# 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

# i CONTENTS

Page

1. I NTRODUCTION 

# ................................................................................................................. 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. F ACILITY 

# O VERVIEW 

# ........................................................................................................ 2-1

2.1 FGD Scrubber Systems ........................................................................................ 2-2

2.2 FGD Wastewater Trea tment System ................................................................... 2-2

3. S AMPLE 

# C OLLECTION 

# ....................................................................................................... 3-1

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

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

3.1.2 Effluent from FGD Wastewat er 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. L ABORATORY 

# A NALYTICAL 

# R ESULTS AND 

# D ISCUSSION 

# ................................................... 4-1

4.1 Measured and Calculated Results for In fluent to FGD Wastewater Treatment

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

4.2 FGD Wastewater Trea tment System ................................................................... 4-2

5. D ATA 

# Q UALITY 

# ............................................................................................................... 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. R EFERENCES 

# ..................................................................................................................... 6-1

Appendix A: A NALYTICAL 

# R ESULTS



# Appendix B: D ATA 

# R EVIEW 

# N ARRATIVES



# Appendix C: P ICTURES 

# F ROM THE 

# S AMPLING 

# E PISODE

# ii LIST OF TABLES

Page

Table 3-1. Sample Collection In formation, Miami Fort ............................................................ 3-10

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

Table 3-3. Field Measurements, Miami Fort ............................................................................. 3-13

Table 3-4. Crosswalk of Sample Number to Sampling Point and Day, Miami Fort ................. 3-15

Table 3-5. Analytical Me thods, Miami Fort .............................................................................. 3-16

Table 3-6. Summary of Sample Container a nd Planned Preservation, Miami Fort .................. 3-17

Table 3-7. Sample Preservation Summary, Miami Fort ............................................................ 3-18

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

Miami Fort .................................................................................................................... . 3-20

Table 3-9. FGD Scrubber System Operati ng Characteristics, Miami Fort ................................ 3-21

Table 3-10. Coal Usage during Samp le Collection, Miami Fort ............................................... 3-22

Table 3-11. Scrubber Slurry Information du ring Sample Collection, Miami Fort .................... 3-23

Table 3-12. FGD Wastewater Tr eatment System Operation Information, Miami Fort ............. 3-24

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 Polluta nts 4-Day Average Data Summary for FGD Wastewater

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

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

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

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

Table 5-2. Field Duplicate Re sults – Effluent fr om FGD Wastewater Treatment System,

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

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

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

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

Wastewater Treatment Syst em, Day 2 Analytical Results, Miami Fort ......................... A-3

# LIST OF TABLES (Continued)

Page

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

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

Table A-4. Biphasic Sample Results for Cla ssicals and Total Meta ls, Influent to FGD

Wastewater Treatment Syst em, 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 FG D Wastewater Treatment System , Day 1 Analytical Results,

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

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

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

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

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

Table A-12. Effluent from FG D 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 Bla nk 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 FG D Wastewater Treatment System , Day 3 Analytical Results,

Miami Fort .................................................................................................................... A-63

# LIST OF TABLES (Continued)

Page

iv Table A-19. Effluent from FG D Wastewater Treatment System , Day 4 Analytical Results,

Miami Fort .................................................................................................................... A-64

# v LIST OF FIGURES

Page

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

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

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

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

Figure C-3. Sample Collection at the Influent to the FGD Wast ewater 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

# 1-1 1. I NTRODUCTION



# 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 generate d by coal-fired steam electric power plants

and evaluate treatment technologi es and best management practic es 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 Fo rt 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 pr esent in the wastewater discharges from steam

electric power plants that substantially cont ribute to the toxic load ings for the industry.

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

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

findings, EPA has focused the sampling progr am on characterizing the untreated FGD

wastewaters and effluent quali ty from technologies designed to treat the wastewater.

1.2 Power Plant Site Selection

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

configurations and characte ristics of the plants.

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

 The plant is a coal-fired pow er 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 (discontinue d prior to the sampling episode),

— Polymer addition,

— Clarification;

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

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

 

# The plant produces a commerc ial-grade gypsum by-product.

# 1-2 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 Ma rch 1, 2010 as part of the detailed study. The

information collected during the pre-sa mpling 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 sa mpling 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 sample s with the Utility

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

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

collected samples on be half of the plant.

# 2-1 2. F ACILITY 

# O VERVIEW



# Miami Fort operates three baseload steam el ectric 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, re spectively, each has a ge nerating capacity of

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

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

Ohio River.

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

FGD scrubber systems to control the sulfur dioxide (SO 2 

# ) 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 scrubbe rs. 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 (NO X 

# ) emissions

from the plant, year round.

The electrostatic precipitators (ESPs) at Miam i 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 fl y ash from all three units. The fly ash and other

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

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

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

landfill located approximately th ree miles away, which is owne d 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 adj acent cells operated in series. Fly ash from

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

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

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

channels for the sluice water to move through th e mass of ash solids coll ected 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 perimete r of the ash channels to allow the solids to

dewater, while the water drains back into th e pond. After the solids ha ve been dewatered, the

plant hauls them to the landfill for disposal. In ad dition 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 ha ve the following configuration:

 Boiler;

 SCR system;

 Air heater;

 Lime injection;

 ESP; and

 FGD scrubber system.

2.1 FGD Scrubber Systems

[CBI information has been removed from this section.]

2.2 FGD Wastewater Treatment System

[CBI information has been removed from this section.]

# 2-3[CBI information has been removed from this section.]Figure 2-1. Chemical Precipitation FGD Wastewater Treatment System, Miami Fort

# 3-1 3. S AMPLE 

# C OLLECTION



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

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

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

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

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

activities.

