing a fly ash beneficiation plant that will 

strip the ammonia from the fly ash and return it back to the plant. In addition, the system will 

separate the ash from the unburned carbon with an electrostatic system. This fly ash 

beneficiation plant is expected to be operating in April 2008. The ESP operation produces no 

direct industrial wastewater discharges. 

 Big Bend operates two FGD systems, which are used to control sulfur dioxide (SO2) 

emissions from all four of the generating units. One of the FGD systems scrubs the flue gas for 

Units 1 and 2, and the other FGD system scrubs the flue gas for Units 3 and 4. The plant installed 

the FGD system on Unit 4 in 1985. However, in 1995, Big Bend retrofitted the system and began 

scrubbing the flue gas from Unit 3 in the same FGD system. Big Bend also installed a FGD 

system for Units 1 and 2 in 2000. Plant personnel estimate that the addition of the FGD system 

for Units 1 and 2 reduces Big Bend’s SO2 emissions by approximately 89 percent, as compared 

to 1998 levels. 

 The wastewater generated from the FGD scrubber systems is treated on site prior to 

discharge to Tampa Bay. In 2000, when Big Bend installed the FGD system on Units 1 and 2, 

the plant also installed a FGD wastewater treatment system to treat the wastewater purge stream 

(the purge stream is needed to remove chlorides from the FGD systems to keep the system below 

30,000 mg/L chlorides). Section 2.1 discusses the FGD scrubber systems and Section 2.2 

discusses the FGD wastewater treatment system. 

2.1 FGD Scrubber System

 Big Bend has two different FGD scrubber systems, one for Units 1 and 2 (“Unit 1&2”), 

and one for Units 3 and 4 (“Unit 3&4”); however, there are some similarities between the two 

different systems. Both systems use a limestone slurry as the sorbent, both are forced oxidation 

systems, and both use dibasic acids (DBA) as additives in the systems. 

 The limestone used in both FGD systems is conveyed to three individual day silos for 

storage, which feed three different ball mills. Each of the three ball mills pulverizes the 

limestone to the same size and consistency. From the ball mills, the limestone slurry is sent to a 

hydroclone that separates the larger limestone particles from the smaller particles. The particles 

that are too large to be sent to the absorber are returned to the ball mill for further processing and 

all other particles are sent to a splitter box that splits the feed for the Unit 1&2 FGD system and 

the Unit 3&4 FGD system. Each FGD system has its own limestone reagent feed tank that holds 

limestone to be sent to the absorber systems. 

 The Unit 3&4 FGD system consists of four double loop, spray/tray absorber towers. 

Initially, only three of the four towers operated at any given time, with the fourth as a spare; 

however, once the plant began scrubbing Unit 3 flue gas in the system, they began operating all 

four towers continuously. Big Bend adds DBA to the limestone reagent feed tank to increase the 
2-3

sulfur dioxide removal from the system; therefore, all the limestone slurry that is sent to the 

absorber contains DBA. The plant adds limestone slurry to the absorbers to keep the pH of the 

scrubber lower loop at approximately 4.2 and the upper loop at approximately 6.0. 

 The Unit 1&2 FGD system was installed in 2000. It consists of one single loop spray/tray 

tower that is 60 feet in diameter and 60 feet tall, with forced oxidation. The absorber tower holds 

approximately 1.3 million gallons of slurry and is one of the largest scrubbers in the United 

States. Big Bend feeds the limestone slurry to the absorbers to keep the pH of the scrubber 

between 5 and 6. In addition, the plant manages the blowdown from the scrubber to maintain the 

scrubber slurry at approximately 20 percent solids (by weight) in the scrubber. 

 The blowdown from the Unit 1&2 scrubber is pumped directly to primary hydroclones. 

The blowdown from the Unit 3&4 scrubber is pumped to quencher blowdown tanks and then 

pumped to a separate set of primary hydroclones. The blowdown from the scrubbers is 

approximately 20 percent solids. The underflow from both of the primary hydroclones is 

transported to the sludge surge tank and contains approximately 50 to 55 percent solids. From the 

sludge surge tank, the gypsum is pumped to rotary drum vacuum filters. As the gypsum is 

transferred to the vacuum filters, it is washed with Sun City Sewage Treatment Plant effluent 

water to reduce the level of chlorides in the gypsum. The rotary drum vacuum filters dry the 

solids to approximately 90 percent solids gypsum product. The gypsum produced by the plant is 

transported to the National Gypsum wallboard manufacturing plant adjacent to Big Bend. 

 The overflows from the two sets of primary hydroclones, which are approximately 6 

percent solids, are combined in the chloride purge feed tank. Most of this wastewater is 

transferred to the return water tank and recycled back to the Unit 1&2 scrubber; however, some 

of the wastewater is pumped to a secondary hydroclone. The underflow from the secondary 

hydroclone is recycled back to the Unit 1&2 scrubber and the overflow (i.e., scrubber purge) is 

transferred to the FGD wastewater treatment system. 

2.2 FGD Wastewater Treatment System

 The overflow from the secondary hydroclones enters the FGD wastewater treatment 

system continuously during normal operations with a fairly consistent flow rate of approximately 

200 to 225 gpm, a solids concentration of approximately 1 to 3 percent solids, and a chlorides 

concentration which varies between 15,000 to 30,000 ppm. When the equalization tank reaches 

high levels, the plant will divert the FGD scrubber purge away from the equalization tank by 

sending it to the return water tank. The Big Bend FGD wastewater treatment system contains the 

following operations: 

• Equalization tank; 

• pH adjustment (lime addition); 

• Ferric chloride addition; 

• Mixing tank; 

• Flocculating polymer addition; 

• Clarification; 

— Overflow to pH adjustment (hydrochloric acid addition); 

— Underflow to filter press; and 

• Filtration. 
2-4

Big Bend estimates that the maximum flow rate from the equalization tank through the 

wastewater treatment system is approximately 230 gpm, with a total equalization tank residence 

time of approximately 8 to 9 hours. Figure 2-1 presents a process flow diagram of the FGD 

wastewater treatment system, as well as the sampling locations for EPA’s sampling episode. Big 

Bend estimates that the residence time of the entire FGD wastewater treatment system (including 

the equalization tank) is approximately 24 to 32 hours. The flow rate entering the wastewater 

treatment system during the sampling episode was approximately 250 gpm; however, 154 gpm 

was off-specification filter press filtrate (with pollutant characteristics similar to treated effluent) 

and only 96 gpm consisted of scrubber purge from the secondary hydroclones. 

 According to Big Bend personnel, the plant controls the level in the equalization tank to 

prevent the tank from overfilling. When the level in the tank reaches high levels, the plant diverts 

the scrubber purge from the secondary hydroclones away from the equalization tanks and 

transfers it to the FGD scrubbers via the return water tank. Because the plant was transferring 

154 gpm of off-specification filter press filtrate to the equalization tank, the plant diverted some 

of the scrubber purge away from the equalization tank and therefore, the 96 gpm of scrubber 

purge is a lower than normal flow rate. When the filter press filtrate meets the turbidity 

specifications, it is transferred to the treated water transfer tank and discharged from the system. 

 The secondary hydroclone overflow is transferred directly to the equalization tank. The 

equalization tank also receives effluent from the treatment system if it did not meet the plant’s 

permit limits and wastewater from the filtrate sump. The filtrate sump wastewater consists of 

filter backwash from the sand filters, off-specification filter press filtrate, wash water from 

polymer storage containers, fume scrubber wastewater from the muriatic acid tank, and 

occasionally material from the sludge storage tank during maintenance. Big Bend typically 

transports the filtrate sump wastewater to the equalization tank 5 times a day at a flow rate of 170 

gpm for approximately 200 minutes per day. 

 The wastewater, at a pH of approximately 6.0, flows from the equalization tank to 

reaction tank 1, where Big Bend adds hydrated lime to raise the pH of the wastewater to 9.0, 

which facilitates heavy metals precipitation. The reaction tank is equipped with an agitator to 

effect rapid mixing and has an average residence time of 60 minutes. 

 From reaction tank 1, the wastewater flows to reaction tank 2, where Big Bend adds 

ferric chloride. The ferric chloride produces iron oxyhydroxide, which causes coprecipitation of 

other trace elements in the water. The overflow from reaction tank 2 is transferred to reaction 

tank 3, which provides low shear agitation. The mixing of the wastewater provides an 

environment to build floc particles to settle in the clarifiers. 

 From reaction tank 3, the wastewater is transferred to the clarifier. A flocculating 

polymer is added to the clarifier feed pump discharge. The primary clarifier, which was added 

after the initial design of the treatment system, is capable of handling all of the wastewater in the 

FGD wastewater treatment system. The two secondary back-up clarifiers are from the original 

design of the FGD wastewater treatment plant and can each handle 50 percent of the wastewater. 

When the primary clarifier was added to the system, Big Bend began using the two secondary 

clarifiers as back-ups; therefore, the plant uses the secondary back-up clarifiers when necessary 

(i.e., during maintenance of the primary clarifier). All three of the clarifiers are designed to have 
2-5

an overflow stream with a maximum TSS level of 100 mg/L and an underflow slurry of 5 to 10 

percent solids. During the sampling episode, the secondary clarifiers were not operating. 

 The overflow from the clarifiers are commingled and transferred to sand gravity filters. 

As the wastewater is pumped to the gravity filters, the plant adds hydrochloric acid to the 

wastewater to ensure the pH is between 6.0 and 9.0. The gravity filters are designed to produce a 

filtrate stream having less than 5 mg/L TSS. The plant continuously backwashes the filters and 

the wastewater from the backwash is transferred to the filtrate sump. 

 From the gravity filters, the wastewater is transferred to the treated water transfer tank 

and discharged from the plant. The plant has the capability to recycle the treated water back to 

the equalization tank if the treated water does not meet the plant’s limits. The discharge from the 

treated water transfer tanks is based on level control; therefore, if the tank is less than 30 percent 

full, the system will not discharge from the treated water transfer tank. The plant commingles the 

effluent from the FGD wastewater treatment system (i.e., treated water transfer tank) with the 

plant’s once-through cooling water prior to discharge. During the sampling episode, the average 

effluent discharge from the FGD wastewater treatment system (prior to commingling with 

cooling water) was approximately 104 gpm; however, the discharge flow rate varied widely 

during the episode, ranging from 2.44 gpm to 253 gpm. 

 The underflow from all three clarifiers is transferred to the sludge storage tank. Big Bend 

dewaters the sludge by pumping it through one of two filter presses. The filter cake is stored on 

site and sold as a by-product. The filtrate is transferred to the treated water tank or to the filtrate 

sump if it does not meet plant specifications. Table 2-1 presents Big Bend’s NPDES permit 

requirements for their internal monitoring point of the effluent from the FGD wastewater 

treatment system, shown as I-130 on Figure 2-1. 

 EPA collected a sample of the influent to Big Bend’s FGD wastewater treatment system 

after the equalization tank, but prior to reaction tank 1 and any chemical addition. EPA also 

collected a sample of the effluent from Big Bend’s FGD wastewater treatment system after the 

treated wastewater effluent tank, but prior to the wastewater commingling with the once-through 

cooling water. 
2-6

Table 2-1. Big Bend NPDES Monitoring Requirements for the FGD Effluent (I-130) 

Parameter 

Daily 

Minimum 

Daily 

Maximum 

Monthly 

Average 

Sample 

Frequency 

Sample 

Type 

Total Suspended Solids NA 30 mg/L NA Quarterly Grab 

Oil & Grease NA 15 mg/L NA Quarterly Grab 

pH 6.0 s.u. 9.0 s.u. NA Quarterly Grab 

Arsenic, Total Recoverable Report (ug/L) Quarterly Grab 

Chromium, Total Recoverable Report (ug/L) Quarterly Grab 

Copper, Total Recoverable Report (ug/L) Quarterly Grab 

Lead, Total Recoverable Report (ug/L) Quarterly Grab 

Mercury, Total Recoverable Report (ug/L) Quarterly Grab 

Nickel, Total Recoverable Report (ug/L) Quarterly Grab 

Selenium, Total Recoverable Report (ug/L) Quarterly Grab 

Alpha, Gross Particle Activity Report (PCI/L) Quarterly Grab 

Radium 226 + Radium 228, Total Report (PCI/L) Quarterly Grab 

Flow Rate Monitor (MGD) Continuous Recorder 

NA – Not applicable. 
2-7 

Figure 2-1. FGD Wastewater Treatment System, Big Bend Power Plant 
3-1

3. SAMPLE COLLECTION

 During the Big Bend sampling episode, the sampling team followed the sample 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 described in the Sampling Plan. 

 During the sampling episode, Unit 3 was shut down due to high opacity readings from the 

unit’s ESP. The unit was shut down on Monday, July 23, 2007 and the sampling occurred on 

Wednesday, July 25, 2007. For more details about the Unit 3 shut down, see Section 3.3. In 

addition, during the sampling episode, the plant was transferring off-specification filter press 

filtrate to the FGD wastewater treatment equalization tank, which caused the plant to transfer 

less of the secondary hydroclone overflow to the FGD wastewater treatment system. During the 

sampling episode 154 gpm of off-specification filter press filtrate and 96 gpm of scrubber purge 

were entering the equalization tank. 

3.1 Sampling Points, Sample Collection Methods, and Field Measurements

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

field measurements obtained for this sampling episode. Additional details are available in 

Section 3 of the Sampling Plan. Figure 2-1 presents a flow diagram of the plant including 

sampling point locations. 

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

collection, sample collection dates and times, and the EPA Sample Control Center (SCC) sample 

numbers. Table 3-2 lists the sampling point numbers and descriptions, the number of samples 

collected, and the pollutant parameters analyzed for this sampling episode. Table 3-3 presents the 

field measurement data collected from each sampling point. 

 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-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 SP-1, SP-2, and SP-3, EPA collected split samples with Big Bend’s representative. 

Prior to the sampling episode, Big Bend personnel installed three-way splitters on the sampling 

taps at the two sampling locations, which allowed for split sample collection. The low-level and 

routine total metals and the classical pollutants were collected as “true” splits (i.e., samples for 

the same analyte were collected simultaneously); however, the low-level and routine dissolved 

metals samples were collected as “multipour” splits, due to difficulties collecting split samples 

through a filter. The “multipour” splits were collected by the following procedure: one-third of 

the EPA sample bottle was filled and then one-third of the “split” bottle was filled. The EPA 

sample bottle and the “split” sample bottle were each in turn then filled with an additional one-
3-2

third sample. Finally, the EPA sample bottle was filled completely and then the “split” bottle was 

filled completely. 

 The field blank samples (SP-4 and SP-5) for the low-level and routine total metals 

samples were not collected as split samples between EPA and Big Bend’s representative. These 

samples were collected using separate blank water and separate tubing. The field blank samples 

for the low-level and routine dissolved metals samples were collected using the “multipour” 

approach, as described previously. For a description of the field blank sample collection 

procedures, see Section 5.2.3. 

 At each of the five sampling points, EPA collected low-level metals sample fractions 

following EPA Method 1669 collection protocols. To collect low-level metals samples, EPA 

donned Tyvek® suits and dust masks (dust masks were worn until all low-level 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 with “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 it 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 E-1, in Appendix E, is a picture of a sampler working inside a 

“cleanbox.” To collect samples, EPA placed the sample bottles and the 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 and closed the sample bottle 

lid and inner bag as quickly as possible within the “cleanbox.” The sample bottles were then 

placed into the outer bag following the “clean hands / dirty hands” protocols. 

3.1.1 Influent to FGD Wastewater Treatment 

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

tap located along the wastewater piping after the equalization tank, but prior to reaction tank 1. 

The sample tap was connected to the top of the pipe on the suction side of the pump from the 

equalization tank. Figure 2-1 identifies the sampling location for SP-1. This sample was 

collected as a grab sample, because the batch discharges from the gypsum dewatering process 

were equalized prior to sample collection and therefore, were expected to be fairly homogenous. 

 During the sample collection at the influent to the FGD wastewater treatment system, the 

sampling team covered the area around the sampling point with tarps to block the sun and cover 

the samplers in case of rain. There was no rain during the sample collection period; however, 

there was a periodic light mist that fell from the return water tank located next to the sampling 

point. There was also a strong wind blowing at the backs of the samplers during portions of the 

sample collection. 

 Prior to collecting samples at the influent to the FGD wastewater treatment system 

(SP-1), the sampling team collected field blanks (SP-4) for low-level total metals and low-level 

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

at the influent to the FGD wastewater treatment system. 
3-3

 EPA collected the wastewater samples at the influent to the FGD wastewater treatment 

system by attaching a 5-foot length of silicone tubing to one of the fittings on the three-way 

splitter at the sample location (Big Bend’s representative attached an identical piece of silicone 

tubing to one of the other fittings). Figure E-2, in Appendix E, is a picture of the three-way 

splitter attached to the sample tap at the influent to the FGD wastewater treatment system 

sampling point. The samplers opened the valves of the sample tap and allowed the sample to 

purge the tubing for four minutes. After the samplers opened the valve to the sampling tap, the 

valve was left open and the flow from the tap did not stop until all samples were collected 

(except HEM/SGT-HEM and the dissolved metals samples). 

 After the four-minute purge time had elapsed, the samplers filled two 10-liter containers 

with sample, which were later used to pump off the low-level and routine dissolved metals 

sample fractions. After filling the 10-liter containers, a member of the sampling team transported 

the two 10-liter containers to the FGD laboratory to allow the solids in the wastewater to settle 

while the remainder of the sampling team stayed at the sample point and continued sample 

collection. Figure E-3, in Appendix E, is a picture of the sampling set-up at the influent to the 

FGD wastewater treatment system. 

 The samplers then collected the low-level total metals, low-level total mercury, low-level 

dissolved mercury, and arsenic/selenium speciation samples in a “cleanbox,” as described in 

Section 3.1. The samplers then collected routine total metals, BOD, Group I, and Group II 

samples by pouring the sample directly from the tubing into the sample bottles without the use of 

a “cleanbox.” To collect the HEM/SGT-HEM samples, the samplers shut off the valve for the 

sample tap, removed the tubing from the fitting, reopened the valve, and filled the sample bottles 

directly from the tap to prevent any oil and grease adhering to the sides of the tubing. 

 During the sample collection, the sampling team collected an aliquot of sample for field 

testing. Sample pH and temperature were measured immediately at the sampling point using a 

pH meter and four-color pH paper. The four-color pH paper was used as an independent check of 

the pH meter to ensure that similar results were measured. After returning to the staging area, the 

sampling team took measurements of free and total residual chlorine using a colorimeter. 

Table 3-3 presents the field measurement data for the influent to the FGD wastewater treatment 

system. The samplers noted that the field test jar was initially cloudy and had a brownish-gray 

appearance when collected. The solids in the sample settled after approximately four minutes, 

leaving a one inch layer at the bottom of the jar. In addition, after the solids settled, the aqueous 

portion of the samples was yellowish in color. 

 The sampling team then moved to the FGD laboratory, where a pump-off station was set 

up, to collect the low-level and routine dissolved metals samples. The pump-off station consisted 

of a length of Teflon® tubing attached to a length of silicone tubing, which was threaded through 

a peristaltic pump. The samplers connected a capsule filter to the end of the silicone tubing. 

Figures E-4 and E-5, in Appendix E, are pictures of the set-up of the pump-off station. Prior to 

collecting any dissolved wastewater samples, the samplers collected a field blank sample (SP-4) 

for low-level dissolved metals. See Section 5.2.3 for a description of the dissolved metals field 

blank sample collection at the influent to the FGD wastewater treatment system. 

 After collecting the field blank samples, the samplers transferred the end of the Teflon® 

tubing into one of the 10-liter containers filled with wastewater from the influent to the FGD 
3-4

wastewater treatment system. By this time, the solids in the wastewater had been settling for 

approximately 1.5 hours (the 10-liter containers had been filled approximately 2 hours earlier), 

and there was approximately a one inch layer of solids at the bottom of the container. 

 The samplers first purged the tubing and filter with approximately 600 mL of sample and 

then collected the routine hexavalent chromium sample, which was collected first because it was 

the only other sample that needed to be preserved prior to shipment. After collecting the routine 

hexavalent chromium sample, the samplers switched capsule filters, purged the new filter with 

approximately 500 mL of sample, and collected the low-level dissolved metals sample. The 

samplers then transferred the end of the Teflon® tubing into the second of the 10-liter containers, 

switched the capsule filter, and purged the tubing and filter with approximately 600 mL of 

sample. Finally, the sampling team collected the routine dissolved metals sample. 

3.1.2 Effluent from FGD Wastewater Treatment 

 The effluent from the FGD wastewater treatment system (SP-2) was collected from a 

sample tap located along the wastewater piping after the treated wastewater effluent tank, but 

prior to commingling with the once-through cooling water. Figure 2-1 identifies the sampling 

location for SP-2. 

 During the sample collection at the effluent from the FGD wastewater treatment system, 

the sampling team covered the area around the sampling point with tents and tarps to block the 

sun and cover the samplers in case of rain. There was no rain during the sample collection 

period. 

 Prior to collecting samples at the effluent from the FGD wastewater treatment system 

(SP-2), the samplers collected field blanks (SP-5) for low-level total metals, low-level total 

mercury, and routine total metals. See Section 5.2.3 for a description of the field blank sample 

collection at the effluent from the FGD wastewater treatment system. 

 EPA collected the wastewater samples at the effluent from the FGD wastewater treatment 

system by attaching a 5-foot length of silicone tubing to one of the fittings on the three-way 

splitter at the sample location (Big Bend’s representative attached an identical piece of silicone 

tubing to one of the other fittings). Figure E-6, in Appendix E, is a picture of a sampler attaching 

the silicone tubing to the three-way splitter. The samplers opened the valves of the sample tap 

and allowed the sample to purge the tubing for 3 minutes. After the samplers opened the valve to 

the sampling tap, the valve was left open and the flow from the tap did not stop until all samples 

were collected (except HEM/SGT-HEM and the dissolved metals samples). Figure E-7, in 

Appendix E, is a picture of the sampling set-up at the effluent from the FGD wastewater 

treatment system. 

 After the three-minute purge time had elapsed, the samplers began collecting the lowlevel total metals samples in a “cleanbox,” as described in Section 3.1. The samplers collected 

low-level total metals, low-level total mercury, and low-level dissolved mercury, as well as the 

field duplicates and QC samples for each of the analytes, and the arsenic/selenium speciation 

samples. Then the samplers filled three 10-liter containers with sample, which were later used to 

pump off the low-level and routine dissolved metals sample fractions. After filling the 10-liter 

containers, a member of the sampling team transported the three containers to the FGD 
3-5

laboratory while the remainder of the sampling team stayed at the sample point and continued 

sample collection. 

 During the sample collection, the sampling team collected an aliquot of sample for field 

testing. Sample pH and temperature were measured immediately at the sampling point using a 

pH meter. After returning to the staging area, the samplers took measurements of free and total 

residual chlorine using a colorimeter. Table 3-3 presents the field measurement data for the 

effluent from the FGD wastewater treatment system. The samplers noted that the sample was 

clear with a yellowish color. 

 The samplers then collected the routine total metals, BOD, Group I, and Group II 

samples, as well as the field duplicates and QC samples for each analyte, by pouring the sample 

directly from the tubing into the sample bottles without the use of a “cleanbox.” To collect the 

HEM/SGT-HEM samples, the samplers shut off the valve for the sample tap, removed the tubing 

from the fitting, reopened the valve, and filled the HEM/SGT-HEM and HEM/SGT-HEM QC 

sample bottles directly from the tap to prevent any oil and grease adhering to the sides of the 

tubing. 

 The sampling team then moved to the FGD laboratory, where a pump-off station was set 

up, to collect the low-level and routine dissolved metals samples. The pump-off station consisted 

of a length of Teflon® tubing attached to a length of silicone tubing, which was threaded through 

a peristaltic pump. The samplers connected a capsule filter to the end of the silicone tubing. 

Figures E-4 and E-5, in Appendix E are pictures of the set-up of the pump-off station. Prior to 

collecting any dissolved wastewater samples, the samplers collected a field blank sample (SP-5) 

for low-level dissolved metals, low-level hexavalent chromium, routine dissolved metals, and 

routine hexavalent chromium. See Section 5.2.3 for a description of the dissolved metals field 

blank sample collection at the effluent to the FGD wastewater treatment system. 

