Sampling Episode Report 

Duke Energy’s 

Miami Fort Station 

North Bend, OH 

Sampling Episode 6560 

Prepared for:

U.S. Environmental Protection Agency

Engineering and Analysis Division 

Office of Water 

1200 Pennsylvania Avenue, NW 

Washington, D.C. 20460 

Prepared by: 

Eastern Research Group, Inc.

14555 Avion Parkway 

Suite 200 

Chantilly, VA 20151 

13 December 2011 

EPA Contract No. 68-C-02-095 

Work Assignment 9-29 
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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. FACILITY OVERVIEW ........................................................................................................ 2-1

2.1 FGD Scrubber Systems ........................................................................................ 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 System ...................................... 3-2

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

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

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

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

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

4.1 Measured and Calculated Results for Influent to FGD Wastewater Treatment 

System Samples ................................................................................................... 4-1

4.2 FGD Wastewater Treatment System ................................................................... 4-2

5. DATA QUALITY ............................................................................................................... 5-14

5.1 Analytical Quality Control ................................................................................. 5-14

5.2 Field Quality Control ......................................................................................... 5-14

5.2.1 Bottle Blanks .......................................................................................... 5-14

5.2.2 Equipment Blanks .................................................................................. 5-15

5.2.3 Field Blanks ........................................................................................... 5-15

5.2.4 Field Duplicates ..................................................................................... 5-17

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

Appendix A: ANALYTICAL RESULTS

Appendix B: DATA REVIEW NARRATIVES 

Appendix C: PICTURES FROM THE SAMPLING EPISODE 
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LIST OF TABLES 

Page 

Table 3-1. Sample Collection Information, Miami Fort ............................................................ 3-10

Table 3-2. Sample Collection at Miami Fort ............................................................................. 3-12

Table 3-3. Field Measurements, Miami Fort ............................................................................. 3-12

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

Table 3-5. Analytical Methods, Miami Fort .............................................................................. 3-15

Table 3-6. Summary of Sample Container and Planned Preservation, Miami Fort .................. 3-16

Table 3-7. Sample Preservation Summary, Miami Fort ............................................................ 3-17

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

Miami Fort ..................................................................................................................... 3-19

Table 3-9. FGD Scrubber System Operating Characteristics, Miami Fort ................................ 3-20

Table 3-10. Coal Usage during Sample Collection, Miami Fort ............................................... 3-21

Table 3-11. Scrubber Slurry Information during Sample Collection, Miami Fort .................... 3-22

Table 3-12. FGD Wastewater Treatment System Operation Information, Miami Fort ............. 3-23

Table 4-1. Influent to FGD Wastewater Treatment System, Miami Fort ................................... 4-4

Table 4-2. Effluent from the FGD Wastewater Treatment System, Miami Fort ........................ 4-7

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

Treatment System, Miami Fort ...................................................................................... 4-11

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

System, Miami Fort ....................................................................................................... 4-12

Table 5-1. Field Blank Analytical Results, Miami Fort............................................................ 5-18

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

Miami Fort ..................................................................................................................... 5-19

Table A-1. Biphasic Sample Results for Classicals and Total Metals, Influent to FGD 

Wastewater Treatment System, Day 1 Analytical Results, Miami Fort ......................... A-1

Table A-2. Biphasic Sample Results for Classicals and Total Metals, Influent to FGD 

Wastewater Treatment System, Day 2 Analytical Results, Miami Fort ......................... A-3
LIST OF TABLES (Continued) 

Page 

iii

Table A-3. Biphasic Sample Results for Classicals and Total Metals, Influent to FGD 

Wastewater Treatment System, Day 3 Analytical Results, Miami Fort ......................... A-5

Table A-4. Biphasic Sample Results for Classicals and Total Metals, Influent to FGD 

Wastewater Treatment System, Day 4 Analytical Results, Miami Fort ......................... A-7

Table A-5. Influent to FGD Wastewater Treatment System, Day 1 Analytical Results, 

Miami Fort ...................................................................................................................... A-9

Table A-6. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, 

Miami Fort .................................................................................................................... A-17

Table A-7. Influent to FGD Wastewater Treatment System, Day 3 Analytical Results, 

Miami Fort .................................................................................................................... A-24

Table A-8. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, 

Miami Fort .................................................................................................................... A-30

Table A-9. Effluent from FGD Wastewater Treatment System, Day 1 Analytical Results, 

Miami Fort .................................................................................................................... A-37

Table A-10. Effluent from FGD Wastewater Treatment System, Day 2 Analytical Results, 

Miami Fort .................................................................................................................... A-40

Table A-11. Effluent from FGD Wastewater Treatment System, Day 3 Analytical Results, 

Miami Fort .................................................................................................................... A-44

Table A-12. Effluent from FGD Wastewater Treatment System, Day 4 Analytical Results, 

Miami Fort .................................................................................................................... A-47

Table A-13. Duplicate of Effluent from FGD Wastewater Treatment System, Day 2 

Analytical Results, Miami Fort ..................................................................................... A-50

Table A-14. Bottle Blank and Equipment Blank Analytical Data, Miami Fort ....................... A-53

Table A-15. Influent to FGD Wastewater Treatment System Field Blank, Day 1 Analytical 

Results, Miami Fort ...................................................................................................... A-58

Table A-16. Effluent from FGD Wastewater Treatment System Field Blank, Day 1 

Analytical Results, Miami Fort ..................................................................................... A-60

Table A-17. Effluent from FGD Wastewater Treatment System Field Blank, Day 2 

Analytical Results, Miami Fort ..................................................................................... A-62

Table A-18. Effluent from FGD Wastewater Treatment System, Day 3 Analytical Results, 

Miami Fort .................................................................................................................... A-63
LIST OF TABLES (Continued) 

Page 

iv

Table A-19. Effluent from FGD Wastewater Treatment System, Day 4 Analytical Results, 

Miami Fort .................................................................................................................... A-64
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LIST OF FIGURES 

Page 

Figure 2-1. Chemical Precipitation FGD Wastewater Treatment System, Miami Fort ............... 2-5

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

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

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

Figure C-3. Sample Collection at the Influent to the FGD Wastewater Treatment System ........C-3

Figure C-4. Sample Collection Set Up at the Pump-Off Station .................................................C-4

Figure C-5. Composite Sample Collection Set Up at the Effluent from the FGD Wastewater 

Treatment System ............................................................................................................C-5
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1. INTRODUCTION

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

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

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

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

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

place July 11 - 16, 2010, at Duke Energy’s Miami Fort Station (Miami Fort), located in North 

Bend, Ohio (Sampling Episode 6560). The focus of Episode 6560 was to characterize the purge 

stream entering the flue gas desulfurization (FGD) wastewater treatment system and the effluent 

from the chemical precipitation system. 

1.1 Background of Detailed Study

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

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

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

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

loadings are associated with wet FGD systems present at coal-fired power plants. Based on these 

findings, EPA has focused the sampling program on characterizing the untreated FGD 

wastewaters and effluent quality from technologies designed to treat the wastewater. 

1.2 Power Plant Site Selection

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

configurations and characteristics of the plants. 

Miami Fort was selected by EPA for sampling based on the following site characteristics: 

 The plant is a coal-fired power plant that burns eastern bituminous coal in each of 

its three generating units; 

 The plant operates limestone forced oxidation wet FGD systems on two of the 

three generating units; 

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

includes the following steps: 

— Equalization and pH adjustment (lime addition), 

— Organosulfide addition, 

— Ferric chloride addition (discontinued prior to the sampling episode), 

— Polymer addition, 

— Clarification; 

 The plant operates selective catalytic reaction (SCR) systems on two of the three 

generating units (the same two that have associated FGD systems); and 

 The plant produces a commercial-grade gypsum by-product. 
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1.3 Sampling Episode Overview

EPA and its technical contractor, Eastern Research Group, Inc. (ERG) conducted a oneday pre-sampling site visit at Miami Fort on March 1, 2010 as part of the detailed study. The 

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

Energy’s Miami Fort Station (Sampling Plan) [1], which describes the sample collection 

procedures used during the sampling episode. 

On Sunday, July 11, 2010, EPA arrived at Miami Fort to meet with plant personnel, 

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

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

Monday through Friday (July 12 - 16, 2010). The following personnel participated in EPA’s 

sample collection activities: 

 Ron Jordan, EPA/EAD; 

 Jezebele Alicea, EPA/EAD; 

 Holly Cannon, ERG; 

 TJ Finseth, ERG; 

 Lydia Lambert, ERG; 

 Jennifer Lewis, ERG; and 

 Jessica Wolford, ERG. 

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

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

industry. During the sampling episode, UWAG acted as Miami Fort’s representative and 

collected samples on behalf of the plant. 
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2. FACILITY OVERVIEW

Miami Fort operates three baseload steam electric generating units and each has a coalfired boiler. Unit 6, which began operation in 1960, has a generating capacity of 175 MW. Units 

7 and 8, which began operation in 1975 and 1978, respectively, each has a generating capacity of 

550 megawatts (MW). All three generating units burn eastern bituminous coal. The plant is 

located in North Bend, Ohio, approximately 20 miles west of Cincinnati, and discharges to the 

Ohio River. 

Approximately three years ago, Miami Fort retrofitted Units 7 and 8 (but not Unit 6) with 

FGD scrubber systems to control the sulfur dioxide (SO2) releases from the plant. The removal 

efficiency of both FGD systems is approximately 96 percent. In addition to the FGD scrubber 

systems, Miami Fort installed an FGD wastewater treatment system to control the discharges of 

the wastewater generated during the operation of the FGD scrubbers. Sections 2.1 and 2.2 further 

discuss the FGD scrubber systems and the FGD wastewater treatment system, respectively. 

Miami Fort retrofitted Units 7 and 8 with SCR systems in 2003 and 2001, respectively. 

The plant operates the SCR systems, which are used to control nitrogen oxide (NOX) emissions 

from the plant, year round. 

The electrostatic precipitators (ESPs) at Miami Fort are particulate control devices that 

are designed to remove greater than 99 percent of the fly ash and other particulates from the flue 

gas. Miami Fort utilizes ESPs to remove the fly ash from all three units. The fly ash and other 

particulates are collected in hoppers. The fly ash from Unit 6 is wet sluiced to the plant’s ash 

pond. The fly ash from Units 7 and 8 is pneumatically conveyed to storage silos. Miami Fort 

sells most of the ash to Ready Mix. Any fly ash that the plant cannot sell is transferred to their 

landfill located approximately three miles away, which is owned and operated by Duke Energy. 

Miami Fort previously had issues with blue plume from the stack, associated with sulfur 

trioxide emissions. The plant now injects lime into the flue gas between the air heater and the 

ESP to control the sulfur trioxide emissions. 

Miami Fort operates an ash pond with two adjacent cells operated in series. Fly ash from 

Unit 6 and bottom ash from all three units are sluiced to the cell nearest the plant. Polymer is 

added to the ash pond near where the sluicing pipes deposit the ash sluice to improve total 

suspended solids (TSS) removals. The plant operates the first cell using equipment to maintain 

channels for the sluice water to move through the mass of ash solids collected in the pond (i.e., 

the rim ditch stacking method). The plant removes the solids that settle out in the channels of the 

ash pond and stacks them in piles along the perimeter of the ash channels to allow the solids to 

dewater, while the water drains back into the pond. After the solids have been dewatered, the 

plant hauls them to the landfill for disposal. In addition to fly ash and bottom ash transport water, 

the ash pond also receives treated FGD wastewater and mill rejects. The ash pond discharges to 

the Ohio River via Outfall 002. 

Unit 6 at Miami Fort has the following configuration: 

 Boiler; 

 Air heater; and 

 ESP. 
2-2

Units 7 and 8 at Miami Fort have the following configuration: 

 Boiler; 

 SCR system; 

 Air heater; 

 Lime injection; 

 ESP; and 

 FGD scrubber system. 

 

2.1 FGD Scrubber Systems

Miami Fort operates two identical wet FGD scrubber systems that treat the flue gas from 

Units 7 and 8. The plant uses limestone slurry as the sorbent for SO2 absorption. Limestone and 

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

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

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

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

is between 20 and 30 percent solids (by weight), is transferred to the limestone slurry feed tank 

and used as fresh limestone slurry in the absorber. Miami Fort also uses lime residual, a 

byproduct from the lime softening process at the City of Hamilton water treatment plant, to make 

the slurry for the FGD process. The lime residual accounts for approximately 10 percent of the 

slurry used in the two units. 

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

pumps transfer the slurry to the various levels of the FGD scrubber (typically two of the three 

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

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

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

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

droplets flow downward until they settle on the first of two dual flow trays, forming a layer of 

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

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

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

second dual flow tray and then continue to flow downward in the scrubber until they reach the 

reaction tank. Miami Fort bubbles air through the reaction tank to oxidize the calcium sulfite to 

calcium sulfate (i.e., gypsum). 

Miami Fort operates the FGD system to maintain a set sulfur dioxide removal of 97 

percent. The system automatically adjusts the slurry feed rate to achieve this removal, which also 

adjusts the pH in the FGD system. The pH in the FGD system is typically around 5 S.U. In 

addition, the plant operates the system to maintain a solids concentration in the scrubber of 21 to 

24 percent weight solids. When the solids concentration exceeds 24 percent, the plant blows 

down some of the gypsum slurry from the scrubber. Miami Fort also blows down some of the 

gypsum slurry to control the chlorides concentration. The chlorides concentration in the 

scrubbers is maintained at approximately 5,000 to 10,000 parts per million (ppm), with a design 

maximum chlorides concentration of 12,000 ppm. Miami Fort transfers the blowdown from the 

scrubbers to the gypsum dewatering operations. 
2-3

Each FGD system has its own gypsum dewatering equipment; therefore, the Unit 7 and 8 

gypsum and wastewater are not commingled until the FGD wastewater treatment system. The 

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

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

of the hydrocyclones and falls downward, while the water exits the top of the hydrocyclones. 

The gypsum from the primary hydrocyclones is transferred to the vacuum belt filters for final 

dewatering. The overflow from the primary hydrocyclones is transferred to secondary 

hydrocyclones. The overflow from the second hydrocyclones is transferred to the FGD 

wastewater treatment system. The underflow from the secondary hydrocyclones is sent to the 

reclaim tanks, which are segregated for each unit, and is reused in the process as make-up water. 

As the gypsum is applied to the vacuum belt filters, Miami Fort washes the gypsum with 

service water to reduce the chlorides in the gypsum to less than 100 ppm. The vacuum belt filters 

dry the gypsum to a moisture content of less than nine percent. The gypsum produced at the plant 

is then sold to Lafarge for wallboard manufacturing. If the gypsum is off-specification or if 

Lafarge refuses to accept the gypsum, the plant can also market the gypsum to the agricultural 

industry. 

2.2 FGD Wastewater Treatment System

The Miami Fort FGD wastewater treatment system is designed to receive intermittent 

transfers of wastewater (secondary hydrocyclone overflow) from the FGD system at a maximum 

design flow rate of 200 gallons per minute (gpm). The actual flow rate through the system 

averages 150 gpm over a 24-hour period. The FGD wastewater treatment system, designed by 

Infilco Degremont, is a chemical precipitation treatment system and contains the following 

treatment operations: 

 Equalization and pH adjustment (lime addition); 

 Organosulfide addition; 

 Polymer addition; and 

 Clarification. 

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

equalization tank at the beginning of the wastewater treatment system. During the sampling 

episode, the FGD influent wastewater was found to contain 1.6 to 3.0 percent solids, had a pH 

between 5 and 7 S.U., and a temperature between 47 and 54 °C. Miami Fort adds lime to the 

equalization tank to raise the pH in the tank to between 8.4 and 8.6 S.U. to precipitate the soluble 

metals as insoluble hydroxides and oxyhydroxides. The equalization tank also receives water 

from the wastewater treatment building sump, which primarily consists of filter press filtrate, and 

flush water from the flushing of the sludge lines. 

From the equalization tank, the wastewater enters the coagulation tank, where 

organosulfide is added. The organosulfide is added to precipitate residual metals as sulfide 

complexes. At the time of the presampling site visit, Miami Fort stated that they were testing the 

Nalco Nalmet® 1689 organosulfide in the FGD wastewater treatment system in place of TMT 

15®. Miami Fort tested the effectiveness of the Nalmet® 1689 by adjusting the feed rate and 

addition amounts, in combination with other FGD wastewater treatment additives (i.e., polymer, 

ferric chloride). Before the sampling episode, the plant optimized the use of Nalmet® 1689, 
2-4

which effectively lowered mercury levels and eliminated the need to add ferric chloride to the 

wastewater treatment system. 

Flow from the coagulation tank splits into two parallel streams that flow to two 

DensaDeg® clarifiers. This type of clarifier has an initial reactor section, where polymer is 

added for coagulation and flocculation to improve solids removals. From the reactor section, the 

wastewater enters the clarification/thickening section of the clarifier, where the solids settle out 

of the wastewater. The sludge is transferred to the sludge holding tank and then processed 

through the filter presses. The filtrate from the filter presses is collected in the wastewater 

treatment building sump and recycled to the equalization tank. The sludge from the filter presses 

is hauled off site for disposal at a different landfill from the one used for the disposal of the ash. 

The clarified wastewater from the two DensaDeg® clarifiers is combined in the effluent 

tank. The wastewater is pumped to the ash pond and discharged via Outfall 002. The transfers to 

the ash pond are based on level control within the effluent tank and are therefore not continuous. 

Figure 2-1 presents the process flow diagram of the FGD wastewater treatment system, as 

well as the sampling points for the Miami Fort sampling episode, which are summarized below: 

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

upstream of the equalization tank (i.e., the sample was collected prior to any 

chemical addition or mixing with recycle streams); 

 A sample of the effluent from the effluent tank downstream of coagulation and 

clarification, just before the treated effluent is sent to the ash pond. 
2-5 

Figure 2-1. Chemical Precipitation FGD Wastewater Treatment System, Miami Fort 
3-1

3. SAMPLE COLLECTION

During the Miami Fort sampling episode, the sampling team followed the collection 

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

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

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

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

activities. 

3.1 Sampling Points, Sample Collection Methods, and Field Measurements

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

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

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

sampling point locations. 

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

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

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

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

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

sample identification and the sample points for each day. 

The sampling points for this episode were: 

 SP-1 Influent to FGD Wastewater Treatment System; 

 SP-2 Effluent from FGD Wastewater Treatment System; 

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

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

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

For all the sampling points, EPA collected split samples with Miami Fort’s representative 

by inserting a “Y” splitter into the sample tubing configuration at each sampling point to allow 

for split sample collection. EPA collected all samples (other than mercury and cyanide) at all 

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

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

therefore, for these samples, EPA and Miami Fort’s representative collected duplicate samples, 

with one filling the bottle immediately after the other. 

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

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

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

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

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

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

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

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

the box and pull the bag over the opening of the box, but is still able to see the sample bottles and 
3-2

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

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

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

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

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

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

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

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

protocols. 