3.1 Sampling Points, Sample Collectio n Methods, and Field Measurements

This section describes the sampling point s, 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, sampli ng point descriptions, type of sample

collection, and sample collection dates and times. Table 3-2 list s 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 th e field measurement data collected from each

sampling point. Table 3-4 presents a crosswalk be tween 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 Wast ewater Treatment System;

 

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

 

# SP-4 Influent to FGD Wastewater Treatme nt System (SP-1) Field Blank; and

 

# SP-5 Effluent from FGD Wa stewater Treatment System (SP-2) Field Blank.

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

by inserting a “Y” splitte r into the sample tubing configurat ion 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., samp les 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 Fo rt’s representative collected duplicate samples,

with one filling the bottle im mediately 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 th at secures itself ope n with clips. The “cleanbox” is double-bagged

with a clear inner bag, enclosed in a translu cent outer bag. The “cleanbo x” is handled using

“clean hands / dirty hands” techniques, where by the inner bag is ha ndled 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 open ing of the box, but is still able to see the sample bottles and

# 3-2 tubing. The “cleanbox” minimizes potential at mospheric contamination during sample

collection. Figure C-1, in Appendix C, is a pictur e 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 seal ed 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 cl osed the sample bottle lid and sealed the inner

bag as quickly as possible with in 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 syst em (SP-1) was collected from a sample tap

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

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

directly to the equali zation tank and, therefore, the sampli ng point upstream of the tank provides

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

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

flow into the equalization tank is not conti nuous. 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 sample s 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 th e influent to the FGD wast ewater treatment system.

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

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

wastewater samples at the influent to the F GD 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 sa mples were collected. The end of the silicone

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

the “Y” splitter. Figure C-2, in Appendix C, is a picture of the tubing att ached 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 samp le tap, opened the valve, and allowed sample to

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

did not close the valve until all samples were coll ected (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 sa mpling 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 containe rs for biochemical oxygen demand (BOD 5 

# ), Group I,

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

Table 3-6 for a list of Group I and Group II analytes. BOD 5 

# , Group I, Group II, and total cyanide

samples were immediately placed on ice after sa mple collection.

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

potassium-iodide starch test stri ps were used to measure for su lfides and oxidants, respectively.

No sulfides or oxidants were detected during th e 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 we re 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 th e silicone tubing, which was a s hort 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” spli tter and two lengths of silicone tubing. This set-up allowed EPA

to collect “true” split samples w ith 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 sa mple 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 c ontainer filled with wastewater from the influent to the FGD wastewater

treatment system. By this time, the solids in th e wastewater had been se ttling for approximately

100 minutes. Approxima tely 0.5- 2 liters 1 

# of sample were pumped through the tubing/filter to

purge the line before collecting samples.

Samplers collected the following dissolved sa mples 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 immedi ately placed on ice after sample collection.

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

represent the FGD scrubber purge from the specific unit that was pur ging 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 wastew ater 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 fo r the sampling location for SP-2). Because the

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

collection.

ERG collected the effluent from FGD wastew ater treatment system composite samples

using two automatic compositors which were prog rammed to collect individual sample volumes

into two 20-liter containers. The compositors we re 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 compos itor to collect sample volume for all classical

analytes (i.e., BOD 5 

# , Group I, and Group II, excluding cy anide). In addition to collecting

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

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

grab sample for cyanide during each compositing period.

On Day 1 only, prior to star ting 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 ch romium (samples were collected in a 20-liter

container and samples were pumped into indi vidual 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 tw o silicone tubing sets to two of the taps

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

to the sample tap, and one end was threaded th rough the automatic comp ositor and connected to

the large composite container. The samplers a ttached 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 en sured that the flow through the tubing during

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

automatic compositors were calibrate d such that they collected 870 mL 2 

# every hour, so that the

projected complete volume would be 20 liters. After calibration, the tubi ng 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 co mpositor 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 plas tic bag was placed on t op 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 gr ab sample every day, ERG collected field blanks

for total mercury samples. See Section 5.2.3 for a de scription 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 ta p for two minutes, the samples were collected directly from the

tap into the sample bottles. Becau se 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; therefor e, duplicate samples were collected. ERG collected another set of total

and dissolved mercury samples every six hours th ereafter over the 24-h our period. The plastic

shroud was replaced for each set of mercury grab samples. After collecti ng 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 thir d set of mercury grabs, ERG collected a total cyanide grab

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

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

split samples with Miami Fort’s representatives; th erefore, 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 su lfides and oxidants, respectively. No sulfides or

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

2 

# The Sampling Plan called for calibrating the compositors to collect 830 mL every hou r; 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 we re 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 me tals 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. a nd placed the samples on ice.

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

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

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

containers were moved to the pump-off area wher e 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 volum e on each day of sample collection.

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

transferred the wastewater coll ected in the 20-liter containe rs into the individual sample

containers at the pump-off area. For this samp ling 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 with in 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 cont ainers. The pump-off station cons isted of a length of Teflon®

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

pump. The sampling team attached a capsule fi lter to the silicone t ubing, which was a short

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

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

silicone tubing. This set-up allowed EPA to co llect “true” split sample s 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 samp les (SP-5) for total and dissolved metals

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

Section 5.2.3 for a description of the field blank sample collection proced ures 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 we re purged with 1-2 liters of

sample, samplers collected the following sample s 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 immedi ately 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 coll ected 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 prev iously filled 20-liter contai ner. After the tubing was purged

with 1-2 liters of sample, samplers fille d containers for biochemical oxygen demand (BOD 5 

# ),

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. BOD 5 

# , Group I, and Group II samples were

immediately placed on ice af ter sample collection.