 After collecting the field blank samples, the samplers transferred the end of the Teflon® 

tubing into one of the 10-liter containers filled with wastewater from the effluent to the FGD 

wastewater treatment system. By this time, the effluent sample had been sitting for 

approximately two hours. 

 The samplers first purged the tubing and filter with approximately 1 liter of sample, after 

which, the samplers collected the low-level dissolved metals sample. Due to the back pressure in 

the filter, the samplers switched to a new capsule filter. The samplers then purged the new filter 

with approximately 1 liter of sample and collected the low-level dissolved metals field duplicate 

and QC samples. The samplers then transferred the end of the Teflon® tubing into the second of 

the 10-liter containers, switched the capsule filter, purged the tubing and filter with 

approximately 1 liter of sample, and collected the low-level hexavalent chromium sample, as 

well as the field duplicate and QC samples. The samplers then switched to a new capsule filter 

and purged the new filter with approximately 1 liter of sample, after which, the samplers 

collected the routine dissolved metals sample. Then the samplers transferred the end of the 

Teflon® tubing into the third of the 10-liter containers, switched the capsule filter, purged the 

tubing and filter with approximately 1 liter of sample, and collected the routine dissolved metals 

field duplicate and QC samples. Finally, the samplers switched the capsule filter, purged the new 

filter with approximately 1 liter of sample, and collected the routine dissolved hexavalent 

chromium sample, as well as the field duplicate and QC samples. 
3-6

3.2 List of Analytes and Sample Preservation

 Analytes in EPA’s Big Bend sampling episode included those in the following classes of 

pollutants: 

• Classicals: 

— Biochemical oxygen demand, 5-day (BOD5), 

— Total suspended solids (TSS), 

— Total dissolved solids (TDS), 

— Sulfate, 

— Chloride, 

— Total Kjeldahl nitrogen (TKN), 

— Ammonia as nitrogen, 

— Nitrate/nitrite as nitrogen, 

— Total phosphorus, 

— Hexane extractable material (HEM), and 

— Silica-gel treated hexane extractable material (SGT-HEM); and 

• Metals: 

— Routine total metals (27 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, yttrium, and zinc), 

— Routine dissolved metals (27 metals), 

— Routine hexavalent chromium, 

— Low-level total mercury, 

— Low-level dissolved mercury, 

— Low-level hexavalent chromium, 

— Low-level total metals (11 metals: antimony, arsenic, cadmium, 

chromium, copper, lead, nickel, selenium, silver, thallium, zinc), and 

— Low-level dissolved metals (11 metals). 

 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 3-4 lists the analytical methods used to determine pollutant 

concentrations. 

 Table 3-5 lists the containers used for sample collection as well as the preservation 

requirements for each sample, and Table 3-6 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. All samples except routine total 

and dissolved metals, low-level total and dissolved metals, low-level total and dissolved 

mercury, and low-level hexavalent chromium samples were placed on ice and cooled to <6°C 

immediately following collection. All dissolved metals samples, except low-level dissolved 

mercury, were filtered in the field. The routine and low-level hexavalent chromium samples were 

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

extraction. The routine hexavalent chromium samples were supposed to be preserved to a pH 

between 9.3 and 9.7 using an ammonium sulfate buffer solution; however, the sampling team 

discontinued preservation for some samples because 10 percent of the sample volume was added 
3-7

before the required pH was achieved (the pH of the preserved samples was approximately 8.7 to 

9.0). The low-level hexavalent chromium samples bottles were prepreserved with 4 mL of 50-

percent NaOH. The Group II and HEM/SGT-HEM samples were preserved with sulfur acid to a 

pH of <2 immediately after collection in the staging area, and the pH was confirmed with fourcolor pH strips. 

3.3 Plant Operational Data

 During the sampling episode at Big Bend, plant personnel provided the sampling team 

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

operational and flow data for the FGD wastewater treatment system. Table 3-7 presents the unit 

operating characteristics, Table 3-8 presents the FGD scrubber system operating characteristics, 

and Table 3-9 presents the FGD wastewater treatment system operating characteristics during the 

sampling episode. In addition, plant personnel provided the sampling team with measured flow 

values at the influent and effluent of the FGD wastewater treatment system during the sampling 

episode. The average flow rate into the FGD wastewater treatment system was approximately 

250 gpm while EPA was collected the influent samples and the average effluent flow rate was 

approximately 104 gpm while EPA collected the effluent samples. The influent flow rate 

consisted of approximately 96 gpm of scrubber purge and 154 gpm of wastewater treatment 

recirculation flow. The flow rate data from 8:00 am to 10:30 am (during effluent sampling) and 

3:00 pm to 4:30 pm (during influent sampling) on the day of sampling is available in 

Appendix D. 

 As noted in Section 3.0, Unit 3 was shut down during the sampling episode due to a high 

opacity reading in Unit 3’s ESP, according to plant personnel. Big Bend has a maximum legal 

limit of 20 percent opacity. The Unit 3 ESP typically operates at 3-6 percent opacity; however, 

on Monday, July 23, 2007, the opacity sensor measurement was 45 percent. Due to the high 

opacity reading, the operators shut down Unit 3; however, after the unit was shut down, the 

opacity sensor continued to measure 45 percent opacity. Therefore, the plant suspected that the 

sensor was not operating properly. 

 Because Unit 3 was not operating during the sampling episode, the scrubber that treats 

Units 3 & 4 was only treating the flue gas from Unit 4. Therefore, during the episode, the flow 

rate of the scrubber blowdown from the scrubber treating Units 3 & 4 was reduced by 

approximately 50 percent. 

3.4 Deviations from the Sampling and Analysis Plan

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

described below: 

• Sample Collection Procedures. EPA planned to collect the influent to the FGD 

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

treatment system (SP-2) by filling the sample bottles directly from the sample tap. 

Instead, EPA collected the samples by attaching silicone tubing to the sample tap 

and running the tubing into a “cleanbox” where the sample bottles were filled, as 

described in Section 3.1. 
3-8

• Field Blank Sample Collection Procedures. EPA planned to collect the field 

blanks for the influent to the FGD wastewater treatment system (SP-4) and the 

effluent from the FGD wastewater treatment system (SP-5) by pouring the blank 

water directly into the sample bottles at the sample location. Because the sample 

collection procedures changed and tubing was used for the for the sample 

collection, the tubing had to be incorporated into the field blank. Therefore, EPA 

used a funnel to pour the blank water through the tubing and into the sample 

bottles, as described in Section 5.2.3. 

• Dissolved Metals Filtration. EPA planned to filter the influent to the FGD 

wastewater treatment samples approximately one hour after the sample was 

collected; however, EPA did not filter the samples until approximately two hours 

later. For the effluent from the FGD wastewater treatment, EPA did not filter the 

samples until two and a half hours after sample collection. 

• Collection Containers for Routine Dissolved Metals. For the effluent from the 

FGD wastewater treatment system, EPA planned to collect volume for the pump 

off of routine dissolved metals and routine hexavalent chromium samples, as well 

as the field duplicate and QC samples, into three 1-gallon containers. However, 

EPA collected the volume into a precleaned 10-liter container. 

• Dissolved Metals Sample Collection Order. During the filtration of the influent 

to the FGD wastewater treatment samples, EPA collected the routine hexavalent 

chromium sample prior to collecting the low-level and routine dissolved metals 

samples because it was the only dissolved sample that needed to be preserved 

prior to shipment. 

• Collection of Low-Level Mercury Field Blank Samples at SP-1. During the 

collection of the low-level total mercury field blank samples at SP-1, the sampling 

team did not don dust masks as required by EPA Method 1669. After the field 

blank sample was collected, EPA realized the error and donned the dust masks 

until the low-level total and dissolved mercury samples were collected. 

• Chlorine Field Test Measurements. When EPA performed the chlorine field test 

measurements for both the influent to the FGD wastewater treatment system (SP1) and the effluent from the FGD wastewater treatment system (SP-2), the 

reaction of the DPD reagent with the wastewater formed a precipitate which 

caused an interference with the measurement. 

• Preservation of Routine Hexavalent Chromium. The routine hexavalent 

chromium samples were supposed to be preserved to a pH between 9.3 and 9.7 

using an ammonium sulfate buffer solution; however, the samplers discontinued 

preservation for some samples because 10 percent of the sample volume was 

added before the required pH was achieved (the pH of the preserved samples was 

approximately 8.7 to 9.0). 
3-9

• Nitrate/Nitrite as Nitrogen Analysis. The analysis of nitrate/nitrite as nitrogen 

was not performed for this sampling episode. The laboratory equipment required 

for the analysis was broken and the equipment could not be repaired before the 

hold time was exceeded. 

Table 3-1. Sample Collection Information, Big Bend 

Sampling 

Point Number Sampling Point Description 

Type of 

Sample 

Sample Collection 

Date and Time SCC Number

SP-1 Influent to FGD Wastewater Treatment 

System 

Grab 07/25/2007 

1510 a and 1710 b 

70320 

SP-2 Effluent from FGD Wastewater Treatment 

System 

Grab 07/25/2007 

0815 a and 1140 b

70321 

SP-3 Duplicate of Effluent from FGD 

Wastewater Treatment System 

Grab 07/25/2007 

0815 a and 1140 b

70322 

SP-4 Influent to FGD Wastewater Treatment 

System Field Blank 

Grab 07/25/2007 

1450 a

 and 1705 b

70323 

SP-5 Effluent from FGD Wastewater Treatment 

System Field Blank 

Grab 07/25/2007 

0745 a

 and 1110 b

70324 

a – Collection of the total metals samples (low-level and routine), low-level dissolved mercury, and classicals. 

b – Collection of the dissolved metals samples (except low-level dissolved mercury). 
3-10 

Table 3-2. Number of Samples Collected by Sampling Point, Big Bend 

Sampling 

Point 

Number 

Sampling Point 

Description 

Low-Level Total Metals 

(11 analytes) 

Low-Level Dissolved 

Metals (11 analytes) 

Low-Level Total 

Mercury 

Low-Level Dissolved 

Mercury 

Low-Level Hexavalent 

Chromium 

Routine Total Metals (27 

analytes) 

Routine Dissolved 

Metals (27 analytes) 

BOD

5 

Group I 

a

Group II 

b

SP-1 Influent to FGD Wastewater 

Treatment System 

1 1 1 1 1 1 1 1 1 

SP-2 Effluent from FGD 

Wastewater Treatment System 

1+QC 1+QC 1+QC 1+QC 1+QC 1+QC 1+QC 1+QC 1+QC 1+QC 

SP-3 Duplicate of Effluent from 

FGD Wastewater Treatment System 

1 1 1 1 1 1 1 1 1 1 

SP-4 Influent to FGD Wastewater 

Treatment System Field Blank 

1 1 1 

SP-5 Effluent from FGD 

Wastewater Treatment System Field Blank 

1 1 1 1 1 1 

Total Number of Samples 5+1QC 5+1QC 5+1QC 3+1QC 3+1QC 5+1QC 5+1QC 3+1QC 3+1QC 3+1QC 

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), and total phosphorus. 

c – The selenium/arsenic speciation results from the sampling episode were not available at the time this report was finalized and therefore are not inc
3-11 

Table 3-3. Field Measurements, Big Bend 

pH 

Sampling Point (S.U.) 

Number 

Sampling Point 

Description Time 

Temp 

°C 

Meter Meter a Strips 

Free Chlorine 

(mg/L) 

Total Chlori

(mg/L) 

SP-1 Influent to FGD 

Wastewater Treatment 

1601 38.2 8.08 8.3 Limit b NA 

SP-2 Effluent from FGD 

Wastewater Treatment 

0942 35.7 6.91 NA 0.15 d NA 

a – The pH meter was calibrated on the morning of July 25, 2007 using pre-packaged buffer solutions at pHs 4.0, 7.0, and 10.0. b – After the N,N’-diethyl-p-phenylenediamine (DPD) powder was added to the sample, a precipitate formed which EPA could not rinswas performed for free residual chlorine, but resulted in a “limit” reading. EPA did not perform the analysis for total residual chlorine. c – Based on the average of monitored flow rate data in one minute intervals provided by Big Bend from 3:00 pm to 4:30 pm (the time treatment system influent samples were collected). d – After the DPD powder was added to the sample, a precipitate formed; however, it settled to the bottom of the vial prior to the readin

the analysis for total residual chlorine. e – Based on the average of monitored flow rate data in one minute intervals provided by Big Bend from 8:00 am to 10:30 am (the time treatment system effluent samples were collected). NA – Not analyzed. Note: At SP-2, the plant has a turbidity meter that is continuously measuring the turbidity of the effluent. During the sampling collectioteam recorded the following turbidity readings: 11.20 to 11.57 NTU at 0756; 10.83 to 11.12 NTU at 0825; and 9.39 NTU at 0928. 
3-12

Table 3-4. Analytical Methods and Procedures for Samples Collected at Big Bend 

Method Number Parameter Method Type 

Classicals 

SM 5210 B Biochemical Oxygen Demand (BOD5) Probe 

SM 2540 D Total Suspended Solids (TSS) Gravimetric 

SM 2540 C Total Dissolved Solids (TDS) Gravimetric 

ASTM D516-90 Sulfate Turbidimetric 

SM 4500–Cl–C Chloride Titrimetric, mercuric 

nitrate 

SM 4500—NH3 F (18th ed.) Ammonia as Nitrogen Distillation, 

potentiometric 

SM 4500—NO3 -H Nitrate/Nitrate as Nitrogen Autoanalyzer 

SM 4500—N,C (18th ed.) Total Kjeldahl Nitrogen (TKN) Digestion, distillation, 

potentiometric 

EPA 365.3 (Rev 1978) Total Phosphorus Digestion, 

spectrophotometric 

EPA 1664A Hexane Extractable Material (HEM) Gravimetric 

EPA 1664A Silica Gel Treated Hexane Extractable Material (SGTHEM) Gravimetric 

Metals 

EPA 1631 Mercury in Water by Oxidation, Purge and Trap, and 

Cold Vapor Atomic Fluorescence Spectrometry 

Oxidation, Purge and 

Trap, and CVAFS 

EPA 1636 Determination of Hexavalent Chromium by Ion 

Chromatography 

Ion Chromatography 

EPA 1638 Determination of Trace Elements in Ambient Waters by 

Inductively Coupled Plasma – Mass Spectroscopy 

(includes antimony, arsenic, cadmium, chromium, 

copper, lead, nickel, selenium, silver, thallium, and zinc) 

ICP/MS 

EPA 200.7, 245.1 Metals by Inductively Coupled Plasma Atomic Emission 

Spectrometry, and Atomic Absorption Spectroscopy 

ICP and CVAA 

ASTM D1687-92 Hexavalent Chromium Colorimetric 

CVAFS – Cold vapor atomic fluorescence spectrometry. 

AA – Atomic Adsorption. 

ICP/MS – Inductively coupled plasma with mass spectrometry. 

ICP – Inductively coupled plasma. 

CVAA – Cold vapor atomic adsorption. 
3-13

Table 3-5. Summary of Sample Container and Planned Preservation 

Parameter Sample Container and Volume On-Site Preservation 

Classicals 

BOD5 One 1-L plastic bottle ≤6oC 

Group I a Two 1-L plastic bottles ≤6EC 

Group II b Two 1-L plastic bottles H2SO4 to pH <2, ≤6EC 

HEM/SGT-HEM Two 1-L wide mouth glass jars H2SO4 to pH <2, ≤6oC 

Metals 

Routine total metals, 27 element 

quantitation (Method 200.7, 200.8, 

200.9, 245.1) 

One 500-mL plastic bottle None 

(acid preserve at laboratory) 

Routine dissolved metals, 27 element 

quantitation (Method 200.7, 200.8, 

200.9, 245.1) 

One 500-mL plastic bottle 0.45 μm filter (performed in field) 

(acid preserve at laboratory) 

Low-level total mercury (Method 1631) Two 250-mL glasses (ultraclean), 

fluoropolymer lined caps 

None 

(acid preserve at laboratory) 

Routine hexavalent chromium One 250-mL plastic bottle 0.45 μm filter (performed in field) 

Ammonium sulfate buffer to pH 9.3 

– 9.7, ≤6EC 

Low-level dissolved mercury (Method 

1631) 

Two 250-mL glasses (ultraclean), 

fluoropolymer lined caps 

None 

(acid preserve and filter at 

laboratory) 

Low-level total elements by ICP/MS (11 

elements, Method 1638) 

One 1-L LDPE (ultraclean), 

fluoropolymer lined cap 

None 

(acid preserve at laboratory) 

Low-level dissolved elements by 

ICP/MS (11 elements, Method 1638) 

One 1-L LDPE (ultraclean), 

fluoropolymer lined cap 

0.45 μm filter (performed in field) 

 (acid preserve at laboratory) 

Low-level hexavalent chromium 

(Method 1636) 

One 500-mL LDPE (ultraclean), 

fluoropolymer lined cap 

0.45 μm filter (performed in field) 

4 mL 50% NaOH per 500 mL 

sample (performed in field) c 

Selenium/arsenic speciation Two 125-mL amber glasses 

(ultraclean) 

None for original sample, ≤6EC 

Duplicate: HCl to pH <2, ≤6EC 

a – Group I includes TSS, TDS, sulfate, and chloride. 

b – Group II includes ammonia as nitrogen, nitrate/nitrite as nitrogen, TKN, and total phosphorus. 

c – Method 1636 has a preservation requirement that the low-level hexavalent chromium sample be cooled to ≤6EC; 

however, EPA did not cool the low-level hexavalent chromium samples due to contamination concerns. 
3-14

Table 3-6. Sample Preservation Summary, Big Bend 

Sampling 

Point 

Number Analysis 

Date and 

Time Chemical 

Initial 

pH 

Final 

pH Amount Added

70320 Group II V1 7/25/07 1935 H2SO4 9 2 175 drops 

70320 Group II V2 7/25/07 1937 H2SO4 9 2 175 drops 

70320 HEM/SGT-HEM 7/25/07 1938 H2SO4 9 2 175 drops 

70320 Routine Hexavalent 

Chromium 

7/25/07 1940 Ammonium 

Sulfate Buffer 

8.5 8.7 250 drops a

70320 Arsenic/Selenium 

Speciation (Duplicate) 

7/25/07 2015 HCl 9 2 50 drops 

70321 Group II V1 7/25/07 1145 H2SO4 7 2 70 drops 

70321 Group II V2 7/25/07 1147 H2SO4 7 2 70 drops 

70321 Group II QC V1 7/25/07 1148 H2SO4 7 2 70 drops 

70321 Group II QC V2 7/25/07 1149 H2SO4 7 2 70 drops 

70321 HEM/SGT-HEM 7/25/07 1150 H2SO4 7 2 70 drops 

70321 HEM/SGT-HEM QC V1 7/25/07 1152 H2SO4 7 2 70 drops 

70321 HEM/SGT-HEM QC V2 7/25/07 1153 H2SO4 7 2 70 drops 

70321 Routine Hexavalent 

Chromium 

7/25/07 1205 Ammonium 

Sulfate Buffer 

7.5 9.0 200 drops a

70321 Routine Hexavalent 

Chromium QC 

7/25/07 1210 Ammonium 

Sulfate Buffer 

7.5 9.0 200 drops a

70321 Arsenic/Selenium 

Speciation (Duplicate) 

7/25/07 2030 HCl 7.5 2 30 drops 

70322 Group II V1 7/25/07 1154 H2SO4 7 2 70 drops 

70322 Group II V2 7/25/07 1155 H2SO4 7 2 70 drops 

70322 Routine Hexavalent 

Chromium 

7/25/07 1300 Ammonium 

Sulfate Buffer 

7.5 9.0 200 drops a

70324 Routine Hexavalent 

Chromium 

7/25/07 1200 Ammonium 

Sulfate Buffer 

6.5 9.5 73 drops 

a – Preservation of this sample was stopped due to excessive buffering of the sample. The pH of the sample was not 

changing with the addition of the ammonium sulfate buffer solution; therefore, the preservation was stopped to 

prevent the sample from being diluted by the preservative. 
3-15 

Table 3-7. Generating Unit Operating Characteristics during Sample Collection, Big Be

Unit 

ID Boiler Type Coal type 

Coal Usage a

(tons/day) 

Source of Coal 

(coal region 

and/or state) 

Capacity 

(MW) 

Electricity 

Production (or 

percent 

capacity) 

SCR 

(No, On, 

Off) 

Parti

Contro

(HS/CS 

B

1 Opposite wall 

fired/ 

Subcritical 

Eastern 

Bituminous 

blend 

3,735 

(3.26% 

Sulfur) 

Eastern 

Illinois/Western 

Kentucky 

Bituminous coal 

400 360 MW (90%) 

@ 

Approximately 

10 AM on 

7/25/2007 

No SCR E

2 Opposite wall 

fired/ 

Subcritical 

Eastern 

Bituminous 

blend 

2,916 

(3.00% 

Sulfur) 

Eastern 

Illinois/Western 

Kentucky 

Bituminous coal 

410 350 MW (85%) 

@ 

Approximately 

10 AM on 

7/25/2007 

No SCR E

3 Opposite wall 

fired/ 

Subcritical 

Eastern 

Bituminous 

blend 

N/A N/A 430 0 MW 

(Unit was shut 

down) 

No SCR ES

4 Tangentially 

fired / 

Subcritical 

Eastern 

Bituminous 

blend 

4,265 

(3.30% 

Sulfur) 

Eastern 

Illinois/Western 

Kentucky 

Bituminous coal 

460 435 MW (95%) 

@ 

Approx 10 AM 

on 7/25/2007 

SCR on E

a – Average of the tons burned on July 24 and July 25, 2007, as provided by Big Bend. b – Unit 3 was not operating due to an issue with the ESP. HS ESP – Hot-side electrostatic precipitator. CS ESP – Cold-side electrostatic precipitator. BH – Baghouse. 
3-16 

Table 3-8. FGD Scrubber System Operating Characteristics, Big Bend 

Unit ID Type of Scrubber Sorbent 

Additives 

(DBA, Formic 

Acid, etc.) 

FGD Make-up Water 

Source 

SO2 Removal 

Percentage 

(%) 

Forced 

Oxidation 

(Yes/No) 

Percent Sol

in Slurry 

(%) 

1-2 a 1 single-loop spraytray absorber tower Limestone DBA Plant recycle water and county effluent mixture 96.3 Yes 22.0 

3-4 b 4 double-loop spraytray absorber towers Limestone DBA Plant recycle water and county effluent mixture 95.8 Yes 19.1 

a – The flue gas from Units 1 and 2 are combined and fed to single absorber tower. b – The flue gas from Units 3 and 4 are combined and then split into the four absorber towers. Note: The plant estimates that the percent solids in the effluent from the primary hydroclones is 5 percent solids and the effluent from tis 2 percent solids. 
3-17

Table 3-9. FGD Wastewater Treatment System Operating Characteristics, Big Bend 

FGD Solids Dewatering (for last cycle prior to sampling or while sampling)

Scrubber slurry blowdown flow rate 1,758 gpm (average) a 

Scrubber slurry blowdown duration Varies 

Scrubber slurry blowdown percent solids 20.6% b 

Dewatering cycle frequency Varies 

Time since last cycle Unit 1&2 scrubber: 07/25/2007 @ 8:00 am 

Unit 3&4 scrubber: 07/25/2007 @ 8:50 am 

Percent hydroclone overflow recycled back to 

scrubber 

Unable to estimate 

FGD Wastewater Treatment System Operation During Sample Collection

Scrubber purge flow rate 96 gpm (average) 

Scrubber purge duration Continuous 

Lime addition 7,852 gpd (35% solids) 

Ferric chloride addition 70 gpd c 

Chemtreat Polymer P813E addition 4.8 gpd 

Hydrochloric acid addition 532 gpd (35.7%) 

Amount of solids generated 12 tpd 

Effluent flow rate 109 gpm (average) 

Frequency of effluent discharge Approximately 40% of the time 

Retention time of equalization tank 8.7 hrs 

Retention time of primary clarifier 18.5 hrs 

Retention time of chemical reaction tanks 2.2 hrs 

Retention time of secondary clarifier Not used during sampling episode 

a – The average scrubber blowdown flow rate for both scrubbers combined. 

b – Average of the percent solids in Unit 1&2 scrubber blowdown (22%) and Unit 3&4 scrubber blowdown 

(19.1%). 

c – 38.6 percent ferric chloride in aqueous solution. 
4-1 

4. LABORATORY ANALYTICAL RESULTS AND DISCUSSION

 This section summarizes and discusses the analytical data collected during this sampling 

episode. Section 4.1 discusses the methods used by the laboratories for the biphasic analysis of 

SP-1 and presents the results of the analyses. Section 4.2 presents the laboratory analytical data 

for the influent to and effluent from the FGD wastewater treatment system. 