3.1.1 Influent to FGD Wastewater Treatment System 

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

located on the piping from the secondary hydrocyclone to the equalization tank. The sample was 

collected prior to the wastewater entering the equalization tank because the plant adds lime 

directly to the equalization tank and, therefore, the sampling point upstream of the tank provides 

the best representation of the FGD scrubber purge from the Miami Fort FGD system. Figure 2-1 

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

flow into the equalization tank is not continuous. In addition, due to the relatively high 

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

split samples using composite sampling techniques. 

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

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

and dissolved metals, and dissolved hexavalent chromium (total and dissolved metals and 

dissolved hexavalent chromium were collected in a 10-liter container and samples were pumped 

into individual bottles later). See Section 5.2.3 for a description of the field blank sample 

collection procedures at the influent to the FGD wastewater treatment system. 

The sampling point was located on the pipe between the secondary hydrocyclone and 

equalization tank, and was only accessible from the top of the equalization tank. To collect the 

wastewater samples at the influent to the FGD wastewater treatment system, the samplers 

attached a 25-foot length of silicone tubing to the sample tap on top of the equalization tank and 

had the tubing run to the ground level where the samples were collected. The end of the silicone 

tubing was fitted with a “Y” splitter, with two additional lengths of silicone tubing attached to 

the “Y” splitter. Figure C-2, in Appendix C, is a picture of the tubing attached to the sample tap 

at the influent to the FGD wastewater treatment system. Figure C-3, in Appendix C, is a picture 

of the sample collection set up at the influent to the FGD wastewater treatment system. The 

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

flow through the tubing for two minutes before beginning to fill sample containers. The samplers 

did not close the valve until all samples were collected (except the dissolved metals samples). On 

Day 2 of the sampling episode, the sampling team set up a tent to cover the samplers/samples 

from rain during the sample collection. 

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

3.1: 

 Total and dissolved mercury; 
3-3

 Total metals by 200.8; and 

 Total metals by 200.7. 

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

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

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

untouched to allow the solids in the wastewater to settle. 

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

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

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

FGD wastewater treatment system. 

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

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

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

samples were immediately placed on ice after sample collection. 

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

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

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

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

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

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

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

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

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

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

to collect “true” split samples with Miami Fort’s representatives. Figure C-4, in Appendix C, is a 

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

On Day 1 only, ERG collected field blank samples (SP-4) for dissolved metals and 

dissolved hexavalent chromium by pumping from a previously filled 10-liter container. See 

Section 5.2.3 for a description of the field blank sample collection procedures at the influent to 

FGD wastewater treatment system. 

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

tubing into the 10-liter container filled with wastewater from the influent to the FGD wastewater 

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

100 minutes. Approximately 0.5- 2 liters1

 of sample were pumped through the tubing/filter to 

purge the line before collecting samples. 

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

Section 3.1: 

 

1

 During Day 1, the capsule filter became clogged, so after the field blank and first sample collection, the filter was 

changed and briefly purged. On Day 2, 3, and 4, the filter/tubing was purged for less than a minute, 1 liter, and 0.5 

liters respectively and there was no need to change the filter. 
3-4

 Dissolved metals by 200.8; 

 Dissolved metals by 200.7; and 

 Dissolved hexavalent chromium. 

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

The samples of the influent to the FGD wastewater treatment system that were collected 

represent the FGD scrubber purge from the specific unit that was purging at the time the samples 

were collected. The following identifies which units are represented by each day of sampling: 

 Day 1 – Unit 8; 

 Day 2 – Unit 7; 

 Day 3 – Unit 8; and 

 Day 4 – Unit 7. 

3.1.2 Effluent from FGD Wastewater Treatment System 

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

located on the suction side of the pump that transfers the wastewater from the effluent tank to the 

ash pond. Miami Fort installed a three-way splitter on the sample tap that had three separate taps 

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

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

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

collection. 

ERG collected the effluent from FGD wastewater treatment system composite samples 

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

into two 20-liter containers. The compositors were programmed to collect 870 milliliters (mL) 

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

off the specific sample volumes into the individual sample containers. 

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

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

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

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

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

grab sample for cyanide during each compositing period. 

On Day 1 only, prior to starting the automatic compositors at the effluent from FGD 

wastewater treatment system (SP-2), the sampling team collected field blanks (SP-5) for total 

and dissolved metals and dissolved hexavalent chromium (samples were collected in a 20-liter 

container and samples were pumped into individual bottles later). See Section 5.2.3 for a 

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

wastewater treatment system. 

Samplers set up the compositors by attaching two silicone tubing sets to two of the taps 

on the three-way splitter. The tubing configuration was set up such that one end was connected 

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

the large composite container. The samplers attached the silicone tubing to the sample tap, 
3-5

opened the valve, and allowed sample to flow through both sets of tubing before calibrating 

either of the automatic compositors. This ensured that the flow through the tubing during 

calibration would be the expected flow through the tubing during sample collection. The 

automatic compositors were calibrated such that they collected 870 mL2

 every hour, so that the 

projected complete volume would be 20 liters. After calibration, the tubing was attached to a 

vented cap on a 20-liter composite container. The sample tap was left open during the entire 

sample collection time period, and the automatic compositor pulled sample as dictated by the 

sampling program. Additionally, the automatic compositor was capable of purging the line back 

through the sample tap between each individual sample aliquot. 

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

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

to minimize contamination. Figure C-5, in Appendix C, is a picture of the composite sampling 

set-up at the effluent from the bioreactor system. 

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

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

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

procedures at the effluent from FGD wastewater treatment system. 

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

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

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

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

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

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

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

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

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

grabs, ERG filled a field test bottle and tested for pH and temperature using a calibrated pH 

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

for the effluent from FGD wastewater treatment system. 

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

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

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

split samples with Miami Fort’s representatives; therefore, duplicate samples were collected. The 

total cyanide sample was immediately preserved. Lead acetate test strips and potassium-iodide 

starch test strips were used to measure for sulfides and oxidants, respectively. No sulfides or 

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

 

2

 The Sampling Plan called for calibrating the compositors to collect 830 mL every hour; however, because the 

pumps that transfer the wastewater from the effluent tank to the ash pond do not operate continuously, the volume of 

water that could be pulled for a specific aliquot varied depending on if the pumps were operating (less volume 

collected) or idle. Therefore, the automatic compositors were calibrated while the pumps were idle and the program 

was set to collect more than 830 mL (specifically 870 mL) to account for the reduced volume that would be 

collected while the pumps were operating. On Day 1, the metals carboy collected 21 liters of sample (the volume of 

the classicals carboy was not noted). On Day 2, the metals and classicals carboys collected 20 and 21 liters, 

respectively. On Day 3, the metals and classicals carboys collected 20 and 21.5 liters, respectively. On Day 4, the 

metals and classicals carboys collected 19.5 and 20 liters, respectively. 
3-6

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

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

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

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

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

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

bottles were filled. The samplers then began setting up the compositors for the next day of 

samples using new tubing sets and composite containers. The automatic compositor was 

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

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

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

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

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

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

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

concentrations in the dissolved metals fractions. 

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

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

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

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

distance downstream of the pump. The samplers then attached another short length of silicone 

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

silicone tubing. This set-up allowed EPA to collect “true” split samples with Miami Fort’s 

representatives. Figure C-4, in Appendix C, is a picture of the set-up at the pump-off station. 

On Day 1 only, ERG collected field blank samples (SP-5) for total and dissolved metals 

and dissolved hexavalent chromium by pumping from a previously filled 20-liter container. See 

Section 5.2.3 for a description of the field blank sample collection procedures at the effluent 

from FGD wastewater treatment system. 

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

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

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

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

3.1: 

 Dissolved metals by 200.8; 

 Dissolved metals by 200.7; and 

 Dissolved hexavalent chromium. 

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

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

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

described in Section 3.1: 

 Total metals by 200.8; and 
3-7

 Total metals by 200.7. 

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

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

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

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

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

immediately placed on ice after sample collection. 

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

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

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

sampling episode. 

3.2 List of Analytes and Sample Preservation

Samples collected at Miami Fort were analyzed for the following pollutants: 

 Classicals: 

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

— Chemical oxygen demand (COD), 

— Total suspended solids (TSS), 

— Total dissolved solids (TDS), 

— Sulfate, 

— Chloride, 

— Total Kjeldahl nitrogen (TKN), 

— Ammonia as nitrogen, 

— Nitrate/nitrite as nitrogen, 

— Total phosphorus, 

— Total cyanide; 

 Total Metals: 

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

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

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

titanium, vanadium, and zinc. 

 Dissolved Metals: 

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

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

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

chemicals, and other sources. Table 3-4 lists the analytical methods used to determine pollutant 

concentrations. 

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

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

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

procedures described in Section 3.4 of the Sampling Plan. Immediately following sample 
3-8

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

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

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

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

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

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

hexavalent chromium samples were preserved with ammonium sulfate buffer solution and 

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

with sulfuric acid to a pH of <2 S.U. in the staging area, and the pH was confirmed with fourcolor pH strips. Each total cyanide sample was tested for sulfides and oxidants immediately after 

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

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

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

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

3.3 Plant Operational Data

During the EPA sampling episode, Miami Fort plant personnel provided the sampling 

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

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

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

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

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

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

3.4 Deviations from the Sampling and Analysis Plan

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

described below: 

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

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

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

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

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

to reach the desired pH. 

 Influent to FGD wastewater treatment system samples (SP-1, Day 2): After 

set up at the sampling location at the influent to FGD wastewater treatment 

system (SP-1), the sampling team had to wait approximately 15 minutes to collect 

the sample because the plant staff switched the pumps that were transferring the 

FGD scrubber purge to the equalization tank. 

 Field test temperature measurement (SP-2, Grab 4, Day 4): At the effluent 

from FGD wastewater treatment system (SP-2), the field temperature 

measurement taken during Grab 4 on Day 4 was only taken with the pH meter 

because the thermometer was misplaced. 
3-9

 Collection of field test measurements (SP-2, Grab 3, Day 2): The field test 

samples taken in conjunction with the Day 2 Grab 3 samples at the effluent from 

FGD wastewater treatment system (SP-2) were taken approximately 7 minutes 

after the grab sample because the effluent wastewater transfer pump kicked on 

immediately after the cyanide sample was taken. The water pressure was too low 

to collect the field test sample while the pump was running, so the samplers 

waited until the pump turned off in order to grab the field test sample. 

 Collection of total mercury (SP-2, Grab 1, Day 1): On Day 1 of sample 

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

bottle cap for the total mercury sample was dropped, but it fell onto the bottle bag 

and did not touch the ground. After the bottle was filled, the cap was used to seal 

the bottle. 

 Filtering and purging the influent to FGD wastewater treatment system 

sample (SP-1): When collecting the dissolved metal samples at the influent to 

FGD wastewater treatment system (SP-1) on Day 1, the capsule filter became 

clogged, so after the field blank and first sample collection, the filter was changed 

and briefly purged. On Day 2, 3, and 4, the filter/tubing was purged for less than a 

minute, 1 liter, and 0.5 liters, respectively, and there was no need to change the 

filter.

 Calibrating the automatic compositors at the effluent from FGD wastewater 

treatment system (SP-2): The Sampling Plan called for calibrating the 

compositors to collect 830 mL every hour; however, because the pumps that 

transfer the wastewater from the effluent tank to the ash pond do not operate 

continuously, the volume of water that could be pulled for a specific aliquot 

varied depending on if the pumps were operating (less volume collected) or idle. 

Therefore, the automatic compositors were calibrated while the pumps were idle 

and the program was set to collect more than 830 mL (specifically 870 mL) to 

account for the reduced volume that would be collected while the pumps were 

operating. 

 Influent to FGD wastewater treatment system dissolved metals samples 

pump-off (SP-1): The suspended solids content in the influent to the FGD 

wastewater treatment system samples was high; therefore, the samplers allowed 

the solids to settle for 100 minutes to two hours, before pumping off the dissolved 

metals samples each day, instead of allowing the solids to settle for one hour as 

the Sampling Plan suggested. 
3-10

Table 3-1. Sample Collection Information, Miami Fort

Sampling 

Point 

Number Sampling Point Description 

Type of 

Sample 

Sample 

Collection Date 

Sample Collection Time

SP-1 Influent to FGD Wastewater Treatment 

System – Day 1 

Grab 7/12/10 0924a and 1149b

Influent to FGD Wastewater Treatment 

System – Day 2 

Grab 7/13/10 1034a and 1247b

Influent to FGD Wastewater Treatment 

System – Day 3 

Grab 7/14/10 0912a and 1143b

Influent to FGD Wastewater Treatment 

System – Day 4 

Grab 7/15/10 0927a and 1137b

SP-2 Effluent from FGD Wastewater 

Treatment System – Day 1 

Composite 7/12/10 

 7/13/10

0731c

0841d

Grab 7/12/10 

 7/13/10 

0752e, 1353f , and 1956 g

0147 h 

Effluent from FGD Wastewater 

Treatment System – Day 2 

Composite 7/13/10 

 7/14/10 

0730c

0806d 

Grab 7/13/10 

7/14/10 

0745e, 1346f , and 1947 g

0147 h 

Effluent from FGD Wastewater 

Treatment System – Day 3 

Composite 7/14/10 

 7/15/10 

0730c

0813d 

Grab 7/14/10 

 7/15/10 

0744e, 1346f , and 1948 g

0150 h 

Effluent from FGD Wastewater 

Treatment System – Day 4 

Composite 7/15/10 

 7/16/10 

0730c

0658d 

Grab 7/15/10 

 7/16/10 

0747e, 1357f , and 1945 g

0145 h 

SP-3 Duplicate of Effluent from FGD 

Wastewater Treatment System – Day 2 

Composite 7/13/10 

 7/14/10 

0731c

0841d

Grab 7/13/10 

 7/14/10 

0746e, 1348f , and 1947 g

0149 h 

SP-4 Influent to FGD Wastewater Treatment 

System Field Blank 

Grab 7/12/10 0910i and 1138j

SP-5 Effluent from FGD Wastewater 

Treatment System Field Blank – Day 1

Composite 7/12/10 

7/13/10

0640k

0829l

Grab 7/12/10 0748m

Effluent from FGD Wastewater 

Treatment System Field Blank – Day 2

Grab 7/13/10 0739m

Effluent from FGD Wastewater 

Treatment System Field Blank – Day 3

Grab 7/14/10 0739m

Effluent from FGD Wastewater 

Treatment System Field Blank – Day 4

Grab 7/15/10 0743m

a

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

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

b

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

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

c Started compositor. 
3-11

d

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

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

classicals (BOD5, Group I, and Group II). e

Start time for the collection of the total and dissolved mercury Grab 1 samples. 

f

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

g

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

h

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

i

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

blank samples. 

j

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

field blank samples. 

k

 Filled 20-L field blank carboy 

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

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

m Start time for the collection of total mercury field blank samples. 
3-12 

Table 3-2. Sample Collection at Miami Fort

Sampling 

Point 

Number Sampling Point Name 

Total Metals 

(EPA Method 200.8 with 

collision cell)

Total Metals 

(EPA Method 200.7) 

Dissolved Metals 

(EPA Method 200.8 with 

collision cell) 

Dissolved Metals 

(EPA Method 200.7) 

Total Mercury 

Dissolved Mercury 

Hexavalent Chromium 

BOD

5

SP-1 Influent to the FGD Wastewater 

Treatment System 

4 4 4 4 4 4 4 4 

SP-2 Effluent from the FGD Wastewater 

Treatment System 

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

SP-3 Duplicate of Effluent from the FGD 

Wastewater Treatment System 

1 1 1 1 1 1 1 1 

SP-4 Field Blank for Influent to the FGD 

Wastewater Treatment System 

1 1 1 1 1 1 

SP-5 Field Blank for Effluent from the 

FGD Wastewater Treatment System 

1 1 1 1 4 1 

Total Number of Samples 11+1QC 11+1QC 11+1QC 11+1QC 14+1QC 9+1QC 11+1QC 9+1QC 9+a Group I includes total suspended solids (TSS), total dissolved solids (TDS), sulfate, and chloride. b Group II includes ammonia as nitrogen, nitrate/nitrite as nitrogen, total Kjeldahl nitrogen (TKN), chemical oxygen demand (COD), and total phosph

Table 3-3. Field Measurements, Miami Fort

Sampling 

Point 

Number 

Sampling Point 

Description Date Time 

Temperature (°C) pH (S.U.) 

Waste Stream 

Flow Rate 

(GPM)b Thermometer Probe Meter 

a Strips 

SP-1 Influent to FGD 

Wastewater Treatment System – Day 1

7/12/2010 0938 53 NAc 5.55 6 148d Samplers noted th

yellow color and solids. No detectetotal cyanide grab
3-13 

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

and 10.0. 

b The SP-2 flow rates provided in the table represent the instantaneous flow at the sampling point during the mercury grab sample colle

0.0 is shown as the flow rate, the effluent wastewater transfer were not operating and therefore, the sample was collected from the tap bfrom the wastewater volume in the effluent tank. 

c Not analyzed. d Scrubber purge flow is a calculated value based on pump discharge pressure provided by the plant. The plant does not have a flow m

rate of the FGD scrubber purge entering the Equalization tank. 

Influent to FGD Wastewater Treatment System – Day 2 

7/13/2010 1047 52.5 50.2 5.56 7 148d Samplers noted th

yellow color. No oxidants in total c

Influent to FGD Wastewater Treatment System – Day 3 

7/14/2010 0933 48 47.5 5.15 6 148d Samplers noted th

yellow color. No oxidants in total c

Influent to FGD Wastewater Treatment System – Day 4 

7/15/2010 0941 54 51 5.51 7 148d No detected sulfi

cyanide grab. 

SP-2 Effluent from FGD 

Wastewater Treatment System – Day 1

7/12/10 0755 43 41.7 8.7 9.5 246.7 Samples were cle

color and did not No detected sulficyanide grab.

7/12/10 1355 43 41 8.63 9 0.0 7/12/10 1956 42 39.9 8.44 9 243.9 7/13/10 0151 44 42.2 8.56 9 0.0 

Effluent from FGD Wastewater Treatment System – Day 2 

7/13/10 0750 44 8.56 9 0.0 Samplers noted th

yellow color. No oxidants in total c

7/13/10 1350 44 42 8.62 9 248.2 7/13/10 2005 45 42.5 8.46 9 0.0 7/14/10 0154 42 39.2 8.62 9 244.5 

Effluent from FGD Wastewater Treatment System – Day 3 

7/14/10 0746 43 40.1 8.55 9 0.0 Samples were cle

did not have any detected sulfides cyanide grab.

7/14/10 1347 44.5 42.5 8.26 9 0.0 7/14/10 1953 44 42.2 8.66 9 0.0 7/15/10 0154 43 40.9 8.38 9 0.0 

Effluent from FGD Wastewater Treatment System – Day 4 

7/15/10 0749 42 40 8.61 9 0.0 Samples were cle

did not have any detected sulfides cyanide grab.