For all analytes, ERG collected QC sample s at the effluent fr om FGD wastewater

treatment system (SP-2) on Day 3 of the samp ling 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 (BOD 5 

# ),

— 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, in cluding contributions from coal , scrubber sorb ents, 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 sampli ng 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 BOD 5 

# , Group I, Group II, dissolved hexavalent chromium,

and total cyanide samples on ice to cool the sa mples 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-pre served prior to extraction at the laboratory. The

hexavalent chromium samples were preserve d 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 te sted for sulfides and oxidants immediately after

sample collection. Because sulfides and oxidants we re 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 sulfid es 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 pr ovided the sampling

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

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

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

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

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

episode, and Table 3-12 presents th e FGD wastewater treatment syst em 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 amm onium sulfate buffer solution was not

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

sulfate buffer solution, followed by as mu ch ammonium hydroxide as necessary

to reach the desired pH.

 

# Influent to FGD wastewater treatm ent system samples (SP-1, Day 2): After

set up at the sampling location at the in fluent to FGD wast ewater 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 measu rement (SP-2, Grab 4, Day 4): At the effluent

from FGD wastewater treatment syst em (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 measu rements (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 orde r to grab the field test sample.

 

# Collection of total mercur y (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 bottl e 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 meta l 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, respectivel y, 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 effl uent 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 opera ting (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 treatmen t 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 allo wing the solids to sett le 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 0924 a 

# and 1149 b



# Influent to FGD Wa stewater Treatment

System – Day 2 Grab 7/13/10 1034 a 

# and 1247 b



# Influent to FGD Wa stewater Treatment

System – Day 3 Grab 7/14/10 0912 a 

# and 1143 b



# Influent to FGD Wa stewater Treatment

System – Day 4 Grab 7/15/10 0927 a 

# and 1137 b



# SP-2 Effluent from FGD Wastewater

Treatment System – Day 1 Composite 7/12/10

7/13/10 0731 c



# 0841 d



# Grab 7/12/10

7/13/10 0752 e 

# , 1353 f 

# , and 1956 g



# 0147 h



# Effluent from FGD Wastewater

Treatment System – Day 2 Composite 7/13/10

7/14/10 0730 c



# 0806 d



# Grab 7/13/10

7/14/10 0745 e 

# , 1346 f 

# , and 1947 g



# 0147 h



# Effluent from FGD Wastewater

Treatment System – Day 3 Composite 7/14/10

7/15/10 0730 c



# 0813 d



# Grab 7/14/10

7/15/10 0744 e 

# , 1346 f 

# , and 1948 g



# 0150 h



# Effluent from FGD Wastewater

Treatment System – Day 4 Composite 7/15/10

7/16/10 0730 c



# 0658 d



# Grab 7/15/10

7/16/10 0747 e 

# , 1357 f 

# , and 1945 g



# 0145 h



# SP-3 Duplicate of Effluent from FGD

Wastewater Treatment System – Day 2 Composite 7/13/10

7/14/10 0731 c



# 0841 d



# Grab 7/13/10

7/14/10 0746 e 

# , 1348 f 

# , and 1947 g



# 0149 h



# SP-4 Influent to FGD Wastewater Treatment

System Field Blank Grab 7/12/10 0910 i 

# and 1138 j



# SP-5 Effluent from FGD Wastewater

Treatment System Field Blank – Day 1 Composite 7/12/10

7/13/10 0640 k



# 0829 l



# Grab 7/12/10 0748 m



# Effluent from FGD Wastewater

Treatment System Field Blank – Day 2 Grab 7/13/10 0739 m



# Effluent from FGD Wastewater

Treatment System Field Blank – Day 3 Grab 7/14/10 0739 m



# Effluent from FGD Wastewater

Treatment System Field Blank – Day 4 Grab 7/15/10 0743 m

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 (BOD 5 

# , 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 (BOD 5 

# , 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.

# 3-12Table 3-2. Sample Collection at Miami FortSamplingPointNumberSampling 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 Group I

a Group II

b Total CyanideSP-1 Influent to the FGD WastewaterTreatment System4 4 4 4 4 4 4 4 4 4 4SP-2 Effluent from the FGD WastewaterTreatment System4+1QC 4+1QC 4+1QC 4+1QC 4+1QC4+1QC 4+1QC 4+1QC 4+1QC 4+1QC4+1QCSP-3 Duplicate of Effluent from the FGDWastewater Treatment System1 1 1 1 1 1 1 1 1 11SP-4 Field Blank for Influent to the FGDWastewater Treatment System1 1 1 1 1 1SP-5 Field Blank for Effluent from theFGD Wastewater Treatment System1 1 1 1 4 1Total Number of Samples 11+1QC 11+1QC 11+1QC 11+1QC 14+1QC 9+1QC 11+1QC 9+1QC 9+1QC 9+1QC 9+1QCaGroup I includes total suspended solids (TSS), total dissolved solids (TDS), sulfate, and chloride.bGroup II includes ammonia as nitrogen, nitrate/nitrite as nitrogen, total Kjeldahlnitrogen (TKN), chemical oxygen demand (COD), and total phosphorus.