 Appendix A provides all analytical results for all samples collected at Big Bend, 

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

limit, but below the reporting limit (i.e., J-values). Appendix B presents the analytical results in a 

format similar to that used in Section 4.2, but with the J-values shown (J-values are not included 

in the tables presented in Section 4.2). 

4.1 Measured and Calculated Results for FGD Influent Samples

 The samples of the influent to the FGD wastewater treatment system were expected to 

contain significant amounts of readily settleable solids, to a large degree consisting of gypsum, 

unreacted limestone, and fly ash. Because of this, EPA was concerned that there could be 

analytical interferences for the metals analyses, since the acid digestion procedures used may not 

be sufficiently rigorous for samples with high solids loads. Therefore, EPA directed its contract 

laboratories to separate the aqueous and solid phases of the sample prior to conducting certain 

analyses, where allowed by the analytical method and if necessary to obtain acceptable analytical 

results. This biphasic approach provides EPA with both measured and calculated pollutant 

concentrations for the following phases of the sample: 

• Aqueous phase; 

• Solid phase; and 

• Total sample. 

The routine metals laboratory, ProChem Analytical (ProChem), and the low-level laboratory, 

Battelle Marine Sciences Laboratory (Battelle), used two different approaches for the biphasic 

analysis because of the different methods used for routine versus low-level metals analyses. This 

section describes the approaches used by each laboratory and presents the results of the analyses. 

Routine Metals and Selected Classicals Analyses 

 ProChem used EPA Method 200.7 to analyze the wastewater samples for routine metals, 

and EPA Method 245.1 to analyze for routine mercury. EPA Method 200.7 states, “Aqueous 

samples containing total suspended solids ≥1% (w/v) should be extracted as a solid type 

sample.” (U.S. EPA, 2001) Because EPA expected the solids content to be greater than one 

percent, ProChem developed an approach for the analysis of the FGD influent samples that 

consisted of filtering the solids from the sample and analyzing the solid and aqueous phases 

separately. To calculate the total sample concentration from the solid and aqueous phase results, 

the laboratory also needed to measure the original sample volume, solid phase weight, and 

filtrate volume. EPA developed the following equation to calculate the individual metal total 

concentrations for the sample. 
4-2 

Sample

Filtrate Filtrate Solid Solid

V

(C V ) (C Wt ) Total SampleConcentration × + × = (4-1) 

where: 

CFiltrate = Concentration of the analyte in the aqueous phase of the sample; 

VFiltrate = Volume of the filtrate; 

CSolid = Concentration of the analyte in the solid phase of the sample; 

WtSolid = Weight of the solids in the sample; and 

VSample = Volume of the original sample. 

ProChem used the same approach for the five classical pollutants that were analyzed as biphasic 

samples: ammonia as nitrogen, chloride, sulfate, total Kjeldahl nitrogen (TKN), and total 

phosphorus. 

Low-Level Metals Analyses 

 Battelle used EPA Method 1638 to analyze the wastewater samples for low-level metals, 

and EPA Method 1631E to analyze for low-level mercury. EPA Method 1638 does not contain 

any language stating how wastewater samples with high solid concentrations should be analyzed; 

therefore, Battelle developed an approach for the analysis of the FGD influent samples that 

minimized potential contamination to the samples. Battelle’s approach consisted of analyzing the 

total metals concentration and dissolved metals concentration for each analyte directly from the 

sample bottles, and calculating the solid phase concentration. By using this approach, the 

laboratory did not have to perform an extra filtration step to determine the individual metals 

concentrations for the various phases in the sample. Battelle did not have any problems with the 

digestion of the solids during the total sample analyses for the Big Bend FGD influent samples. 

 To calculate the solid phase concentration from the total and dissolved phase results, 

Battelle also measured the TSS level in the total metals sample bottle. EPA used the following 

equation to calculate the individual metal solid phase concentrations for the sample: 

TSS

Total Diss

Solid C

C - C C = (4-2) 

where: 

CSolid = Concentration of the metal in the solid phase of the sample; 

CTotal = Total concentration of the metal in the sample; 

CDiss = Concentration of the metal in the dissolved phase of the sample; and 

CTSS = TSS concentration of the sample. 

Analytical Deviations 

 During the analysis of the Big Bend FGD influent samples, ProChem did not measure the 

original sample volume and filtrate volume for the routine total metals samples, which were 

needed for the calculation of the total sample concentration. Because ProChem did not have 

extra sample volume to reanalyze the samples, extra sample volume from the low-level total 

metals sample bottles at Battelle were shipped to ProChem for the reanalysis of routine total 

metals. When performing the reanalysis using Battelle’s extra sample volume, ProChem used the 

same approach as Battelle (i.e., analyzing the total sample directly), because the laboratory 
4-3 

determined that the suspended solids present in the sample were at a concentration less than one 

percent; therefore, the phase separation was not required by EPA Method 200.7. The laboratory 

analyzed the total metals directly from the sample bottle. The laboratory had already analyzed 

the dissolved metals concentration; therefore, a solid concentration was calculated using 

Equation 4-2. 

 Table 4-1 presents the results of the biphasic analysis for low-level total metals and 

routine total metals (except routine total mercury, which is discussed below) in the FGD influent 

samples. Only those analytes that were detected at the influent to the FGD wastewater treatment 

system (at levels above the reporting limit) are included in the table. Results are rounded to three 

significant figures. Appendix Table A-1 presents all the analytical results from the FGD influent 

(SP-1) sample analysis, including results that were measured above the method detection limit, 

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

 For the biphasic classical analyses, ProChem did not measure the original sample volume 

and filtrate volume, which were needed for the calculation of the total sample concentration, and 

they did not have extra sample volume to reanalyze the classicals. Although additional sample 

volume was available for the reanalysis of mercury, by the time the error was recognized, the 

holding time for the mercury analysis had expired. 

 To determine the total sample results for the classical analytes, EPA calculated the 

sample volume using the sample weight and sample density. EPA was also able to calculate the 

filtrate volume using data that had already been collected by the laboratory. Therefore, the 

classical analytes total concentrations were calculated using Equation 4-1 without making any 

assumptions. For the routine total mercury concentration, EPA had to estimate the sample 

volume to calculate the filtrate volume needed for the calculation. As a best available estimate, 

EPA assumed that the sample volume was 500 mL, based on the sample bottle size, knowing that 

the actual volume of sample collected may have been less than or greater than 500 mL 

 Table 4-2 presents the results of the biphasic analysis for routine total mercury and 

Table 4-3 presents the results of the biphasic analysis for ammonia as nitrogen, chloride, sulfate, 

TKN, and total phosphorus in the FGD influent samples. Only those analytes that were detected 

at the influent to the FGD wastewater treatment system (at levels above the reporting limit) are 

included in the table. Results are rounded to three significant figures. Appendix Table A-1 

presents all the analytical results from the FGD influent (SP-1) sample analysis, including Jvalues. 

 ProChem performed a filtration blank associated with the biphasic sample separation 

process for the FGD influent (SP-1) sample analysis. For the blank, ProChem poured blank water 

through the filter used for the separation and analyzed the filtered blank water for routine 

mercury (note: routine mercury is the only analytical result from the filtration blank that is 

applicable to the biphasic analysis because all other metals were analyzed without the biphasic 

separation). Mercury was not measured in the filtration blank sample above the reporting limit, 

indicating that there was no contamination from the filtration process. Appendix Table A-2 

presents the routine mercury analytical result from the filtration blank. 
4-4 

4.2 FGD Wastewater Treatment System

 Table 4-4 presents the analytical results of the classical pollutants at the influent to and 

effluent from the FGD wastewater treatment system (SP-1 and SP-2). Table 4-5 presents the 

analytical results of the routine and low-level metals at the influent to and effluent from the FGD 

wastewater treatment system (SP-1 and SP-2). Only those analytes that were detected in one or 

more samples (at levels above the reporting limit) for the sampling episode are included in the 

table. Results are rounded to three significant digits. If an analyte was measured above the 

method detection limit, but below the report limit, “NQ” is reported followed by the samplespecific report limit in parentheses. If an analyte was not detected in a sample above the method 

detection limit, “ND” is reported followed by the sample-specific report limit in parentheses. 

Note that the results presented in Tables 4-4 and 4-5 are not paired results, meaning that sample 

collection across the treatment system was not timed to reflect the amount of time it takes the 

wastewater to pass through the treatment system (approximately 24-32 hours). 

 Appendix Tables A-1, A-3, and A-4 present all the analytical results from the FGD 

influent (SP-1), FGD effluent (SP-2), and FGD effluent duplicate (SP-3) sample analyses, 

including J-values. Appendix Table B-1 presents the analytical results for the metal analytes in a 

format similar to Table 4-5; however, Table B-1 also include results where analytes were 

measured above the method detection limit, but below the reporting limit (i.e., J-values). 
4-5 

Table 4-1. Biphasic Sample Results for Low-Level Total Metals and Routine Total Metals 

Measured Above the Report Limit, FGD Influent, Big Bend 

Analyte

Dissolved Sample Result 

(ug/L) 

Calculated Solid Phase Result 

(mg/kg) 

Total Sample Result 

(ug/L) 

Low-level Total Metals 

Antimony 21.9 NQ (0.837) 24.9 

Arsenic 137 NQ (6.28) 165 

Cadmium 190 10.0 238 

Chromium ND (160) 136 651 L 

Copper NQ (40.0) 16.2 103 

Lead ND (10.0) 14.6 69.9 

Mercury 0.206 3.38 16.4 

Nickel 1,030 322 2,570 

Selenium 3,280 NQ (41.8) 3,470 

Thallium 39.4 NQ (0.837) 39.8 

Zinc ND (100) 391 1,870 

Routine Total Metals 

Aluminum ND (50.0) 6,280 31,200 

Antimony 33.9 5.75 62.5 

Arsenic 18.6 11.4 75.5 

Barium 1,820 ND (0.402) 1,590 

Beryllium NQ (5.00) 2.07 12.9 

Boron 618,000 NQ (2,010) 626,000 

Cadmium 179 9.05 224 

Calcium 4,470,000 447,000 6,690,000 

Chromium NQ (10.0) 151 757 

Cobalt NQ (50.0) 28.2 172 

Copper 27.2 18.7 120 

Iron NQ (100) 4,730 23,500 

Lead NQ (50.0) 12.6 69.1 

Magnesium 4,110,000 145,000 4,830,000 

Manganese 9,610 2,470 21,900 

Molybdenum 581 7.44 618 

Nickel 851 249 2,090 

Selenium 3,610 109 4,150 

Sodium 1,970,000 113,000 2,530,000 

Thallium 14.3 ND (2.01) ND (10.0) 

Titanium 12.5 82.0 420 

Vanadium 108 124 724 

Yttrium ND (5.00) 49.3 245 

Zinc 16.8 306 1,540 

L – Sample result between 5x and 10x blank result. 

ND – Not detected (number in parenthesis is the report limit). 

NQ – Analyte was measured above the method detection limit, but below the report limit (number in parenthesis is the report 

limit). The analytical result is presented in Appendix A with a J flag designation. 
4-6 

Table 4-2. Biphasic Sample Results for Routine Total Mercury, FGD Influent, Big Bend 

Analyte 

Aqueous Phase Result 

(ug/L) 

Solid Phase Result 

(mg/kg) 

Calculated Total 

Sample (ug/L) 

Routine Total Metals 

Mercury ND (10.0) 0.220 NJ (10.0) 

ND – Not detected (number in parenthesis is the report limit). 

NJ – The analyte concentration was calculated using the filtered aqueous and/or the filtered solid analytical results, 

including J-values, if applicable, and was determined to be less than the calculated sample-specific report limit 

(number in parenthesis is the report limit). The calculated result is presented in Appendix A with a CJ flag 

designation. 

Table 4-3. Biphasic Sample Results for Classical Analytes Measured Above the Report 

Limit, FGD Influent, Big Bend 

Analyte 

Aqueous Phase Result 

(mg/L) 

Solid Phase Result 

(mg/kg) 

Calculated Total 

Sample (mg/L) 

Classical Pollutants 

Ammonia As Nitrogen (NH3-N) 31.7 20.4 31.5 

Total Kjeldahl Nitrogen (TKN) 47.4 319 51.6 

Chloride 24,500 11,000 24,200 

Sulfate 2,300 67,600 3,590 

Total Phosphorus 0.390 39.4 0.990 

Table 4-4. Classical Pollutants Measured Above the Report Limit for the FGD 

Wastewater Treatment System, Big Bend 

Analyte Method Unit 

FGD Influent 

(SP-1) 

FGD Effluent 

(SP-2/SP-3)a 

Classical Pollutants 

Ammonia As Nitrogen (NH3-N) 4500-NH3F MG/L 31.5 24.1

Total Kjeldahl Nitrogen (TKN) 4500-N,C MG/L 51.6 98.7 

Biochemical Oxygen Demand (BOD) 5210B MG/L 1,370 >1,720

Chloride 4500-CL-C MG/L 24,200 22,500

Hexane Extractable Material (HEM) 1664A MG/L ND (6.00) 6.00

Sulfate D516-90 MG/L 3,590 1,920

Total Dissolved Solids (TDS) 2540 C MG/L 44,600 40,600

Total Phosphorus 365.3 MG/L 0.990 0.355

Total Suspended Solids (TSS) 2540 D MG/L 4,970 31.5

a – The FGD effluent results represent the average of the FGD effluent and the duplicate of the FGD effluent 

analytical measurements. 

> – Result above measurement range. 

NA – Not analyzed. 

ND – Not detected (number in parenthesis is the report limit). 

Note: Results shown are not paired samples. See Section 4.2.
4-7 

a – The FGD effluent results represent the average of the FGD effluent and the duplicate of the FGD effluent analytical measurements. 

NA – Not analyzed. ND – Not detected (number in parenthesis is the report limit). NJ – The analyte concentration was calculated using the filtered aqueous and/or the filtered solid analytical results, including J-values, 

determined to be less than the calculated sample-specific report limit (number in parenthesis is the report limit). The calculated result is with a CJ flag designation. NQ – Analyte was measured above the method detection limit, but below the report limit (number in parenthesis is the report limit). Thpresented in Appendix A with a J flag designation. A designation of “NQ” for the average FGD effluent indicates that the original FGD duplicate of the FGD effluent is flagged as a J-value. The analytical result for the original FGD effluent and/or the duplicate of the FGD 

Appendix A with a J flag designation. R – MS/MSD % Recovery outside method acceptance criteria. T – MS/MSD RPD outside method acceptance criteria. < – Average result includes at least one non-detect value. (Calculation uses detection limit for non-detected results). 

L – Sample result between 5x and 10x blank result. Note: Results shown are not paired samples. See Section 4.2. 

Table 4-5. Metals Measured Above the Report Limit for the FGD Wastewater Treatment System

FGD Influent (SP-1) FGD Effluent 

Analyte Method Unit Total Dissolved Total 

Routine Metals Aluminum 200.7 UG/L 31,200 ND (50.0) ND (50.0) Antimony 200.7 UG/L 62.5 33.9 22.1 R Arsenic 200.7 UG/L 75.5 18.6 NQ (10.0) Barium 200.7 UG/L 1,590 1,820 1,490 Beryllium 200.7 UG/L 12.9 NQ (5.00) NQ (5.00) Boron 200.7 UG/L 626,000 618,000 369,000 Cadmium 200.7 UG/L 224 179 24.9 Calcium 200.7 UG/L 6,690,000 4,470,000 4,420,000 Chromium 200.7 UG/L 757 NQ (10.0) NQ (10.0) Hexavalent Chromium D1687-92 UG/L NA 24.0 NA Cobalt 200.7 UG/L 172 NQ (50.0) NQ (50.0) Copper 200.7 UG/L 120 27.2 <10.3 Iron 200.7 UG/L 23,500 NQ (100) NQ (100) Lead 200.7 UG/L 69.1 NQ (50.0) NQ (50.0) Magnesium 200.7 UG/L 4,830,000 4,110,000 2,510,000 Manganese 200.7 UG/L 21,900 9,610 60.1 
4-8 

a – The FGD effluent results represent the average of the FGD effluent and the duplicate of the FGD effluent analytical measurements. 

NA – Not analyzed. ND – Not detected (number in parenthesis is the report limit). NJ – The analyte concentration was calculated using the filtered aqueous and/or the filtered solid analytical results, including J-values, 

determined to be less than the calculated sample-specific report limit (number in parenthesis is the report limit). The calculated result is with a CJ flag designation. NQ – Analyte was measured above the method detection limit, but below the report limit (number in parenthesis is the report limit). Thpresented in Appendix A with a J flag designation. A designation of “NQ” for the average FGD effluent indicates that the original FGD duplicate of the FGD effluent is flagged as a J-value. The analytical result for the original FGD effluent and/or the duplicate of the FGD 

Appendix A with a J flag designation. R – MS/MSD % Recovery outside method acceptance criteria. T – MS/MSD RPD outside method acceptance criteria. < – Average result includes at least one non-detect value. (Calculation uses detection limit for non-detected results). 

L – Sample result between 5x and 10x blank result. Note: Results shown are not paired samples. See Section 4.2. 

Table 4-5. Metals Measured Above the Report Limit for the FGD Wastewater Treatment System

FGD Influent (SP-1) FGD Effluent 

Analyte Method Unit Total Dissolved Total 

Mercury 245.1 UG/L NJ (10.0) ND (10.0) ND (10.0) Molybdenum 200.7 UG/L 618 581 450 R Nickel 200.7 UG/L 2,090 851 221 Selenium 200.7 UG/L 4,150 3,610 2,910 R Sodium 200.7 UG/L 2,530,000 1,970,000 1,590,000 Thallium 200.7 UG/L ND (10.0) 14.3 16.8 Titanium 200.7 UG/L 420 12.5 13.5 Vanadium 200.7 UG/L 724 108 NQ (20.0) Yttrium 200.7 UG/L 245 ND (5.00) ND (5.00) Zinc 200.7 UG/L 1,540 16.8 ND (10.0) Low-Level Metals Antimony 1638 UG/L 24.9 21.9 14.2 Arsenic 1638 UG/L 165 137 68.0 Cadmium 1638 UG/L 238 190 25.8 Chromium 1638 UG/L 651 L ND (160) NQ (80.0) Hexavalent Chromium 1636 UG/L NA NA NA Copper 1638 UG/L 103 NQ (40.0) NQ (20.0) 
4-9 

a – The FGD effluent results represent the average of the FGD effluent and the duplicate of the FGD effluent analytical measurements. 

NA – Not analyzed. ND – Not detected (number in parenthesis is the report limit). NJ – The analyte concentration was calculated using the filtered aqueous and/or the filtered solid analytical results, including J-values, 

determined to be less than the calculated sample-specific report limit (number in parenthesis is the report limit). The calculated result is with a CJ flag designation. NQ – Analyte was measured above the method detection limit, but below the report limit (number in parenthesis is the report limit). Thpresented in Appendix A with a J flag designation. A designation of “NQ” for the average FGD effluent indicates that the original FGD duplicate of the FGD effluent is flagged as a J-value. The analytical result for the original FGD effluent and/or the duplicate of the FGD 

Appendix A with a J flag designation. R – MS/MSD % Recovery outside method acceptance criteria. T – MS/MSD RPD outside method acceptance criteria. < – Average result includes at least one non-detect value. (Calculation uses detection limit for non-detected results). 

L – Sample result between 5x and 10x blank result. Note: Results shown are not paired samples. See Section 4.2. 

Table 4-5. Metals Measured Above the Report Limit for the FGD Wastewater Treatment System

FGD Influent (SP-1) FGD Effluent 

Analyte Method Unit Total Dissolved Total 

Lead 1638 UG/L 69.9 ND (10.0) ND (5.00) Mercury 1631E UG/L 16.4 0.206 0.156 Nickel 1638 UG/L 2,570 1,030 381 Selenium 1638 UG/L 3,470 3,280 2,500 Thallium 1638 UG/L 39.8 39.4 31.1 Zinc 1638 UG/L 1,870 ND (100) NQ (50.0) 
5-1 

5. DATA QUALITY

 QA/QC procedures applicable to the Big Bend sampling episode are outlined in the 

Quality Assurance Project Plan for the Steam Electric Detailed Study (QAPP) [2]. This section 

describes the QC procedures used to assess the precision and accuracy of the analytical data 

presented in Section 4 and Appendices A and B. 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

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

during this episode. EPA’s Sample Control Center (SCC) verified that the performances of the 

laboratories selected by EPA was acceptable by conducting QC checks of the analytical data as 

specified by the SCC’s Quality Assurance Project Plan dated 15 February 2008. SCC data 

review chemists prepared written data review narratives describing any qualifications of the 

analytical data from this episode. The data review narratives are included in Appendix C. 

5.2 Field Quality Control

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

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

Tables presented in this section include results for only certain analytes (e.g., only those detected 

in the respective field QC sample or those detected during the sampling episode). Appendix A 

contains the results for all analytes, both detected and nondetected. 

5.2.1 Bottle Blanks 

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

bottles. Bottle blanks were collected and analyzed for low-level metals by the supplier of the precleaned bottles, Albion Environmental. 

 Albion Environmental collected the bottle blanks for the low-level metals sample bottles 

(1000 mL LDPE), the low-level hexavalent chromium samples bottles (500 mL LDPE), and the 

speciation sample bottles (125 mL amber glass bottles) by filling the pre-cleaned bottle to the 

neck with ASTM Type 1 water, preserving the sample with nitric acid to a pH <2, and allowing 

the sample to sit for at least 72 hours. Albion Environmental then analyzed the samples using 

EPA Method 1638. 

 Albion Environmental collected the bottle blanks for the 4-liter blank water bottles by 

filling the pre-cleaned bottle with ASTM Type 1 water and allowing it to soak for approximately 

24 hours. Albion Environmental then poured a representative aliquot into a pre-cleaned LDPE 

sample bottle, preserved the sample with nitric acid to a pH <2, and allowed the sample to sit for 

at least 72 hours. Albion Environmental then analyzed the samples using EPA Method 1638. 

 Albion Environmental collected the bottle blanks for the low-level mercury sample 

bottles (250 flint glass bottles and 1-L borosilicate glass bottles) by filling the pre-cleaned bottle 

to the neck with ASTM Type 1 water, preserving the sample with bromine monochloride, and 
5-2 

allowing the sample to sit for at least 24 hours. Albion Environmental then analyzed the samples 

using EPA Method 1631E. 

 Albion Environmental collected the bottle blank for the 10-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, Albion Environmental 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-liter container and poured a 

representative sample into a pre-cleaned sample bottle (a LDPE bottle for low-level metals and a 

glass bottle for low-level mercury). The blank samples were then preserved and analyzed 

according to the analytical methods (i.e., EPA Method 1638 or 1631E), as described above for 

the other bottle blank samples. 

 No metals were detected in the bottle blank, indicating that there was no contamination 

from the sample containers. Appendix Table A-5 presents all of the analytical results from the 

bottle blank and equipment blank analyses for all of the equipment used for the collection of 

low-level samples. 

5.2.2 Equipment Blanks 

 EPA collects equipment blanks to evaluate possible contamination from the equipment 

used for sample collection. EPA did not collect specific equipment blanks for this sampling 

program; however, the field blanks as collected (as described in Section 5.2.3) include the 

sampling equipment. In addition, Albion Environmental collected and analyzed equipment 

blanks for low-level metals for each type of pre-cleaned equipment supplied for the episode. 

 Albion Environmental collected the equipment blanks for the capsule filters and 

fabricated tubing sets by pumping approximately 500 mL of ASTM Type 1 water through the 

pre-cleaned filter or tubing set and discarding the water. Albion Environmental then pumped 

additional water through the pre-cleaned filter or tubing set into a pre-cleaned bottle (a LDPE 

bottle for low-level metals and a glass bottle for low-level mercury). The blank samples were 

then preserved and analyzed according to the analytical methods (EPA Method 1638 or 1631E), 

as described in Section 5.2.1 for the bottle blank samples. For the fabricated tubing sets, Albion 

Environmental collected and analyzed equipment blanks for the individual components of the 

tubing sets, the assembled tubing sets, or both. 