7/15/10 1358 44 42 8.49 9 251.3 7/15/10 1950 45 42.3 8.53 9 0.0 7/16/10 0150 45 42.4 8.55 9 250.0 
3-14

Table 3-4. Crosswalk of Sample Number to Sampling Point and Day, Miami Fort

Sample Number Sample Point Sample Description 

71741 SP-1, Day 1 Influent to FGD Wastewater Treatment System - Day 1 

71742 SP-1, Day 2 Influent to FGD Wastewater Treatment System - Day 2 

71743 SP-1, Day 3 Influent to FGD Wastewater Treatment System - Day 3 

71744 SP-1, Day 4 Influent to FGD Wastewater Treatment System - Day 4 

71745 SP-2, Day 1 Effluent to FGD Wastewater Treatment System - Day 1 

71746 SP-2, Day 2 Effluent to FGD Wastewater Treatment System - Day 2 

71747 SP-2, Day 3 Effluent to FGD Wastewater Treatment System - Day 3 

71748 SP-2, Day 4 Effluent to FGD Wastewater Treatment System - Day 4 

71749 SP-3, Day 2 Duplicate of Effluent to FGD Wastewater Treatment System - Day 2 

71750 SP-4, Day 1 Influent to FGD Wastewater Treatment System Field Blank - Day 1 

71751 SP-5, Day 1 Effluent to FGD Wastewater Treatment System Field Blank - Day 1 

71752 SP-5, Day 2 Effluent to FGD Wastewater Treatment System Field Blank - Day 2 

71753 SP-5, Day 3 Effluent to FGD Wastewater Treatment System Field Blank - Day 3 

71754 SP-5, Day 4 Effluent to FGD Wastewater Treatment System Field Blank - Day 4 
3-15

Table 3-5. Analytical Methods, Miami Fort

Parameter Method Number 

Classicals

Biochemical oxygen demand (BOD5) SM 5210 B 

Chemical oxygen demand (COD) EPA 410.4 

Total suspended solids (TSS) SM 2540 D 

Total dissolved solids (TDS) SM 2540 C 

Sulfate EPA 300.0 

Chloride EPA 300.0 

Ammonia as nitrogen EPA 350.1 

Nitrate/nitrate as nitrogen EPA 353.2 

Total Kjeldahl nitrogen (TKN) EPA 351.2 

Total phosphorus EPA 365.1 

Total cyanide SM 4500 CN E 

Total and Dissolved Metals

Mercury EPA 1631E 

Hexavalent chromium (dissolved only) EPA 218.6 

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

nickel, selenium, silver, thallium, vanadium, and zinc 

EPA 200.8 with collision cell 

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

molybdenum, sodium, tin, and titanium 

EPA 200.7 
3-16

Table 3-6. Summary of Sample Container and Planned Preservation, Miami Fort 

Parameter 

Sample 

Container and 

Volume 

QC Sample 

Container and 

Volume On-Site Preservation 

Classicals 

BOD5 One 1-L plastic 

bottle 

One 1-L plastic 

bottle 

≤6C 

Group I a One 1-L plastic 

bottles 

One 1-L plastic 

bottles 

≤6C 

Group II b Two 1-L plastic 

bottles 

Two 1-L plastic 

bottles 

H2SO4 to pH <2 S.U., ≤6C 

Total cyanide One 1-L plastic 

bottle 

One 1-L plastic 

bottles 

Dilution until sulfide is not detected, 

NaAsO2 until total chlorine is not 

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

≤6C 

Metals 

Total metals (EPA Method 200.8 with 

collision cell) 

One 500-mL 

plastic bottle 

No additional 

volume needed 

None 

(acid preserve at laboratory) 

Total metals (EPA Method 200.7) One 500-mL 

plastic bottle 

No additional 

volume needed 

None 

(acid preserve at laboratory) 

Dissolved metals (EPA Method 200.8 

with collision cell) 

One 500-mL 

plastic bottle 

No additional 

volume needed 

0.45-μm filter (performed in field) 

(acid preserve at laboratory) 

Dissolved metals (EPA Method 200.7) One 500-mL 

plastic bottle 

No additional 

volume needed 

0.45-μm filter (performed in field) 

(acid preserve at laboratory) 

Total mercury: None 

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

glass bottle 

No additional 

volume needed 

Influent samples and field blank 

samples 

Two 250-mL 

glass bottle 

No additional 

volume needed 

Dissolved mercury: None 

(filter and acid preserve at 

laboratory) Manual composite grab samples Four 125-mL 

glass bottle 

No additional 

volume needed 

Influent samples One 250-mL 

glass bottle 

No additional 

volume needed 

Hexavalent chromium One 250-mL 

plastic bottle 

No additional 

volume needed 

0.45-μm filter (performed in field) 

Ammonium sulfate buffer to 

pH 9.3 – 9.7 S.U., ≤6C 

a

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

b

 Group II includes ammonia as nitrogen, COD, nitrate/nitrite as nitrogen, TKN, and total phosphorus.
3-17 

Table 3-7. Sample Preservation Summary, Miami Fort

Sampling Point 

Number Analysis Date 

Chemical 

Added Initial pH Final pH 

Amount 

Added 

(drops) 

71741 Group II Volume 1 7/12/10 H2SO4 7 <2 250 

71741 Group II Volume 2 7/12/10 H2SO4 7 <2 200 

71741 Hexavalent Chromium 7/12/10 (NH4)2SO4

Buffer 

6.5 6.8 100 

NH4OH 6.8 9.5 25 

71750 Hexavalent Chromium 7/12/10 (NH4)2SO4

Buffer 

6.5 8.5 100 

NH4OH 8.5 9.5 4 

71741 Total Cyanide 7/12/10 NaOH 7 10 200 

71745 Total Cyanide 7/12/10 NaOH 9 10 9 

71742 Group II Volume 1 7/13/10 H2SO4 7 2 150 

71742 Group II Volume 2 7/13/10 H2SO4 7 2 150 

71745 Group II Volume 1 7/13/10 H2SO4 9.5 <2 75 

71745 Group II Volume 2 7/13/10 H2SO4 9.5 <2 75 

71742 Hexavalent Chromium 7/13/10 (NH4)2SO4

Buffer 

6.5 7.1 100 

NH4OH 7.1 9.7 67 

71745 Hexavalent Chromium 7/13/10 (NH4)2SO4

Buffer 

8.7 8.7 100 

NH4OH 8.7 9.3 10 

71751 Hexavalent Chromium 7/13/10 (NH4)2SO4

Buffer 

6.5 8.5 50 

NH4OH 8.5 9.7 20 

71742 Total Cyanide 7/13/10 NaOH 6.5 10 400 

71746 Total Cyanide 7/13/10 NaOH 9 10 10 

71749 Total Cyanide 7/13/10 NaOH 9 10 10 

71743 Group II Volume 1 7/14/10 H2SO4 6 <2 200 

71743 Group II Volume 2 7/14/10 H2SO4 6 <2 200 

71746 Group II Volume 1 7/14/10 H2SO4 9 2 100 

71746 Group II Volume 2 7/14/10 H2SO4 9 2 100 

71749 Group II Volume 2 7/14/10 H2SO4 9 2 100 

71749 Group II Volume 1 7/14/10 H2SO4 9 2 100 

71743 Hexavalent Chromium 7/14/10 (NH4)2SO4

Buffer 

6.5 7.1 100 

NH4OH 7.1 9.7 60 

71746 Hexavalent Chromium 7/14/10 (NH4)2SO4

Buffer 

8.7 8.7 100 

NH4OH 8.7 9.5 15 
3-18 

Table 3-7. Sample Preservation Summary, Miami Fort

Sampling Point 

Number Analysis Date 

Chemical 

Added Initial pH Final pH 

Amount 

Added 

(drops) 

71749 Hexavalent Chromium 7/14/10 (NH4)2SO4

Buffer 

8.7 8.7 100 

NH4OH 8.7 9.7 15 

71743 Total Cyanide 7/14/10 NaOH 6 10 500 

71747 Total Cyanide 7/14/10 NaOH 9 10 7 

71747 Total Cyanide - QC 7/14/10 NaOH 9 10 7 

71744 Group II Volume 1 7/15/10 H2SO4 6 2 150 

71744 Group II Volume 2 7/15/10 H2SO4 6 2 150 

71747 Group II Volume 1 7/15/10 H2SO4 9 2 100 

71747 Group II Volume 2 7/15/10 H2SO4 9 2 100 

71747 Group II Volume 1 - QC 7/15/10 H2SO4 9 2 100 

71747 Group II Volume 2 - QC 7/15/10 H2SO4 9 2 100 

71744 Hexavalent Chromium 7/15/10 (NH4)2SO4

Buffer 

6.5 7.1 100 

NH4OH 7.1 9.5 120 

71747 Hexavalent Chromium - QC 7/15/10 (NH4)2SO4

Buffer 

8.7 8.7 100 

NH4OH 8.7 9.7 30 

71744 Total Cyanide 7/15/10 NaOH 6.5 10 500 

71748 Total Cyanide 7/15/10 NaOH 8.5 10 12 

71748 Group II Volume 2 7/16/10 H2SO4 9 2 125 

71748 Group II Volume 1 7/16/10 H2SO4 6.0 2 55 

71748 Hexavalent Chromium 7/16/10 (NH4)2SO4

Buffer 

8.7 8.7 100 

NH4OH 8.7 9.5 30 
3-19 

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

Unit ID Boiler Type 

Capacity 

(MW) 

Electricity Production 

(MW) 

(or Percent Capacity %)

SCR 

(No, On, Off) 

Particulate Control System 

(HS/CS ESP, or BH) 

7 Opposed Firing 550 538 MW On CS ESP 

8 Opposed Firing 550 545 MW On CS ESP 

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

Table 3-9. FGD Scrubber System Operating Characteristics, Miami Fort 

Unit ID 

Wet FGD 

System (Yes/No) 

Type of 

Scrubber 

Forced 

Oxidation 

(Yes/No) Sorbent 

Additives (DBA, 

formic acid, 

etc.) 

FGD Make-up 

Water Source 

SO2 Rem

Percen

7 Yes Spray Yes Limestone None Ohio River 97.4 8 Yes Spray Yes Limestone None Ohio River 96.9 
3-21

Table 3-10. Coal Usage during Sample Collection, Miami Fort 

Day of 

Sampling Unit ID Coal Type 

Amount of Coal 

Used During Day 

of Sampling 

(tpd) 

Source of Coal 

(Coal Region 

and/or State) 

Percent 

Sulfur in 

Coal 

(%) 

Chlorine Content of 

Coal 

(ppm) 

1 

7 Bituminous 3635 Tons 

Northern 

Appalachian/ 

Illinois Basin 

3.36% 

(Dry) 1070 ppm (Dry) 

8 Bituminous 5331 Tons Northern 

Appalachian 

4.05% 

(Dry) 574 ppm (dry) 

2 

7 Bituminous 4865 Tons 

Northern 

Appalachian/ 

Illinois Basin 

3.44% 

(Dry) 635 ppm (Dry) 

8 Bituminous 3678 Tons Northern 

Appalachian 

4.04% 

(Dry) 582 ppm (Dry) 

3 

7 Bituminous 5417 Tons 

Northern 

Appalachian/ 

Illinois Basin 

3.77% 

(Dry) 354 ppm (Dry) 

8 Bituminous 5165 Tons Northern 

Appalachian 

4.10% 

(Dry) 569 ppm (Dry) 

4 

7 Bituminous 6937 Tons 

Northern 

Appalachian/ 

Illinois Basin 

3.48% 

(Dry) 584 ppm (Dry) 

8 Bituminous 3382 Tons Northern 

Appalachian 

3.96% 

(Dry) 561 ppm (Dry) 
3-22

Table 3-11. Scrubber Slurry Information during Sample Collection, Miami Fort

Day of 

Sampling 

FGD 

System ID 

Associated 

Unit IDs 

Scrubber Slurry 

Blowdown Flow Rate 

Scrubber 

Slurry 

Percent 

Solids 

Time of 

Dewatering 

During 

Sampling Day 

Percent 

Filtrate 

Recycled 

Back to 

Scrubber 

Flow Rate 

(gpm) Duration 

1 

7 7 1269 17 hrs 23.3 Dewatered 2 times 100 % 

8 8 1104 24 hrs 23.5 Dewatered 3 times 100 %

2 

7 7 1240 17 hrs 22.7 Dewatered 3 times 100 %

8 8 1096 21 hrs 22.9 Dewatered 2 times 100 %

3 

7 7 1273 13 hrs 22.7 Dewatered 3 times 100 %

8 8 1114 19 hrs 22.2 Dewatered 2 times 100 %

4 

7 7 1270 19 hrs 22.5 Dewatered 3 times 100 %

8 8 1116 20 hrs 22.4 Dewatered 2 times 100 %
3-23 

Table 3-12. FGD Wastewater Treatment System Operation Information, Miami Fort

Day of Sampling 

Scrubber Purge Chemical Usage 

Flow Rate (gpm) b Duration Lime a Ferric Chloride 

Organosulfide: 

Nalmet 1689 c

Polyme

776

1 148 14 hrs pH – 8.5 N/A 20 ppm/5.0 gal 13/2

3.3/5

2 148 15 hrs pH – 8.6 N/A 20 ppm/5.2 gal 13/1

3.4/2

3 148 11 hrs pH – 8.5 N/A 20 ppm/4.9 gal 13/1

3.2/2

4 148 16 hrs pH – 8.5 N/A 20 ppm/4.3 gal 13/1

2.8/2

a Lime usage is approximately 9,000 lbs/day. b Scrubber purge flow is a calculated value based on pump discharge pressure. c Organosulfide and polymer usage are calculated values based on dosing set points. 
4-1 

4. LABORATORY ANALYTICAL RESULTS AND DISCUSSION

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

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

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

SP-1. 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 Miami Fort, 

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

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

4.1 Measured and Calculated Results for Influent to FGD Wastewater Treatment 

System 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, ERG 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 measured or calculated pollutant 

concentrations for the following phases of the sample: 

 Aqueous phase; 

 Solid phase; and 

 Total sample. 

The metals and classicals laboratory, TestAmerica Laboratories - Denver (TestAmerica), 

and the mercury laboratory, Frontier Global Sciences (Frontier), used two different approaches 

for the biphasic analysis. This section describes the approaches used by each laboratory and 

presents the results of the analyses. 

Metals and Classicals Analyses 

TestAmerica used EPA Methods 200.7 and 200.8 to analyze the wastewater samples for 

metals. Both EPA Methods 200.7 and 200.8 state, “Aqueous samples containing total suspended 

solids ≥1% (w/v) should be extracted as a solid type sample.” [3, 4] Because EPA expected the 

solids content to be greater than one percent, TestAmerica developed an approach for the 

analysis of the FGD influent samples that consisted of performing a pressure filtration to separate 

the solids from the sample and analyzing the solid and aqueous phases separately. TestAmerica 

also dried the solids prior to analysis, so the solid concentration is on a dry-weight basis. 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. 

TestAmerica used the same approach for the seven classical pollutants that were analyzed 

as biphasic samples: ammonia as nitrogen, chloride, sulfate, nitrate/nitrite, total cyanide, total 

Kjeldahl nitrogen (TKN), and total phosphorus. 

Mercury Analyses 

Frontier used EPA Method 1631E to analyze the wastewater samples for mercury. EPA 

Method 1631E does not contain any language stating how wastewater samples with high solid 

concentrations should be analyzed; therefore, Frontier developed an approach for the analysis of 

the FGD influent samples that minimized potential contamination to the samples. Frontier’s 

approach consisted of using a centrifuge to separate the solids from the sample and analyzing the 

solid and aqueous phases separately. Frontier did not dry the solids prior to analysis, so the solid 

concentration is on a wet-weight basis. 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 used Equation 4-1 to calculate the 

individual total mercury concentrations for the sample. 

Appendix Tables A-1 through A-4 present the results of the biphasic analysis for 

ammonia as nitrogen, nitrate/nitrite, chloride, sulfate, nitrate/nitrite, total cyanide, TKN, total 

phosphorus, total metals, and total mercury for each of the four days of sampling. Results are 

rounded to three significant figures. 

4.2 FGD Wastewater Treatment System

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

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

calculated 4-day average result for each analyte for the sampling point. The total metal results 

presented in Table 4-1 represent the calculated total result for all analytes for which biphasic 

separation was performed. Table 4-2 presents the analytical results for all classical and metal 

analytes for the four days of sampling at the effluent from the FGD wastewater treatment system 

(SP-2). 

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

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

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

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

sample-specific quantitation limit in parentheses. 
4-3 

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

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

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

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

difference (RPD). 

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

averages, ERG used the following methodology: 

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

together; 

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

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

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

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

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

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

the average of the sample-specific quantitation limits; and 

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

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

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

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

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

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

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

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

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

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

system. 

Appendix Tables A-5 through A-13 present all the analytical results from the influent to 

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

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

Note: The total metals results and the results for certain classical analytes (i.e., ammonia as nitrogen, nitrate/nitrite, chloride, sulfate, nitrate/nitrite, totphosphorus) represent the total result that was calculated based on the results of the solid and aqueous phase of the samples. See Section 4.1 for more < - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

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

value. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. 

Table 4-1. Influent to FGD Wastewater Treatment System, Miami Fort 

Analyte Units Method 

Influent to FGD Wastewater Treatment System 

Day 1 Day 2 Day 3 D

Classicals Ammonia mg/L 350.1 5.21 6.12 7.90 6.0Nitrate Nitrite as N mg/L 353.2 71.7 86.6 74.9 82Nitrogen, Total Kjeldahl mg/L 351.2 40.5 52.6 47.6 40Biochemical Oxygen Demand mg/L 5210B NQ (2.50) NQ (2.50) 3.30 ND (2Chemical Oxygen Demand mg/L 410.4 620 670 910 72Chloride mg/L 300.0 9,000 9,800 9,600 9,6Sulfate mg/L 300.0 18,000 21,000 32,000 24,0Cyanide, Total mg/L 4500 CN E 0.255 0.644 2.05 0.1Total Dissolved Solids mg/L 2540C 56,000 68,000 59,000 50,0Total Suspended Solids mg/L 2540D 16,000 30,000 20,000 19,0Phosphorus, Total mg/L 365.1 0.476 7.68 NQ (0.191) 6.5Total Metals Aluminum ug/L 200.7, 6010B 561,000 626,000 687,000 497,Antimony ug/L 200.8, 6020 NQ (10.3) NQ (11.0) NQ (13.4) NQ (9Arsenic ug/L 200.8, 6020 937 896 1,310 69Barium ug/L 200.7, 6010B 7,640 7,510 10,400 6,4Beryllium ug/L 200.7, 6010B 27.6 28.3 41.8 22Boron ug/L 200.7, 6010B 624,000 803,000 844,000 762,Cadmium ug/L 200.8, 6020 342 426 522 39Calcium ug/L 200.7, 6010B 1,340,000 1,350,000 2,060,000 1,140Chromium ug/L 200.8, 6020 4,000 4,460 4,430 3,6Cobalt ug/L 200.7, 6010B 425 503 632 45Copper ug/L 200.8, 6020 1,350 1,520 1,670 1,2Iron ug/L 200.7, 6010B 911,000 965,000 1,030,000 766,Lead ug/L 200.8, 6020 756 842 887 65Magnesium ug/L 200.7, 6010B 7,870,000 9,210,000 11,800,000 9,010
4-5 

Note: The total metals results and the results for certain classical analytes (i.e., ammonia as nitrogen, nitrate/nitrite, chloride, sulfate, nitrate/nitrite, totphosphorus) represent the total result that was calculated based on the results of the solid and aqueous phase of the samples. See Section 4.1 for more < - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

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

value. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. 