# 3-13Table 3-3. Field Measurements, Miami FortSamplingPointNumberSampling PointDescriptionDateTimeTemperature (°C)pH (S.U.)Waste StreamFlow Rate(GPM)bNotesThermometerProbeMeteraStripsSP-1 Influent to FGDWastewater TreatmentSystem – Day 17/12/2010 093853NAc5.55 6 148dSamplers noted that the samples had ayellow color and appeared to be high insolids. No detected sulfides or oxidants intotal cyanide grab.Influent to FGDWastewater TreatmentSystem – Day 27/13/2010 104752.550.25.56 7 148dSamplers noted that the samples had a lightyellow color. No detected sulfides oroxidants in total cyanide grab.Influent to FGDWastewater TreatmentSystem – Day 37/14/2010 09334847.55.15 6 148dSamplers noted that the samples had a lightyellow color. No detected sulfides oroxidants in total cyanide grab.Influent to FGDWastewater TreatmentSystem – Day 47/15/2010 094154515.51 7 148dNo detected sulfides or oxidants in totalcyanide grab.SP-2 Effluent from FGDWastewater TreatmentSystem – Day 17/12/10 07554341.78.7 9.5246.7Samples were clear with a light yellowcolor and did not have any visible solids.No detected sulfides or oxidants in totalcyanide grab.7/12/10 135543418.63 90.07/12/10 19564239.98.44 9 243.97/13/10 01514442.28.56 9 0.0Effluent from FGDWastewater TreatmentSystem – Day 27/13/10 0750448.56 9 0.0 Samplers noted that the samples had a lightyellow color. No detected sulfides oroxidants in total cyanide grab.7/13/10 135044428.62 9 248.27/13/10 20054542.58.46 9 0.07/14/10 01544239.28.62 9 244.5Effluent from FGDWastewater TreatmentSystem – Day 37/14/10 07464340.18.55 9 0.0 Samples were clear with a yellow tint anddid not have any observed particulates. Nodetected sulfides or oxidants in totalcyanide grab.7/14/10 134744.542.58.26 9 0.07/14/10 19534442.28.66 9 0.07/15/10 01544340.98.38 9 0.0Effluent from FGDWastewater TreatmentSystem – Day 47/15/10 074942408.61 9 0.0 Samples were clear with a yellow tint anddid not have any observed particulates. Nodetected sulfides or oxidants in totalcyanide grab.7/15/10 135844428.49 9 251.37/15/10 19504542.38.53 9 0.07/16/10 01504542.48.55 9 250.0

# 3-14aThe pH meter was calibrated prior to the sampling episode and once every day during the sampling episode using prepackaged buffer solutions at pH 4.0, 7.0,and 10.0.bThe SP-2 flow rates provided in the table represent the instantaneous flow at the sampling point during the mercury grab sample collection. For the times when0.0 is shown as the flow rate, the effluent wastewater transferwere not operating and therefore, the sample was collected fromthe tap based on the head pressurefrom the wastewater volumein the effluent tank.cNot analyzed.dScrubber purge flow is a calculated value based on pump discharge pressure provided by the plant. The plant does not have a flow meter that measures the flowrate of the FGD scrubber purge entering the Equalization tank.

# 3-15 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 Wastewat er Treatment System Field Blank - Day 1

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

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

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

71754 SP-5, Day 4 Effluent to FGD Wastewat er Treatment System Field Blank - Day 4

# 3-16 Table 3-5. Analytical Methods, Miami Fort

Parameter Method Number

Classicals

Biochemical oxygen demand (BOD 5 

# ) 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

# 3-17 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

BOD 5 

# 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 H 2 

# SO 4 

# 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,

NaAsO 2 

# 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

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

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, nitr ate/nitrite as ni trogen, TKN, and total phosphorus.