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

contamination from the sampling equipment. Appendix Table A-5 presents all of the analytical 

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

collection of low-level samples. 

5.2.3 Field Blanks 

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

contamination caused by sampling equipment, sampling equipment decontamination procedures, 
5-3 

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

samples for the low-level and routine metals analyses, including both total and dissolved metals1

. 

 The low-level and routine total metals field blank samples for the influent to the FGD 

Wastewater Treatment System (SP-4) and the effluent from the FGD Wastewater Treatment 

System (SP-5) were collected by pouring ASTM Type 1 water through a precleaned funnel 

attached to the silicone tubing used for sample collection. The sampling team shrouded the blank 

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

potential atmospheric deposition. In addition, the sample bottles were placed in a “cleanbox” to 

prevent potential atmospheric deposition. Figure E-8, in Appendix E, is a picture of the samplers 

collecting the field blanks at the effluent from the FGD wastewater treatment system. The ASTM 

Type 1 water flowed through the funnel and tubing, and was poured into the sample bottles. EPA 

collected the field blank samples separately from the Big Bend representative’s field blank 

samples. Split samples were not collected for the field blank samples because the sample split 

was performed at the tap outlet, not within the sample tubing. 

 The low-level and routine dissolved metals field blank samples for the influent to the 

FGD Wastewater Treatment System (SP-4) and the effluent from the FGD Wastewater 

Treatment System (SP-5) were collected by pumping ASTM Type 1 water through the pump-off 

tubing used for the dissolved metals sample collection and a capsule filter. The container holding 

the ASTM Type 1 water was placed in a large plastic bag and the tubing was placed directly into 

the container. The large plastic bag was closed off as quickly as possible to minimize potential 

atmospheric deposition. The sample bottles were placed in a “cleanbox” and the ASTM Type 1 

water was pumped through the tubing, capsule filter, and poured into the sample bottles. EPA 

collected the field blank samples as “multipour” split samples with Big Bend’s representative, 

using the same procedure discussed in the sample collection description (Section 3.1). 

 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 reporting limit are 

included in the table. Results are rounded to three significant digits. Appendix Tables A-6 and A7 present all the analytical results for the field blanks from the FGD influent (SP-1) and FGD 

effluent (SP-2) sample analyses, including all qualified results and all results that were measured 

above the method detection limit, but below the reporting limit (i.e., J-values). 

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 relative percent difference (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. 

 

1 EPA did not collect a low-level dissolved mercury field blank sample in the field 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 low-level dissolved mercury sample. 

Mercury was detected at a concentration of 0.000334 ug/L in the filtration blank; however, this concentration is 

below the report limit of 0.0005 ug/L. Therefore, this sample result is flagged as a J-value. 
5-4 

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, duplicate samples (SP-3) for all analytes (except 

HEM/SGT-HEM) were collected from the effluent from the FGD Wastewater Treatment System 

(SP-2). Table 5-2 presents analytical results and the RPD for SP-2 and SP-3 and includes 

analytical results for only those analytes that were detected in one or more samples for the 

sampling episode. Results are rounded to three significant digits. Appendix Tables A-3 and A-4 

present all the analytical results for the FGD effluent and FGD effluent duplicate sample 

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

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

Table 5-1. Field Blank Results Measured Above the Report Limit, Big Bend 

Analyte Sample Point Method Unit

Concentration 

(ug/L) 

Routine Total Metals 

Calcium FGD Effluent 200.7 UG/L 863 

Magnesium FGD Effluent 200.7 UG/L 750 

Routine Dissolved Metals 

Boron FGD Effluent 200.7 UG/L 2,430 

Calcium FGD Effluent 200.7 UG/L 20,200 

Magnesium FGD Effluent 200.7 UG/L 17,800 

Sodium FGD Effluent 200.7 UG/L 8,730 

Low-Level Dissolved Metals 

Chromium FGD Effluent 1638 UG/L 2.15 

Copper FGD Effluent 1638 UG/L 1.11 

Hexavalent Chromium FGD Effluent 1636 UG/L 6.27 

Zinc FGD Effluent 1638 UG/L 0.650 
5-5 

> – Result above measurement range. NA – Not analyzed. NC – Not calculated. ND – Not detected (number in parenthesis is the report limit). NQ – Analyte was measured above the method detection limit, but below the report limit (number in parenthesis is the report limit). Thpresented in Appendix A with a J flag designation. R – MS/MSD % Recovery outside method acceptance criteria. T – MS/MSD RPD outside method acceptance criteria. < – Average result includes at least one non-detect value. (Calculation uses detection limit for non-detected results). 

Table 5-2. Field Duplicate Results, Big Bend 

Analyte

Original FGD Effluent 

Concentration 

Duplicate FGD Effluent 

Concentration Average Result 

Relat

Diffe

Classical Pollutants Ammonia As Nitrogen (NH3-N) 23.9 24.2 24.1 Total Kjeldahl Nitrogen (TKN) 102 95.3 98.7 Biochemical Oxygen Demand (BOD)

1,440 >2,000 >1,720 

Chloride 22,000 23,000 22,500 Hexane Extractable Material (HEM)

6.00 NA 6.00 

Silica Gel Treated HEM (SGTHEM) ND (6.00) NA ND (6.00) Sulfate 1,820 2,020 1,920 Total Dissolved Solids (TDS) 40,700 40,400 40,600 Total Phosphorus 0.390 0.320 0.355 Total Suspended Solids (TSS) 42.0 21.0 31.5 Routine Total Metals Aluminum ND (50.0) ND (50.0) ND (50.0) Antimony 22.3 R 21.9 22.1 Arsenic NQ (10.0) NQ (10.0) ND (10.0) Barium 1,570 1,410 1,490 Beryllium NQ (5.00) NQ (5.00) ND (5.00) Boron 346,000 391,000 369,000 Cadmium 26.0 23.7 24.9 
5-6 

> – Result above measurement range. NA – Not analyzed. NC – Not calculated. ND – Not detected (number in parenthesis is the report limit). NQ – Analyte was measured above the method detection limit, but below the report limit (number in parenthesis is the report limit). Thpresented in Appendix A with a J flag designation. R – MS/MSD % Recovery outside method acceptance criteria. T – MS/MSD RPD outside method acceptance criteria. < – Average result includes at least one non-detect value. (Calculation uses detection limit for non-detected results). 

Table 5-2. Field Duplicate Results, Big Bend 

Analyte

Original FGD Effluent 

Concentration 

Duplicate FGD Effluent 

Concentration Average Result 

Relat

Diffe

Calcium 4,210,000 4,620,000 4,420,000 Chromium NQ (10.0) NQ (10.0) ND (10.0) Cobalt NQ (50.0) NQ (50.0) ND (50.0) Copper 10.5 NQ (10.0) < 10.3 Iron NQ (100) NQ (100) ND (100) Lead NQ (50.0) NQ (50.0) ND (50.0) Magnesium 2,470,000 2,550,000 2,510,000 Manganese 63.1 57.0 60.1 Mercury ND (10.0) ND (10.0) ND (10.0) Molybdenum 470 R 429 450 Nickel 231 210 221 Selenium 3,020 R 2,790 2,910 Sodium 1,530,000 1,650,000 1,590,000 Thallium 17.4 16.2 16.8 Titanium 13.7 13.2 13.5 Vanadium NQ (20.0) NQ (20.0) ND (20.0) Yttrium ND (5.00) ND (5.00) ND (5.00) Zinc ND (10.0) ND (10.0) ND (10.0) Routine Dissolved Metals Aluminum ND (50.0) ND (50.0) ND (50.0) Antimony 21.1 T 20.4 20.8 Arsenic 11.1 R,T 10.5 10.8 
5-7 

> – Result above measurement range. NA – Not analyzed. NC – Not calculated. ND – Not detected (number in parenthesis is the report limit). NQ – Analyte was measured above the method detection limit, but below the report limit (number in parenthesis is the report limit). Thpresented in Appendix A with a J flag designation. R – MS/MSD % Recovery outside method acceptance criteria. T – MS/MSD RPD outside method acceptance criteria. < – Average result includes at least one non-detect value. (Calculation uses detection limit for non-detected results). 

Table 5-2. Field Duplicate Results, Big Bend 

Analyte

Original FGD Effluent 

Concentration 

Duplicate FGD Effluent 

Concentration Average Result 

Relat

Diffe

Barium 1,400 1,410 1,410 Beryllium NQ (5.00) NQ (5.00) ND (5.00) Boron 401,000 392,000 397,000 Cadmium 19.5 19.1 19.3 Calcium 5,180,000 5,240,000 5,210,000 Chromium NQ (10.0) NQ (10.0) ND (10.0) Hexavalent Chromium ND (2.00) ND (2.00) ND (2.00) Cobalt NQ (50.0) NQ (50.0) ND (50.0) Copper NQ (10.0) NQ (10.0) ND (10.0) Iron NQ (100) NQ (100) ND (100) Lead NQ (50.0) NQ (50.0) ND (50.0) Magnesium 2,910,000 2,940,000 2,930,000 Manganese 55.6 55.5 55.6 Mercury ND (10.0) ND (10.0) ND (10.0) Molybdenum 431 T 429 430 Nickel 210 209 210 Selenium 2,860 R 2,860 2,860 Sodium 1,850,000 1,910,000 1,880,000 Thallium 14.2 10.8 12.5 Titanium 13.2 14.1 13.7 Vanadium NQ (20.0) NQ (20.0) ND (20.0) Yttrium ND (5.00) ND (5.00) ND (5.00) 
5-8 

> – Result above measurement range. NA – Not analyzed. NC – Not calculated. ND – Not detected (number in parenthesis is the report limit). NQ – Analyte was measured above the method detection limit, but below the report limit (number in parenthesis is the report limit). Thpresented in Appendix A with a J flag designation. R – MS/MSD % Recovery outside method acceptance criteria. T – MS/MSD RPD outside method acceptance criteria. < – Average result includes at least one non-detect value. (Calculation uses detection limit for non-detected results). 

Table 5-2. Field Duplicate Results, Big Bend 

Analyte

Original FGD Effluent 

Concentration 

Duplicate FGD Effluent 

Concentration Average Result 

Relat

Diffe

Zinc ND (10.0) ND (10.0) ND (10.0) Low-Level Total Metals Antimony 14.1 14.2 14.2 Arsenic 67.0 68.9 68.0 Cadmium 25.7 25.9 25.8 Chromium NQ (80.0) NQ (80.0) ND (80.0) Copper NQ (20.0) NQ (20.0) ND (20.0) Lead ND (5.00) ND (5.00) ND (5.00) Mercury 0.154 0.157 0.156 Nickel 363 399 381 Selenium 2,500 2,500 2,500 Thallium 31.0 31.2 31.1 Zinc NQ (50.0) NQ (50.0) ND (50.0) Low-Level Dissolved Metals Antimony 13.3 14.1 13.7 Arsenic 73.0 71.7 72.4 Cadmium 22.1 22.2 22.2 Chromium NQ (80.0) NQ (80.0) ND (80.0) Hexavalent Chromium ND (5.00) ND (5.00) ND (5.00) Copper NQ (20.0) NQ (20.0) ND (20.0) Lead ND (5.00) ND (5.00) ND (5.00) Mercury 0.0708 0.0668 0.0688 
5-9 

> – Result above measurement range. NA – Not analyzed. NC – Not calculated. ND – Not detected (number in parenthesis is the report limit). NQ – Analyte was measured above the method detection limit, but below the report limit (number in parenthesis is the report limit). Thpresented in Appendix A with a J flag designation. R – MS/MSD % Recovery outside method acceptance criteria. T – MS/MSD RPD outside method acceptance criteria. < – Average result includes at least one non-detect value. (Calculation uses detection limit for non-detected results). 

Table 5-2. Field Duplicate Results, Big Bend 

Analyte

Original FGD Effluent 

Concentration 

Duplicate FGD Effluent 

Concentration Average Result 

Relat

Diffe

Nickel 402 390 396 Selenium 2,560 2,550 2,560 Thallium 31.3 31.6 31.5 Zinc NQ (50.0) NQ (50.0) ND (50.0) 
6-1

6. REFERENCES

1. Eastern Research Group, Inc., 2007. Sampling Plan, Tampa Electric Company’s Big 

Bend Station. July 10. DCN 04815A1. EPA-HQ-OW-2006-0071-0630.1. 

2. Eastern Research Group, Inc., 2007. Quality Assurance Project Plan for the Steam 

Electric Detailed Study. September 25. DCN 05079. EPA-HQ-OW-2006-0071-0724. 

3. U.S. EPA. 2001. Method 200.7: Trace Elements in Water, Solids, and Biosolids, by 

Inductively Coupled Plasma-Atomic Emission Spectrometry. Revision 5.0. EPA-821-R01-010. January. 
Appendix A 

ANALYTICAL RESULTS 
A-1 

CJ – Calculated J-value. The J-value was calculated using the filtered aqueous and/or the filtered solid analytical results, including J-va

one of the sample fraction analytical results (i.e., filtered aqueous and/or filtered solid concentration) was measured above the method dcalculated total sample concentration is less than the calculated sample-specific report limit. NA – Not applicable. Calculated value. NC – A sample-specific MDL was not calculated for the analyte. ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is presentmetals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit). J – Result measured above the MDL, but less than the reporting limit. L – Sample result between 5x and 10x blank result. 

Table A-1. FGD Influent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor

Sample-Specific 

MDL 

Sample-Specifi

RL 

Classical Pollutants – Total Ammonia As Nitrogen (NH3-N) 4500-NH3F MG/L NA NP NP Total Kjeldahl Nitrogen (TKN) 4500-N,C MG/L NA NP NP Biochemical Oxygen Demand (BOD) 5210B MG/L 300 NP NP Chloride 4500-CL-C MG/L NA NP NP Hexane Extractable Material (HEM) 1664A MG/L 1 NP NP Sulfate D516-90 MG/L NA NP NP Total Dissolved Solids (TDS) 2540 C MG/L 1 NP NP Total Phosphorus 365.3 MG/L NA NP NP Total Suspended Solids (TSS) 2540 D MG/L 1 NP NP Classical Pollutants – Solid (wet weight) Ammonia As Nitrogen (NH3-N) 4500-NH3F MG/KG 1 NP NP Total Kjeldahl Nitrogen (TKN) 4500-N,C MG/KG 1 NP NP Chloride 4500-CL-C MG/KG 1 NP NP Sulfate D516-90 MG/KG 50 NP NP Total Phosphorus 365.3 MG/KG 1 NP NP Classical Pollutants – Filtered Aqueous Ammonia As Nitrogen (NH3-N) 4500-NH3F MG/L 1 NP NP Total Kjeldahl Nitrogen (TKN) 4500-N,C MG/L 1 NP NP 
A-2 

CJ – Calculated J-value. The J-value was calculated using the filtered aqueous and/or the filtered solid analytical results, including J-va

one of the sample fraction analytical results (i.e., filtered aqueous and/or filtered solid concentration) was measured above the method dcalculated total sample concentration is less than the calculated sample-specific report limit. NA – Not applicable. Calculated value. NC – A sample-specific MDL was not calculated for the analyte. ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is presentmetals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit). J – Result measured above the MDL, but less than the reporting limit. L – Sample result between 5x and 10x blank result. 

Table A-1. FGD Influent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor

Sample-Specific 

MDL 

Sample-Specifi

RL 

Chloride 4500-CL-C MG/L 50 NP NP Sulfate D516-90 MG/L 100 NP NP Total Phosphorus 365.3 MG/L 1 NP NP Routine Metals – Total Aluminum 200.7 UG/L 1 10.6 50.0 Antimony 200.7 UG/L 1 0.700 20.0 Arsenic 200.7 UG/L 1 0.500 10.0 Barium 200.7 UG/L 1 0.100 2.00 Beryllium 200.7 UG/L 1 0.500 5.00 Boron 200.7 UG/L 100 270 10,000 Cadmium 200.7 UG/L 1 0.100 5.00 Calcium 200.7 UG/L 100 510 5,000 Chromium 200.7 UG/L 1 0.200 10.0 Cobalt 200.7 UG/L 1 0.600 50.0 Copper 200.7 UG/L 1 0.200 10.0 Iron 200.7 UG/L 1 5.40 100 Lead 200.7 UG/L 1 0.700 50.0 Magnesium 200.7 UG/L 10 89.0 2,000 Manganese 200.7 UG/L 10 2.00 150 
A-3 

CJ – Calculated J-value. The J-value was calculated using the filtered aqueous and/or the filtered solid analytical results, including J-va

one of the sample fraction analytical results (i.e., filtered aqueous and/or filtered solid concentration) was measured above the method dcalculated total sample concentration is less than the calculated sample-specific report limit. NA – Not applicable. Calculated value. NC – A sample-specific MDL was not calculated for the analyte. ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is presentmetals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit). J – Result measured above the MDL, but less than the reporting limit. L – Sample result between 5x and 10x blank result. 

Table A-1. FGD Influent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor

Sample-Specific 

MDL 

Sample-Specifi

RL 

Mercury 245.1 UG/L NA NC 10.0 Molybdenum 200.7 UG/L 1 0.200 10.0 Nickel 200.7 UG/L 1 1.10 50.0 Selenium 200.7 UG/L 1 0.600 5.00 Silver 200.7 UG/L 1 0.400 20.0 Sodium 200.7 UG/L 10 405 5,000 Thallium 200.7 UG/L 1 0.500 10.0 Tin 200.7 UG/L 1 0.400 30.0 Titanium 200.7 UG/L 1 0.200 10.0 Vanadium 200.7 UG/L 1 0.600 20.0 Yttrium 200.7 UG/L 1 0.200 5.00 Zinc 200.7 UG/L 1 0.200 10.0 Routine Metals – Dissolved Aluminum 200.7 UG/L 1 10.6 50.0 Antimony 200.7 UG/L 1 0.700 20.0 Arsenic 200.7 UG/L 1 0.500 10.0 Barium 200.7 UG/L 1 0.100 2.00 Beryllium 200.7 UG/L 1 0.500 5.00 Boron 200.7 UG/L 100 270 10,000 
A-4 

CJ – Calculated J-value. The J-value was calculated using the filtered aqueous and/or the filtered solid analytical results, including J-va

one of the sample fraction analytical results (i.e., filtered aqueous and/or filtered solid concentration) was measured above the method dcalculated total sample concentration is less than the calculated sample-specific report limit. NA – Not applicable. Calculated value. NC – A sample-specific MDL was not calculated for the analyte. ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is presentmetals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit). J – Result measured above the MDL, but less than the reporting limit. L – Sample result between 5x and 10x blank result. 

Table A-1. FGD Influent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor

Sample-Specific 

MDL 

Sample-Specifi

RL 

Cadmium 200.7 UG/L 1 0.100 5.00 Calcium 200.7 UG/L 100 510 5,000 Chromium 200.7 UG/L 1 0.200 10.0 Hexavalent Chromium D1687-92 UG/L 1 1.00 2.00 Cobalt 200.7 UG/L 1 0.600 50.0 Copper 200.7 UG/L 1 0.200 10.0 Iron 200.7 UG/L 1 5.40 100 Lead 200.7 UG/L 1 0.700 50.0 Magnesium 200.7 UG/L 100 890 20,000 Manganese 200.7 UG/L 1 0.200 15.0 Mercury 245.1 UG/L 50 2.50 10.0 Molybdenum 200.7 UG/L 1 0.200 10.0 Nickel 200.7 UG/L 1 1.10 50.0 Selenium 200.7 UG/L 1 0.600 5.00 Silver 200.7 UG/L 1 0.400 20.0 Sodium 200.7 UG/L 100 4,050 50,000 Thallium 200.7 UG/L 1 0.500 10.0 Tin 200.7 UG/L 1 0.400 30.0 Titanium 200.7 UG/L 1 0.200 10.0 
A-5 

CJ – Calculated J-value. The J-value was calculated using the filtered aqueous and/or the filtered solid analytical results, including J-va

one of the sample fraction analytical results (i.e., filtered aqueous and/or filtered solid concentration) was measured above the method dcalculated total sample concentration is less than the calculated sample-specific report limit. NA – Not applicable. Calculated value. NC – A sample-specific MDL was not calculated for the analyte. ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is presentmetals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit). J – Result measured above the MDL, but less than the reporting limit. L – Sample result between 5x and 10x blank result. 

Table A-1. FGD Influent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor

Sample-Specific 

MDL 

Sample-Specifi

RL 

Vanadium 200.7 UG/L 1 0.600 20.0 Yttrium 200.7 UG/L 1 0.200 5.00 Zinc 200.7 UG/L 1 0.200 10.0 Routine Metals – Filtered Aqueous Mercury 245.1 UG/L 50 2.50 10.0 Routine Metals – Solid (wet weight) Mercury 245.5 MG/KG 1 0.00600 0.0200 Routine Metals – Solid (dry weight) Aluminum 200.7 MG/KG NA 2.13 10.1 Antimony 200.7 MG/KG NA 0.141 4.02 Arsenic 200.7 MG/KG NA 0.101 2.01 Barium 200.7 MG/KG NA 0.0201 0.402 Beryllium 200.7 MG/KG NA 0.101 1.01 Boron 200.7 MG/KG NA 54.3 2,010 Cadmium 200.7 MG/KG NA 0.0201 1.01 Calcium 200.7 MG/KG NA 103 1,010 Chromium 200.7 MG/KG NA 0.0402 2.01 Cobalt 200.7 MG/KG NA 0.121 10.1 Copper 200.7 MG/KG NA 0.0402 2.01 
A-6 

CJ – Calculated J-value. The J-value was calculated using the filtered aqueous and/or the filtered solid analytical results, including J-va

one of the sample fraction analytical results (i.e., filtered aqueous and/or filtered solid concentration) was measured above the method dcalculated total sample concentration is less than the calculated sample-specific report limit. NA – Not applicable. Calculated value. NC – A sample-specific MDL was not calculated for the analyte. ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is presentmetals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit). J – Result measured above the MDL, but less than the reporting limit. L – Sample result between 5x and 10x blank result. 

Table A-1. FGD Influent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor

Sample-Specific 

MDL 

Sample-Specifi

RL 

Iron 200.7 MG/KG NA 1.09 20.1 Lead 200.7 MG/KG NA 0.141 10.1 Magnesium 200.7 MG/KG NA 179 4,020 Manganese 200.7 MG/KG NA 0.402 30.2 Molybdenum 200.7 MG/KG NA 0.0402 2.01 Nickel 200.7 MG/KG NA 0.221 10.1 Selenium 200.7 MG/KG NA 0.121 1.01 Silver 200.7 MG/KG NA 0.0805 4.02 Sodium 200.7 MG/KG NA 815 10,100 Thallium 200.7 MG/KG NA 0.101 2.01 Tin 200.7 MG/KG NA 0.0805 6.04 Titanium 200.7 MG/KG NA 0.0402 2.01 Vanadium 200.7 MG/KG NA 0.121 4.02 Yttrium 200.7 MG/KG NA 0.0402 1.01 Zinc 200.7 MG/KG NA 0.0402 2.01 Low-Level Metals – Total Antimony 1638 UG/L 200 1.40 4.00 Arsenic 1638 UG/L 200 3.04 30.0 Cadmium 1638 UG/L 200 0.200 20.0 
A-7 

CJ – Calculated J-value. The J-value was calculated using the filtered aqueous and/or the filtered solid analytical results, including J-va

one of the sample fraction analytical results (i.e., filtered aqueous and/or filtered solid concentration) was measured above the method dcalculated total sample concentration is less than the calculated sample-specific report limit. NA – Not applicable. Calculated value. NC – A sample-specific MDL was not calculated for the analyte. ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is presentmetals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit). J – Result measured above the MDL, but less than the reporting limit. L – Sample result between 5x and 10x blank result. 