Table 4-1. Influent to FGD Wastewater Treatment System, Miami Fort 

Analyte Units Method 

Influent to FGD Wastewater Treatment System 

Day 1 Day 2 Day 3 D

Manganese ug/L 200.7, 6010B 93,100 105,000 157,000 96,0Mercury ng/L 1631E, FGS-069 166,000 148,000 231,000 44,0Molybdenum ug/L 200.7, 6010B 506 540 641 40Nickel ug/L 200.8, 6020 2,580 2,980 3,610 2,5Selenium ug/L 200.8, 6020 3,400 3,650 3,330 2,9Silver ug/L 200.8, 6020 NQ (6.06) NQ (6.50) NQ (7.47) NQ (Sodium ug/L 200.7, 6010B 355,000 427,000 502,000 404,Thallium ug/L 200.8, 6020 52.8 56.4 93.5 46Tin ug/L 200.7, 6010B NQ (403) NQ (430) NQ (460) NQ (Titanium ug/L 200.7, 6010B 2,020 2,050 4,140 1,8Vanadium ug/L 200.8, 6020 4,010 4,220 4,440 3,2Zinc ug/L 200.8, 6020 13,900 16,300 20,200 14,5Dissolved Metals Aluminum ug/L 200.7 4,200 B 2,400 B 29,000 B 2,8Antimony ug/L 200.8 3.40 3.30 3.70 2.8Arsenic ug/L 200.8 4.40 4.90 6.60 5.5Barium ug/L 200.7 140 140 180 15Beryllium ug/L 200.7 4.70 4.10 12.0 4.6Boron ug/L 200.7 650,000 B 690,000 B 820,000 730,Cadmium ug/L 200.8 340 390 510 42Calcium ug/L 200.7 690,000 670,000 620,000 640,Chromium ug/L 200.8 ND (8.00) ND (8.00) ND (8.00) ND (Chromium (VI) ug/L 218.6 ND (10.0) ND (10.0) ND (10.0) ND (Cobalt ug/L 200.7 340 360 490 38Copper ug/L 200.8 54.0 50.0 110 55Iron ug/L 200.7 NQ (200) ND (200) NQ (200) ND (Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2
4-6 

Note: The total metals results and the results for certain classical analytes (i.e., ammonia as nitrogen, nitrate/nitrite, chloride, sulfate, nitrate/nitrite, totphosphorus) represent the total result that was calculated based on the results of the solid and aqueous phase of the samples. See Section 4.1 for more < - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

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

value. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. 

Table 4-1. Influent to FGD Wastewater Treatment System, Miami Fort 

Analyte Units Method 

Influent to FGD Wastewater Treatment System 

Day 1 Day 2 Day 3 D

Magnesium ug/L 200.7 7,900,000 8,400,000 11,000,000 8,900Manganese ug/L 200.7 100,000 100,000 170,000 110,Mercury ng/L 1631E 1,110 1,830 1,600 1,9Molybdenum ug/L 200.7 120 110 130 90Nickel ug/L 200.8 1,700 1,700 2,500 2,0Selenium ug/L 200.8 290 330 330 30Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2Sodium ug/L 200.7 360,000 380,000 480,000 400,Thallium ug/L 200.8 25.0 26.0 49.0 26Tin ug/L 200.7 NQ (200) ND (200) ND (200) ND (Titanium ug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (2Vanadium ug/L 200.8 12.0 13.0 20.0 16Zinc ug/L 200.8 6,300 6,200 11,000 7,6
4-7 

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

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

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

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

B – Analyte was found in the blank and sample. C – pH upon receipt was less than 10 S.U. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. S – Seed correction blank recovery low. 

Table 4-2. Effluent from the FGD Wastewater Treatment System, Miami Fort 

Analyte Units Method

Effluent from the FGD Wastewater System 

Day 1 Day 2 Day 3 Day 4 

ClassicalsAmmonia mg/L 350.1 4.80 5.40 5.50 5.30 Nitrate Nitrite as N mg/L 353.2 55.0 295 58.0 61.0 Nitrogen, Total Kjeldahl mg/L 351.2 21.0 B 22.0 21.0 B 24.0 Biochemical Oxygen Demand mg/L 5210B 6.70 9.00 6.90 *,Min 4.60 Chemical Oxygen Demand mg/L 410.4 570 480 560 F,Min 510 Chloride mg/L 300.0 5,300 7,500 7,300 7,400 Sulfate mg/L 300.0 8,400 13,000 13,000 14,000 Cyanide, Total mg/L 4500 CN E 0.210 B < 1.23 0.600 B,C 1.50 Total Dissolved Solids mg/L 2540C 29,000 29,500 28,000 33,000 Total Suspended Solids mg/L 2540D 17.0 8.80 8.40 B 22.0 Phosphorus, Total mg/L 365.1 0.0960 B 0.123 0.180 B,F,Min 0.0750 Total MetalsAluminum ug/L 200.7 NQ (200) < 180 330 NQ (200) Antimony ug/L 200.8 6.80 6.95 5.70 5.80 Arsenic ug/L 200.8 4.30 4.85 4.90 4.40 Barium ug/L 200.7 150 155 160 150 Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.00) Boron ug/L 200.7 300,000 B 320,000 320,000 B,F,4 330,000 Cadmium ug/L 200.8 ND (4.00) ND (4.00) ND (4.00) ND (4.00) Calcium ug/L 200.7 890,000 850,000 840,000 800,000 Chromium ug/L 200.8 17.0 16.5 14.0 16.0 
4-8 

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

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

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

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

B – Analyte was found in the blank and sample. C – pH upon receipt was less than 10 S.U. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. S – Seed correction blank recovery low. 

Table 4-2. Effluent from the FGD Wastewater Treatment System, Miami Fort 

Analyte Units Method

Effluent from the FGD Wastewater System 

Day 1 Day 2 Day 3 Day 4 

Cobalt ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND (20.0) Copper ug/L 200.8 ND (4.00) ND (4.00) ND (4.00) ND (4.00) Iron ug/L 200.7 NQ (200) NQ (200) 260 NQ (200) Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.00) Magnesium ug/L 200.7 5,600,000 B 5,550,000 5,500,000 B,F,4 5,700,000 Manganese ug/L 200.7 170 B 89.0 280 B 100 Mercury ng/L 1631E 101 105 148 165 Molybdenum ug/L 200.7 220 200 180 150 Nickel ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.00) Selenium ug/L 200.8 560 535 800 4 480 Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) F,Min ND (2.00) Sodium ug/L 200.7 370,000 365,000 360,000 4 360,000 Thallium ug/L 200.8 14.0 14.0 14.0 12.0 Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (200) Titanium ug/L 200.7 ND (20.0) NQ (20.0) NQ (20.0) NQ (20.0) Vanadium ug/L 200.8 16.0 17.5 16.0 18.0 Zinc ug/L 200.8 ND (10.0) ND (10.0) ND (10.0) ND (10.0) Dissolved MetalsAluminum ug/L 200.7 ND (200) NQ (200) ND (200) ND (200) Antimony ug/L 200.8 7.80 6.80 6.60 5.80 Arsenic ug/L 200.8 4.80 < 3.00 4.80 4.70 Barium ug/L 200.7 140 145 150 150 
4-9 

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

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

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

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

B – Analyte was found in the blank and sample. C – pH upon receipt was less than 10 S.U. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. S – Seed correction blank recovery low. 

Table 4-2. Effluent from the FGD Wastewater Treatment System, Miami Fort 

Analyte Units Method

Effluent from the FGD Wastewater System 

Day 1 Day 2 Day 3 Day 4 

Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.00) Boron ug/L 200.7 300,000 B 325,000 320,000 F,4 330,000 Cadmium ug/L 200.8 ND (4.00) ND (4.00) ND (4.00) ND (4.00) Calcium ug/L 200.7 880,000 835,000 840,000 4 820,000 Chromium ug/L 200.8 14.0 14.0 15.0 ^ 15.0 Chromium (VI) ug/L 218.6 7.04 7.34 7.61 6.71 Cobalt ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND (20.0) Copper ug/L 200.8 NQ (4.00) NQ (4.00) ND (4.00) ND (4.00) Iron ug/L 200.7 ND (200) ND (200) ND (200) ND (200) Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.00) Magnesium ug/L 200.7 5,500,000 5,750,000 5,600,000 F,4 6,000,000 Manganese ug/L 200.7 160 B 84.0 250 B 93.0 Mercury ng/L 1631E 49.7 61.5 71.3 84.5 Molybdenum ug/L 200.7 210 195 170 150 Nickel ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.00) Selenium ug/L 200.8 560 495 640 4 530 Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) F,Min ND (2.00) Sodium ug/L 200.7 350,000 350,000 350,000 360,000 Thallium ug/L 200.8 14.0 14.0 13.0 12.0 Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (200) Titanium ug/L 200.7 ND (50.0) NQ (60.0) NQ (20.0) NQ (20.0) Vanadium ug/L 200.8 16.0 17.0 14.0 ^ 15.0 
4-10 

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

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

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

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

B – Analyte was found in the blank and sample. C – pH upon receipt was less than 10 S.U. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. S – Seed correction blank recovery low. 

Table 4-2. Effluent from the FGD Wastewater Treatment System, Miami Fort 

Analyte Units Method

Effluent from the FGD Wastewater System 

Day 1 Day 2 Day 3 Day 4 

Zinc ug/L 200.8 ND (10.0) ND (10.0) ND (10.0) ND (10.0) 
4-11 

< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

Analyte Units Method

Influent to FGD 

Wastewater Treatment 

System (SP-1)

4-Day Average

Effl

FGD Waste

Syst

4-Da

ClassicalsAmmonia mg/L 350.1 6.32 Nitrate Nitrite as N mg/L 353.2 79.0 Nitrogen, Total Kjeldahl mg/L 351.2 45.4 Biochemical Oxygen Demand mg/L 5210B < 1.70 Chemical Oxygen Demand mg/L 410.4 730 Chloride mg/L 300.0 9,500 Sulfate mg/L 300.0 23,800 Cyanide, Total mg/L 4500 CN E 0.787 < Total Dissolved Solids mg/L 2540C 58,300 Total Suspended Solids mg/L 2540D 21,300 Phosphorus, Total mg/L 365.1 < 3.69 
4-12 

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

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

value. 

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

Analyte Units Method

Influent to FGD 

Wastewater Treatment

System (SP-1)

4-Day Average

Efflu

FGD Waste

Syst

4-Da

Total Dissolved Total 

MetalsAluminum ug/L 200.7 593,000 9,600 < 178 Antimony ug/L 200.8 NQ (11.0) 3.30 6.31 Arsenic ug/L 200.8 960 5.35 4.61 Barium ug/L 200.7 7,990 153 154 Beryllium ug/L 200.7 30.0 6.35 ND (2.00) Boron ug/L 200.7 758,000 723,000 318,000 Cadmium ug/L 200.8 422 415 ND (4.00) Calcium ug/L 200.7 1,470,000 655,000 845,000 Chromium ug/L 200.8 4,130 ND (8.00) 15.9 Chromium (VI) ug/L 218.6 NA ND (10.0) NA Cobalt ug/L 200.7 505 393 ND (20.0) Copper ug/L 200.8 1,440 67.3 ND (4.00) Iron ug/L 200.7 918,000 NQ (200) < 140 Lead ug/L 200.8 784 ND (2.00) ND (2.00) Magnesium ug/L 200.7 9,470,000 9,050,000 5,590,000 Manganese ug/L 200.7 113,000 120,000 160 Mercury ng/L 1631E 147,000 1,630 130 Molybdenum ug/L 200.7 523 113 188 Nickel ug/L 200.8 2,930 1,980 NQ (4.00) Selenium ug/L 200.8 3,330 313 594 Silver ug/L 200.8 NQ (6.42) ND (2.00) ND (2.00) Sodium ug/L 200.7 422,000 405,000 364,000 Thallium ug/L 200.8 62.2 31.5 13.5 Tin ug/L 200.7 NQ (426) NQ (200) ND (200) 
4-13 

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

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

value. 

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

Analyte Units Method

Influent to FGD 

Wastewater Treatment

System (SP-1)

4-Day Average

Efflu

FGD Waste

Syst

4-Da

Total Dissolved Total 

Titanium ug/L 200.7 2,510 NQ (20.0) NQ (20.0) Vanadium ug/L 200.8 3,990 15.3 16.9 Zinc ug/L 200.8 16,200 7,780 ND (10.0) 
5-14 

5. DATA QUALITY

Quality assurance/quality control (QA/QC) procedures applicable to the Miami Fort 

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

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

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

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

QC standard checks. 

5.1 Analytical Quality Control

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

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

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

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

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

5.2 Field Quality Control

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

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

5.2.1 Bottle Blanks 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

No metals were detected in the bottle blanks, except for aluminum in two of the three 10-

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

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

ug/L); therefore, this contamination did not affect the results of the sampling episode. Appendix 
5-15 

Table A-14 presents all of the analytical results from the bottle blank analyses for the bottles 

used to collect the metals and mercury samples. 

5.2.2 Equipment Blanks 

EPA collects equipment blanks to evaluate possible contamination from the equipment 

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

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

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

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

precleaned equipment supplied for the episode. 

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

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

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

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

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

blank samples. 

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

contamination from the sampling equipment. Appendix Table A-14 presents all of the analytical 

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

collection of metals and mercury samples. 

5.2.3 Field Blanks 

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

contamination from sampling equipment, sampling equipment decontamination procedures, 

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

samples for the total and dissolved metals, dissolved hexavalent chromium, and total and 

dissolved mercury samples3

. 

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

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

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

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

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

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

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

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

 

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

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

filtering the sample, which is assessed as the field blank for the dissolved mercury sample. Mercury was detected at 

a concentration of 0.25 ng/L in the filtration blank performed for the fourth day of samples, which includes the 

influent to the FGD wastewater treatment system (Day 4), the third and fourth grab sample for the effluent from 

FGD wastewater treatment system (Day 3), and the first and second grab samples for effluent from FGD wastewater 

treatment system (Day 4). Mercury was not detected above the method detection limit (0.24 ng/L) in the filtration 

blanks performed for the first, second, third, or fifth day of samples.
5-16 

as “true” split samples with Miami Fort’s representative, using the same procedure discussed in 

the sample collection description (Section 3.1). 

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

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

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

composite container. After approximately 100 minutes, the sampling team began pumping off 

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

the tubing and filter were purged with 750 mL of blank water. The sample bottles were placed in 

a “cleanbox” and the ASTM Type 1 water was pumped through the tubing, capsule filter, and 

“Y” splitter, and into the sample bottles. EPA collected the field blank samples as “true” split 

samples with Miami Fort’s representative, using the same procedure discussed in the sample 

collection description (Section 3.1). 

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

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

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

the sample bottles under the clear plastic bag. 

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

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

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

composite container was used with a pump to fill the field blank composite container. Prior to 

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

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

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

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

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

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

After 24 hours, the ASTM Type 1 water in the field blank composite container was 

pumped off into the individual sample bottles. The sample bottles were placed in a “cleanbox” 

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

sample bottles. EPA collected the field blank samples as “true” split samples with Miami Fort’s 

representative, using the same procedure discussed in the sample collection description (Section 

3.1). Prior to filling the sample bottles, the tubing was purged with approximately one liter of 

ASTM Type 1 water. First the samplers collected the total metals by 200.8 and total metals by 

200.7 field blank samples. Then the sampling team attached a filter to the tubing set and purged 

the tubing with approximately 0.75 liter of ASTM Type 1 water. The samplers then collected the 

dissolved metals by 200.8, dissolved metals by 200.7, and dissolved hexavalent chromium field 

blank samples. 

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

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

included in the table. Results are rounded to three significant digits. Appendix Tables A-15 

through A-19 present all the analytical results for the field blanks from each of the sampling 

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

detection limit, but below the quantitation limit (i.e., J-values). 
5-17 

5.2.4 Field Duplicates 

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

precision for the episode. Field duplicate samples are separate samples collected from the same 

location as the original sample. The duplicate is filled immediately after the original sample and 

is stored and analyzed independently. The RPD between the two sample results is examined to 

determine the precision of the data. EPA used the following equation to calculate the RPD for 

the duplicate sample results. 

100

2

S D

S D

RPD (%) 





 



 

  (5-1) 

where: 

S = concentration of the analyte from original sample analysis; 

D = concentration of the analyte from the duplicate sample analysis; and 

RPD = relative percent difference between the original and duplicate sample 

result. 