# 3-18 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 H 2 

# SO 4 

# 7 <2 250

71741 Group II Volume 2 7/12/10 H 2 

# SO 4 

# 7 <2 200

71741 Hexavalent Chromium 7/12/10 (NH 4 

# ) 2 

# SO 4



# Buffer 6.5 6.8 100

NH 4 

# OH 6.8 9.5 25

71750 Hexavalent Chromium 7/12/10 (NH 4 

# ) 2 

# SO 4



# Buffer 6.5 8.5 100

NH 4 

# OH 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 H 2 

# SO 4 

# 7 2 150

71742 Group II Volume 2 7/13/10 H 2 

# SO 4 

# 7 2 150

71745 Group II Volume 1 7/13/10 H 2 

# SO 4 

# 9.5 <2 75

71745 Group II Volume 2 7/13/10 H 2 

# SO 4 

# 9.5 <2 75

71742 Hexavalent Chromium 7/13/10 (NH 4 

# ) 2 

# SO 4



# Buffer 6.5 7.1 100

NH 4 

# OH 7.1 9.7 67

71745 Hexavalent Chromium 7/13/10 (NH 4 

# ) 2 

# SO 4



# Buffer 8.7 8.7 100

NH 4 

# OH 8.7 9.3 10

71751 Hexavalent Chromium 7/13/10 (NH 4 

# ) 2 

# SO 4



# Buffer 6.5 8.5 50

NH 4 

# OH 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 H 2 

# SO 4 

# 6 <2 200

71743 Group II Volume 2 7/14/10 H 2 

# SO 4 

# 6 <2 200

71746 Group II Volume 1 7/14/10 H 2 

# SO 4 

# 9 2 100

71746 Group II Volume 2 7/14/10 H 2 

# SO 4 

# 9 2 100

71749 Group II Volume 2 7/14/10 H 2 

# SO 4 

# 9 2 100

71749 Group II Volume 1 7/14/10 H 2 

# SO 4 

# 9 2 100

71743 Hexavalent Chromium 7/14/10 (NH 4 

# ) 2 

# SO 4



# Buffer 6.5 7.1 100

NH 4 

# OH 7.1 9.7 60

71746 Hexavalent Chromium 7/14/10 (NH 4 

# ) 2 

# SO 4



# Buffer 8.7 8.7 100

NH 4 

# OH 8.7 9.5 15

# 3-19 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 (NH 4 

# ) 2 

# SO 4



# Buffer 8.7 8.7 100

NH 4 

# OH 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 H 2 

# SO 4 

# 6 2 150

71744 Group II Volume 2 7/15/10 H 2 

# SO 4 

# 6 2 150

71747 Group II Volume 1 7/15/10 H 2 

# SO 4 

# 9 2 100

71747 Group II Volume 2 7/15/10 H 2 

# SO 4 

# 9 2 100

71747 Group II Volume 1 - QC 7/15/10 H 2 

# SO 4 

# 9 2 100

71747 Group II Volume 2 - QC 7/15/10 H 2 

# SO 4 

# 9 2 100

71744 Hexavalent Chromium 7/15/10 (NH 4 

# ) 2 

# SO 4



# Buffer 6.5 7.1 100

NH 4 

# OH 7.1 9.5 120

71747 Hexavalent Chromium - QC 7/15/10 (NH 4 

# ) 2 

# SO 4



# Buffer 8.7 8.7 100

NH 4 

# OH 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 H 2 

# SO 4 

# 9 2 125

71748 Group II Volume 1 7/16/10 H 2 

# SO 4 

# 6.0 2 55

71748 Hexavalent Chromium 7/16/10 (NH 4 

# ) 2 

# SO 4



# Buffer 8.7 8.7 100

NH 4 

# OH 8.7 9.5 30

# 3-20 Table 3-8. Generating Unit Operating Charact eristics 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 elect rostatic precipitator.

# 3-21Table 3-9. FGD Scrubber System Operating Characteristics, Miami FortUnit IDWet FGDSystem (Yes/No)Type ofScrubberForcedOxidation(Yes/No)SorbentAdditives (DBA,formic acid,etc.)FGD Make-upWater SourceSO2RemovalPercentageType of SolidsSeparation7 Yes Spray Yes LimestoneNone Ohio River 97.4 %SecondaryHydrocyclones8 Yes Spray Yes LimestoneNone Ohio River 96.9 %SecondaryHydrocyclones

# 3-22 Table 3-10. Coal Usage during Sa mple 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)

# 3-23 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 CBI CBI CBI CBI CBI

8 8 CBI CBI CBI CBI CBI

2 7 7 CBI CBI CBI CBI CBI

8 8 CBI CBI CBI CBI CBI

3 7 7 CBI CBI CBI CBI CBI

8 8 CBI CBI CBI CBI CBI

4 7 7 CBI CBI CBI CBI CBI

8 8 CBI CBI CBI CBI CBI

# 3-24Table 3-12. FGD Wastewater Treatment System Operation Information, Miami FortDay of SamplingScrubber PurgeChemical UsageFlow Rate (gpm)bDurationLimeaFerric ChlorideOrganosulfide:Nalmet 1689cPolymer: Nalco7766+cAcid1 CBI CBI CBI CBI CBI CBI CBI2 CBI CBI CBI CBI CBI CBI CBI3 CBI CBI CBI CBI CBI CBI CBI4 CBI CBI CBI CBI CBI CBI CBIaLime usage is approximately [CBI information has been removed] lbs/day.bScrubber purge flow is a calculated value based on pump discharge pressure.cOrganosulfide and polymer usage are calculated values based on dosing set points.

# 4-1 4. L ABORATORY 

# A NALYTICAL 

# R ESULTS AND 

# D ISCUSSION



# 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 th e biphasic analysis of

SP-1. Section 4.2 presents the laborat ory analytical data for the infl uent 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 a nd all results that were measur ed above the method detection

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

4.1 Measured and Calculated Results for In fluent to FGD Wastewater Treatment

System Samples

The samples of the influent to the FGD wast ewater treatment system were expected to

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

unreacted limestone, and fly ash. Because of th is, 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 solid s loads. Therefore, ERG directed its contract

laboratories to separate the aque ous and solid phases of the samp le 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, Test America Laboratories - Denver (TestAmerica),

and the mercury laboratory, Frontier Global Scien ces (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 consiste d of performing a pressure filtration to separate

the solids from the sample and analyzing the so lid and aqueous phases separately. TestAmerica

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

calculate the total sample concentration from th e solid and aqueous phase results, the laboratory

also needed to measure the original sample vol ume, solid phase weight, and filtrate volume. EPA

developed the following equation to calculate the individual metal total concentrations for the

sample.

# 4-2 Sample Solid Solid Filtrate Filtrate



# V ) Wt (C ) V (C ion Concentrat Sample Total   

 

# (4-1)

where:

C Filtrate 

# = concentration of the analyte in the aqueous phase of the sample;

V Filtrate 

# = volume of the filtrate;

C Solid 

# = concentration of the analyte in the solid phase of the sample;

Wt Solid 

# = weight of the solids in the sample; and

V Sample 

# = volume of the original sample.

TestAmerica used the same approach for the se ven 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 a ny language stating how wastewat er samples with high solid

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

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

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

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

concentration is on a wet-weight basis. To cal culate 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 volum e. EPA used Equation 4-1 to calculate the

individual total mercury con centrations for the sample.

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

ammonia as nitrogen, nitrate/nitrit e, 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 wast ewater 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 e ffluent from the FGD wast ewater treatment system

(SP-2).