Table A-1. FGD Influent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor

Sample-Specific 

MDL 

Sample-Specifi

RL 

Chromium 1638 UG/L 200 16.6 160 Copper 1638 UG/L 200 0.800 40.0 Lead 1638 UG/L 200 0.200 10.0 Mercury 1631E UG/L 1,000 0.188 0.500 Nickel 1638 UG/L 200 2.60 200 Selenium 1638 UG/L 200 3.20 200 Silver 1638 UG/L 200 0.400 20.0 Thallium 1638 UG/L 200 0.0800 4.00 Zinc 1638 UG/L 200 41.8 100 Low-Level Metals – Dissolved Antimony 1638 UG/L 200 1.40 4.00 Arsenic 1638 UG/L 200 3.04 30.0 Cadmium 1638 UG/L 200 0.200 20.0 Chromium 1638 UG/L 200 16.6 160 Copper 1638 UG/L 200 0.800 40.0 Lead 1638 UG/L 200 0.200 10.0 Mercury 1631E UG/L 100 0.0188 0.0500 Nickel 1638 UG/L 200 2.60 200 Selenium 1638 UG/L 200 3.20 200 
A-8 

CJ – Calculated J-value. The J-value was calculated using the filtered aqueous and/or the filtered solid analytical results, including J-va

one of the sample fraction analytical results (i.e., filtered aqueous and/or filtered solid concentration) was measured above the method dcalculated total sample concentration is less than the calculated sample-specific report limit. NA – Not applicable. Calculated value. NC – A sample-specific MDL was not calculated for the analyte. ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is presentmetals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit). J – Result measured above the MDL, but less than the reporting limit. L – Sample result between 5x and 10x blank result. 

Table A-1. FGD Influent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor

Sample-Specific 

MDL 

Sample-Specifi

RL 

Silver 1638 UG/L 200 0.400 20.0 Thallium 1638 UG/L 200 0.0800 4.00 Zinc 1638 UG/L 200 41.8 100 Low-Level Metals – Solid (dry weight) Antimony 1638 MG/KG NA 0.293 0.837 Arsenic 1638 MG/KG NA 0.636 6.28 Cadmium 1638 MG/KG NA 0.0460 4.19 Chromium 1638 MG/KG NA 3.47 33.5 Copper 1638 MG/KG NA 0.167 8.37 Lead 1638 MG/KG NA 0.0418 2.09 Mercury 1631E MG/KG NA 0.105 0.0393 Nickel 1638 MG/KG NA 0.544 41.8 Selenium 1638 MG/KG NA 0.667 41.8 Silver 1638 MG/KG NA 0.0837 4.19 Thallium 1638 MG/KG NA 0.0167 0.837 Zinc 1638 MG/KG NA 8.75 20.9 
A-9 

Table A-2. ProChem Biphasic Filtration Blank Analytical Results, Big Bend 

Analyte Method Unit 

Dilution 

Factor 

Sample-Specific 

MDL 

Sample-Specific 

RL Concentration 

Mercury 245.1 UG/L 1 0.0500 0.200 ND (0.200) U 

ND – Not detected (number in parenthesis is the report limit). 

U – Result below the MDL. Number shown in parentheses is the reporting limit). 
A-10 

ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is present

metals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit).

R – MS/MSD % Recovery outside method acceptance criteria. J – Result measured above the MDL, but less than the reporting limit. T – MS/MSD RPD outside method acceptance criteria. 

Table A-3. FGD Effluent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor 

SampleSpecific MDL Sample- Specific RL 

Classical Pollutants – Total Ammonia As Nitrogen (NH3-N) 4500-NH3F MG/L 1 NP NP Total Kjeldahl Nitrogen (TKN) 4500-N,C MG/L 1 NP NP Biochemical Oxygen Demand (BOD) 5210B MG/L 300 NP NP Chloride 4500-CL-C MG/L 50 NP NP Hexane Extractable Material (HEM) 1664A MG/L 1 NP NP Silica Gel Treated HEM (SGT-HEM) 1664A MG/L 1 NP NP Sulfate D516-90 MG/L 50 NP NP Total Dissolved Solids (TDS) 2540 C MG/L 1 NP NP Total Phosphorus 365.3 MG/L 1 NP NP Total Suspended Solids (TSS) 2540 D MG/L 1 NP NP Routine Metals – Total Aluminum 200.7 UG/L 1 10.6 50.0 Antimony 200.7 UG/L 1 0.700 20.0 Arsenic 200.7 UG/L 1 0.500 10.0 Barium 200.7 UG/L 1 0.100 2.00 Beryllium 200.7 UG/L 1 0.500 5.00 Boron 200.7 UG/L 100 270 10,000 Cadmium 200.7 UG/L 1 0.100 5.00 Calcium 200.7 UG/L 100 510 5,000 Chromium 200.7 UG/L 1 0.200 10.0 Cobalt 200.7 UG/L 1 0.600 50.0 
A-11 

ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is present

metals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit).

R – MS/MSD % Recovery outside method acceptance criteria. J – Result measured above the MDL, but less than the reporting limit. T – MS/MSD RPD outside method acceptance criteria. 

Table A-3. FGD Effluent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor 

SampleSpecific MDL Sample- Specific RL 

Copper 200.7 UG/L 1 0.200 10.0 Iron 200.7 UG/L 1 5.40 100 Lead 200.7 UG/L 1 0.700 50.0 Magnesium 200.7 UG/L 100 890 20,000 Manganese 200.7 UG/L 1 0.200 15.0 Mercury 245.1 UG/L 50 2.50 10.0 Molybdenum 200.7 UG/L 1 0.200 10.0 Nickel 200.7 UG/L 1 1.10 50.0 Selenium 200.7 UG/L 1 0.600 5.00 Silver 200.7 UG/L 1 0.400 20.0 Sodium 200.7 UG/L 100 4,050 50,000 Thallium 200.7 UG/L 1 0.500 10.0 Tin 200.7 UG/L 1 0.400 30.0 Titanium 200.7 UG/L 1 0.200 10.0 Vanadium 200.7 UG/L 1 0.600 20.0 Yttrium 200.7 UG/L 1 0.200 5.00 Zinc 200.7 UG/L 1 0.200 10.0 Routine Metals – Dissolved Aluminum 200.7 UG/L 1 10.6 50.0 Antimony 200.7 UG/L 1 0.700 20.0 Arsenic 200.7 UG/L 1 0.500 10.0 Barium 200.7 UG/L 1 0.100 2.00 
A-12 

ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is present

metals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit).

R – MS/MSD % Recovery outside method acceptance criteria. J – Result measured above the MDL, but less than the reporting limit. T – MS/MSD RPD outside method acceptance criteria. 

Table A-3. FGD Effluent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor 

SampleSpecific MDL Sample- Specific RL 

Beryllium 200.7 UG/L 1 0.500 5.00 Boron 200.7 UG/L 100 270 10,000 Cadmium 200.7 UG/L 1 0.100 5.00 Calcium 200.7 UG/L 100 510 5,000 Chromium 200.7 UG/L 1 0.200 10.0 Hexavalent Chromium D1687-92 UG/L 1 1.00 2.00 Cobalt 200.7 UG/L 1 0.600 50.0 Copper 200.7 UG/L 1 0.200 10.0 Iron 200.7 UG/L 1 5.40 100 Lead 200.7 UG/L 1 0.700 50.0 Magnesium 200.7 UG/L 100 890 20,000 Manganese 200.7 UG/L 1 0.200 15.0 Mercury 245.1 UG/L 50 2.50 10.0 Molybdenum 200.7 UG/L 1 0.200 10.0 Nickel 200.7 UG/L 1 1.10 50.0 Selenium 200.7 UG/L 1 0.600 5.00 Silver 200.7 UG/L 1 0.400 20.0 Sodium 200.7 UG/L 100 4,050 50,000 Thallium 200.7 UG/L 1 0.500 10.0 Tin 200.7 UG/L 1 0.400 30.0 Titanium 200.7 UG/L 1 0.200 10.0 Vanadium 200.7 UG/L 1 0.600 20.0 
A-13 

ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is present

metals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit).

R – MS/MSD % Recovery outside method acceptance criteria. J – Result measured above the MDL, but less than the reporting limit. T – MS/MSD RPD outside method acceptance criteria. 

Table A-3. FGD Effluent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor 

SampleSpecific MDL Sample- Specific RL 

Yttrium 200.7 UG/L 1 0.200 5.00 Zinc 200.7 UG/L 1 0.200 10.0 Low-Level Metals – Total Antimony 1638 UG/L 100 0.700 2.00 Arsenic 1638 UG/L 100 1.52 15.0 Cadmium 1638 UG/L 100 0.100 10.0 Chromium 1638 UG/L 100 8.30 80.0 Copper 1638 UG/L 100 0.400 20.0 Lead 1638 UG/L 100 0.100 5.00 Mercury 1631E UG/L 1 0.000188 0.000500 Nickel 1638 UG/L 100 1.30 100 Selenium 1638 UG/L 100 1.60 100 Silver 1638 UG/L 100 0.200 10.0 Thallium 1638 UG/L 100 0.0400 2.00 Zinc 1638 UG/L 100 20.9 50.0 Low-Level Metals – Dissolved Antimony 1638 UG/L 100 0.700 2.00 Arsenic 1638 UG/L 100 1.52 15.0 Cadmium 1638 UG/L 100 0.100 10.0 Chromium 1638 UG/L 100 8.30 80.0 Hexavalent Chromium 1636 UG/L 10 3.50 5.00 Copper 1638 UG/L 100 0.400 20.0 
A-14 

ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is present

metals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit).

R – MS/MSD % Recovery outside method acceptance criteria. J – Result measured above the MDL, but less than the reporting limit. T – MS/MSD RPD outside method acceptance criteria. 

Table A-3. FGD Effluent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor 

SampleSpecific MDL Sample- Specific RL 

Lead 1638 UG/L 100 0.100 5.00 Mercury 1631E UG/L 1 0.000188 0.000500 Nickel 1638 UG/L 100 1.30 100 Selenium 1638 UG/L 100 1.60 100 Silver 1638 UG/L 100 0.200 10.0 Thallium 1638 UG/L 100 0.0400 2.00 Zinc 1638 UG/L 100 20.9 50.0 
A-15 

> – Result above measurement range. ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is present

metals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit). J – Result measured above the MDL, but less than the reporting limit. 

Table A-4. Duplicate of FGD Effluent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor Sample-Specific MDL Sample-Specific R

Classical Pollutants – Total Ammonia As Nitrogen (NH3-N) 4500-NH3F MG/L 1 NP NP Total Kjeldahl Nitrogen (TKN) 4500-N,C MG/L 1 NP NP Biochemical Oxygen Demand (BOD) 5210B MG/L 300 NP NP Chloride 4500-CL-C MG/L 50 NP NP Sulfate D516-90 MG/L 50 NP NP Total Dissolved Solids (TDS) 2540 C MG/L 1 NP NP Total Phosphorus 365.3 MG/L 1 NP NP Total Suspended Solids (TSS) 2540 D MG/L 1 NP NP Routine Metals – Total Aluminum 200.7 UG/L 1 10.6 50.0 Antimony 200.7 UG/L 1 0.700 20.0 Arsenic 200.7 UG/L 1 0.500 10.0 Barium 200.7 UG/L 1 0.100 2.00 Beryllium 200.7 UG/L 1 0.500 5.00 Boron 200.7 UG/L 100 270 10,000 Cadmium 200.7 UG/L 1 0.100 5.00 Calcium 200.7 UG/L 100 510 5,000 Chromium 200.7 UG/L 1 0.200 10.0 Cobalt 200.7 UG/L 1 0.600 50.0 Copper 200.7 UG/L 1 0.200 10.0 Iron 200.7 UG/L 1 5.40 100 Lead 200.7 UG/L 1 0.700 50.0 Magnesium 200.7 UG/L 100 890 20,000 Manganese 200.7 UG/L 1 0.200 15.0 
A-16 

> – Result above measurement range. ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is present

metals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit). J – Result measured above the MDL, but less than the reporting limit. 

Table A-4. Duplicate of FGD Effluent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor Sample-Specific MDL Sample-Specific R

Mercury 245.1 UG/L 50 2.50 10.0 Molybdenum 200.7 UG/L 1 0.200 10.0 Nickel 200.7 UG/L 1 1.10 50.0 Selenium 200.7 UG/L 1 0.600 5.00 Silver 200.7 UG/L 1 0.400 20.0 Sodium 200.7 UG/L 100 4,050 50,000 Thallium 200.7 UG/L 1 0.500 10.0 Tin 200.7 UG/L 1 0.400 30.0 Titanium 200.7 UG/L 1 0.200 10.0 Vanadium 200.7 UG/L 1 0.600 20.0 Yttrium 200.7 UG/L 1 0.200 5.00 Zinc 200.7 UG/L 1 0.200 10.0 Routine Metals – Dissolved Aluminum 200.7 UG/L 1 10.6 50.0 Antimony 200.7 UG/L 1 0.700 20.0 Arsenic 200.7 UG/L 1 0.500 10.0 Barium 200.7 UG/L 1 0.100 2.00 Beryllium 200.7 UG/L 1 0.500 5.00 Boron 200.7 UG/L 100 270 10,000 Cadmium 200.7 UG/L 1 0.100 5.00 Calcium 200.7 UG/L 100 510 5,000 Chromium 200.7 UG/L 1 0.200 10.0 Hexavalent Chromium D1687-92 UG/L 1 1.00 2.00 Cobalt 200.7 UG/L 1 0.600 50.0 Copper 200.7 UG/L 1 0.200 10.0 
A-17 

> – Result above measurement range. ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is present

metals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit). J – Result measured above the MDL, but less than the reporting limit. 

Table A-4. Duplicate of FGD Effluent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor Sample-Specific MDL Sample-Specific R

Iron 200.7 UG/L 1 5.40 100 Lead 200.7 UG/L 1 0.700 50.0 Magnesium 200.7 UG/L 100 890 20,000 Manganese 200.7 UG/L 1 0.200 15.0 Mercury 245.1 UG/L 50 2.50 10.0 Molybdenum 200.7 UG/L 1 0.200 10.0 Nickel 200.7 UG/L 1 1.10 50.0 Selenium 200.7 UG/L 1 0.600 5.00 Silver 200.7 UG/L 1 0.400 20.0 Sodium 200.7 UG/L 100 4,050 50,000 Thallium 200.7 UG/L 1 0.500 10.0 Tin 200.7 UG/L 1 0.400 30.0 Titanium 200.7 UG/L 1 0.200 10.0 Vanadium 200.7 UG/L 1 0.600 20.0 Yttrium 200.7 UG/L 1 0.200 5.00 Zinc 200.7 UG/L 1 0.200 10.0 Low-Level Metals – Total Antimony 1638 UG/L 100 0.700 2.00 Arsenic 1638 UG/L 100 1.52 15.0 Cadmium 1638 UG/L 100 0.100 10.0 Chromium 1638 UG/L 100 8.30 80.0 Copper 1638 UG/L 100 0.400 20.0 Lead 1638 UG/L 100 0.100 5.00 Mercury 1631E UG/L 1 0.000188 0.000500 Nickel 1638 UG/L 100 1.30 100 
A-18 

> – Result above measurement range. ND – Not detected (number in parenthesis is the report limit). NP – Not provided. The sample-specific MDL and sample-specific RL are only provided for the metal analytes because EPA is present

metals that are quantified below the report limit. For this analyte, only values above the report limit are presented. If the analyte was nolimit, the report limit is presented in parentheses in the concentration column. U – Result below the MDL. Number shown in parentheses is the reporting limit). J – Result measured above the MDL, but less than the reporting limit. 

Table A-4. Duplicate of FGD Effluent Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor Sample-Specific MDL Sample-Specific R

Selenium 1638 UG/L 100 1.60 100 Silver 1638 UG/L 100 0.200 10.0 Thallium 1638 UG/L 100 0.0400 2.00 Zinc 1638 UG/L 100 20.9 50.0 Low-Level Metals – Dissolved Antimony 1638 UG/L 100 0.700 2.00 Arsenic 1638 UG/L 100 1.52 15.0 Cadmium 1638 UG/L 100 0.100 10.0 Chromium 1638 UG/L 100 8.30 80.0 Hexavalent Chromium 1636 UG/L 10 3.50 5.00 Copper 1638 UG/L 100 0.400 20.0 Lead 1638 UG/L 100 0.100 5.00 Mercury 1631E UG/L 1 0.000188 0.000500 Nickel 1638 UG/L 100 1.30 100 Selenium 1638 UG/L 100 1.60 100 Silver 1638 UG/L 100 0.200 10.0 Thallium 1638 UG/L 100 0.0400 2.00 Zinc 1638 UG/L 100 20.9 50.0 
ND – Not detected (number in parenthesis is the report limit). 

A-19 

Table A-5. Bottle Blank and Equipment Blank Analytical Data, Big Bend 

Analyte Method Process Units Concentration 

LDPE 1000 ml Plastic Bottles – Bottle Blank (for low-level metals samples)

Aluminum EPA 1638 Dissolved UG/L ND (2.0) 

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 500 ml Plastic Bottles – Bottle Blank (for low-level hexavalent chromium samples)

Aluminum EPA 1638 Dissolved UG/L ND (2.0) 

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) 
ND – Not detected (number in parenthesis is the report limit). 

A-20 

Table A-5. Bottle Blank and Equipment Blank Analytical Data, Big Bend 

Analyte Method Process Units Concentration 

Flint 125 ml Amber Glass Bottles – Bottle Blank (for speciation samples)

Aluminum EPA 1638 Dissolved UG/L ND (2.0) 

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) 

Flint 250 ml Glass Bottles – Bottle Blank (for low-level mercury samples)

Mercury EPA 1631E Total Recoverable UG/L ND (0.00020) 

Capsule Filter – Equipment Blank (for dissolved low-level metals sample collection)

Aluminum EPA 1638 Dissolved UG/L ND (2.0) 

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) 

Mercury EPA 1631E Dissolved UG/L ND (0.00020) 

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) 
ND – Not detected (number in parenthesis is the report limit). 

A-21 

Table A-5. Bottle Blank and Equipment Blank Analytical Data, Big Bend 

Analyte Method Process Units Concentration 

Zinc EPA 1638 Dissolved UG/L ND (0.50) 

LDPE 4000 ml Plastic Bottles – Bottle Blank (for low-level metals field blank water)

Aluminum EPA 1638 Dissolved UG/L ND (2.0) 

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) 

Borosilicate 1000 ml Glass Bottles – Bottle Blank (for low-level mercury field blank water)

Mercury EPA 1631E Total Recoverable UG/L ND (0.00020) 

LDPE 10 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) 

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) 

Mercury EPA 1631E Total Recoverable UG/L ND (0.00020) 

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) 
ND – Not detected (number in parenthesis is the report limit). 

A-22 

Table A-5. Bottle Blank and Equipment Blank Analytical Data, Big Bend 

Analyte Method Process Units Concentration 

Vanadium EPA 1638 Dissolved UG/L ND (1.0) 

Zinc EPA 1638 Dissolved UG/L ND (0.50) 

Pump-Off Tubing Set – Equipment Blank (Teflon® and silicone tubing for dissolved sample collection for 

low-level metals)

Aluminum EPA 1638 Dissolved UG/L ND (2.0) 

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) 

Mercury EPA 1631E Total Recoverable UG/L ND (0.00020) 

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) 

C-Flex Tubing Set – Equipment Blank (silicone tubing for sample collection for low-level mercury and 

metals from sample taps)

Aluminum EPA 1638 Dissolved UG/L ND (2.0) 

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) 

Mercury EPA 1631E Total Recoverable UG/L ND (0.00020) 

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) 
ND – Not detected (number in parenthesis is the report limit). 

A-23 

Table A-5. Bottle Blank and Equipment Blank Analytical Data, Big Bend 

Analyte Method Process Units Concentration 

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) 
A-24 

ND – Not detected (number in parenthesis is the report limit). U – Result below the MDL. Number shown in parentheses is the reporting limit). J – Result measured above the MDL, but less than the reporting limit. 

Table A-6. FGD Influent Field Blank Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor 

Sample-Specific 

MDL 

Sample-Specific 

RL C

Low-Level Metals – Total Antimony 1638 UG/L 1 0.00700 0.0200 Arsenic 1638 UG/L 1 0.0152 0.150 Cadmium 1638 UG/L 1 0.00100 0.100 Chromium 1638 UG/L 1 0.0830 0.800 Copper 1638 UG/L 1 0.00400 0.200 Lead 1638 UG/L 1 0.00100 0.0500 Mercury 1631E UG/L 1 0.000188 0.000500 Nickel 1638 UG/L 1 0.0130 1.00 Selenium 1638 UG/L 1 0.0160 1.00 Silver 1638 UG/L 1 0.00200 0.100 Thallium 1638 UG/L 1 0.000400 0.0200 Zinc 1638 UG/L 1 0.209 0.500 Low-Level Metals – Dissolved Antimony 1638 UG/L 1 0.00700 0.0200 Arsenic 1638 UG/L 1 0.0152 0.150 Cadmium 1638 UG/L 1 0.00100 0.100 Chromium 1638 UG/L 1 0.0830 0.800 Copper 1638 UG/L 1 0.00400 0.200 Lead 1638 UG/L 1 0.00100 0.0500 Nickel 1638 UG/L 1 0.0130 1.00 Selenium 1638 UG/L 1 0.0160 1.00 Silver 1638 UG/L 1 0.00200 0.100 Thallium 1638 UG/L 1 0.000400 0.0200 Zinc 1638 UG/L 1 0.209 0.500 
A-25 

ND – Not detected (number in parenthesis is the report limit). J – Result measured above the MDL, but less than the reporting limit. U – Result below the MDL. Number shown in parentheses is the reporting limit). 

Table A-7. FGD Effluent Field Blank Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor 

SampleSpecific MDL Sample-Specific RL C

Routine Metals – Total Aluminum 200.7 UG/L 1 10.6 50.0 Antimony 200.7 UG/L 1 0.700 20.0 Arsenic 200.7 UG/L 1 0.500 10.0 Barium 200.7 UG/L 1 0.100 2.00 Beryllium 200.7 UG/L 1 0.500 5.00 Boron 200.7 UG/L 1 2.70 100 Cadmium 200.7 UG/L 1 0.100 5.00 Calcium 200.7 UG/L 1 5.10 50.0 Chromium 200.7 UG/L 1 0.200 10.0 Cobalt 200.7 UG/L 1 0.600 50.0 Copper 200.7 UG/L 1 0.200 10.0 Iron 200.7 UG/L 1 5.40 100 Lead 200.7 UG/L 1 0.700 50.0 Magnesium 200.7 UG/L 1 8.90 200 Manganese 200.7 UG/L 1 0.200 15.0 Mercury 245.1 UG/L 1 0.0500 0.200 Molybdenum 200.7 UG/L 1 0.200 10.0 Nickel 200.7 UG/L 1 1.10 50.0 Selenium 200.7 UG/L 1 0.600 5.00 Silver 200.7 UG/L 1 0.400 20.0 Sodium 200.7 UG/L 1 40.5 500 Thallium 200.7 UG/L 1 0.500 10.0 Tin 200.7 UG/L 1 0.400 30.0 Titanium 200.7 UG/L 1 0.200 10.0 Vanadium 200.7 UG/L 1 0.600 20.0 
A-26 

ND – Not detected (number in parenthesis is the report limit). J – Result measured above the MDL, but less than the reporting limit. U – Result below the MDL. Number shown in parentheses is the reporting limit). 

Table A-7. FGD Effluent Field Blank Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor 

SampleSpecific MDL Sample-Specific RL C

Yttrium 200.7 UG/L 1 0.200 5.00 Zinc 200.7 UG/L 1 0.200 10.0 Routine Metals – Dissolved Aluminum 200.7 UG/L 1 10.6 50.0 Antimony 200.7 UG/L 1 0.700 20.0 Arsenic 200.7 UG/L 1 0.500 10.0 Barium 200.7 UG/L 1 0.100 2.00 Beryllium 200.7 UG/L 1 0.500 5.00 Boron 200.7 UG/L 1 2.70 100 Cadmium 200.7 UG/L 1 0.100 5.00 Calcium 200.7 UG/L 1 5.10 50.0 Chromium 200.7 UG/L 1 0.200 10.0 Hexavalent Chromium D1687-92 UG/L 1 1.00 2.00 Cobalt 200.7 UG/L 1 0.600 50.0 Copper 200.7 UG/L 1 0.200 10.0 Iron 200.7 UG/L 1 5.40 100 Lead 200.7 UG/L 1 0.700 50.0 Magnesium 200.7 UG/L 1 8.90 200 Manganese 200.7 UG/L 1 0.200 15.0 Mercury 245.1 UG/L 1 0.0500 0.200 Molybdenum 200.7 UG/L 1 0.200 10.0 Nickel 200.7 UG/L 1 1.10 50.0 Selenium 200.7 UG/L 1 0.600 5.00 Silver 200.7 UG/L 1 0.400 20.0 Sodium 200.7 UG/L 1 40.5 500 Thallium 200.7 UG/L 1 0.500 10.0 
A-27 

ND – Not detected (number in parenthesis is the report limit). J – Result measured above the MDL, but less than the reporting limit. U – Result below the MDL. Number shown in parentheses is the reporting limit). 