During this sampling episode, EPA collected duplicate samples for the effluent from 

FGD wastewater treatment system (SP-3) during Day 2 of the sampling episode. The duplicate 

samples were analyzed for all analytes. Table 5-2 presents analytical results and the RPD for SP3. Results are rounded to three significant digits. Appendix Tables A-10 and A-13 present all the 

analytical results for the effluent from FGD wastewater treatment system (SP-2) Day 2 and the 

duplicate of the effluent from FGD wastewater treatment system (SP-3) sample analyses, 

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

limit, but below the quantitation limit (i.e., J-values). 
5-18 

Table 5-1. Field Blank Analytical Results, Miami Fort 

Analyte Sample Description Method Units 

Total MetalsMagnesium Effluent from FGD Wastewater Treatment System Field Blank - Day 1 200.7 ug/L Mercury Influent to FGD Wastewater Treatment System Field Blank - Day 1 1631E ng/L 
5-19 

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

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

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

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. MI – Matrix interferences present. Min – Minimum value. V – Serial dilution is not within control limits

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

Analyte Method Units

Original Effluent from 

FGD Wastewater 

Treatment System, Day 

2 Concentration (SP-2) 

Duplicate

Effluent from FGD 

Wastewater 

Treatment System 

Concentration 

(SP-3)

Aver

Resu

ClassicalsAmmonia 350.1 mg/L 5.30 5.50 5.4Nitrate Nitrite as N 353.2 mg/L 290 300 29Nitrogen, Total Kjeldahl 351.2 mg/L 21.0 B 23.0 B 22.Biochemical Oxygen Demand 5210B mg/L 8.40 9.60 9.0Chemical Oxygen Demand 410.4 mg/L 400 560 48Chloride 300.0 mg/L 7,500 7,500 7,50Sulfate 300.0 mg/L 13,000 13,000 13,0Cyanide, Total 4500 CN E mg/L 2.40 B NQ (0.100) B < 1.Total Dissolved Solids 2540C mg/L 32,000 27,000 29,5Total Suspended Solids 2540D mg/L 10.0 7.60 8.8Phosphorus, Total 365.1 mg/L 0.180 B 0.0650 B 0.12Total MetalsAluminum 200.7 ug/L 260 NQ (200) < 18Antimony 200.8 ug/L 6.90 7.00 6.9Arsenic 200.8 ug/L 5.60 4.10 4.8Barium 200.7 ug/L 150 160 15Beryllium 200.7 ug/L ND (2.00) ND (2.00) ND (2Boron 200.7 ug/L 320,000 B,F,4 320,000 B 320,0Cadmium 200.8 ug/L ND (4.00) ND (4.00) ND (4
5-20 

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

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

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

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. MI – Matrix interferences present. Min – Minimum value. V – Serial dilution is not within control limits

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

Analyte Method Units

Original Effluent from 

FGD Wastewater 

Treatment System, Day 

2 Concentration (SP-2) 

Duplicate

Effluent from FGD 

Wastewater 

Treatment System 

Concentration 

(SP-3)

Aver

Resu

Calcium 200.7 ug/L 840,000 4 860,000 850,0Chromium 200.8 ug/L 16.0 17.0 16.Cobalt 200.7 ug/L ND (20.0) ND (20.0) ND (2Copper 200.8 ug/L ND (4.00) ND (4.00) ND (4Iron 200.7 ug/L NQ (200) NQ (200) NQ (2Lead 200.8 ug/L ND (2.00) ND (2.00) ND (2Magnesium 200.7 ug/L 5,500,000 B,F,4 5,600,000 B 5,550Manganese 200.7 ug/L 88.0 B 90.0 B 89.Mercury 1631E ng/L 99.8 110 10Molybdenum 200.7 ug/L 200 200 20Nickel 200.8 ug/L NQ (4.00) NQ (4.00) NQ (4Selenium 200.8 ug/L 540 V,4,MI 530 53Silver 200.8 ug/L ND (2.00) F,Min ND (2.00) ND (2Sodium 200.7 ug/L 360,000 4 370,000 365,0Thallium 200.8 ug/L 14.0 14.0 14.Tin 200.7 ug/L ND (200) ND (200) ND (2Titanium 200.7 ug/L ND (20.0) NQ (20.0) NQ (2Vanadium 200.8 ug/L 17.0 18.0 17.Zinc 200.8 ug/L ND (10.0) ND (10.0) ND (1Dissolved Metals
5-21 

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

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

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

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. MI – Matrix interferences present. Min – Minimum value. V – Serial dilution is not within control limits

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

Analyte Method Units

Original Effluent from 

FGD Wastewater 

Treatment System, Day 

2 Concentration (SP-2) 

Duplicate

Effluent from FGD 

Wastewater 

Treatment System 

Concentration 

(SP-3)

Aver

Resu

Aluminum 200.7 ug/L NQ (200) B ND (200) NQ (2Antimony 200.8 ug/L 6.80 6.80 6.8Arsenic 200.8 ug/L NQ (4.00) 4.00 < 3.Barium 200.7 ug/L 150 140 14Beryllium 200.7 ug/L ND (2.00) ND (2.00) ND (2Boron 200.7 ug/L 330,000 F,4 320,000 325,0Cadmium 200.8 ug/L ND (4.00) ND (4.00) ND (4Calcium 200.7 ug/L 860,000 810,000 835,0Chromium 200.8 ug/L 14.0 14.0 14.Chromium (VI) 218.6 ug/L 7.32 7.35 7.3Cobalt 200.7 ug/L ND (20.0) ND (20.0) ND (2Copper 200.8 ug/L ND (4.00) NQ (4.00) NQ (4Iron 200.7 ug/L ND (200) ND (200) ND (2Lead 200.8 ug/L ND (2.00) ND (2.00) ND (2Magnesium 200.7 ug/L 5,900,000 F,4 5,600,000 5,750Manganese 200.7 ug/L 87.0 B 81.0 B 84.Mercury 1631E ng/L 63.1 59.9 61.Molybdenum 200.7 ug/L 200 190 19Nickel 200.8 ug/L NQ (4.00) NQ (4.00) NQ (4Selenium 200.8 ug/L 520 V,4,MI 470 49
5-22 

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

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

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

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. MI – Matrix interferences present. Min – Minimum value. V – Serial dilution is not within control limits

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

Analyte Method Units

Original Effluent from 

FGD Wastewater 

Treatment System, Day 

2 Concentration (SP-2) 

Duplicate

Effluent from FGD 

Wastewater 

Treatment System 

Concentration 

(SP-3)

Aver

Resu

Silver 200.8 ug/L ND (2.00) F,Min ND (2.00) ND (2Sodium 200.7 ug/L 360,000 340,000 350,0Thallium 200.8 ug/L 14.0 14.0 14.Tin 200.7 ug/L ND (200) ND (200) ND (2Titanium 200.7 ug/L NQ (20.0) ND (100.0) NQ (6Vanadium 200.8 ug/L 16.0 18.0 17.Zinc 200.8 ug/L ND (10.0) ND (10.0) ND (1
6-1

6. REFERENCES

1. Eastern Research Group, Inc., 2010. Sampling Plan, Duke Energy’s Miami Fort Station. 

July 1. DCN SE00501. 

2. Eastern Research Group, Inc., 2010. Quality Assurance Project Plan for the Steam 

Electric Effluent Guidelines Rulemaking. (October). DCN SE00058. 

3. U.S. EPA. 2001. Method 200.7: Determination of Metals and Trace Elements in Water 

and Wastes by Inductively Coupled Plasma – Atomic Emission Spectrometry. Revision 

4.4. 

4. U.S. EPA. 1994. Method 200.7: Determination of Trace Elements in Waters and Wastes 

by Inductively Coupled Plasma - Mass Spectrometry. Revision 5.4. 
Appendix A 

ANALYTICAL RESULTS 
A-1 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). V – Serial dilution is not within control limits. 

Table A-1. Biphasic Sample Results for Classicals and Total Metals, Influent to FGD 

Wastewater Treatment System, Day 1 Analytical Results, Miami Fort 

Analyte

Aqueous Phase Result 

(mg/L)

Solid Phase Result 

(mg/kg)

Calculated T

Result (mg

ClassicalsAmmonia 5.1 H,P,Est 24 H,P,Est 5.21Nitrate Nitrite as N 77 H,P,Est 49 H,P,Est 71.7Nitrogen, Total Kjeldahl 24 H,P,Est 830 H,P,Est 40.5Cyanide, Total 0.27 B,H,P,Est 0.35 J,B,H,P 0.255Phosphorus, Total 0.01 J,B,H,P 21 H,P,Est 0.476Total MetalsAluminum 6,000 25,000 561,000Antimony 3.1 0.16 J 6.4Arsenic 4.1 42 937Barium 88 F,Min 340 B 7,640Beryllium 3.4 1.1 27.6Boron 660,000 B,4 860 B 624,000Cadmium 320 2.2 342Calcium 610,000 35,000 B 1,340,000Chromium ND (8) U 180 ^ 4,000Cobalt 320 5.9 425Copper 42 59 1,350Iron ND (200) U 41,000 911,000
A-2 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). V – Serial dilution is not within control limits. 

Table A-1. Biphasic Sample Results for Classicals and Total Metals, Influent to FGD 

Wastewater Treatment System, Day 1 Analytical Results, Miami Fort 

Analyte

Aqueous Phase Result 

(mg/L)

Solid Phase Result 

(mg/kg)

Calculated T

Result (mg

Lead ND (2) U 34 756Magnesium 8,100,000 4 20,000 7,870,000Manganese 95,000 B,4 270 93,100Mercury 2,920 7,570 166,000Molybdenum 140 17 506Nickel 1,500 4 54 2,580Selenium 320 V,4,MI 140 3,400Silver ND (2) U,F,Min 0.14 J 3.11Sodium 360,000 1,100 355,000Thallium 14 1.8 B 52.8Tin 11 J 2.3 J 61.2Titanium ND (20) U 91 2,020Vanadium 8.7 J 180 4,010Zinc 5,200 B,4 410 13,900
A-3 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-2. Biphasic Sample Results for Classicals and Total Metals, Influent to FGD Waste

Treatment System, Day 2 Analytical Results, Miami Fort 

Analyte

Aqueous Phase 

Result 

(mg/L)

Solid Phase Result

(mg/kg)

Calculated Tot

Result (mg/L)

ClassicalsAmmonia 5.3 P,Est 28 H,P,Est 6.12Nitrate Nitrite as N 83 P,Est 64 H,P,Est 86.6Nitrogen, Total Kjeldahl 31 H,P,Est 840 H,P,Est 52.6Cyanide, Total 0.62 B,H,P,Est 0.33 J,B,H,P 0.644Phosphorus, Total 0.008 J,B,H,P 310 H,P,Est 7.68Total MetalsAluminum 6,600 B 25,000 626,000Antimony 2.7 0.15 J 6.48Arsenic 4.4 36 896Barium 83 300 B 7,510Beryllium 3.5 1 28.3Boron 760,000 B 980 B 803,000Cadmium 360 2.3 426Calcium 590,000 B 30,000 B 1,350,000Chromium ND (8) U 180 ^ 4,460Cobalt 360 5.4 503Copper 59 59 1,520Iron ND (200) U 39,000 965,000Lead 0.82 J 34 842Magnesium 8,500,000 20,000 9,210,000Manganese 96,000 B 260 105,000Mercury 2,990 7,330 148,000Molybdenum 140 16 540
A-4 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-2. Biphasic Sample Results for Classicals and Total Metals, Influent to FGD Waste

Treatment System, Day 2 Analytical Results, Miami Fort 

Analyte

Aqueous Phase 

Result 

(mg/L)

Solid Phase Result

(mg/kg)

Calculated Tot

Result (mg/L)

Nickel 1,600 54 2,980Selenium 420 130 3,650Silver ND (2) U 0.14 J 3.47Sodium 390,000 1,100 427,000Thallium 14 1.7 B 56.4Tin 6.1 J 2.2 J 60.7Titanium ND (20) U 83 2,050Vanadium 9.9 J 170 4,220Zinc 6,000 B 410 16,300
A-5 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-3. Biphasic Sample Results for Classicals and Total Metals, Influent to FGD Waste

Treatment System, Day 3 Analytical Results, Miami Fort

Analyte

Aqueous Phase Result 

(mg/L)

Solid Phase Result

(mg/kg)

Calculated Tot

Result (mg/L

ClassicalsAmmonia 7.7 P,Est 26 P,Est 7.9Nitrate Nitrite as N 79 P,Est 56 P,Est 74.9Nitrogen, Total Kjeldahl 29 P,Est 700 P,Est 47.6Cyanide, Total 2.2 B,H,P,Est 0.37 J,B,H,P 2.05Phosphorus, Total 0.013 J,B,P 1.9 J,P 0.068Total MetalsAluminum 40,000 B 22,000 4 687,000Antimony 3.6 0.16 J,F,Min 8.06Arsenic 7.2 44 1,310Barium 80 350 B 10,400Beryllium 10 1.1 41.8Boron 880,000 B 950 B,4 844,000Cadmium 500 2 522Calcium 570,000 B 52,000 B,4 2,060,000Chromium ND (8) U 150 4,^ 4,430Cobalt 500 5.7 632Copper 86 54 1,670Iron ND (200) U 35,000 4 1,030,000Lead 0.82 J 30 887Magnesium 12,000,000 23,000 11,800,000Manganese 160,000 B 300 157,000
A-6 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-3. Biphasic Sample Results for Classicals and Total Metals, Influent to FGD Waste

Treatment System, Day 3 Analytical Results, Miami Fort

Analyte

Aqueous Phase Result 

(mg/L)

Solid Phase Result

(mg/kg)

Calculated Tot

Result (mg/L

Mercury 3,640 5,990 231,000Molybdenum 150 17 641Nickel 2,400 47 3,610Selenium 410 100 3,330Silver ND (2) U 0.14 J,F,Min 4.14Sodium 500,000 1,300 502,000Thallium 34 2.1 B 93.5Tin ND (200) U 2.4 J 70.9Titanium ND (20) U 140 F Max 4,140Vanadium 14 150 4 4,440Zinc 11,000 B 340 4 20,200
A-7 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-4. Biphasic Sample Results for Classicals and Total Metals, Influent to FGD Wastewa

Treatment System, Day 4 Analytical Results, Miami Fort 

Analyte

Aqueous Phase Result 

(mg/L)

Solid Phase Result

(mg/kg)

Calculated Total 

Result (mg/L)

ClassicalsAmmonia 6.2 P,Est 23 P,Est 6.06Nitrate Nitrite as N 90 P,Est 65 P,Est 82.8Nitrogen, Total Kjeldahl 26 P,Est 900 P,Est 40.8Cyanide, Total 0.21 B,H,P,Est 0.42 J,B,H,P 0.198Phosphorus, Total 0.012 J,B,P 340 P,Est 6.52Total MetalsAluminum 20,000 B 25,000 497,000Antimony 2.5 0.14 J 4.95Arsenic 5.9 36 695Barium 100 330 B 6,410Beryllium 3.6 1 22.4Boron 820,000 B 990 B 762,000Cadmium 380 2.7 396Calcium 600,000 B 31,000 B 1,140,000Chromium ND (8) U 190 ^ 3,640Cobalt 390 5.5 459Copper 72 60 1,210Iron ND (200) U 40,000 766,000Lead ND (2) U 34 651Magnesium 9,500,000 21,000 9,010,000Manganese 100,000 B 280 96,000Mercury 4,370 4,990 44,000Molybdenum 110 16 406
A-8 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-4. Biphasic Sample Results for Classicals and Total Metals, Influent to FGD Wastewa

Treatment System, Day 4 Analytical Results, Miami Fort 

Analyte

Aqueous Phase Result 

(mg/L)

Solid Phase Result

(mg/kg)

Calculated Total 

Result (mg/L)