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

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

sample above the method detection limit, the resu lt 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 wastew ater 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 averag e of the original and the duplicate samp le results. Table 5-2 presents the

analytical results for the original and duplicat e 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 quantitati on limit, then all results were averaged

together;

 

# If at least one result was above the quan titation 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 repo rted 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 de tection limit, then the sample-specific

quantitation limits for all results were aver aged 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 fo r all classical analytes for the influent to

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

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

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

(SP-1) and the effluent from th e 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), th e effluent from the FGD wastewater treatment

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

# 4-4Note: The total metals results and the results for certain classical analytes (i.e., ammonia as nitrogen, nitrate/nitrite, chloride, sulfate, nitrate/nitrite, total cyanide, TKN, totalphosphorus) represent the total result that was calculated based onthe results of the solid and aqueous phase of the samples.See Section 4.1 for more details.< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 at least one result is a Jvalue.* - 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 FortAnalyteUnitsMethodInfluent to FGD Wastewater Treatment System (SP-1)Day 1Day 2Day 3Day 44-DayAverageClassicalsAmmonia mg/L 350.1 5.21 6.12 7.90 6.06 6.32Nitrate Nitrite as N mg/L 353.2 71.7 86.6 74.9 82.8 79.0Nitrogen, Total Kjeldahl mg/L 351.2 40.5 52.6 47.6 40.8 45.4Biochemical Oxygen Demand mg/L 5210B NQ (2.50) NQ (2.50) 3.30 ND (2.00) * < 1.70Chemical Oxygen Demand mg/L 410.4 620 670 910 720 730Chloride mg/L 300.0 9,000 9,800 9,600 9,600 9,500Sulfate mg/L 300.0 18,000 21,000 32,000 24,000 23,800Cyanide, Total mg/L 4500 CN E 0.255 0.644 2.05 0.198 0.787Total Dissolved Solids mg/L 2540C 56,000 68,000 59,000 50,000 58,300Total Suspended Solids mg/L 2540D 16,000 30,000 20,000 19,000 21,300Phosphorus, Total mg/L 365.1 0.476 7.68 NQ (0.191) 6.52 < 3.69Total MetalsAluminum ug/L 200.7, 6010B 561,000 626,000 687,000 497,000 593,000Antimony ug/L 200.8, 6020 NQ (10.3) NQ (11.0) NQ (13.4) NQ (9.47) NQ (11.0)Arsenic ug/L 200.8, 6020 937 896 1,310 695 960Barium ug/L 200.7, 6010B 7,640 7,510 10,400 6,410 7,990Beryllium ug/L 200.7, 6010B 27.6 28.3 41.8 22.4 30.0Boron ug/L 200.7, 6010B 624,000 803,000 844,000 762,000 758,000Cadmium ug/L 200.8, 6020 342 426 522 396 422Calcium ug/L 200.7, 6010B 1,340,000 1,350,000 2,060,000 1,140,000 1,470,000Chromium ug/L 200.8, 6020 4,000 4,460 4,430 3,640 4,130Cobalt ug/L 200.7, 6010B 425 503 632 459 505Copper ug/L 200.8, 6020 1,350 1,520 1,670 1,210 1,440Iron ug/L 200.7, 6010B 911,000 965,000 1,030,000 766,000 918,000Lead ug/L 200.8, 6020 756 842 887 651 784Magnesium ug/L 200.7, 6010B 7,870,000 9,210,000 11,800,000 9,010,000 9,470,000

# 4-5Note: The total metals results and the results for certain classical analytes (i.e., ammonia as nitrogen, nitrate/nitrite, chloride, sulfate, nitrate/nitrite, total cyanide, TKN, totalphosphorus) represent the total result that was calculated based onthe results of the solid and aqueous phase of the samples.See Section 4.1 for more details.< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 at least one result is a Jvalue.* - 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 FortAnalyteUnitsMethodInfluent to FGD Wastewater Treatment System (SP-1)Day 1Day 2Day 3Day 44-DayAverageManganese ug/L 200.7, 6010B 93,100 105,000 157,000 96,000 113,000Mercury ng/L 1631E, FGS-069 166,000 148,000 231,000 44,000 147,000Molybdenum ug/L 200.7, 6010B 506 540 641 406 523Nickel ug/L 200.8, 6020 2,580 2,980 3,610 2,560 2,930Selenium ug/L 200.8, 6020 3,400 3,650 3,330 2,920 3,330Silver ug/L 200.8, 6020 NQ (6.06) NQ (6.50) NQ (7.47) NQ (5.64) NQ (6.42)Sodium ug/L 200.7, 6010B 355,000 427,000 502,000 404,000 422,000Thallium ug/L 200.8, 6020 52.8 56.4 93.5 46.2 62.2Tin ug/L 200.7, 6010B NQ (403) NQ (430) NQ (460) NQ (411) NQ (426)Titanium ug/L 200.7, 6010B 2,020 2,050 4,140 1,820 2,510Vanadium ug/L 200.8, 6020 4,010 4,220 4,440 3,270 3,990Zinc ug/L 200.8, 6020 13,900 16,300 20,200 14,500 16,200Dissolved MetalsAluminum ug/L 200.7 4,200 B 2,400 B 29,000 B 2,800 B 9,600Antimony ug/L 200.8 3.40 3.30 3.70 2.80 3.30Arsenic ug/L 200.8 4.40 4.90 6.60 5.50 5.35Barium ug/L 200.7 140 140 180 150 153Beryllium ug/L 200.7 4.70 4.10 12.0 4.60 6.35Boron ug/L 200.7 650,000 B 690,000 B 820,000 730,000 723,000Cadmium ug/L 200.8 340 390 510 420 415Calcium ug/L 200.7 690,000 670,000 620,000 640,000 655,000Chromium ug/L 200.8 ND (8.00) ND (8.00) ND (8.00) ND (8.00) ^ ND (8.00)Chromium (VI) ug/L 218.6 ND (10.0) ND (10.0) ND (10.0) ND (10.0) ND (10.0)Cobalt ug/L 200.7 340 360 490 380 393Copper ug/L 200.8 54.0 50.0 110 55.0 67.3Iron ug/L 200.7 NQ (200) ND (200) NQ (200) ND (200) NQ (200)Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.00) ND (2.00)