Table A-7. FGD Effluent Field Blank Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor 

SampleSpecific MDL Sample-Specific RL C

Tin 200.7 UG/L 1 0.400 30.0 Titanium 200.7 UG/L 1 0.200 10.0 Vanadium 200.7 UG/L 1 0.600 20.0 Yttrium 200.7 UG/L 1 0.200 5.00 Zinc 200.7 UG/L 1 0.200 10.0 Low-Level Metals – Total Antimony 1638 UG/L 1 0.00700 0.0200 Arsenic 1638 UG/L 1 0.0152 0.150 Cadmium 1638 UG/L 1 0.00100 0.100 Chromium 1638 UG/L 1 0.0830 0.800 Copper 1638 UG/L 1 0.00400 0.200 Lead 1638 UG/L 1 0.00100 0.0500 Mercury 1631E UG/L 1 0.000188 0.000500 Nickel 1638 UG/L 1 0.0130 1.00 Selenium 1638 UG/L 1 0.0160 1.00 Silver 1638 UG/L 1 0.00200 0.100 Thallium 1638 UG/L 1 0.000400 0.0200 Zinc 1638 UG/L 1 0.209 0.500 Low-Level Metals – Dissolved Antimony 1638 UG/L 1 0.00700 0.0200 Arsenic 1638 UG/L 1 0.0152 0.150 Cadmium 1638 UG/L 1 0.00100 0.100 Chromium 1638 UG/L 1 0.0830 0.800 Hexavalent Chromium 1636 UG/L 5 1.75 2.50 Copper 1638 UG/L 1 0.00400 0.200 Lead 1638 UG/L 1 0.00100 0.0500 
A-28 

ND – Not detected (number in parenthesis is the report limit). J – Result measured above the MDL, but less than the reporting limit. U – Result below the MDL. Number shown in parentheses is the reporting limit). 

Table A-7. FGD Effluent Field Blank Analytical Data, Big Bend 

Analyte Method Unit Dilution Factor 

SampleSpecific MDL Sample-Specific RL C

Nickel 1638 UG/L 1 0.0130 1.00 Selenium 1638 UG/L 1 0.0160 1.00 Silver 1638 UG/L 1 0.00200 0.100 Thallium 1638 UG/L 1 0.000400 0.0200 Zinc 1638 UG/L 1 0.209 0.500 
Appendix B 

ANALYTICAL DATA FOR METALS, FGD WASTEWATER 
B-1 

CJ – Calculated J-value. The J-value was calculated using the filtered aqueous and/or the filtered solid analytical results, including J-values, if applicabsample fraction analytical results (i.e., filtered aqueous and/or filtered solid concentration) was measured above the method detection limit, and the calconcentration is less than the calculated sample-specific report limit. L – Sample result between 5x and 10x blank result. J - Result measured above the MDL, but less than the reporting limit. R – MS/MSD % Recovery outside method acceptance criteria. T – MS/MSD RPD outside method acceptance criteria. U - Result below the MDL. Number shown in parentheses is the reporting limit). NA – Not analyzed. ND – Not detected (number in parenthesis is the report limit). Note: Results shown are not paired samples. See Section 4.2. 

Table B-1. Analytical Results for Metals in the FGD Wastewater Treatment System, Big B

FGD Influent (SP-1) Original FGD Effluent (SP-2) Duplicat

Analyte Method Unit Total Dissolved Total Dissolved Total 

Routine Metals Aluminum 200.7 UG/L 31,200 ND (50.0) U ND (50.0) U ND (50.0) U ND (50.0) Antimony 200.7 UG/L 62.5 33.9 22.3 R 21.1 T 21.9 Arsenic 200.7 UG/L 75.5 18.6 9.73 J 11.1 R,T 9.01 Barium 200.7 UG/L 1,590 1,820 1,570 1,400 1,410 Beryllium 200.7 UG/L 12.9 2.60 J 1.80 J 1.81 J 1.77 Boron 200.7 UG/L 626,000 618,000 346,000 401,000 391,000 Cadmium 200.7 UG/L 224 179 26.0 19.5 23.7 Calcium 200.7 UG/L 6,690,000 4,470,000 4,210,000 5,180,000 4,620,000 Chromium 200.7 UG/L 757 7.84 J 1.31 J 1.24 J 1.49 Hexavalent Chromium D1687-92 UG/L NA 24.0 NA ND (2.00) U NA Cobalt 200.7 UG/L 172 32.0 J 3.05 J 2.30 J 2.68 Copper 200.7 UG/L 120 27.2 10.5 7.82 J 8.56 Iron 200.7 UG/L 23,500 16.5 J 57.4 J 44.6 J 54.7 Lead 200.7 UG/L 69.1 6.33 J 4.97 J 3.96 J 2.97 Magnesium 200.7 UG/L 4,830,000 4,110,000 2,470,000 2,910,000 2,550,000 Manganese 200.7 UG/L 21,900 9,610 63.1 55.6 57.0 Mercury 245.1 UG/L 0.968 CJ ND (10.0) U ND (10.0) U ND (10.0) U ND (10.0) Molybdenum 200.7 UG/L 618 581 470 R 431 T 429 Nickel 200.7 UG/L 2,090 851 231 210 210 Selenium 200.7 UG/L 4,150 3,610 3,020 R 2,860 R 2,790 Silver 200.7 UG/L ND (20.0) U ND (20.0) U ND (20.0) U ND (20.0) U ND (20.0) 
B-2 

CJ – Calculated J-value. The J-value was calculated using the filtered aqueous and/or the filtered solid analytical results, including J-values, if applicabsample fraction analytical results (i.e., filtered aqueous and/or filtered solid concentration) was measured above the method detection limit, and the calconcentration is less than the calculated sample-specific report limit. L – Sample result between 5x and 10x blank result. J - Result measured above the MDL, but less than the reporting limit. R – MS/MSD % Recovery outside method acceptance criteria. T – MS/MSD RPD outside method acceptance criteria. U - Result below the MDL. Number shown in parentheses is the reporting limit). NA – Not analyzed. ND – Not detected (number in parenthesis is the report limit). Note: Results shown are not paired samples. See Section 4.2. 

Table B-1. Analytical Results for Metals in the FGD Wastewater Treatment System, Big B

FGD Influent (SP-1) Original FGD Effluent (SP-2) Duplicat

Analyte Method Unit Total Dissolved Total Dissolved Total 

Sodium 200.7 UG/L 2,530,000 1,970,000 1,530,000 1,850,000 1,650,000 Thallium 200.7 UG/L ND (10.0) U 14.3 17.4 14.2 16.2 Tin 200.7 UG/L 9.48 J 4.89 J 3.48 R 2.84 J 2.08 Titanium 200.7 UG/L 420 12.5 13.7 13.2 13.2 Vanadium 200.7 UG/L 724 108 9.64 R 8.38 J 8.09 Yttrium 200.7 UG/L 245 ND (5.00) U ND (5.00) U ND (5.00) U ND (5.00) Zinc 200.7 UG/L 1,540 16.8 ND (10.0) U ND (10.0) U ND (10.0) Low-Level Metals Antimony 1638 UG/L 24.9 21.9 14.1 13.3 14.2 Arsenic 1638 UG/L 165 137 67.0 73.0 68.9 Cadmium 1638 UG/L 238 190 25.7 22.1 25.9 Chromium 1638 UG/L 651 L ND (160) U 35.7 J 29.0 J 38.5 Hexavalent Chromium 1636 UG/L NA NA NA ND (5.00) U NA Copper 1638 UG/L 103 25.4 J 13.8 J 13.6 J 13.5 Lead 1638 UG/L 69.9 ND (10.0) U ND (5.00) U ND (5.00) U ND (5.00) Mercury 1631E UG/L 16.4 0.206 0.154 0.0708 0.157 Nickel 1638 UG/L 2,570 1,030 363 402 399 Selenium 1638 UG/L 3,470 3,280 2,500 2,560 2,500 Silver 1638 UG/L ND (20.0) U ND (20.0) U 2.07 J 2.92 J 3.74 Thallium 1638 UG/L 39.8 39.4 31.0 31.3 31.2 Zinc 1638 UG/L 1,870 ND (100) U 34.1 J 31.0 J 31.8 
Appendix C 

DATA REVIEW NARRATIVES
Computer Sciences Corporation 

www.csc.com 

6101 Stevenson Avenue 

Alexandria, Virginia 22304 

703.461.2000 Fax 703.461.2020 

MEMORANDUM

DATE: December 5, 2007 

TO: Ron Jordan, Project Officer 

 EPA EAD 

FROM: Sara Clark, Quality Assurance Chemist 

Computer Sciences Corporation 

SUBJECT: Data Review Narrative for Classical Analyses for the Steam Electric Study, Episode 6547 

OVERVIEW

Under EPA Contract Number 68-C-03-058, ProChem Analytical, Inc. submitted classical wet chemistry 

data for four samples in Episode 6547. Sample 70320, identified as FGD influent, was expected to 

contain a significant and variable particulate concentration. EPA and industry representatives were 

concerned that the variable nature of the sample would 1) complicate the collection of a representative 

sample for both EPA and industry analyses and 2) lead to analytical interferences. Therefore, for some 

classical analyses (those with a phase listed in Table 1), the laboratory was directed by EPA to separate 

the FGD influent sample into an aqueous-phase and a solid-phase and analyze each. The two sets of 

results (filtered aqueous and filtered solid phases) are provided in the analytical database, as are 

calculated total results (derived by combining filtered aqueous and filtered solid phase results). 

Table 1 provides a complete listing of samples, matrices, descriptions, sampling dates, phases, and the 

required analytes. 

Table 1 - Sample Identifiers, Descriptions, Sampling Dates and Analytes

EPA Sample # Matrix Sample Description Sampling 

Date Phase Analytes

70320 Aqueous SP-1 – FGD Influent 7/25/07 NA 

BOD (SM 5210B), HEM 

(1664A), SGT-HEM 

(1664A), Hexavalent 

Chromium (ASTM D1687-

92), TSS (SM 2540D), and 

TDS (SM 2540C) 

70320 Aqueous SP-1 – FGD Influent 7/25/07 Filtered 

Aqueous 

Chloride (SM 4500-Cl-

 C), 

Sulfate (ASTM D516-90), 

TKN (SM 4500-N C), 

Ammonia (SM 4500-NH3 

F), Total Phosphorus 

(365.3), and Nitrate/Nitrite 

(SM 4500-NO3 H) 

70320 Aqueous SP-1 – FGD Influent 7/25/07 Filtered 

Solid 

Chloride (SM 4500-Cl- C), 

Sulfate (ASTM D516-90), 

TKN (SM 4500-N C), 

Ammonia (SM 4500-NH3 

F), Total Phosphorus 

(365.3), Nitrate/Nitrite (SM 

4500-NO3 H) and Total 

Solids (2540B) 
2

Table 1 - Sample Identifiers, Descriptions, Sampling Dates and Analytes

EPA Sample # Matrix Sample Description Sampling 

Date Phase Analytes

70320 Aqueous SP-1 – FGD Influent NA Calculated 

Total 

Chloride (SM 4500-Cl-

 C), 

Sulfate (ASTM D516-90), 

TKN (SM 4500-N C), 

Ammonia (SM 4500-NH3 

F), Total Phosphorus 

(365.3), and Nitrate/Nitrite 

(SM 4500-NO3 H) 

70321 Aqueous SP-2 – FGD 

Effluent 7/25/07 NA 

BOD (SM 5210B), HEM 

(1664A), SGT-HEM 

(1664A), Hexavalent 

Chromium (ASTM D1687-

92), TSS (SM 2540D), 

TDS (SM 2540C), 

Chloride (SM 4500-Cl-

 C), 

Total Phosphorus (365.3), 

TKN (SM 4500-N C), 

Nitrate/Nitrite (SM 4500-

NO3 H), Ammonia (SM 

4500-NH3 F), and Sulfate 

(ASTM D516-90) 

70322 Aqueous SP-3 – FGD 

Effluent Duplicate 7/25/07 NA 

BOD (SM 5210B), 

Hexavalent Chromium 

(ASTM D1687-92), TSS 

(SM 2540D), TDS (SM 

2540C), Chloride (SM 

4500-Cl-

 C), Total 

Phosphorus (365.3), TKN 

(SM 4500-N C), 

Nitrate/Nitrite (SM 4500-

NO3 H), Ammonia (SM 

4500-NH3 F), and Sulfate 

(ASTM D516-90) 

70324 Aqueous SP-4 – FGD 

Effluent Field Blank 7/25/07 NA Hexavalent Chromium 

(ASTM D1687-92) 

NA= Not Applicable. In the Phase column, only one result exists in the EPA database for this sample/analyte 

combination. 

These data have been reviewed in accordance with CSC’s Data Review Guidelines for Classical Wet 

Chemistry Analyses (DR-02 Revision 2, September 1, 2007) and with the specifications listed in the 

contract. All data are of acceptable quality with the qualifiers described below and detailed in the data 

review summary table (Table 2). 

SUMMARY

All samples were analyzed within the contract-specified holding times for all classical wet chemistry 

parameters as directed on the accompanying traffic reports, except for Nitrate/Nitrite analysis. 

Nitrate/Nitrite analysis was requested for samples 70320 filtered solid and filtered aqueous phases, 70321, 

and 70322. Data were not submitted due to instrument failure. 

 
3

The calibration and continuing calibration standards were successfully analyzed. Laboratory blanks were 

performed for each analysis, and there was no contamination detected above the laboratory reporting 

limits with the exception of the samples described below. An effluent field blank was analyzed for 

hexavalent chromium and the analyte was not detected above the ML. The QC samples, including the 

ongoing precision and recovery sample (OPR) and matrix spike/matrix spike duplicate (MS/MSD) 

samples, demonstrated that laboratory performance for these analyses was acceptable with the exception 

of the samples described below. 

DATA ISSUES 

SGT-HEM 

The MS and MSD recoveries for sample 70321 were 161% and 176% respectively, above the contract 

acceptance criteria range of 64-132%. Because the sample result was a non-detect respectively, the high 

bias did not affect the data; CSC considers the sample result to be considered acceptable without 

qualification. 

The OPR recovery (170%) associated with sample 70321 was above the contract acceptance criteria range 

of 64-132%. The sample result was a non-detect, therefore the high recovery does not affect the data; the 

sample result is considered acceptable without qualification. 

TKN

TKN was detected in the laboratory preparation blank at a concentration of 0.17 mg/L, which is greater 

than the ML of .1 mg/L. The TKN results for the samples are greater than ten times the preparation blank 

result. Because the presence of the analyte in the blank does not adversely affect the data when the result 

is greater than ten times the associated blank, the TKN data are acceptable without qualification for the 

following associated samples: 70320 filtered aqueous and filtered solid phases, 70321, and 70322. 

TSS 

The TSS result for the FGD effluent sample 70321 was 42 mg/L. The laboratory duplicate result for this 

sample was 21 mg/L. The relative percent difference (RPD) value for sample 70321 and the duplicate is 

66.7%, which is above the contract acceptance criteria of 20%. A reanalysis for sample 70321 was 

performed with similar results confirming the initial analysis. CSC believes that this difference was 

caused by the fact that the laboratory performed the initial and duplicate analyses from different bottles. 

Based on the high RPD, CSC considers the TSS result for sample 70321 to be an estimated value. 

BOD 

The field duplicate effluent sample 70322 BOD result was > 2000 mg/L, due to insufficient sample 

dilution. CSC recommends that the value be qualified as a minimum in the EPA database. 

The BOD sample result for the effluent sample 70321 was 1440 mg/L. The laboratory duplicate result for 

this sample was > 2000 mg/L (again, a minimum due to insufficient dilution). The RPD for sample 

70321 and the laboratory duplicate is > 32%, which is above the contract acceptance criteria of 20%; the 

field duplicate result+ would indicate a similar high RPD. Based on this, CSC recommends that the BOD 

result for sample 70321 be considered an estimated value. 
4

Field Duplicate 

The RPD between samples 70321 (FGD effluent) and 70322 (FGD effluent duplicate) for the following 

analytes were: BOD (33%), total phosphorus (22%) and TSS (67%). CSC does not routinely qualify 

results based on field duplicate RPD. 

TECHNICAL NOTES 

Phase Separation and Calculations 

As described in the phase separation document, EPA’s contract laboratory was asked to measure and 

record the following data as part of the phase separation process: 

• Original sample weight 

• Original sample volume 

• Net weight of solid phase on the filter 

• Filtrate weight 

• Filtrate volume 

These data were required elements of the formula used to calculate a total result; there should be one set 

of these records for each of Group I and Group II analyses. The laboratory failed to provide those items 

listed in bold above. 

CSC calculated the total results for the FGD Influent sample using the following formula: 

Several variables were not recorded by the laboratory as requested—most importantly, the original 

sample volume and filtrate volume. In discussion with the lab, CSC was able to calculate the missing 

variables based on other information that the laboratory was able to provide, including the original sample 

density, original sample weight, and the solid phase weight. This series of calculations are as follows and 

detailed in the phase separation data elements table (Table 3): 

• Original sample weight = (Original sample volume) x (Original sample density) 

• Filtrate weight = (Original sample weight) - (Solid-phase weight) 

• Filtrate volume = (Filtrate weight) / (Original sample density) 

In generating the classicals “Calculated Total” results for the Steam Electric Study, CSC used all values 

greater than the ML. However, if any concentration was affected by contamination in an associated blank 

at less than 5 times the associated blank result, it was changed to a zero before going through the 

calculation, per CSC's data review protocols. Negative values submitted by the laboratory were not used 

in the calculations. 

Please note that the results for the various phases will be labeled in the PROCEDUR field of the EPA 

database as “FILTERED AQUEOUS”, “FILTERED SOLID (WET WEIGHT)”, and “CALCULATED 

TOTAL”. 

Vol. L

(Conc. mg/L x Vol. L) (Conc. mg/kg Wt. kg) Total SampleConcentration mg/L

original sample

Filtrate Filtrate + solid phase × solid phase =
5

Minimum Levels 

When two results are mathematically combined to obtain a Calculated Total result, CSC will report the 

larger of the two MLs associated with each result as the Calculated Total ML. 

Percent Solids 

The laboratory was asked to provide separate percent solids measurements for each sample bottle that was 

phase-separated. However, because this request was received after sample analysis was initiated, the 

laboratory was unable to measure a valid percent solids for the Group 2 bottle. In Table 3, the percent 

solid result is provided for the Group 1 bottle to convert solid phase wet weight basis values to dry weight 

results, and was not used to generate the “Calculated Total” results. 

If you have any questions regarding the analyses of these samples or the review of these data, please 

contact Barbara Beard by telephone at (703) 461-2154, by facsimile at (703) 461-8056, or by email at 

bbeard2@csc.com. 

cc: Brian D’Amico, EPA 

Marla Smith, EPA 

Brian Englert, EPA 

Beverly Randolph, EPA 

Nelson Andrews, EPA 

Deb Bartram, ERG 

TJ Finseth, ERG 

 Lynn Walters, CSC 

 Barbara Beard, CSC 

 Table 2

Data Review Summary Table 

Episode: 6547 Analysis: Classicals 

Industry: Steam Electric Study Reviewer: Sara Clark 

Sample Analyte Action Reason CSC Qual Level

70321 TSS Estimated value 

RPD exceeds the 

contract-specified 

criteria 

NA 42 mg/L 

70321 BOD Estimated value 

RPD exceeds the 

contract-specified 

criteria 

NA 1440 mg/L 

70322 BOD Minimum value Result above 

measurement range > 2000 mg/L 

NA= Not Applicable 
6

 Table 3 

 Phase Separation Data Elements 

Episode: 6547 Analysis: Classicals 

Industry: Steam Electric Study Reviewer: Sara Clark 

Group number I II 

Sample number 70320 70320 

Original sample vol (mL) 928a

 952a 

Net weight of solid phase on the filter (g) 18.33 14.75 

Density (g/mL) 1.0022 1.0022 

Original sample weight (g) 930 954 

Filtrate weight (g) 912a

 939a 

Filtrate volume (mL) 910a

 937a 

Percent Solid (of solid phase) (%) 45.4 NA 

 

 a Derived value. Calculated using lab measured results (if available), or otherwise estimated

 NA: Not applicable 
Computer Sciences Corporation 

www.csc.com 

6101 Stevenson Avenue 

Alexandria, Virginia 22304 

703.461.2000 Fax 703.461.2020 

MEMORANDUM 

DATE: December 5, 2007 

TO: Ron Jordan, Work Assignment Manager 

 EPA EAD 

FROM: Maria A. Vargas, Quality Assurance Chemist

Computer Sciences Corporation 

SUBJECT: Data Review Narrative for Total and Dissolved Metals Analyses for the Steam Electric 

Study, Episode 6547 

Under EPA contract number 68-C-03-044, ProChem Analytical submitted data for the analysis of metals 

by EPA Method 200.7 and mercury by Method 245.1. Four aqueous samples in this episode were 

analyzed for total and dissolved metals. Sample 70320, identified as FGD influent, was expected to 

contain a significant and variable particulate concentration. EPA and industry representatives were 

concerned that the variable nature of the sample would 1) complicate the collection of a representative 

sample for both EPA and industry analyses and 2) lead to analytical interferences. Therefore the 

laboratory was directed by EPA to separate the FGD influent sample into an aqueous-phase and a solidphase, and analyze each for mercury. The two sets of results (filtered aqueous and filtered solid phases) 

are provided in the analytical database, including the calculated total result (derived by combining filtered 

aqueous and filtered solid phase results). 

Table 1 provides a list of samples, matrices, descriptions, sampling dates, phases, and the required 

analytical methods.

Table 1 - Sample Identifiers, Descriptions, Sampling Dates, and Analysis Methods

EPA Sample # Matrix Sample Description Sampling 

Date Phase Methods

7/25/2007 Dissolved 200.7, 245.1 

7/25/2007 Filtered Solid 

7/25/2007 Filtered Aqueous 

70320 Aqueous FGD Influent 

NA Calculated Total 

245.1 

Dissolved 70321 Aqueous FGD Effluent 7/25/2007 Total 200.7, 245.1 

Dissolved 

70322 Aqueous FGD Effluent-Duplicate 7/25/2007 Total 200.7, 245.1 

Dissolved 70324 Aqueous FGD Effluent-Field Blank 7/25/2007 Total 200.7, 245.1 

NA= Not applicable 

These data have been reviewed in accordance with CSC's Data Review Guidelines for Metals Analyses 

(November 2004), the EAD contract, and with the specifications listed in EPA Methods 200.7 (Rev. 5.0), 

and 245.1 (03/83). All data are of acceptable quality with the qualifiers described below and detailed in 

the data review summary table (Table 2). 
2

SUMMARY 

All four samples were successfully analyzed within the contract-specified holding times. The method 

detection limit (MDL) study was performed and was within the contract-specified criteria. Both aqueous 

and solid phase initial precision and recovery (IPR) analysis were performed and were within the contract 

criteria. 

Calibration curves, calibration standards, and calibration blanks were successfully analyzed, with the 

exceptions noted below. Preparation blanks performed for each analysis detected no contamination above 

the laboratory’s reporting limits. QC samples, including ongoing precision and recovery (OPR) samples, 

matrix spike (MS) samples, matrix spike duplicate (MSD) samples, and laboratory serial dilution samples 

demonstrated that laboratory performance for these analyses was acceptable, with the exception of the 

issues described below and summarized in Table 2. The MS/MSD analyses were performed on the total 

and dissolved fractions of sample 70321. 