Nickel 1,700 53 2,560Selenium 470 130 2,920Silver ND (2) U 0.12 J 2.3Sodium 420,000 1,200 404,000Thallium 15 1.7 B 46.2Tin ND (200) U 2.3 J 44.1Titanium ND (20) U 95 1,820Vanadium 14 170 3,270Zinc 6,700 B 440 14,500
A-9 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-5. Influent to FGD Wastewater Treatment System, Day 1 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Classical Pollutants - TotalAmmonia 350.1 mg/l NA 0.192 2.05 5.21Nitrate Nitrite as N 353.2 mg/l NA 0.182 1.14 71.7Nitrogen, Total Kjeldahl 351.2 mg/l NA 3.02 15.9 40.5Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 2 Chemical Oxygen Demand 410.4 mg/L 10 41 200 620Chloride 300.0 mg/L 500 130 1,500 9,000Sulfate 300.0 mg/L 500 120 2,500 18,000Cyanide, Total 4500 CN E mg/l NA 0.0205 0.102 0.255Total Dissolved Solids 2540C mg/L 1 470 1,000 56,000Total Suspended Solids 2540D mg/L 1 55 200 16,000Phosphorus, Total 365.1 mg/l NA 0.0224 0.153 0.476Classicals Pollutants - Solid (dry weight)Ammonia 350.1 mg/Kg 1 4.1 9.9 24 Nitrate Nitrite as N 353.2 mg/Kg 1 0.36 10 49 Nitrogen, Total Kjeldahl 351.2 mg/Kg 10 120 510 830 Cyanide, Total 4500 CN E mg/Kg 1 0.095 0.46 0.35 
A-10 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-5. Influent to FGD Wastewater Treatment System, Day 1 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Phosphorus, Total 365.1 mg/Kg 1 0.8 4.8 21 Classicals Pollutants -Filtered AqueousAmmonia 350.1 mg/L 1 0.11 2 5.1 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 77 Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.38 5 24 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.27 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.01 Metals - Calculated TotalAluminum 200.7, 6010B ug/L NA 42 403 561,000Antimony 200.8, 6020 ug/L NA 1.26 10.3 6.4Arsenic 200.8, 6020 ug/L NA 27.8 315 937Barium 200.7, 6010B ug/L NA 3.96 40.3 7,640Beryllium 200.7, 6010B ug/L NA 1.38 12.9 27.6Boron 200.7, 6010B ug/L NA 265 5,700 624,000Cadmium 200.8, 6020 ug/L NA 1.5 7.89 342Calcium 200.7, 6010B ug/L NA 374 1,480 1,340,000Chromium 200.8, 6020 ug/L NA 43 114 4,000
A-11 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-5. Influent to FGD Wastewater Treatment System, Day 1 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Cobalt 200.7, 6010B ug/L NA 3.21 40.3 425Copper 200.8, 6020 ug/L NA 38.7 137 1,350Iron 200.7, 6010B ug/L NA 114 517 911,000Lead 200.8, 6020 ug/L NA 10.2 81.8 756Magnesium 200.7, 6010B ug/L NA 577 9,620 7,870,000Manganese 200.7, 6010B ug/L NA 14.1 481 93,100Mercury 1631E, FGS-069 ng/L NA 1,670 4,530 166,000Molybdenum 200.7, 6010B ug/L NA 7.25 81.1 506Nickel 200.8, 6020 ug/L NA 1.88 10.1 2,580Selenium 200.8, 6020 ug/L NA 6.12 24.8 3,400Silver 200.8, 6020 ug/L NA 1.41 6.06 3.11Sodium 200.7, 6010B ug/L NA 1,450 20,300 355,000Thallium 200.8, 6020 ug/L NA 0.58 6.06 52.8Tin 200.7, 6010B ug/L NA 24.4 403 61.2Titanium 200.7, 6010B ug/L NA 4.58 40.3 2,020Vanadium 200.8, 6020 ug/L NA 22 276 4,010Zinc 200.8, 6020 ug/L NA 204 625 13,900
A-12 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-5. Influent to FGD Wastewater Treatment System, Day 1 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Metals - DissolvedAluminum 200.7 ug/L 2 9.4 200 4,200 Antimony 200.8 ug/L 2 0.72 2 3.4Arsenic 200.8 ug/L 2 1.2 4 4.4Barium 200.7 ug/L 2 2.5 20 140Beryllium 200.7 ug/L 2 0.71 2 4.7Boron 200.7 ug/L 500 1,700 50,000 650,000 Cadmium 200.8 ug/L 5 2.9 10 340Calcium 200.7 ug/L 2 69 400 690,000Chromium 200.8 ug/L 2 3.3 8 ND (8) Chromium (VI) 218.6 ug/L 5 1.96 10 ND (10) Cobalt 200.7 ug/L 2 1.1 20 340Copper 200.8 ug/L 2 0.96 4 54Iron 200.7 ug/L 2 32 200 47 Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 500 5,400 100,000 7,900,000Manganese 200.7 ug/L 500 130 5,000 100,000
A-13 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-5. Influent to FGD Wastewater Treatment System, Day 1 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Mercury 1631E ng/L 500 124 260 1,110Molybdenum 200.7 ug/L 2 1.6 40 120Nickel 200.8 ug/L 25 11 50 1,700Selenium 200.8 ug/L 5 1.6 10 290Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 360,000Thallium 200.8 ug/L 2 0.47 2 25Tin 200.7 ug/L 2 4.8 200 8.7 Titanium 200.7 ug/L 2 1.6 20 3.2 Vanadium 200.8 ug/L 2 1.7 10 12Zinc 200.8 ug/L 100 200 500 6,300Metals - Filtered AqueousAluminum 200.7 ug/L 2 9.4 200 6,000Antimony 200.8 ug/L 2 0.72 2 3.1Arsenic 200.8 ug/L 2 1.2 4 4.1Barium 200.7 ug/L 2 2.5 20 88 Beryllium 200.7 ug/L 2 0.71 2 3.4
A-14 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-5. Influent to FGD Wastewater Treatment System, Day 1 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Boron 200.7 ug/L 50 170 5,000 660,000 Cadmium 200.8 ug/L 2 1.2 4 320Calcium 200.7 ug/L 2 69 400 610,000Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 320Copper 200.8 ug/L 2 0.96 4 42Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 50 540 10,000 8,100,000 Manganese 200.7 ug/L 50 13 500 95,000 Mercury 1631E ng/L 500 124 260 2,920Molybdenum 200.7 ug/L 2 1.6 40 140Nickel 200.8 ug/L 2 0.89 4 1,500 Selenium 200.8 ug/L 2 0.62 4 320 Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 360,000Thallium 200.8 ug/L 2 0.47 2 14
A-15 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-5. Influent to FGD Wastewater Treatment System, Day 1 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Tin 200.7 ug/L 2 4.8 200 11 Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 8.7 Zinc 200.8 ug/L 20 41 100 5,200 Metals - Solid (dry weight)Aluminum 6010B mg/kg 1 1.5 9.9 25,000Antimony 6020 mg/kg 2 0.027 0.38 0.16 Arsenic 6020 mg/kg 25 1.2 14 42Barium 6010B mg/kg 1 0.075 0.99 340 Beryllium 6010B mg/kg 1 0.033 0.5 1.1Boron 6010B mg/kg 5 4.9 50 860 Cadmium 6020 mg/kg 2 0.018 0.19 2.2Calcium 6010B mg/kg 1 14 50 35,000 Chromium 6020 mg/kg 25 1.8 4.8 180 Cobalt 6010B mg/kg 1 0.099 0.99 5.9Copper 6020 mg/kg 25 1.7 6 59Iron 6010B mg/kg 1 3.8 15 41,000
A-16 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-5. Influent to FGD Wastewater Treatment System, Day 1 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Lead 6020 mg/kg 25 0.43 3.6 34Magnesium 6010B mg/kg 1 3.7 20 20,000Manganese 6010B mg/kg 1 0.099 0.99 270Mercury FGS-069 ng/g 4,000 71.9 198 7,570Molybdenum 6010B mg/kg 1 0.26 2 17Nickel 6020 mg/kg 2 0.048 0.29 54Selenium 6020 mg/kg 2 0.25 0.95 140Silver 6020 mg/kg 2 0.039 0.19 0.14 Sodium 6010B mg/kg 1 58 500 1,100Thallium 6020 mg/kg 2 0.0067 0.19 1.8 Tin 6010B mg/kg 1 0.9 9.9 2.3 Titanium 6010B mg/kg 1 0.14 0.99 91Vanadium 6020 mg/kg 25 0.92 12 180Zinc 6020 mg/kg 25 7.5 24 410
A-17 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-6. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Classical Pollutants - TotalAmmonia 350.1 mg/l NA 0.214 2.3 6.12Nitrate Nitrite as N 353.2 mg/l NA 0.203 1.27 86.6Nitrogen, Total Kjeldahl 351.2 mg/l NA 3.36 18 52.6Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 1.9 Chemical Oxygen Demand 410.4 mg/L 10 41 200 670Chloride 300.0 mg/L 500 130 1,500 9,800Sulfate 300.0 mg/L 500 120 2,500 21,000Cyanide, Total 4500 CN E mg/l NA 0.0232 0.116 0.644Total Dissolved Solids 2540C mg/L 1 470 1,000 68,000Total Suspended Solids 2540D mg/L 1 55 200 30,000Phosphorus, Total 365.1 mg/l NA 0.208 1.29 7.68Classicals Pollutants - Solid (dry weight)Ammonia 350.1 mg/Kg 1 4.1 10 28 Nitrate Nitrite as N 353.2 mg/Kg 1 0.35 9.9 64 Nitrogen, Total Kjeldahl 351.2 mg/Kg 10 120 520 840 Cyanide, Total 4500 CN E mg/Kg 1 0.11 0.53 0.33 Phosphorus, Total 365.1 mg/Kg 10 8.2 50 310 Classicals Pollutants -Filtered AqueousAmmonia 350.1 mg/L 1 0.11 2 5.3 
A-18 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-6. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 83 Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.38 5 31 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.62 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.008 Metals - Calculated TotalAluminum 200.7, 6010B ug/L NA 44.3 430 626,000Antimony 200.8, 6020 ug/L NA 1.36 11 6.48Arsenic 200.8, 6020 ug/L NA 28.5 351 896Barium 200.7, 6010B ug/L NA 4.27 43 7,510Beryllium 200.7, 6010B ug/L NA 1.47 13.2 28.3Boron 200.7, 6010B ug/L NA 286 6,240 803,000Cadmium 200.8, 6020 ug/L NA 1.65 8.55 426Calcium 200.7, 6010B ug/L NA 392 1,520 1,350,000Chromium 200.8, 6020 ug/L NA 45.5 120 4,460Cobalt 200.7, 6010B ug/L NA 3.38 43 503Copper 200.8, 6020 ug/L NA 40.6 143 1,520Iron 200.7, 6010B ug/L NA 119 551 965,000Lead 200.8, 6020 ug/L NA 10.9 86.2 842Magnesium 200.7, 6010B ug/L NA 638 10,700 9,210,000Manganese 200.7, 6010B ug/L NA 15.6 535 105,000
A-19 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-6. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Mercury 1631E, FGS-069 ng/L NA 1,520 4,120 148,000Molybdenum 200.7, 6010B ug/L NA 7.58 85.5 540Nickel 200.8, 6020 ug/L NA 2.05 10.8 2,980Selenium 200.8, 6020 ug/L NA 6.58 26.4 3,650Silver 200.8, 6020 ug/L NA 1.52 6.5 3.47Sodium 200.7, 6010B ug/L NA 1,520 21,400 427,000Thallium 200.8, 6020 ug/L NA 0.638 6.5 56.4Tin 200.7, 6010B ug/L NA 25.5 430 60.7Titanium 200.7, 6010B ug/L NA 4.86 43 2,050Vanadium 200.8, 6020 ug/L NA 23.3 283 4,220Zinc 200.8, 6020 ug/L NA 196 621 16,300Metals - DissolvedAluminum 200.7 ug/L 2 9.4 200 2,400 Antimony 200.8 ug/L 2 0.72 2 3.3Arsenic 200.8 ug/L 2 1.2 4 4.9Barium 200.7 ug/L 2 2.5 20 140Beryllium 200.7 ug/L 2 0.71 2 4.1Boron 200.7 ug/L 500 1,700 50,000 690,000 Cadmium 200.8 ug/L 5 2.9 10 390Calcium 200.7 ug/L 2 69 400 670,000
A-20 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-6. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Chromium 200.8 ug/L 2 3.3 8 ND (8) Chromium (VI) 218.6 ug/L 5 1.96 10 ND (10) Cobalt 200.7 ug/L 2 1.1 20 360Copper 200.8 ug/L 2 0.96 4 50Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 500 5,400 100,000 8,400,000Manganese 200.7 ug/L 500 130 5,000 100,000Mercury 1631E ng/L 500 124 260 1,830Molybdenum 200.7 ug/L 2 1.6 40 110Nickel 200.8 ug/L 25 11 50 1,700Selenium 200.8 ug/L 5 1.6 10 330Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 380,000Thallium 200.8 ug/L 2 0.47 2 26Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 2.1 Vanadium 200.8 ug/L 2 1.7 10 13Zinc 200.8 ug/L 100 200 500 6,200
A-21 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-6. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Metals - Filtered AqueousAluminum 200.7 ug/L 2 9.4 200 6,600 Antimony 200.8 ug/L 2 0.72 2 2.7Arsenic 200.8 ug/L 2 1.2 4 4.4Barium 200.7 ug/L 2 2.5 20 83Beryllium 200.7 ug/L 2 0.71 2 3.5Boron 200.7 ug/L 50 170 5,000 760,000 Cadmium 200.8 ug/L 2 1.2 4 360Calcium 200.7 ug/L 2 69 400 590,000 Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 360Copper 200.8 ug/L 2 0.96 4 59Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 0.82 Magnesium 200.7 ug/L 50 540 10,000 8,500,000Manganese 200.7 ug/L 50 13 500 96,000 Mercury 1631E ng/L 500 124 260 2,990Molybdenum 200.7 ug/L 2 1.6 40 140Nickel 200.8 ug/L 2 0.89 4 1,600Selenium 200.8 ug/L 2 0.62 4 420
A-22 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-6. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 390,000Thallium 200.8 ug/L 2 0.47 2 14Tin 200.7 ug/L 2 4.8 200 6.1 Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 9.9 Zinc 200.8 ug/L 10 20 50 6,000 Metals - Solid (dry weight)Aluminum 6010B mg/kg 1 1.4 9.1 25,000Antimony 6020 mg/kg 2 0.025 0.36 0.15 Arsenic 6020 mg/kg 25 1.1 14 36Barium 6010B mg/kg 1 0.069 0.91 300 Beryllium 6010B mg/kg 1 0.03 0.45 1Boron 6010B mg/kg 5 4.5 45 980 Cadmium 6020 mg/kg 2 0.017 0.18 2.3Calcium 6010B mg/kg 1 13 45 30,000 Chromium 6020 mg/kg 25 1.7 4.5 180 Cobalt 6010B mg/kg 1 0.091 0.91 5.4Copper 6020 mg/kg 25 1.6 5.6 59Iron 6010B mg/kg 1 3.5 14 39,000
A-23 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-6. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Lead 6020 mg/kg 25 0.41 3.4 34Magnesium 6010B mg/kg 1 3.4 18 20,000Manganese 6010B mg/kg 1 0.091 0.91 260Mercury FGS-069 ng/g 4,000 71.1 196 7,330Molybdenum 6010B mg/kg 1 0.24 1.8 16Nickel 6020 mg/kg 2 0.046 0.27 54Selenium 6020 mg/kg 2 0.24 0.9 130Silver 6020 mg/kg 2 0.037 0.18 0.14 Sodium 6010B mg/kg 1 54 450 1,100Thallium 6020 mg/kg 2 0.0063 0.18 1.7 Tin 6010B mg/kg 1 0.83 9.1 2.2 Titanium 6010B mg/kg 1 0.13 0.91 83Vanadium 6020 mg/kg 25 0.87 11 170Zinc 6020 mg/kg 25 7.1 23 410
A-24 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-7. Influent to FGD Wastewater Treatment System, Day 3 Analytical Results, Miam

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Classical Pollutants – TotalAmmonia 350.1 mg/l NA 0.223 2.15 7.9Nitrate Nitrite as N 353.2 mg/l NA 0.186 1.22 74.9Nitrogen, Total Kjeldahl 351.2 mg/l NA 3.9 19.4 47.6Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 3.3Chemical Oxygen Demand 410.4 mg/L 10 41 200 910Chloride 300.0 mg/L 500 130 1,500 9,60Sulfate 300.0 mg/L 1,000 230 5,000 32,00Cyanide, Total 4500 CN E mg/l NA 0.0218 0.109 2.05Total Dissolved Solids 2540C mg/L 1 470 1,000 59,00Total Suspended Solids 2540D mg/L 1 55 200 20,00Phosphorus, Total 365.1 mg/l NA 0.0286 0.191 0.06Classicals Pollutants - Solid (dry weight)Ammonia 350.1 mg/Kg 1 4.1 10 26 Nitrate Nitrite as N 353.2 mg/Kg 1 0.35 9.9 56 Nitrogen, Total Kjeldahl 351.2 mg/Kg 10 120 500 700 Cyanide, Total 4500 CN E mg/Kg 1 0.11 0.55 0.37 Phosphorus, Total 365.1 mg/Kg 1 0.81 4.9 1.9 Classicals Pollutants -Filtered AqueousAmmonia 350.1 mg/L 1 0.11 2 7.7 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 79 Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.38 5 29 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 2.2 
A-25 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-7. Influent to FGD Wastewater Treatment System, Day 3 Analytical Results, Miam

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.01Metals - Calculated TotalAluminum 200.7, 6010B ug/L NA 50.1 460 687,0Antimony 200.8, 6020 ug/L NA 1.46 13.4 8.06Arsenic 200.8, 6020 ug/L NA 30.1 358 1,31Barium 200.7, 6010B ug/L NA 4.41 46 10,40Beryllium 200.7, 6010B ug/L NA 1.57 15.7 41.8Boron 200.7, 6010B ug/L NA 293 6,020 844,0Cadmium 200.8, 6020 ug/L NA 1.64 9.32 522Calcium 200.7, 6010B ug/L NA 2,010 7,170 2,060,0Chromium 200.8, 6020 ug/L NA 47.4 123 4,43Cobalt 200.7, 6010B ug/L NA 3.77 46 632Copper 200.8, 6020 ug/L NA 42.2 148 1,67Iron 200.7, 6010B ug/L NA 136 599 1,030,0Lead 200.8, 6020 ug/L NA 11 87.5 887Magnesium 200.7, 6010B ug/L NA 604 9,830 11,800,Manganese 200.7, 6010B ug/L NA 14.8 491 157,0Mercury 1631E, FGS-069 ng/L NA 2,860 7,810 231,0Molybdenum 200.7, 6010B ug/L NA 8.57 93.2 641Nickel 200.8, 6020 ug/L NA 2.27 12.3 3,61Selenium 200.8, 6020 ug/L NA 10.6 47.2 3,33Silver 200.8, 6020 ug/L NA 1.7 7.47 4.14Sodium 200.7, 6010B ug/L NA 1,790 23,200 502,0
A-26 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-7. Influent to FGD Wastewater Treatment System, Day 3 Analytical Results, Miam

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Thallium 200.8, 6020 ug/L NA 0.636 7.47 93.5Tin 200.7, 6010B ug/L NA 29.6 460 70.9Titanium 200.7, 6010B ug/L NA 5.32 46 4,14Vanadium 200.8, 6020 ug/L NA 23.7 296 4,44Zinc 200.8, 6020 ug/L NA 36.6 102 20,20Metals - DissolvedAluminum 200.7 ug/L 10 47 1,000 29,00Antimony 200.8 ug/L 2 0.72 2 3.7Arsenic 200.8 ug/L 2 1.2 4 6.6Barium 200.7 ug/L 2 2.5 20 180Beryllium 200.7 ug/L 2 0.71 2 12Boron 200.7 ug/L 500 1,700 50,000 820,0Cadmium 200.8 ug/L 50 29 100 510Calcium 200.7 ug/L 2 69 400 620,0Chromium 200.8 ug/L 2 3.3 8 ND (Chromium (VI) 218.6 ug/L 5 1.96 10 ND (1Cobalt 200.7 ug/L 2 1.1 20 490Copper 200.8 ug/L 2 0.96 4 110Iron 200.7 ug/L 2 32 200 42 Lead 200.8 ug/L 2 0.73 2 ND (Magnesium 200.7 ug/L 500 5,400 100,000 11,000,Manganese 200.7 ug/L 500 130 5,000 170,0Mercury 1631E ng/L 500 124 260 1,60
A-27 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-7. Influent to FGD Wastewater Treatment System, Day 3 Analytical Results, Miam

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Molybdenum 200.7 ug/L 2 1.6 40 130Nickel 200.8 ug/L 50 22 100 2,50Selenium 200.8 ug/L 5 1.6 10 330Silver 200.8 ug/L 2 0.59 2 ND (Sodium 200.7 ug/L 2 180 10,000 480,0Thallium 200.8 ug/L 2 0.47 2 49Tin 200.7 ug/L 2 4.8 200 ND (2Titanium 200.7 ug/L 2 1.6 20 1.8 Vanadium 200.8 ug/L 2 1.7 10 20Zinc 200.8 ug/L 200 410 1,000 11,00Metals - Filtered AqueousAluminum 200.7 ug/L 2 9.4 200 40,00Antimony 200.8 ug/L 2 0.72 2 3.6Arsenic 200.8 ug/L 2 1.2 4 7.2Barium 200.7 ug/L 2 2.5 20 80Beryllium 200.7 ug/L 2 0.71 2 10Boron 200.7 ug/L 50 170 5,000 880,0Cadmium 200.8 ug/L 2 1.2 4 500Calcium 200.7 ug/L 2 69 400 570,0Chromium 200.8 ug/L 2 3.3 8 ND (Cobalt 200.7 ug/L 2 1.1 20 500Copper 200.8 ug/L 2 0.96 4 86Iron 200.7 ug/L 2 32 200 ND (2
A-28 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-7. Influent to FGD Wastewater Treatment System, Day 3 Analytical Results, Miam

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Lead 200.8 ug/L 2 0.73 2 0.82 Magnesium 200.7 ug/L 50 540 10,000 12,000,Manganese 200.7 ug/L 50 13 500 160,0Mercury 1631E ng/L 500 124 260 3,64Molybdenum 200.7 ug/L 2 1.6 40 150Nickel 200.8 ug/L 2 0.89 4 2,40Selenium 200.8 ug/L 10 3.1 20 410Silver 200.8 ug/L 2 0.59 2 ND (Sodium 200.7 ug/L 2 180 10,000 500,0Thallium 200.8 ug/L 2 0.47 2 34Tin 200.7 ug/L 2 4.8 200 ND (2Titanium 200.7 ug/L 2 1.6 20 ND (2Vanadium 200.8 ug/L 2 1.7 10 14Zinc 200.8 ug/L 10 20 50 11,00Metals - Solid (dry weight)Aluminum 6010B mg/kg 1 1.4 9.3 22,00Antimony 6020 mg/kg 2 0.027 0.39 0.16 Arsenic 6020 mg/kg 20 0.98 12 44Barium 6010B mg/kg 1 0.071 0.93 350 Beryllium 6010B mg/kg 1 0.031 0.47 1.1Boron 6010B mg/kg 5 4.6 47 950 Cadmium 6020 mg/kg 2 0.018 0.19 2Calcium 6010B mg/kg 5 66 230 52,00
A-29 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-7. Influent to FGD Wastewater Treatment System, Day 3 Analytical Results, Miam