# 4-6Note: The total metals results and the results for certain classical analytes (i.e., ammonia as nitrogen, nitrate/nitrite, chloride, sulfate, nitrate/nitrite, total cyanide, TKN, totalphosphorus) represent the total result that was calculated based onthe results of the solid and aqueous phase of the samples.See Section 4.1 for more details.< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 at least one result is a Jvalue.* - 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 FortAnalyteUnitsMethodInfluent to FGD Wastewater Treatment System (SP-1)Day 1Day 2Day 3Day 44-DayAverageMagnesium ug/L 200.7 7,900,000 8,400,000 11,000,000 8,900,000 9,050,000Manganese ug/L 200.7 100,000 100,000 170,000 110,000 120,000Mercury ng/L 1631E 1,110 1,830 1,600 1,990 1,630Molybdenum ug/L 200.7 120 110 130 90.0 113Nickel ug/L 200.8 1,700 1,700 2,500 2,000 1,980Selenium ug/L 200.8 290 330 330 300 313Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.00) ND (2.00)Sodium ug/L 200.7 360,000 380,000 480,000 400,000 405,000Thallium ug/L 200.8 25.0 26.0 49.0 26.0 31.5Tin ug/L 200.7 NQ (200) ND (200) ND (200) ND (200) NQ (200)Titanium ug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.0)Vanadium ug/L 200.8 12.0 13.0 20.0 16.0 ^ 15.3Zinc ug/L 200.8 6,300 6,200 11,000 7,600 7,780

# 4-7Note: The Day 2 results represent the average of the original sample and the field duplicate (SP-3). See Section 5.2.4 for theanalytical results for the individual samples.< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 at least one result is a Jvalue.* - 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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 FortAnalyteUnitsMethodEffluent from the FGD Wastewater System (SP-2)Day 1Day 2Day 3Day 44-Day AverageClassicalsAmmoniamg/L350.14.805.405.505.305.25Nitrate Nitrite as Nmg/L353.255.029558.061.0117Nitrogen, Total Kjeldahlmg/L351.221.0B22.021.0B24.0B22.0Biochemical Oxygen Demandmg/L5210B6.709.006.90*,Min4.60S,*,Min6.80Chemical Oxygen Demandmg/L410.4570480560F,Min510530Chloridemg/L300.05,3007,5007,3007,4006,880Sulfatemg/L300.08,40013,00013,00014,00012,100Cyanide, Totalmg/L4500 CN E0.210B< 1.230.600B,C1.50B< 0.884Total Dissolved Solidsmg/L2540C29,00029,50028,00033,00029,900Total Suspended Solidsmg/L2540D17.08.808.40B22.014.1Phosphorus, Totalmg/L365.10.0960B0.1230.180B,F,Min0.0750B0.118Total MetalsAluminumug/L200.7NQ (200)< 180330NQ (200)< 178Antimonyug/L200.86.806.955.705.806.31Arsenicug/L200.84.304.854.904.404.61Bariumug/L200.7150155160150154Berylliumug/L200.7ND (2.00)ND (2.00)ND (2.00)ND (2.00)ND (2.00)Boronug/L200.7300,000B320,000320,000B,F,4330,000B318,000Cadmiumug/L200.8ND (4.00)ND (4.00)ND (4.00)ND (4.00)ND (4.00)Calciumug/L200.7890,000850,000840,000800,000845,000Chromiumug/L200.817.016.514.016.015.9

# 4-8Note: The Day 2 results represent the average of the original sample and the field duplicate (SP-3). See Section 5.2.4 for theanalytical results for the individual samples.< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 at least one result is a Jvalue.* - 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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 FortAnalyteUnitsMethodEffluent from the FGD Wastewater System (SP-2)Day 1Day 2Day 3Day 44-Day AverageCobaltug/L200.7ND (20.0)ND (20.0)ND (20.0)ND (20.0)ND (20.0)Copperug/L200.8ND (4.00)ND (4.00)ND (4.00)ND (4.00)ND (4.00)Ironug/L200.7NQ (200)NQ (200)260NQ (200)< 140Leadug/L200.8ND (2.00)ND (2.00)ND (2.00)ND (2.00)ND (2.00)Magnesiumug/L200.75,600,000B5,550,0005,500,000B,F,45,700,000B5,590,000Manganeseug/L200.7170B89.0280B100B160Mercuryng/L1631E101105148165130Molybdenumug/L200.7220200180150188Nickelug/L200.8NQ (4.00)NQ (4.00)NQ (4.00)NQ (4.00)NQ (4.00)Seleniumug/L200.85605358004480594Silverug/L200.8ND (2.00)ND (2.00)ND (2.00)F,MinND (2.00)ND (2.00)Sodiumug/L200.7370,000365,000360,0004360,000364,000Thalliumug/L200.814.014.014.012.013.5Tinug/L200.7ND (200)ND (200)ND (200)ND (200)ND (200)Titaniumug/L200.7ND (20.0)NQ (20.0)NQ (20.0)NQ (20.0)NQ (20.0)Vanadiumug/L200.816.017.516.018.016.9Zincug/L200.8ND (10.0)ND (10.0)ND (10.0)ND (10.0)ND (10.0)Dissolved MetalsAluminumug/L200.7ND (200)NQ (200)ND (200)ND (200)NQ (200)Antimonyug/L200.87.806.806.605.806.75Arsenicug/L200.84.80< 3.004.804.70< 4.33Bariumug/L200.7140145150150146