DATA ISSUES

Method and Analytical Blanks

Several analytes were detected in the preparation blanks (PB), initial calibration blanks (ICBs), and 

continuing calibration blanks (CCBs) associated with the samples in this Episode at concentrations 

greater than the respective MDLs, but less than the method-specified MLs. The data quality is affected as 

follows: 

• Sample Results Greater than Ten Times Blank Results or Analyte Not Detected in Sample: CSC 

does not consider the presence of the analyte in the blank to adversely affect the data in cases 

where the sample results are greater than ten times the associated blank results or where the 

analyte is not detected in associated samples. Several samples fall into this category, but because 

CSC considers such data to be acceptable without qualification, these cases do not merit further 

detail. 

ML Standards 

The recovery of mercury (135%) in the aqueous minimum level standard was above the contract-specified 

criteria of 120%. However, because mercury was not detected in any of the samples in this episode, CSC 

considers the results to be unaffected by this potential high recovery. 

 

Quarterly Quality Control Samples (QCS)

The recovery of calcium (106%) in the quarterly quality control sample (QCS) was marginally above the 

contract-specified criteria (95-105%). The QCS recovery of nickel (94%) and thallium (94%) were 

slightly below the contract-specified criteria (95-105%). However, because the OPR and CCVs were all 

within contract specified criteria, and they are each prepared from separate standard sources, CSC 

recommends that sample data be included in the database without qualification. 

Field Duplicate 

The relative percent difference (RPD) between samples 70322 (FGD effluent duplicate) and 70321 (FGD 

effluent) for dissolved thallium was 27%. CSC does not routinely qualify results based on field duplicate 

RPD. 
3

Matrix Performance 

The relative percent difference (RPD) between the matrix spike and matrix spike duplicate for dissolved 

cadmium (21%) in sample 70321 was marginally above the contract-specified acceptance criteria of 20%. 

CSC considers the result for dissolved cadmium in sample 70321 to be of acceptable quality. 

The MS recovery of dissolved antimony (133%) and molybdenum (135%) in sample 70321 were above 

the contract-specified acceptance criteria of 125%. The MSD recovery of dissolved antimony (162%) 

and molybdenum (255%) in sample 70321 were also above the acceptance criteria. CSC recommends 

that the results for dissolved antimony and molybdenum in sample 70321 be considered of acceptable 

quality but may be maximum values. 

 

The MS recovery of dissolved arsenic (140%) in sample 70321 was above the contract-specified 

acceptance criteria of 125%. The related MSD recovery (177%) and RPD (22%) were also above the 

acceptance criteria. CSC recommends that the result for dissolved arsenic in sample 70321 be considered 

an estimated value. 

The MS recovery of dissolved yttrium (37%) in sample 70321 was below the contract-specified 

acceptance criteria of 75%. The related MSD recovery (135%) and RPD (114%) were above the 

acceptance criteria. Because dissolved yttrium was not detected, CSC recommends that the result in 

sample 70321 be included in the database without qualification. 

The MS recovery of dissolved selenium (126%) in sample 70321 was marginally above the contractspecified criteria of 125%. CSC recommends that the result for dissolved selenium in sample 70321 be 

considered of acceptable quality but may be a maximum value. 

The MS recovery of dissolved aluminum (112%) in sample 70321 was within the contract-specified 

criteria of 75-125%. The related MSD recovery (61%) was below the acceptance criteria. The RPD 

(60%) between the MS and MSD was above the 20% criteria. Since dissolved aluminum was not 

detected, CSC recommends that the result for aluminum in sample 70321 be included in the database 

without qualification. 

The MS recoveries of total antimony (139%) and arsenic (146%) in sample 70321 were above the 

contract-specified acceptance criteria of 125%. The MSD recoveries of total antimony (129%) and 

arsenic (134%) in sample 70321 were also above the acceptance criteria. Since total arsenic was not 

detected, CSC recommends that the result in sample 70321 be included in the database without 

qualification. CSC recommends that the total antimony result in sample 70321 be considered of 

acceptable quality but may be a maximum value. 

The MS recovery of total molybdenum (102%) in sample 70321 was within the contract-specified 

acceptance criteria of 75-125%. The related MSD recovery (69%) was below the acceptance criteria. The 

RPD (6%) between the MS and MSD was within the contract-specified criteria. CSC recommends that 

the result for total molybdenum in sample 70321 be considered a minimum value. 

The MS recovery of total selenium (123%) in sample 70321 was within the contract-specified acceptance 

criteria of 75-125%. The related MSD recovery (131%) was above the acceptance criteria. CSC 

recommends that the result for total selenium in sample 70321 be considered a maximum value. 
4

Serial Dilutions 

The serial dilution percent differences for dissolved copper in sample 70321 (55%) and total copper 

(22%) were above the contract-specified criteria of 10%. However, the MS/MSD recoveries were within 

the criteria for both total and dissolved copper. CSC does not qualify sample data based on serial dilution 

results alone and believes that no further action is required. 

Field Blanks/Filter Blanks 

Boron, calcium, magnesium, and sodium were detected in the dissolved field filter blank sample (70324) 

at concentrations greater than the contract-specified MLs. Calcium and magnesium were the only two 

analytes detected in the total field filter blank (70324). Per EPA request, CSC does not qualify sample 

data or results based on field and filter blanks results. 

TECHNICAL NOTE 

Phase Separation and Calculations 

As described in the phase separation document, EPA’s contract laboratory was asked to measure and 

record the following data as part of the phase separation process: 

• Original sample weight 

• Original sample volume 

• Net weight of solid phase on the filter 

• Filtrate weight 

• Filtrate volume 

The laboratory failed to provide those items listed in bold above. 

CSC calculated the total result for the FGD Influent sample using the following formula: 

Since the laboratory provided only the solid-phase weight, CSC estimated the original sample volume to 

be 500 mL, based on the bottle size, and because the laboratory reported that the bottles were full upon 

receipt. The filtrate volume was calculated using this estimated original volume, solid-phase weight, and 

the density of the original sample measured by the laboratory. This series of calculations are as follows 

and detailed in the phase separation data elements table (Table 3): 

• Original sample weight = (Original sample volume) x (Original sample density) 

• Filtrate weight = (Original sample weight) - (Solid weight) 

• Filtrate volume = (Filtrate weight) / (Original sample density) 

As a result, calculated total data for mercury will be qualified as estimated for sample 70320. 

Additionally, CSC requested that the laboratory measure the volume of a 500-mL bottle of the type used 

for these samples, to further refine the sample volume estimate. A discussion of the uncertainty 

introduced by the volume assumption is included below. 

Vol. L

(Conc. μg/L x Vol. L) (Conc. mg/kg 1000μg/mg x Wt. kg) Total SampleConcentration μg/L

originalsample

Filtrate Filtrate + solid × solid =
5

• According to the laboratory, a 500-mL bottle filled to the rim holds about 510 mL (to the nearest 

mL). 

• Allowing for some variability among the 500-mL bottles and the levels to which each was filled in 

the field, we assume that a “full” bottle holds 500 mL ± 10 mL. 

• Recalculating the results from Episode 6547 using 510 mL as the original volume yields results that 

are 4 % higher than those calculated assuming 490 mL. 

• Therefore, for the metals results in Episode 6547, the volume estimation introduces an error of ± 4 %. 

That difference is well within the expected analytical uncertainty and at least 5 times lower than 

typical acceptance limits for laboratory duplicate analyses (i.e., 20%). 

In the generation of the routine metals “Calculated Total” results, at EPA's request, CSC included 

concentrations that were greater than the MDL but less than the ML. However, if any concentration was 

affected by contamination in an associated blank at less than 5 times the associated blank result, it was 

changed to a zero before going through the calculation, per CSC's data review protocols. Negative values 

submitted by the laboratory were not used in the calculations. 

Please note that the results for the various phases will be labeled in the PROCEDUR field of the EPA 

database as “FILTERED AQUEOUS”, “FILTERED SOLID (WET WEIGHT)”, and “CALCULATED 

TOTAL”. 

Minimum Levels 

When two results are mathematically combined to obtain a Calculated Total result, CSC will report the 

larger of the two MLs associated with each result as the Calculated Total ML. 

Due to severe matrix interferences, the laboratory analyzed several samples at 50-fold dilutions for 

mercury. The affected samples are as follows: filtered aqueous phase and dissolved mercury for sample 

70320; total and dissolved mercury for sample 70321; and total and dissolved mercury for sample 70322. 

Reporting limits for these results have been adjusted for dilution. 

Percent Solids 

CSC notes that there was so little particulate in the bottles sent for the metals analysis of sample 70320 

that ProChem could not determine the percent solids on the filtered solid phase of that sample because the 

majority of the original sample was consumed in analysis. Therefore, for this sample, a percent solids 

evaluation was performed from the Group I influent bottle and summarized in Table 3. The percent solid 

result is provided to convert if desired, solid phase wet weight basis values to dry weight results, and was 

not used to generate the “Calculated Total” results. 

If you have any questions regarding the analyses of these samples or the review of these data, please 

contact Barbara Beard by telephone at (703) 461-2154, by facsimile at (703) 461-8056, or by email at 

bbeard2@csc.com. 

cc: Brian D’Amico, EPA Deb Bartram, ERG 

Beverly Randolph, EPA TJ Finseth, ERG 

Marla Smith, EPA Lynn Walters, CSC 

Nelson Andrews, EPA Barbara Beard, CSC 

Brian Englert, EPA 
6

 

Table 2 

Data Review Summary Table

Episode: 6547 Analysis: Metals

Industry: Steam Electric Study Reviewer: Maria A. Vargas 

Sample Analyte Action Reason CSC Qual Level

70320 

calculated total Hg Estimated value Estimated value used in calculation of total. NA ND 

70321 total Sb Maximum value MS/MSD %R above 

contract-specified criteria NA 22.3 μg/L 

70321 total Mo Minimum value MSD %R below contractspecified criteria NA 470 μg/L 

70321 total Se Maximum value MSD %R above contractspecified criteria NA 3,020 μg/L 

Sb 21.1 μg/L 70321 dissolved 

Mo 

Maximum value MS/MSD %R above 

contract-specified criteria NA 

431 μg/L 

70321 dissolved As Estimated value MS/MSD and RPD above 

contract-specified criteria NA 11.1 μg/L 

70321 dissolved Se Maximum value MS %R above contractspecified criteria NA 2,860 μg/L 

NA= Not Applicable 

ND= Not detected 
7

 Table 3 

 Phase Separation Data Elements 

Episode: 6547 Analysis: Metals 

Industry: Steam Electric Study Reviewer: Maria A. Vargas 

Sample number 70320 

Original sample vol (mL) 500a

Net weight of solid phase on the filter (g) 2.2 

Density (g/mL) 1.0022 

Original sample weight (g) 501.1a

Filtrate weight (g) 498.9a

Filtrate volume (mL) 497.8a

Percent Solid (of solid phase) (%) 45.4b

 

 a

 Derived value. Calculated using lab measured results (if available), or otherwise estimated 

 b

 Value calculated from the Group I bottle 
Computer Sciences Corporation 

www.csc.com

MEMORANDUM 

DATE: January 08, 2008 

TO: Ron Jordan, Work Assignment Manager 

 EPA EAD 

FROM: Lisa White, Quality Assurance Chemist 

Computer Sciences Corporation 

SUBJECT: Data Review Narrative for Total Metals Analyses for the Steam Electric Study, Episodes 

6547 and 6548

Under EPA contract number 68-C-03-044, ProChem Analytical submitted data for the analysis of total 

metals by EPA Method 200.7 for aqueous sample 70320 in Episode 6547 and aqueous sample 70420 in

Episode 6548. Because influent samples for this study were expected to be highly variable in solids 

content, EPA chose to obtain results for the solid phase as well. The solid phase results for sample 70320 

and 70420 were not directly analyzed, but rather calculated from total, dissolved, and TSS results. 

Please note that the results for mercury by Method 245.1 and dissolved metals by Method 200.7 for these 

samples were previously delivered under a separate Data Review Narrative. 

Table 1 provides a list of samples, episodes, matrices, descriptions, sampling dates, phase, and the 

required analytical methods.

Table 1 - Sample Identifiers, Descriptions, Sampling Dates, and Analysis Methods

EPA 

Sample #

Episode 

# Matrix Sample Description Sampling

Date Phase Method

7/25/07 Total

70320 6547 Aqueous FGD Influent

NA Calculated Solid

200.7 

8/22/07 Total

70420 6548 Aqueous FGD Influent

NA Calculated Solid

200.7 

NA = Not Applicable 

These data have been reviewed in accordance with CSC's Data Review Guidelines for Metals Analyses 

(November 2004); the EAD contract; and with the specifications listed in EPA Methods 200.7 (Rev. 5.0). 

All data are of acceptable quality with the qualifiers described below and detailed in the data review 

summary table (Table 2). 

 

SUMMARY 

All samples were successfully analyzed within the method-specified holding times. The method detection

limit (MDL) studies and initial precision and recovery (IPR) analyses were performed and met the 

contract-specified criteria. Calibration curves, calibration standards, and calibration blanks were 

successfully analyzed. Preparation blanks performed for each analysis detected no contamination above 

the laboratory’s reporting limits. QC samples, including ongoing precision and recovery (OPR) samples, 

matrix spike (MS) samples, matrix spike duplicate (MSD) samples, and laboratory serial dilution samples 

demonstrated that laboratory performance for these analyses was acceptable, with the exception of the 

6101 Stevenson Avenue 

Alexandria, Virginia 22304 

703.461.2000 Fax 703.461.2020
2

issues described below and summarized in Table 2. The MS/MSD analyses were performed on sample 

70420. 

DATA ISSUES

Method and Analytical Blanks

Several analytes were detected in the preparation blanks (PBs), initial calibration blanks (ICBs), and 

continuing calibration blanks (CCBs) associated with the samples in this episode at concentrations greater 

than the respective MDLs, but less than the method-specified MLs. The data quality is affected as 

follows: 

• Sample Results Greater than Ten Times Blank Results or Analyte Not Detected in Sample: CSC 

does not consider the presence of the analyte in the blank to adversely affect the data in cases 

where the sample results are greater than ten times the associated blank results or where the 

analyte is not detected in associated samples. Several samples fall into this category, but because 

CSC considers such data to be acceptable without qualification, these cases do not merit further 

detail. 

Matrix Performance 

MS/MSD and Serial Dilution analyses were performed on samples 70420. 

The percent recoveries for total barium in the MS and MSD (18% and 9% respectively) for sample 70420 

were below contract-specified criteria of 75%. In addition, the serial dilution percent difference for total 

barium (16%) was above the contract-specified criteria of 10%. The combination of spike recovery 

failure and serial dilution failure indicates severe matrix interferences. Therefore, CSC recommends that 

the result for total barium in sample 70420 be considered an estimated value. 

 

The percent recovery for total titanium (126%) in the MS for sample 70420 was slightly above the 

contract-specified criteria of 125%. In addition, the serial dilution percent difference (19%) was above the 

contract-specified criteria of 10%. The combination of spike recovery failure and serial dilution failure 

indicates severe matrix interferences. Therefore, CSC recommends that the result for total titanium in 

sample 70420 be considered an estimated value. 

The percent recovery for total nickel (73%) in the MSD for sample 70420 was slightly below the 

contract-specified criteria of 75%. In addition, the serial dilution percent difference (16%) was above the 

contract-specified criteria of 10%. The combination of spike recovery failure and serial dilution failure 

indicates severe matrix interferences. Therefore, CSC recommends that the result for total nickel in 

sample 70420 be considered an estimated value. 

The percent recovery for total selenium (47%) in the MSD for sample 70420 was below the contractspecified criteria of 75%. CSC recommends that the result for total selenium in sample 70420 be 

considered of acceptable quality, but may be a minimum value. 

Total thallium was not recovered in the MS or MSD for sample 70420. In addition, the analyte was not 

detected in the unspiked sample. The laboratory suspected that the increased solids in the sample 

(chloride in particular) were likely the cause. Zero percent recoveries in the matrix spike samples indicate 

significant methodological problems that preclude successful analysis of thallium. Therefore, CSC 

recommends that the results for total thallium and calculated solid thallium in sample 70420 be excluded 

from the database. 
3

The serial dilution percent differences for several analytes were above the contract-specified criteria of 

10% in sample 70420. These instances are as follows: total chromium (14%), cobalt (17%), copper 

(15%), lead (12%), molybdenum (12%), sodium (11%), vanadium (26%), and zinc (17%). In these cases, 

MS/MSD percent recoveries were within acceptable criteria. CSC recommends that the results for these 

analytes be included in the database without qualification.

 TECHNICAL NOTES 

Solid Phase Calculations 

CSC calculated the solid phase results using the following formula:

ug mg

mg kg

TSS mg L

Conc g L Conc g L

original sample

Total Dissolved

10 /

10 /

/

( . / . / ) Solid phase concentration (mg/kg) 3

6

× − = μ μ

In the generation of the Calculated Solid result, at EPA's request, CSC included Total and Dissolved 

concentrations that were greater than the MDL but less than the ML unless both factors in the calculations 

were less than the ML. However, if any concentration was affected by contamination in an associated 

blank at less than 5 times the associated blank result, it was changed to a zero before going through the 

calculation, per CSC's data review protocols. Negative values submitted by the laboratory were not used 

in the calculations. 

The results for the various phases will be labeled in the PROCEDUR field of the EPA database as 

“DISSOLVED”, “TOTAL”, and “CALCULATED SOLID (DRY WEIGHT)”. 

The TSS result for sample 70320 in Episode 6547 is 4970 mg/L. The TSS result for sample 70420 in 

Episode 6548 is 13300 mg/L. 

Minimum Levels 

When two results are mathematically combined to obtain a Calculated Solid result, CSC will report the 

larger of the two MLs associated with each result as the Calculated Solid ML. 

In order to alleviate expected matrix effects, the laboratory performed a 2-fold dilution on sample 70420 

in Episode 6548. MLs are adjusted appropriately.

If you have any questions regarding the analyses of these samples or the review of these data, please 

contact Barbara Beard by telephone at (703) 461-2154, by facsimile at (703) 461-8056, or by email at 

bbeard2@csc.com.

cc: Brian D’Amico, EPA Deb Bartram, ERG 

Beverly Randolph, EPA TJ Finseth, ERG 

Marla Smith, EPA Lynn Watlers, CSC 

Nelson Andrews, EPA Barbara Beard, CSC 

Brian Englert, EPA 

 
4

Table 2 

Data Review Summary Table

Episode: 6547, 6548 Analysis: Metals

Industry: Steam Electric Study Reviewer: Lisa White 

Sample Analyte Action Reason CSC Qual Level

70420 Total Ba Estimated Value 

MS and MSD %R below 

contract-specified criteria; 

Serial Dilution %D above 

contract-specified criteria 

NA See Database 

70420 

Calculated solid Ba Estimated Value 

Dissolved component is a 

Minimum Value; 

Total component is an 

Estimated Value 

NA See Database 

70420 Total Tl Exclude Zero %R in MS and MSD EXCLUDE NA 

70420 

Calculated Solid Tl Exclude Not Calculable EXCLUDE NA 

70420 Total Ti Estimated Value 

MS %R above contractspecified criteria; 

Serial Dilution %D above 

contract-specified criteria 

NA See Database 

70420 

Calculated solid Ti Estimated Value Total component is an 

Estimated Value NA See Database 

70420 Total Ni Estimated Value 

MSD %R below contractspecified criteria; 

Serial Dilution %D above 

contract-specified criteria 

NA See Database 

70420 

Calculated solid Ni Estimated Value Total component is an 

Estimated Value NA See Database 

70420 Total Se Minimum Value MSD %R below contractspecified criteria NA See Database 

70420 

Calculated solid Se Estimated Value 

Total component is a 

Minimum value; 

 Dissolved component is 

an Estimated Value 

NA See Database 

NA= Not applicable 

 
Computer Sciences Corporation 

www.csc.com 

6101 Stevenson Avenue 

Alexandria, Virginia 22304 

703.461.2000 Fax 703.461.2020 

MEMORANDUM 

DATE: December 4, 2007 

TO: Ron Jordan, Work Assignment Manager 

 EPA EAD 

FROM: Cris Robinson, Quality Assurance Chemist 

Computer Sciences Corporation 

SUBJECT: Data Review Narrative for Trace Metals Analyses for the Steam Electric Study, Episode 

6547 

Under EPA contract number 68-C-03-046, Battelle Marine Sciences submitted data for the analyses of 

trace metals. All five aqueous samples in this episode were analyzed for total mercury (Hg) by Method 

1631E. Three of the five (effluent, effluent duplicate, and effluent field blank) were analyzed for 

hexavalent chromium by Method 1636 and total metals including antimony (Sb), arsenic (As), cadmium 

(Cd), copper (Cu), chromium (Cr), lead (Pb), nickel (Ni), selenium (Se), silver (Ag), thallium (Tl), and 

zinc (Zn) by Method 1638 (ICP-MS). Several samples were analyzed for dissolved metals as well as 

total. Because FGD influent samples for this study were expected to be highly variable in solids content, 

EPA chose to obtain results for this phase as well. The solid-phase results for sample 70320 were not 

directly analyzed, but rather calculated from total, dissolved, and TSS results.

Table 1 - Sample Identifiers, Descriptions, Sampling Dates, and Analysis Methods 

EPA Sample # Matrix Sample Description Sampling Date Phase Methods

Total 1631E 

7/25/07 

70320 Aqueous FGD influent Dissolved 1631E 

NA Calculated Solid 1631E 

Total 1631E, 1638

70321 Aqueous FGD effluent 7/25/07 Dissolved 1631E, 1638

NA 1636 

Total 1631E, 1638

70322 Aqueous FGD effluent duplicate 7/25/07 Dissolved 1631E, 1638

NA 1636 

70323 Aqueous FGD influent field blank 7/25/07 NA 1631E 

Total 1631E, 1638

70324 Aqueous FGD effluent field blank 7/25/07 Dissolved 1636, 1638 

NA 1636 

NA = Not applicable

These data have been reviewed in accordance with CSC's Data Review Guidelines for Metals Analyses 

(November 2004), with the EAD contract, and with the specifications listed in EPA Methods 1631E (Aug 

2002), 1636 (Jan 1996), and 1638 (Jan 1996). All data are of acceptable quality with the qualifiers 

described below. 
2

SUMMARY

All 5 samples were successfully analyzed within the method-specified holding times, and initial precision 

and recovery (IPR) analyses and method detection limit (MDL) studies were acceptably performed. 

Except for instances detailed below, all QC samples, including ongoing precision and recovery samples 

(OPR), matrix spike and matrix spike duplicate (MS/MSD) samples, and quality control samples (QCS) 

were within method specified criteria. The MS/MSD analysis was performed on sample 70321. 

Calibration curves and calibration verification standards were successfully analyzed. 

All calibration and preparation blanks were free of contamination above the report limit (minimum level 

or ML). Some analytes were detected at levels above the reporting limit in the field blanks. These blanks 

are discussed in detail below. 

DATA ISSUES

Method and Analytical Blanks

Several analytes were detected in the preparation blanks (PB), initial calibration blanks (ICBs), and 

continuing calibration blanks (CCBs) associated with the samples in this episode at concentrations greater 

than the respective MDLs, but less than the method-specified MLs. The data quality is affected as 

follows: 

• Sample Results Greater than Ten Times Blank Results or Analyte Not Detected in Sample: CSC 

does not consider the presence of the analyte in the blank to adversely affect the data in cases 

where the sample results are greater than ten times the associated blank results or where the 

analyte is not detected in associated samples. Several samples fall into this category, but because 

CSC considers such data to be acceptable without qualification, these cases do not merit further 

detail. 

Field Blanks 

CSC reviewed results from two field blanks. Sample 70323 (influent field blank) exhibited no results 

above the ML. Dissolved chromium, dissolved copper and dissolved zinc were detected at levels above 

the ML in field-filtered sample 70324 (effluent field blank). Hexavalent chromium was detected above 

the ML in sample 70324. Per EPA request, CSC does not qualify results based on field blank 

contamination. 

TSS Duplicate 

Due to lab error, a duplicate for TSS analyses was not performed. Blank and LCS results for TSS were 

acceptable. Because TSS is a secondary analyte used only in the calculation of solid-phase mercury 

results, CSC has not qualified the TSS results because of this omission. 