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Chromium 6020 mg/kg 20 1.5 3.9 150 Cobalt 6010B mg/kg 1 0.093 0.93 5.7Copper 6020 mg/kg 20 1.4 4.9 54Iron 6010B mg/kg 1 3.6 14 35,00Lead 6020 mg/kg 20 0.35 2.9 30Magnesium 6010B mg/kg 1 3.5 19 23,00Manganese 6010B mg/kg 1 0.093 0.93 300Mercury FGS-069 ng/g 4,000 72.1 199 5,99Molybdenum 6010B mg/kg 1 0.24 1.9 17Nickel 6020 mg/kg 2 0.049 0.29 47Selenium 6020 mg/kg 2 0.26 0.97 100Silver 6020 mg/kg 2 0.039 0.19 0.14 Sodium 6010B mg/kg 1 55 470 1,30Thallium 6020 mg/kg 2 0.0068 0.19 2.1 Tin 6010B mg/kg 1 0.85 9.3 2.4 Titanium 6010B mg/kg 1 0.13 0.93 140 Vanadium 6020 mg/kg 20 0.75 9.7 150 Zinc 6020 mg/kg 2 0.61 1.9 340 
A-30 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-8. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Classical Pollutants - TotalAmmonia 350.1 mg/l NA 0.178 2 6.06Nitrate Nitrite as N 353.2 mg/l NA 0.179 1.1 82.8Nitrogen, Total Kjeldahl 351.2 mg/l NA 2.64 14.5 40.8Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) Chemical Oxygen Demand 410.4 mg/L 10 41 200 720Chloride 300.0 mg/L 500 130 1,500 9,600Sulfate 300.0 mg/L 500 120 2,500 24,000Cyanide, Total 4500 CN E mg/l NA 0.0202 0.101 0.198Total Dissolved Solids 2540C mg/L 1 470 1,000 50,000Total Suspended Solids 2540D mg/L 1 92 330 19,000Phosphorus, Total 365.1 mg/l NA 0.163 1 6.52Classicals Pollutants - Solid (dry weight)Ammonia 350.1 mg/Kg 1 4.1 10 23 Nitrate Nitrite as N 353.2 mg/Kg 1 0.35 9.9 65 Nitrogen, Total Kjeldahl 351.2 mg/Kg 10 120 520 900 Cyanide, Total 4500 CN E mg/Kg 1 0.11 0.54 0.42 Phosphorus, Total 365.1 mg/Kg 10 8.3 50 340 Classicals Pollutants -Filtered AqueousAmmonia 350.1 mg/L 1 0.11 2 6.2 
A-31 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-8. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 90 Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.38 5 26 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.21 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.012 Metals - Calculated TotalAluminum 200.7, 6010B ug/L NA 44.9 411 497,000Antimony 200.8, 6020 ug/L NA 1.19 9.47 4.95Arsenic 200.8, 6020 ug/L NA 26 291 695Barium 200.7, 6010B ug/L NA 4.09 41.1 6,410Beryllium 200.7, 6010B ug/L NA 1.43 13.7 22.4Boron 200.7, 6010B ug/L NA 271 5,720 762,000Cadmium 200.8, 6020 ug/L NA 1.45 7.46 396Calcium 200.7, 6010B ug/L NA 407 1,550 1,140,000Chromium 200.8, 6020 ug/L NA 39.4 103 3,640Cobalt 200.7, 6010B ug/L NA 3.3 41.1 459Copper 200.8, 6020 ug/L NA 35.3 122 1,210Iron 200.7, 6010B ug/L NA 121 545 766,000Lead 200.8, 6020 ug/L NA 9.28 72.7 651Magnesium 200.7, 6010B ug/L NA 578 9,540 9,010,000Manganese 200.7, 6010B ug/L NA 14.1 476 96,000
A-32 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-8. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Mercury 1631E, FGS-069 ng/L NA 691 1,830 44,000Molybdenum 200.7, 6010B ug/L NA 7.58 84.1 406Nickel 200.8, 6020 ug/L NA 1.76 9.37 2,560Selenium 200.8, 6020 ug/L NA 5.54 22.6 2,920Silver 200.8, 6020 ug/L NA 1.3 5.64 2.3Sodium 200.7, 6010B ug/L NA 1,580 20,900 404,000Thallium 200.8, 6020 ug/L NA 0.56 5.64 46.2Tin 200.7, 6010B ug/L NA 25.4 411 44.1Titanium 200.7, 6010B ug/L NA 4.9 41.1 1,820Vanadium 200.8, 6020 ug/L NA 19.7 239 3,270Zinc 200.8, 6020 ug/L NA 168 524 14,500Metals - DissolvedAluminum 200.7 ug/L 2 9.4 200 2,800 Antimony 200.8 ug/L 2 0.72 2 2.8Arsenic 200.8 ug/L 2 1.2 4 5.5Barium 200.7 ug/L 2 2.5 20 150Beryllium 200.7 ug/L 2 0.71 2 4.6Boron 200.7 ug/L 500 1,700 50,000 730,000Cadmium 200.8 ug/L 5 2.9 10 420Calcium 200.7 ug/L 2 69 400 640,000
A-33 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-8. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Chromium 200.8 ug/L 2 3.3 8 ND (8) Chromium (VI) 218.6 ug/L 5 1.96 10 ND (10) Cobalt 200.7 ug/L 2 1.1 20 380Copper 200.8 ug/L 2 0.96 4 55Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 500 5,400 100,000 8,900,000Manganese 200.7 ug/L 500 130 5,000 110,000Mercury 1631E ng/L 500 124 260 1,990Molybdenum 200.7 ug/L 2 1.6 40 90Nickel 200.8 ug/L 25 11 50 2,000Selenium 200.8 ug/L 5 1.6 10 300Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 400,000Thallium 200.8 ug/L 2 0.47 2 26Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 2 Vanadium 200.8 ug/L 2 1.7 10 16 Zinc 200.8 ug/L 25 51 120 7,600Metals - Filtered Aqueous
A-34 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-8. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Aluminum 200.7 ug/L 2 9.4 200 20,000 Antimony 200.8 ug/L 2 0.72 2 2.5Arsenic 200.8 ug/L 2 1.2 4 5.9Barium 200.7 ug/L 2 2.5 20 100Beryllium 200.7 ug/L 2 0.71 2 3.6Boron 200.7 ug/L 50 170 5,000 820,000 Cadmium 200.8 ug/L 2 1.2 4 380Calcium 200.7 ug/L 2 69 400 600,000 Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 390Copper 200.8 ug/L 2 0.96 4 72Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 50 540 10,000 9,500,000Manganese 200.7 ug/L 50 13 500 100,000 Mercury 1631E ng/L 500 124 260 4,370Molybdenum 200.7 ug/L 2 1.6 40 110Nickel 200.8 ug/L 2 0.89 4 1,700Selenium 200.8 ug/L 2 0.62 4 470Silver 200.8 ug/L 2 0.59 2 ND (2) 
A-35 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-8. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Sodium 200.7 ug/L 2 180 10,000 420,000Thallium 200.8 ug/L 2 0.47 2 15Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 14Zinc 200.8 ug/L 10 20 50 6,700 Metals - Solid (dry weight)Aluminum 6010B mg/kg 1 1.9 12 25,000Antimony 6020 mg/kg 2 0.028 0.4 0.14 Arsenic 6020 mg/kg 25 1.3 15 36Barium 6010B mg/kg 1 0.095 1.2 330 Beryllium 6010B mg/kg 1 0.041 0.62 1Boron 6010B mg/kg 5 6.1 62 990 Cadmium 6020 mg/kg 2 0.019 0.2 2.7Calcium 6010B mg/kg 1 18 62 31,000 Chromium 6020 mg/kg 25 1.9 5 190 Cobalt 6010B mg/kg 1 0.12 1.2 5.5Copper 6020 mg/kg 25 1.8 6.2 60Iron 6010B mg/kg 1 4.8 19 40,000Lead 6020 mg/kg 25 0.45 3.7 34
A-36 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-8. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, Miami For

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Magnesium 6010B mg/kg 1 4.6 25 21,000Manganese 6010B mg/kg 1 0.12 1.2 280Mercury FGS-069 ng/g 4,000 71.9 198 4,990Molybdenum 6010B mg/kg 1 0.32 2.5 16Nickel 6020 mg/kg 2 0.05 0.3 53Selenium 6020 mg/kg 2 0.26 0.99 130Silver 6020 mg/kg 2 0.04 0.2 0.12 Sodium 6010B mg/kg 1 74 620 1,200Thallium 6020 mg/kg 2 0.007 0.2 1.7 Tin 6010B mg/kg 1 1.1 12 2.3 Titanium 6010B mg/kg 1 0.18 1.2 95Vanadium 6020 mg/kg 25 0.95 12 170Zinc 6020 mg/kg 25 7.8 25 440
A-37 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-9. Effluent from FGD Wastewater Treatment System, Day 1 Analytical Results, Miami F

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentratio

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 4.8Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 55Nitrogen, Total Kjeldahl 351.2 mg/L 4 0.31 4 21 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 6.7Chemical Oxygen Demand 410.4 mg/L 10 41 200 570Chloride 300.0 mg/L 500 130 1,500 5,300Sulfate 300.0 mg/L 500 120 2,500 8,400Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.21 Total Dissolved Solids 2540C mg/L 1 47 100 29,000Total Suspended Solids 2540D mg/L 1 1.1 4 17Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.096 Total MetalsAluminum 200.7 ug/L 2 9.4 200 180 Antimony 200.8 ug/L 2 0.72 2 6.8Arsenic 200.8 ug/L 2 1.2 4 4.3Barium 200.7 ug/L 2 2.5 20 150Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 500 1,700 50,000 300,000 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 890,000Chromium 200.8 ug/L 2 3.3 8 17Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 ND (4) 
A-38 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-9. Effluent from FGD Wastewater Treatment System, Day 1 Analytical Results, Miami F

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentratio

Iron 200.7 ug/L 2 32 200 110 Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 50 540 10,000 5,600,000 Manganese 200.7 ug/L 2 0.51 20 170 Mercury 1631E ng/L 20 4.87 10.2 101Molybdenum 200.7 ug/L 2 1.6 40 220Nickel 200.8 ug/L 2 0.89 4 3.4 Selenium 200.8 ug/L 2 0.62 4 560Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 370,000Thallium 200.8 ug/L 2 0.47 2 14Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 16Zinc 200.8 ug/L 2 4.1 10 ND (10) Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) Antimony 200.8 ug/L 2 0.72 2 7.8Arsenic 200.8 ug/L 2 1.2 4 4.8Barium 200.7 ug/L 2 2.5 20 140Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 50 170 5,000 300,000 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 880,000
A-39 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-9. Effluent from FGD Wastewater Treatment System, Day 1 Analytical Results, Miami F

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentratio

Chromium 200.8 ug/L 2 3.3 8 14Chromium (VI) 218.6 ug/L 1 0.39 2 7.04Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 1.4 Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 50 540 10,000 5,500,000Manganese 200.7 ug/L 2 0.51 20 160 Mercury 1631E ng/L 20 4.87 10.2 49.7Molybdenum 200.7 ug/L 2 1.6 40 210Nickel 200.8 ug/L 2 0.89 4 2.2 Selenium 200.8 ug/L 2 0.62 4 560Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 350,000Thallium 200.8 ug/L 2 0.47 2 14Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 5 4.1 50 ND (50) Vanadium 200.8 ug/L 2 1.7 10 16Zinc 200.8 ug/L 2 4.1 10 ND (10) 
A-40 

ND – Not detected (number in parentheses is the quantitation limit). 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). V – Serial dilution is not within control limits. 

Table A-10. Effluent from FGD Wastewater Treatment System, Day 2 Analytical Results, Mia

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Conce

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 5.3Nitrate Nitrite as N 353.2 mg/L 50 0.95 5 290Nitrogen, Total Kjeldahl 351.2 mg/L 4 0.31 4 21 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 8.4Chemical Oxygen Demand 410.4 mg/L 10 41 200 400Chloride 300.0 mg/L 500 130 1,500 7,500Sulfate 300.0 mg/L 500 120 2,500 13,000Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 2.4 Total Dissolved Solids 2540C mg/L 1 47 100 32,000Total Suspended Solids 2540D mg/L 1 1.1 4 10Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.18 Total MetalsAluminum 200.7 ug/L 2 9.4 200 260Antimony 200.8 ug/L 2 0.72 2 6.9Arsenic 200.8 ug/L 2 1.2 4 5.6Barium 200.7 ug/L 2 2.5 20 150Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 100 330 10,000 320,000 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 840,000 
A-41 

ND – Not detected (number in parentheses is the quantitation limit). 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). V – Serial dilution is not within control limits. 

Table A-10. Effluent from FGD Wastewater Treatment System, Day 2 Analytical Results, Mia

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Conce

Chromium 200.8 ug/L 2 3.3 8 16Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 ND (4) Iron 200.7 ug/L 2 32 200 110 Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 100 1,100 20,000 5,500,000 Manganese 200.7 ug/L 2 0.51 20 88 Mercury 1631E ng/L 20 4.87 10.2 99.8Molybdenum 200.7 ug/L 2 1.6 40 200Nickel 200.8 ug/L 2 0.89 4 3.3 Selenium 200.8 ug/L 2 0.62 4 540 Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 360,000 Thallium 200.8 ug/L 2 0.47 2 14Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 17Zinc 200.8 ug/L 2 4.1 10 ND (10) Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 24 Antimony 200.8 ug/L 2 0.72 2 6.8
A-42 

ND – Not detected (number in parentheses is the quantitation limit). 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). V – Serial dilution is not within control limits. 

Table A-10. Effluent from FGD Wastewater Treatment System, Day 2 Analytical Results, Mia

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Conce

Arsenic 200.8 ug/L 2 1.2 4 3.8 Barium 200.7 ug/L 2 2.5 20 150Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 50 170 5,000 330,000 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 860,000Chromium 200.8 ug/L 2 3.3 8 14Chromium (VI) 218.6 ug/L 1 0.39 2 7.32Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 ND (4) Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 50 540 10,000 5,900,000 Manganese 200.7 ug/L 2 0.51 20 87 Mercury 1631E ng/L 20 4.97 10.4 63.1Molybdenum 200.7 ug/L 2 1.6 40 200Nickel 200.8 ug/L 2 0.89 4 2.2 Selenium 200.8 ug/L 2 0.62 4 520 Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 360,000Thallium 200.8 ug/L 2 0.47 2 14
A-43 

ND – Not detected (number in parentheses is the quantitation limit). 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). V – Serial dilution is not within control limits. 

Table A-10. Effluent from FGD Wastewater Treatment System, Day 2 Analytical Results, Mia

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Conce

Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 4.5 Vanadium 200.8 ug/L 2 1.7 10 16Zinc 200.8 ug/L 2 4.1 10 ND (10) 
A-44 

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

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-11. Effluent from FGD Wastewater Treatment System, Day 3 Analytical Results, Mia

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 5.5Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 58Nitrogen, Total Kjeldahl 351.2 mg/L 4 0.31 4 21 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 6.9 Chemical Oxygen Demand 410.4 mg/L 10 41 200 56Chloride 300.0 mg/L 500 130 1,500 7,30Sulfate 300.0 mg/L 500 120 2,500 13,0Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.6 Total Dissolved Solids 2540C mg/L 1 47 100 28,0Total Suspended Solids 2540D mg/L 1 1.1 4 8.4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.1Total MetalsAluminum 200.7 ug/L 2 9.4 200 33Antimony 200.8 ug/L 2 0.72 2 5.7Arsenic 200.8 ug/L 2 1.2 4 4.9Barium 200.7 ug/L 2 2.5 20 16Beryllium 200.7 ug/L 2 0.71 2 ND Boron 200.7 ug/L 100 330 10,000 320,0Cadmium 200.8 ug/L 2 1.2 4 ND Calcium 200.7 ug/L 2 69 400 840,0Chromium 200.8 ug/L 2 3.3 8 14Cobalt 200.7 ug/L 2 1.1 20 ND (Copper 200.8 ug/L 2 0.96 4 ND Iron 200.7 ug/L 2 32 200 26Lead 200.8 ug/L 2 0.73 2 ND 
A-45 

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

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-11. Effluent from FGD Wastewater Treatment System, Day 3 Analytical Results, Mia

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Magnesium 200.7 ug/L 100 1,100 20,000 5,500Manganese 200.7 ug/L 2 0.51 20 28Mercury 1631E ng/L 100 24.4 51 14Molybdenum 200.7 ug/L 2 1.6 40 18Nickel 200.8 ug/L 2 0.89 4 2.9 Selenium 200.8 ug/L 10 3.1 20 80Silver 200.8 ug/L 2 0.59 2 ND Sodium 200.7 ug/L 2 180 10,000 360,0Thallium 200.8 ug/L 2 0.47 2 14Tin 200.7 ug/L 2 4.8 200 ND (2Titanium 200.7 ug/L 2 1.6 20 7.5 Vanadium 200.8 ug/L 2 1.7 10 16Zinc 200.8 ug/L 2 4.1 10 ND (Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 ND (2Antimony 200.8 ug/L 2 0.72 2 6.6Arsenic 200.8 ug/L 2 1.2 4 4.8Barium 200.7 ug/L 2 2.5 20 15Beryllium 200.7 ug/L 2 0.71 2 ND Boron 200.7 ug/L 50 170 5,000 320,0Cadmium 200.8 ug/L 2 1.2 4 ND Calcium 200.7 ug/L 2 69 400 840,0Chromium 200.8 ug/L 2 3.3 8 15 Chromium (VI) 218.6 ug/L 1 0.39 2 7.6Cobalt 200.7 ug/L 2 1.1 20 ND (Copper 200.8 ug/L 2 0.96 4 ND 
A-46 

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

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-11. Effluent from FGD Wastewater Treatment System, Day 3 Analytical Results, Mia

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Iron 200.7 ug/L 2 32 200 ND (2Lead 200.8 ug/L 2 0.73 2 ND Magnesium 200.7 ug/L 50 540 10,000 5,600Manganese 200.7 ug/L 2 0.51 20 25Mercury 1631E ng/L 20 4.87 10.2 71.Molybdenum 200.7 ug/L 2 1.6 40 17Nickel 200.8 ug/L 2 0.89 4 2.3 Selenium 200.8 ug/L 10 3.1 20 64Silver 200.8 ug/L 2 0.59 2 ND Sodium 200.7 ug/L 2 180 10,000 350,0Thallium 200.8 ug/L 2 0.47 2 13Tin 200.7 ug/L 2 4.8 200 ND (2Titanium 200.7 ug/L 2 1.6 20 4.6 Vanadium 200.8 ug/L 2 1.7 10 14 Zinc 200.8 ug/L 2 4.1 10 ND (
A-47 

ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. S – Seed correction blank recovery low. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-12. Effluent from FGD Wastewater Treatment System, Day 4 Analytical Results, Mia

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 5.Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 6Nitrogen, Total Kjeldahl 351.2 mg/L 4 0.31 4 24 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 4.Chemical Oxygen Demand 410.4 mg/L 10 41 200 51Chloride 300.0 mg/L 500 130 1,500 7,4Sulfate 300.0 mg/L 500 120 2,500 14,0Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 1.Total Dissolved Solids 2540C mg/L 1 47 100 33,0Total Suspended Solids 2540D mg/L 1 2.2 8 22Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.0Total MetalsAluminum 200.7 ug/L 2 9.4 200 53 Antimony 200.8 ug/L 2 0.72 2 5.Arsenic 200.8 ug/L 2 1.2 4 4.Barium 200.7 ug/L 2 2.5 20 15Beryllium 200.7 ug/L 2 0.71 2 ND Boron 200.7 ug/L 100 330 10,000 330,Cadmium 200.8 ug/L 2 1.2 4 ND Calcium 200.7 ug/L 2 69 400 800,Chromium 200.8 ug/L 2 3.3 8 16Cobalt 200.7 ug/L 2 1.1 20 ND (Copper 200.8 ug/L 2 0.96 4 ND Iron 200.7 ug/L 2 32 200 13Lead 200.8 ug/L 2 0.73 2 ND Magnesium 200.7 ug/L 100 1,100 20,000 5,700
A-48 

ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. S – Seed correction blank recovery low. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-12. Effluent from FGD Wastewater Treatment System, Day 4 Analytical Results, Mia

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Manganese 200.7 ug/L 2 0.51 20 10Mercury 1631E ng/L 100 24.1 50.5 16Molybdenum 200.7 ug/L 2 1.6 40 15Nickel 200.8 ug/L 2 0.89 4 2.Selenium 200.8 ug/L 2 0.62 4 48Silver 200.8 ug/L 2 0.59 2 ND Sodium 200.7 ug/L 2 180 10,000 360,Thallium 200.8 ug/L 2 0.47 2 12Tin 200.7 ug/L 2 4.8 200 ND (Titanium 200.7 ug/L 2 1.6 20 6.Vanadium 200.8 ug/L 2 1.7 10 18Zinc 200.8 ug/L 2 4.1 10 ND (Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 ND (Antimony 200.8 ug/L 2 0.72 2 5.Arsenic 200.8 ug/L 2 1.2 4 4.Barium 200.7 ug/L 2 2.5 20 15Beryllium 200.7 ug/L 2 0.71 2 ND Boron 200.7 ug/L 50 170 5,000 330,Cadmium 200.8 ug/L 2 1.2 4 ND Calcium 200.7 ug/L 2 69 400 820,Chromium 200.8 ug/L 2 3.3 8 15 Chromium (VI) 218.6 ug/L 1 0.39 2 6.7Cobalt 200.7 ug/L 2 1.1 20 ND (Copper 200.8 ug/L 2 0.96 4 ND Iron 200.7 ug/L 2 32 200 ND (Lead 200.8 ug/L 2 0.73 2 ND 
A-49 

ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. S – Seed correction blank recovery low. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-12. Effluent from FGD Wastewater Treatment System, Day 4 Analytical Results, Mia

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Magnesium 200.7 ug/L 50 540 10,000 6,000Manganese 200.7 ug/L 2 0.51 20 93 Mercury 1631E ng/L 20 4.83 10.1 84Molybdenum 200.7 ug/L 2 1.6 40 15Nickel 200.8 ug/L 2 0.89 4 1.Selenium 200.8 ug/L 2 0.62 4 53Silver 200.8 ug/L 2 0.59 2 ND Sodium 200.7 ug/L 2 180 10,000 360,Thallium 200.8 ug/L 2 0.47 2 12Tin 200.7 ug/L 2 4.8 200 ND (Titanium 200.7 ug/L 2 1.6 20 4.Vanadium 200.8 ug/L 2 1.7 10 15 Zinc 200.8 ug/L 2 4.1 10 ND (
A-50 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-13. Duplicate of Effluent from FGD Wastewater Treatment System, Day 2 Analytical Resul

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 50 0.95 5 Nitrogen, Total Kjeldahl 351.2 mg/L 4 0.31 4 Biochemical Oxygen Demand 5210B mg/L 1 0.59 5 Chemical Oxygen Demand 410.4 mg/L 10 41 200 Chloride 300.0 mg/L 500 130 1,500 Sulfate 300.0 mg/L 500 120 2,500 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 100 330 10,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 100 1,100 20,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 20 4.87 10.2 Molybdenum 200.7 ug/L 2 1.6 40 
A-51 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-13. Duplicate of Effluent from FGD Wastewater Treatment System, Day 2 Analytical Resul

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL 

Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 0.39 2 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 20 4.87 10.2 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 5 1.6 10 
A-52 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-13. Duplicate of Effluent from FGD Wastewater Treatment System, Day 2 Analytical Resul

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL 

Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 10 8.2 100 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

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

A-53 

Table A-14. Bottle Blank and Equipment Blank Analytical Data, Miami Fort

Analyte Method Process Units Concentration 

HDPE 250 ml Plastic Bottles – Bottle Blank (for metals and hexavalent chromium samples) 

Aluminum EPA 1638 Total Recoverable ug/L ND (4.0) 

Antimony EPA 1638 Total Recoverable ug/L ND (0.020) 

Arsenic EPA 1638 Total Recoverable ug/L ND (0.15) 

Barium EPA 1638 Total Recoverable ug/L ND (0.20) 

Beryllium EPA 1638 Total Recoverable ug/L ND (0.060) 

Boron EPA 1638 Total Recoverable ug/L ND (3.0) 

Cadmium EPA 1638 Total Recoverable ug/L ND (0.020) 

Calcium EPA 1638 Total Recoverable ug/L ND (40) 

Chromium EPA 1638 Total Recoverable ug/L ND (0.10) 

Cobalt EPA 1638 Total Recoverable ug/L ND (0.10) 

Copper EPA 1638 Total Recoverable ug/L ND (0.10) 

Iron EPA 1638 Total Recoverable ug/L ND (10) 

Lead EPA 1638 Total Recoverable ug/L ND (0.040) 

Magnesium EPA 1638 Total Recoverable ug/L ND (2.5) 

Manganese EPA 1638 Total Recoverable ug/L ND (0.10) 

Molybdenum EPA 1638 Total Recoverable ug/L ND (0.060) 

Nickel EPA 1638 Total Recoverable ug/L ND (0.10) 

Selenium EPA 1638 Total Recoverable ug/L ND (0.60) 

Silver EPA 1638 Total Recoverable ug/L ND (0.020) 

Sodium EPA 1638 Total Recoverable ug/L ND (20) 

Thallium EPA 1638 Total Recoverable ug/L ND (0.0050) 

Tin EPA 1638 Total Recoverable ug/L ND (0.10) 

Titanium EPA 1638 Total Recoverable ug/L ND (0.50) 

Vanadium EPA 1638 Total Recoverable ug/L ND (0.10) 

Zinc EPA 1638 Total Recoverable ug/L ND (0.20) 

HDPE 500 ml Plastic Bottles – Bottle Blank (for metals samples) 

Aluminum EPA 1638 Total Recoverable ug/L ND (4.0) 

Antimony EPA 1638 Total Recoverable ug/L ND (0.020) 

Arsenic EPA 1638 Total Recoverable ug/L ND (0.15) 

Barium EPA 1638 Total Recoverable ug/L ND (0.20) 

Beryllium EPA 1638 Total Recoverable ug/L ND (0.060) 

Boron EPA 1638 Total Recoverable ug/L ND (3.0) 

Cadmium EPA 1638 Total Recoverable ug/L ND (0.020) 

Calcium EPA 1638 Total Recoverable ug/L ND (40) 

Chromium EPA 1638 Total Recoverable ug/L ND (0.10) 

Cobalt EPA 1638 Total Recoverable ug/L ND (0.10) 

Copper EPA 1638 Total Recoverable ug/L ND (0.10) 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

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

A-54 

Table A-14. Bottle Blank and Equipment Blank Analytical Data, Miami Fort

Analyte Method Process Units Concentration 

Iron EPA 1638 Total Recoverable ug/L ND (10) 

Lead EPA 1638 Total Recoverable ug/L ND (0.040) 

Magnesium EPA 1638 Total Recoverable ug/L ND (2.5) 

Manganese EPA 1638 Total Recoverable ug/L ND (0.10) 

Molybdenum EPA 1638 Total Recoverable ug/L ND (0.060) 

Nickel EPA 1638 Total Recoverable ug/L ND (0.10) 

Selenium EPA 1638 Total Recoverable ug/L ND (0.60) 

Silver EPA 1638 Total Recoverable ug/L ND (0.020) 

Sodium EPA 1638 Total Recoverable ug/L ND (20) 

Thallium EPA 1638 Total Recoverable ug/L ND (0.0050) 

Tin EPA 1638 Total Recoverable ug/L ND (0.10) 

Titanium EPA 1638 Total Recoverable ug/L ND (0.50) 

Vanadium EPA 1638 Total Recoverable ug/L ND (0.10) 

Zinc EPA 1638 Total Recoverable ug/L ND (0.20) 

125 ml Glass Bottles – Bottle Blank (for mercury composite samples)

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

250 ml Glass Bottles – Bottle Blank (for mercury grab samples)

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

LDPE 10 L Composite Bottles – Bottle Blank (sample composite bottle for dissolved/filtration pump-off)

Aluminuma EPA 1638 Dissolved ug/L 4.71 

Antimony EPA 1638 Dissolved ug/L ND (0.50) 

Arsenic EPA 1638 Dissolved ug/L ND (0.50) 

Barium EPA 1638 Dissolved ug/L ND (0.10) 

Beryllium EPA 1638 Dissolved ug/L ND (0.10) 

Cadmium EPA 1638 Dissolved ug/L ND (0.10) 

Chromium EPA 1638 Dissolved ug/L ND (1.0) 

Cobalt EPA 1638 Dissolved ug/L ND (0.10) 

Copper EPA 1638 Dissolved ug/L ND (0.30) 

Lead EPA 1638 Dissolved ug/L ND (0.050) 

Manganese EPA 1638 Dissolved ug/L ND (0.50) 

Molybdenum EPA 1638 Dissolved ug/L ND (0.50) 

Nickel EPA 1638 Dissolved ug/L ND (0.50) 

Selenium EPA 1638 Dissolved ug/L ND (2.0) 

Silver EPA 1638 Dissolved ug/L ND (0.10) 

Thallium EPA 1638 Dissolved ug/L ND (0.050) 

Vanadium EPA 1638 Dissolved ug/L ND (1.0) 

Zinc EPA 1638 Dissolved ug/L ND (0.50) 

LDPE 20 L Composite Bottles – Bottle Blank (sample composite bottle for dissolved/filtration pump-off)

Aluminum EPA 1638 Dissolved ug/L ND (2.0) 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

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

A-55 

Table A-14. Bottle Blank and Equipment Blank Analytical Data, Miami Fort

Analyte Method Process Units Concentration 

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) 

Sample Tap Tubing Set – Equipment Blank (seven feet of #73 silicone tubing, Y-splitter, and two pieces of 5 

feet of #24 silicone tubing for sample collection for mercury and metals from sample taps) 

Aluminum EPA 1638 Total Recoverable ug/L ND (4.0) 

Antimony EPA 1638 Total Recoverable ug/L ND (0.020) 

Arsenic EPA 1638 Total Recoverable ug/L ND (0.15) 

Barium EPA 1638 Total Recoverable ug/L ND (0.20) 

Beryllium EPA 1638 Total Recoverable ug/L ND (0.060) 

Boron EPA 1638 Total Recoverable ug/L ND (3.0) 

Cadmium EPA 1638 Total Recoverable ug/L ND (0.020) 

Calcium EPA 1638 Total Recoverable ug/L ND (40) 

Chromium EPA 1638 Total Recoverable ug/L ND (0.10) 

Cobalt EPA 1638 Total Recoverable ug/L ND (0.10) 

Copper EPA 1638 Total Recoverable ug/L ND (0.10) 

Iron EPA 1638 Total Recoverable ug/L ND (10) 

Lead EPA 1638 Total Recoverable ug/L ND (0.040) 

Magnesium EPA 1638 Total Recoverable ug/L ND (2.5) 

Manganese EPA 1638 Total Recoverable ug/L ND (0.10) 

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

Molybdenum EPA 1638 Total Recoverable ug/L ND (0.060) 

Nickel EPA 1638 Total Recoverable ug/L ND (0.10) 

Selenium EPA 1638 Total Recoverable ug/L ND (0.60) 

Silver EPA 1638 Total Recoverable ug/L ND (0.020) 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

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

A-56 

Table A-14. Bottle Blank and Equipment Blank Analytical Data, Miami Fort

Analyte Method Process Units Concentration 

Sodium EPA 1638 Total Recoverable ug/L ND (20) 

Thallium EPA 1638 Total Recoverable ug/L ND (0.0050) 

Tin EPA 1638 Total Recoverable ug/L ND (0.10) 

Titanium EPA 1638 Total Recoverable ug/L ND (0.50) 

Vanadium EPA 1638 Total Recoverable ug/L ND (0.10) 

Zinc EPA 1638 Total Recoverable ug/L ND (0.20) 

Pump-Off Tubing Set – Equipment Blank (Three feet of Teflon® tubing, 10 feet of #73 silicone tubing, Ysplitter, and two pieces of 5 feet of #24 silicone tubing for total and dissolved sample collection for metals)

Aluminum EPA 1638 Total Recoverable ug/L ND (4.0) 

Antimony EPA 1638 Total Recoverable ug/L ND (0.020) 

Arsenic EPA 1638 Total Recoverable ug/L ND (0.15) 

Barium EPA 1638 Total Recoverable ug/L ND (0.20) 

Beryllium EPA 1638 Total Recoverable ug/L ND (0.060) 

Boron EPA 1638 Total Recoverable ug/L ND (3.0) 

Cadmium EPA 1638 Total Recoverable ug/L ND (0.020) 

Calcium EPA 1638 Total Recoverable ug/L ND (40) 

Chromium EPA 1638 Total Recoverable ug/L ND (0.10) 

Cobalt EPA 1638 Total Recoverable ug/L ND (0.10) 

Copper EPA 1638 Total Recoverable ug/L ND (0.10) 

Iron EPA 1638 Total Recoverable ug/L ND (10) 

Lead EPA 1638 Total Recoverable ug/L ND (0.040) 

Magnesium EPA 1638 Total Recoverable ug/L ND (2.5) 

Manganese EPA 1638 Total Recoverable ug/L ND (0.10) 

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

Molybdenum EPA 1638 Total Recoverable ug/L ND (0.060) 

Nickel EPA 1638 Total Recoverable ug/L ND (0.10) 

Selenium EPA 1638 Total Recoverable ug/L ND (0.60) 

Silver EPA 1638 Total Recoverable ug/L ND (0.020) 

Sodium EPA 1638 Total Recoverable ug/L ND (20) 

Thallium EPA 1638 Total Recoverable ug/L ND (0.0050) 

Tin EPA 1638 Total Recoverable ug/L ND (0.10) 

Titanium EPA 1638 Total Recoverable ug/L ND (0.50) 

Vanadium EPA 1638 Total Recoverable ug/L ND (0.10) 

Zinc EPA 1638 Total Recoverable ug/L ND (0.20) 

T-Splitter Tubing Set – Equipment Blank (Ten feet of #73 silicone tubing, T-splitter, six feet of #73 silicone 

tubing, and 15 feet of #73 silicone tubing for total and dissolved sample collection for metal composites)

Aluminum EPA 1638 Total Recoverable ug/L ND (4.0) 

Antimony EPA 1638 Total Recoverable ug/L ND (0.020) 

Arsenic EPA 1638 Total Recoverable ug/L ND (0.15) 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

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

A-57 

Table A-14. Bottle Blank and Equipment Blank Analytical Data, Miami Fort

Analyte Method Process Units Concentration 

Barium EPA 1638 Total Recoverable ug/L ND (0.20) 

Beryllium EPA 1638 Total Recoverable ug/L ND (0.060) 

Boron EPA 1638 Total Recoverable ug/L ND (3.0) 

Cadmium EPA 1638 Total Recoverable ug/L ND (0.020) 

Calcium EPA 1638 Total Recoverable ug/L ND (40) 

Chromium EPA 1638 Total Recoverable ug/L ND (0.10) 

Cobalt EPA 1638 Total Recoverable ug/L ND (0.10) 

Copper EPA 1638 Total Recoverable ug/L ND (0.10) 

Iron EPA 1638 Total Recoverable ug/L ND (10) 

Lead EPA 1638 Total Recoverable ug/L ND (0.040) 

Magnesium EPA 1638 Total Recoverable ug/L ND (2.5) 

Manganese EPA 1638 Total Recoverable ug/L ND (0.10) 

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

Molybdenum EPA 1638 Total Recoverable ug/L ND (0.060) 

Nickel EPA 1638 Total Recoverable ug/L ND (0.10) 

Selenium EPA 1638 Total Recoverable ug/L ND (0.60) 

Silver EPA 1638 Total Recoverable ug/L ND (0.020) 

Sodium EPA 1638 Total Recoverable ug/L ND (20) 

Thallium EPA 1638 Total Recoverable ug/L ND (0.0050) 

Tin EPA 1638 Total Recoverable ug/L ND (0.10) 

Titanium EPA 1638 Total Recoverable ug/L ND (0.50) 

Vanadium EPA 1638 Total Recoverable ug/L ND (0.10) 

Zinc EPA 1638 Total Recoverable ug/L ND (0.20) 
A-58 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-15. Influent to FGD Wastewater Treatment System Field Blank, Day 1 Analytical Results

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL C

Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 NBeryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 NCopper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 Molybdenum 200.7 ug/L 2 1.6 40 NNickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 ND Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 NTitanium 200.7 ug/L 2 1.6 20 NVanadium 200.8 ug/L 2 1.7 10 NZinc 200.8 ug/L 2 4.1 10 NDissolved MetalsAluminum 200.7 ug/L 2 9.4 200 NAntimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 
A-59 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-15. Influent to FGD Wastewater Treatment System Field Blank, Day 1 Analytical Results

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL C

Barium 200.7 ug/L 2 2.5 20 NBeryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 0.39 2 Cobalt 200.7 ug/L 2 1.1 20 NCopper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 NLead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Molybdenum 200.7 ug/L 2 1.6 40 NNickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 NTitanium 200.7 ug/L 2 1.6 20 NVanadium 200.8 ug/L 2 1.7 10 NZinc 200.8 ug/L 2 4.1 10 N
A-60 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. Est – Estimated value. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-16. Effluent from FGD Wastewater Treatment System Field Blank, Day 1 Analytical Resul

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL 

Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 
A-61 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. Est – Estimated value. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-16. Effluent from FGD Wastewater Treatment System Field Blank, Day 1 Analytical Resul

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL 

Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 0.39 2 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
A-62 

ND – Not detected (number in parentheses is the quantitation limit). U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-17. Effluent from FGD Wastewater Treatment System Field Blank, Day 2 Analytical Resul

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL 

Total MetalsMercury 1631E ng/L 1 0.24 0.5 
A-63 

ND – Not detected (number in parentheses is the quantitation limit). U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-18. Effluent from FGD Wastewater Treatment System, Day 3 Analytical Results, Mia

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL C

Total MetalsMercury 1631E ng/L 1 0.24 0.5 N
A-64 

ND – Not detected (number in parentheses is the quantitation limit). U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-19. Effluent from FGD Wastewater Treatment System, Day 4 Analytical Results, Mia

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL C

Total MetalsMercury 1631E ng/L 1 0.24 0.5 N
Appendix B 

DATA REVIEW NARRATIVES 
Appendix C 

PICTURES FROM THE SAMPLING EPISODE 
C-1 

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

 
C-2 

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

System 

 
C-3 

Figure C-3. Sample Collection at the Influent to the FGD Wastewater Treatment System 

 
C-4 

Figure C-4. Sample Collection Set Up at the Pump-Off Station 

 
C-5 

Figure C-5. Composite Sample Collection Set Up at the Effluent from the FGD Wastewater 

Treatment System