Laboratory Duplicate 

The RPD for chromium (32%) for a laboratory duplicate performed on dissolved metals sample 70321 

was above the internal laboratory limit (25%). However, because the MS/MSD performed on this sample 

produced an acceptable RPD, and Method 1638 does not specify limits for laboratory duplicates, CSC 

considers the associated result acceptable without qualification. 
3

Field Duplicate 

Field duplicate RPD values were above the method-specified limit (20%) for the following duplicate 

pairs: 

• 70321 and 70322 (effluent and effluent field duplicate) total metals results for Ag (58%) and Cr 

(35%). Note that because Method 1638 does not list chromium as an analyte, there are no 

method-specified limits for chromium field duplicate RPD. In these cases, CSC defaults to the 

limit specified for the other analytes in the method—20%. 

• 70321 and 70322 (effluent and effluent field duplicate) dissolved metals results for Ag (32%). 

CSC does not routinely qualify results based on field duplicate RPD failure. 

TECHNICAL NOTES 

Sample Temperature 

Trace metals samples were not chilled during shipment for this study. 

Additional Analytes 

Two additional analytes, arsenic and chromium, were included for evaluation by Method 1638. Because 

they are not specified in the method, the MLs for these (0.15 μg/L and 0.80 μg/L, respectively) were set 

well above the laboratory-determined MDL. 

Minimum Levels 

A precipitate formed after preservation in dissolved field samples for Method 1638 analysis. Therefore, 

in order to alleviate expected matrix effects, the laboratory performed a 100-fold dilution on all samples 

on which Method 1638 was performed, except the FGD effluent field blank sample 70324. MLs are 

adjusted appropriately. 

Solid-Phase Calculations 

CSC calculated the solid-phase results using the following formula: 

The results for the various phases will be labeled in the PROCEDUR field of the EPA database as 

“DISSOLVED”, “TOTAL”, and “CALCULATED SOLID (DRY WEIGHT)”. 

In the generation of the Calculated Solid result, at EPA's request, CSC included Total and Dissolved 

concentrations that were greater than the MDL but less than the ML. However, if any concentration was 

affected by contamination in an associated blank at less than 5 times the associated blank result, it was 

changed to a zero before going through the calculation, per CSC's data review protocols. Negative values 

submitted by the laboratory were not used in the calculations. 

original sample

Total Dissolved

TSS mg L

Conc g L Conc g L ng g

/

( . / . / ) 1000 / Solid phase concentration (ng/mg or μg/g) μ − μ × μ =
4

When two results are mathematically combined to obtain a Calculated Solid result, CSC will report the 

larger of the two MLs associated with each result as the Calculated Solid ML. 

The TSS result for the sample 70320 bottle analyzed for mercury is 4779 mg/L. 

If you have any questions regarding the analyses of these samples or the review of these data, please 

contact Barbara Beard by telephone at (703) 461-2154, facsimile at (703) 461-8056, or via email at 

bbeard2@csc.com. 

cc: Brian Damico, EPA 

 Beverly Randolph, EPA 

Marla Smith, EPA 

Nelson Andrews, EPA 

Brian Englert, EPA 

Deb Bartram, ERG 

TJ Finseth, ERG 

Lynn Walters, CSC 

Barbara Beard, CSC 
Computer Sciences Corporation 

www.csc.com 

6101 Stevenson Avenue 

Alexandria, Virginia 22304 

703.461.2000 Fax 703.461.2020 

MEMORANDUM 

DATE: December 10, 2007 

TO: Ron Jordan, Work Assignment Manager 

 EPA EAD 

FROM: Cris Robinson, Quality Assurance Chemist 

Computer Sciences Corporation 

SUBJECT: Data Review Narrative for Method 1638 Trace Metals Analyses for the Steam Electric 

Study, Episode 6547, FGD Influent Samples 

Under EPA contract number 68-C-03-046, Battelle Marine Sciences submitted data for the analyses of 

trace metals. Analysis of the two samples reviewed in this narrative by Method 1638 was requested by 

EPA at a later date than the rest of the samples in Episode 6547. This narrative only evaluates Method 

1638 results for sample 70320 and 70323. Other analyses for these and other samples in Episode 6547 

are covered in a previous narrative. 

These two samples were analyzed for total metals including antimony (Sb), arsenic (As), cadmium (Cd), 

copper (Cu), chromium (Cr), lead (Pb), nickel (Ni), selenium (Se), silver (Ag), thallium (Tl), and zinc 

(Zn) by Method 1638 (ICP-MS). Sample 70320 was analyzed for dissolved and total metals. Because 

the FGD influent samples for this study were expected to be highly variable in solids content, EPA chose 

to obtain results for this phase as well. The solid-phase results for sample 70320 were not directly 

analyzed, but rather calculated from the total, dissolved, and TSS results.

Table 1 - Sample Identifiers, Descriptions, Sampling Dates, and Analysis Methods 

EPA Sample # Matrix Sample Description Sampling Date Phase Methods

Total 

7/25/07 

70320 Aqueous FGD Influent Dissolved 

NA Calculated Solid 

Total 

70323 Aqueous FGD Influent Field Blank 7/25/07 

Dissolved 

1638 

NA = Not applicable

These data have been reviewed in accordance with CSC's Data Review Guidelines for Metals Analyses 

(November 2004), with the EAD contract, and with the specifications listed in EPA Method 1638 (Jan 

1996). All data are of acceptable quality with the qualifiers described below and detailed in the data 

review summary table (Table 2). 

SUMMARY

Both samples were successfully analyzed within the method-specified holding times, and initial precision 

and recovery (IPR) analyses and method detection limit (MDL) studies were acceptably performed. 

Except for instances detailed below, all QC samples, including laboratory control samples (LCS), matrix 

spike and matrix spike duplicate (MS/MSD) samples, and quality control samples (QCS) were within 

contract-specified criteria. The MS/MSD analyses for this Episode were performed on samples 70321 
2

and 70322, and evaluated in a previous narrative. All method preparation blanks detected no 

contamination above the laboratory’s reporting limits. All calibration blanks were free of contamination 

above the report limit (minimum level or ML). These blanks are discussed in detail below. 

DATA ISSUES

Method and Analytical Blanks

Several analytes were detected in the preparation blanks (PB), initial calibration blanks (ICBs), and 

continuing calibration blanks (CCBs) associated with the samples in this Episode at concentrations 

greater than the respective MDLs, but less than the method-specified MLs. The data quality is affected as 

follows: 

• Sample Results Greater than Five Times but Less than Ten Times Blank Results: CSC considers 

these results to be of acceptable quality, but they may be maximum values. One instance of blank 

contamination at this level is detailed below. The affected samples and analytes are as follows: 

70320 total Cr. 

• Sample Results Greater than Ten Times Blank Results or Analyte Not Detected in Sample: CSC 

does not consider the presence of the analyte in the blank to adversely affect the data in cases 

where the sample results are greater than ten times the associated blank results or where the 

analyte is not detected in associated samples. Several samples fall into this category, but because 

CSC considers such data to be acceptable without qualification, these cases do not merit further 

detail. 

CCV 

One continuing calibration verification standard (CCV) recovery for silver (108)% was slightly above 

method-specified limits (81-107). However, all reported sample results associated with this CCV were 

not detected; therefore no samples are qualified. 

TSS Duplicate 

Due to lab error, a duplicate for TSS analyses was not performed. Blank and LCS results for TSS were 

acceptable. Because TSS is a secondary analyte used only in the calculation of solid-phase metals results, 

no data will be qualified by this omission. 

TECHNICAL NOTES 

Sample Temperature 

Trace metals samples were not chilled during shipment for this study. 

Additional Analytes 

Two additional analytes, arsenic and chromium, were included for evaluation by Method 1638. Because 

they are not specified in the method, the MLs for these (0.15 μg/L and 0.80 μg/L, respectively) were set 

well above the laboratory-determined MDL. 
3

Minimum Levels 

For dissolved and total sample 70320, the lab diluted 200-fold in order to alleviate expected matrix effects 

caused by high dissolved solids (dissolved solids content was assumed to be high because the lab 

observed precipitation in dissolved sample bottles). MLs are adjusted appropriately. 

Solid-Phase Calculations 

CSC calculated the solid-phase results by the following formula: 

The results for the various phases will be labeled in the PROCEDUR field of the EPA database as 

“DISSOLVED”, “TOTAL”, and “CALCULATED SOLID (DRY WEIGHT)”. 

When two results are mathematically combined to obtain a Calculated Solid result, CSC will report the 

larger of the two MLs associated with each result as the Calculated Solid ML. 

In the generation of the Calculated Solid result, at EPA's request, CSC included Total and Dissolved 

concentrations that were greater than the MDL but less than the ML. However, if any concentration was 

affected by contamination in an associated blank at less than 5 times the associated blank result, it was 

changed to a zero before going through the calculation, per CSC's data review protocols. Negative values 

submitted by the laboratory were not used in the calculations. 

Note that because the Method 1638 samples in this episode were held and analyzed at a later time at the 

request of EPA, the bottles had been preserved before a TSS was requested. Because preservation affects 

the solids content of a sample, a TSS was not performed; rather, the TSS result from the sample 70320 

bottle analyzed for mercury (4779 mg/L) was used in calculation of Method 1638 solid phase results. 

If you have any questions regarding the analyses of these samples or the review of these data, please 

contact Barbara Beard by telephone at (703) 461-2154, facsimile at (703) 461-8056, or via email at 

bbeard2@csc.com. 

cc: Brian Damico, EPA 

 Beverly Randolph, EPA 

Marla Smith, EPA 

Nelson Andrews, EPA 

Brian Englert, EPA 

Deb Bartram, ERG 

TJ Finseth, ERG 

Lynn Walters, CSC 

Barbara Beard, CSC 

original sample

Total Dissolved

TSS mg L

Conc ng L Conc ng L

/

( . / . / ) Solid phase concentration (ng/mg or μg/g) − =
4

Table 2 

Data Review Summary Table

Episode: 6547 Analysis: Trace Metals

Industry: STELEC Study Reviewer: Cris Robinson 

Sample Analyte Action Reason CSC Qual Level

70320 Total Cr Maximum value Sample result >5x and 

<10x blank result NA See Database 

70320 

Calculated Solid Cr Maximum value Associated total result is a 

maximum NA See Database 

NA = Not applicable 
Appendix D 

FGD WASTEWATER TREATMENT SYSTEM FLOW RATE DATA 
D-1 

Table D-1. Flow Data during FGD Wastewater Treatment Effluent Sample Collection, 

Big Bend 

Date Time 

FGD WWT Influent Flow Rate

(gpm) 

FGD WWT Effluent Flow Rate

(gpm) 

July 25, 2007 8:00 AM 252 14 

July 25, 2007 8:01 AM 252 14 

July 25, 2007 8:02 AM 251 251 

July 25, 2007 8:03 AM 251 248 

July 25, 2007 8:04 AM 251 245 

July 25, 2007 8:05 AM 251 242 

July 25, 2007 8:06 AM 251 65 

July 25, 2007 8:07 AM 251 17 

July 25, 2007 8:08 AM 251 16 

July 25, 2007 8:09 AM 251 16 

July 25, 2007 8:10 AM 251 15 

July 25, 2007 8:11 AM 251 15 

July 25, 2007 8:12 AM 251 14 

July 25, 2007 8:13 AM 251 239 

July 25, 2007 8:14 AM 250 242 

July 25, 2007 8:15 AM 250 245 

July 25, 2007 8:16 AM 250 249 

July 25, 2007 8:17 AM 250 13 

July 25, 2007 8:18 AM 250 13 

July 25, 2007 8:19 AM 250 13 

July 25, 2007 8:20 AM 250 14 

July 25, 2007 8:21 AM 250 14 

July 25, 2007 8:22 AM 250 14 

July 25, 2007 8:23 AM 250 14 

July 25, 2007 8:24 AM 250 249 

July 25, 2007 8:25 AM 250 249 

July 25, 2007 8:26 AM 249 250 

July 25, 2007 8:27 AM 249 250 

July 25, 2007 8:28 AM 249 6 

July 25, 2007 8:29 AM 249 7 

July 25, 2007 8:30 AM 249 9 

July 25, 2007 8:31 AM 249 10 

July 25, 2007 8:32 AM 249 11 

July 25, 2007 8:33 AM 249 13 

July 25, 2007 8:34 AM 249 252 

July 25, 2007 8:35 AM 249 252 

July 25, 2007 8:36 AM 249 253 

July 25, 2007 8:37 AM 249 253 

July 25, 2007 8:38 AM 248 212 
D-2 

Table D-1. Flow Data during FGD Wastewater Treatment Effluent Sample Collection, 

Big Bend 

Date Time 

FGD WWT Influent Flow Rate

(gpm) 

FGD WWT Effluent Flow Rate

(gpm) 

July 25, 2007 8:39 AM 248 7 

July 25, 2007 8:40 AM 248 8 

July 25, 2007 8:41 AM 248 9 

July 25, 2007 8:42 AM 248 10 

July 25, 2007 8:43 AM 248 12 

July 25, 2007 8:44 AM 248 13 

July 25, 2007 8:45 AM 248 250 

July 25, 2007 8:46 AM 248 251 

July 25, 2007 8:47 AM 248 251 

July 25, 2007 8:48 AM 248 252 

July 25, 2007 8:49 AM 248 253 

July 25, 2007 8:50 AM 247 12 

July 25, 2007 8:51 AM 247 13 

July 25, 2007 8:52 AM 247 14 

July 25, 2007 8:53 AM 247 15 

July 25, 2007 8:54 AM 247 16 

July 25, 2007 8:55 AM 247 17 

July 25, 2007 8:56 AM 247 251 

July 25, 2007 8:57 AM 247 251 

July 25, 2007 8:58 AM 247 252 

July 25, 2007 8:59 AM 247 252 

July 25, 2007 9:00 AM 247 25 

July 25, 2007 9:01 AM 247 23 

July 25, 2007 9:02 AM 246 21 

July 25, 2007 9:03 AM 246 19 

July 25, 2007 9:04 AM 246 17 

July 25, 2007 9:05 AM 246 15 

July 25, 2007 9:06 AM 246 249 

July 25, 2007 9:07 AM 246 250 

July 25, 2007 9:08 AM 12 251 

July 25, 2007 9:09 AM 7 252 

July 25, 2007 9:10 AM 7 253 

July 25, 2007 9:11 AM 6 15 

July 25, 2007 9:12 AM 6 15 

July 25, 2007 9:13 AM 166 14 

July 25, 2007 9:14 AM 243 14 

July 25, 2007 9:15 AM 243 14 

July 25, 2007 9:16 AM 243 14 

July 25, 2007 9:17 AM 243 14 
D-3 

Table D-1. Flow Data during FGD Wastewater Treatment Effluent Sample Collection, 

Big Bend 

Date Time 

FGD WWT Influent Flow Rate

(gpm) 

FGD WWT Effluent Flow Rate

(gpm) 

July 25, 2007 9:18 AM 243 14 

July 25, 2007 9:19 AM 243 14 

July 25, 2007 9:20 AM 243 14 

July 25, 2007 9:21 AM 243 14 

July 25, 2007 9:22 AM 243 14 

July 25, 2007 9:23 AM 243 14 

July 25, 2007 9:24 AM 244 14 

July 25, 2007 9:25 AM 244 14 

July 25, 2007 9:26 AM 244 14 

July 25, 2007 9:27 AM 244 14 

July 25, 2007 9:28 AM 244 14 

July 25, 2007 9:29 AM 244 14 

July 25, 2007 9:30 AM 244 13 

July 25, 2007 9:31 AM 244 13 

July 25, 2007 9:32 AM 244 13 

July 25, 2007 9:33 AM 244 13 

July 25, 2007 9:34 AM 244 110 

July 25, 2007 9:35 AM 244 250 

July 25, 2007 9:36 AM 244 248 

July 25, 2007 9:37 AM 244 245 

July 25, 2007 9:38 AM 244 243 

July 25, 2007 9:39 AM 244 240 

July 25, 2007 9:40 AM 244 31 

July 25, 2007 9:41 AM 244 18 

July 25, 2007 9:42 AM 244 23 

July 25, 2007 9:43 AM 244 28 

July 25, 2007 9:44 AM 245 33 

July 25, 2007 9:45 AM 245 245 

July 25, 2007 9:46 AM 245 247 

July 25, 2007 9:47 AM 245 249 

July 25, 2007 9:48 AM 245 250 

July 25, 2007 9:49 AM 245 252 

July 25, 2007 9:50 AM 245 4 

July 25, 2007 9:51 AM 245 9 

July 25, 2007 9:52 AM 245 14 

July 25, 2007 9:53 AM 245 19 

July 25, 2007 9:54 AM 245 24 

July 25, 2007 9:55 AM 245 198 

July 25, 2007 9:56 AM 245 244 
D-4 

Table D-1. Flow Data during FGD Wastewater Treatment Effluent Sample Collection, 

Big Bend 

Date Time 

FGD WWT Influent Flow Rate

(gpm) 

FGD WWT Effluent Flow Rate

(gpm) 

July 25, 2007 9:57 AM 245 246 

July 25, 2007 9:58 AM 245 248 

July 25, 2007 9:59 AM 245 251 

July 25, 2007 10:00 AM 245 13 

July 25, 2007 10:01 AM 245 13 

July 25, 2007 10:02 AM 245 13 

July 25, 2007 10:03 AM 245 13 

July 25, 2007 10:04 AM 246 13 

July 25, 2007 10:05 AM 246 13 

July 25, 2007 10:06 AM 246 13 

July 25, 2007 10:07 AM 246 13 

July 25, 2007 10:08 AM 246 247 

July 25, 2007 10:09 AM 246 248 

July 25, 2007 10:10 AM 246 250 

July 25, 2007 10:11 AM 246 252 

July 25, 2007 10:12 AM 246 2 

July 25, 2007 10:13 AM 246 5 

July 25, 2007 10:14 AM 246 7 

July 25, 2007 10:15 AM 246 9 

July 25, 2007 10:16 AM 246 11 

July 25, 2007 10:17 AM 246 13 

July 25, 2007 10:18 AM 246 249 

July 25, 2007 10:19 AM 246 250 

July 25, 2007 10:20 AM 246 251 

July 25, 2007 10:21 AM 246 252 

July 25, 2007 10:22 AM 246 14 

July 25, 2007 10:23 AM 247 14 

July 25, 2007 10:24 AM 247 14 

July 25, 2007 10:25 AM 247 14 

July 25, 2007 10:26 AM 247 14 

July 25, 2007 10:27 AM 247 13 

July 25, 2007 10:28 AM 247 235 

July 25, 2007 10:29 AM 247 248 

July 25, 2007 10:30 AM 247 249 
D-5 

Table D-2. Flow Data during FGD Wastewater Treatment Influent Sample Collection, 

Big Bend 

Date Time 

FGD WWT Influent Flow Rate

(gpm) 

FGD WWT Effluent Flow Rate

(gpm) 

July 25, 2007 3:00 PM 251 4 

July 25, 2007 3:01 PM 251 6 

July 25, 2007 3:02 PM 251 8 

July 25, 2007 3:03 PM 251 10 

July 25, 2007 3:04 PM 251 12 

July 25, 2007 3:05 PM 251 245 

July 25, 2007 3:06 PM 251 243 

July 25, 2007 3:07 PM 251 242 

July 25, 2007 3:08 PM 251 241 

July 25, 2007 3:09 PM 251 239 

July 25, 2007 3:10 PM 251 13 

July 25, 2007 3:11 PM 251 13 

July 25, 2007 3:12 PM 251 13 

July 25, 2007 3:13 PM 251 13 

July 25, 2007 3:14 PM 251 13 

July 25, 2007 3:15 PM 251 122 

July 25, 2007 3:16 PM 251 250 

July 25, 2007 3:17 PM 251 250 

July 25, 2007 3:18 PM 251 250 

July 25, 2007 3:19 PM 251 250 

July 25, 2007 3:20 PM 251 14 

July 25, 2007 3:21 PM 251 14 

July 25, 2007 3:22 PM 251 14 

July 25, 2007 3:23 PM 251 13 

July 25, 2007 3:24 PM 251 13 

July 25, 2007 3:25 PM 251 13 

July 25, 2007 3:26 PM 251 13 

July 25, 2007 3:27 PM 251 250 

July 25, 2007 3:28 PM 251 250 

July 25, 2007 3:29 PM 251 251 

July 25, 2007 3:30 PM 251 251 

July 25, 2007 3:31 PM 251 10 

July 25, 2007 3:32 PM 251 11 

July 25, 2007 3:33 PM 251 12 

July 25, 2007 3:34 PM 251 14 

July 25, 2007 3:35 PM 251 15 

July 25, 2007 3:36 PM 251 16 

July 25, 2007 3:37 PM 251 246 

July 25, 2007 3:38 PM 251 247 
D-6 

Table D-2. Flow Data during FGD Wastewater Treatment Influent Sample Collection, 

Big Bend 

Date Time 

FGD WWT Influent Flow Rate

(gpm) 

FGD WWT Effluent Flow Rate

(gpm) 

July 25, 2007 3:39 PM 251 249 

July 25, 2007 3:40 PM 251 250 

July 25, 2007 3:41 PM 251 252 

July 25, 2007 3:42 PM 251 3 

July 25, 2007 3:43 PM 251 5 

July 25, 2007 3:44 PM 251 7 

July 25, 2007 3:45 PM 251 9 

July 25, 2007 3:46 PM 251 11 

July 25, 2007 3:47 PM 251 238 

July 25, 2007 3:48 PM 251 241 

July 25, 2007 3:49 PM 251 243 

July 25, 2007 3:50 PM 251 246 

July 25, 2007 3:51 PM 251 248 

July 25, 2007 3:52 PM 251 10 

July 25, 2007 3:53 PM 251 2 

July 25, 2007 3:54 PM 251 4 

July 25, 2007 3:55 PM 251 7 

July 25, 2007 3:56 PM 251 9 

July 25, 2007 3:57 PM 251 11 

July 25, 2007 3:58 PM 251 249 

July 25, 2007 3:59 PM 251 248 

July 25, 2007 4:00 PM 251 247 

July 25, 2007 4:01 PM 251 246 

July 25, 2007 4:02 PM 251 36 

July 25, 2007 4:03 PM 251 17 

July 25, 2007 4:04 PM 251 16 

July 25, 2007 4:05 PM 251 15 

July 25, 2007 4:06 PM 251 14 

July 25, 2007 4:07 PM 251 13 

July 25, 2007 4:08 PM 251 204 

July 25, 2007 4:09 PM 251 252 

July 25, 2007 4:10 PM 251 252 

July 25, 2007 4:11 PM 251 252 

July 25, 2007 4:12 PM 250 252 

July 25, 2007 4:13 PM 250 3 

July 25, 2007 4:14 PM 250 4 

July 25, 2007 4:15 PM 250 6 

July 25, 2007 4:16 PM 250 8 

July 25, 2007 4:17 PM 250 10 
D-7 

Table D-2. Flow Data during FGD Wastewater Treatment Influent Sample Collection, 

Big Bend 

Date Time 

FGD WWT Influent Flow Rate

(gpm) 

FGD WWT Effluent Flow Rate

(gpm) 

July 25, 2007 4:18 PM 250 11 

July 25, 2007 4:19 PM 250 242 

July 25, 2007 4:20 PM 250 247 

July 25, 2007 4:21 PM 250 246 

July 25, 2007 4:22 PM 250 244 

July 25, 2007 4:23 PM 250 243 

July 25, 2007 4:24 PM 250 20 

July 25, 2007 4:25 PM 250 21 

July 25, 2007 4:26 PM 250 22 

July 25, 2007 4:27 PM 250 23 

July 25, 2007 4:28 PM 250 24 

July 25, 2007 4:29 PM 250 25 

July 25, 2007 4:30 PM 250 244 
Appendix E 

PICTURES FROM THE SAMPLING EPISODE 
E-1 

Figure E-1. Sampler Working Inside a “Cleanbox” 
E-2 

Figure E-2. Three-Way Splitter at the Influent to FGD Wastewater Treatment System 
E-3 

Figure E-3. Sampling Set Up at the Influent to FGD Wastewater Treatment System (SP-1) 
E-4 

Figure E-4. Pump-Off Station for Dissolved Metals Sample Collection 
E-5 

Figure E-5. Collection of Dissolved Metals Samples at Pump-Off Station 
E-6 

Figure E-6. Three-Way Splitter at the Effluent from FGD Wastewater Treatment System 
E-7 

Figure E-7. Sampling Set Up at Effluent from FGD Wastewater Treatment System (SP-2) 
E-8 

Figure E-8. Field Blank Collection at Effluent from FGD Wastewater Treatment (SP-5)