# 4-9Note: The Day 2 results represent the average of the original sample and the field duplicate (SP-3). See Section 5.2.4 for theanalytical results for the individual samples.< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 at least one result is a Jvalue.* - 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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 FortAnalyteUnitsMethodEffluent from the FGD Wastewater System (SP-2)Day 1Day 2Day 3Day 44-Day AverageBerylliumug/L200.7ND (2.00)ND (2.00)ND (2.00)ND (2.00)ND (2.00)Boronug/L200.7300,000B325,000320,000F,4330,000319,000Cadmiumug/L200.8ND (4.00)ND (4.00)ND (4.00)ND (4.00)ND (4.00)Calciumug/L200.7880,000835,000840,0004820,000844,000Chromiumug/L200.814.014.015.0^15.0^14.5Chromium (VI)ug/L218.67.047.347.616.717.17Cobaltug/L200.7ND (20.0)ND (20.0)ND (20.0)ND (20.0)ND (20.0)Copperug/L200.8NQ (4.00)NQ (4.00)ND (4.00)ND (4.00)NQ (4.00)Ironug/L200.7ND (200)ND (200)ND (200)ND (200)ND (200)Leadug/L200.8ND (2.00)ND (2.00)ND (2.00)ND (2.00)ND (2.00)Magnesiumug/L200.75,500,0005,750,0005,600,000F,46,000,0005,710,000Manganeseug/L200.7160B84.0250B93.0B147Mercuryng/L1631E49.761.571.384.566.8Molybdenumug/L200.7210195170150181Nickelug/L200.8NQ (4.00)NQ (4.00)NQ (4.00)NQ (4.00)NQ (4.00)Seleniumug/L200.85604956404530556Silverug/L200.8ND (2.00)ND (2.00)ND (2.00)F,MinND (2.00)ND (2.00)Sodiumug/L200.7350,000350,000350,000360,000353,000Thalliumug/L200.814.014.013.012.013.3Tinug/L200.7ND (200)ND (200)ND (200)ND (200)ND (200)Titaniumug/L200.7ND (50.0)NQ (60.0)NQ (20.0)NQ (20.0)NQ (37.5)Vanadiumug/L200.816.017.014.0^15.0^15.5

# 4-10Note: The Day 2 results represent the average of the original sample and the field duplicate (SP-3). See Section 5.2.4 for theanalytical results for the individual samples.< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 at least one result is a Jvalue.* - 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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 FortAnalyteUnitsMethodEffluent from the FGD Wastewater System (SP-2)Day 1Day 2Day 3Day 44-Day AverageZincug/L200.8ND (10.0)ND (10.0)ND (10.0)ND (10.0)ND (10.0)

# 4-11< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).Table 4-3.Classical Pollutants 4-Day Average Data Summaryfor FGD Wastewater Treatment System, Miami FortAnalyteUnitsMethodInfluent to FGDWastewater TreatmentSystem (SP-1)4-Day AverageEffluent fromFGD Wastewater TreatmentSystem (SP-2)4-Day AverageClassicalsAmmoniamg/L350.16.325.25Nitrate Nitrite as Nmg/L353.279.0117Nitrogen, Total Kjeldahlmg/L351.245.422.0Biochemical Oxygen Demandmg/L5210B< 1.706.80Chemical Oxygen Demandmg/L410.4730530Chloridemg/L300.09,5006,880Sulfatemg/L300.023,80012,100Cyanide, Totalmg/L4500 CN E0.787< 0.884Total Dissolved Solidsmg/L2540C58,30029,900Total Suspended Solidsmg/L2540D21,30014.1Phosphorus, Totalmg/L365.1< 3.690.118

# 4-12< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).NA – Not analyzed.ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 at least one result is a Jvalue.Table 4-4.Metal Pollutants 4-Day Average Data Summary for FGD Wastewater Treatment System, Miami FortAnalyteUnitsMethodInfluent to FGDWastewater TreatmentSystem (SP-1)4-Day AverageEffluent fromFGD Wastewater TreatmentSystem (SP-2)4-Day AverageTotalDissolvedTotalDissolvedMetalsAluminumug/L200.7593,0009,600< 178NQ (200)Antimonyug/L200.8NQ (11.0)3.306.316.75Arsenicug/L200.89605.354.61< 4.33Bariumug/L200.77,990153154146Berylliumug/L200.730.06.35ND (2.00)ND (2.00)Boronug/L200.7758,000723,000318,000319,000Cadmiumug/L200.8422415ND (4.00)ND (4.00)Calciumug/L200.71,470,000655,000845,000844,000Chromiumug/L200.84,130ND (8.00)15.914.5Chromium (VI)ug/L218.6NAND (10.0)NA7.17Cobaltug/L200.7505393ND (20.0)ND (20.0)Copperug/L200.81,44067.3ND (4.00)NQ (4.00)Ironug/L200.7918,000NQ (200)< 140ND (200)Leadug/L200.8784ND (2.00)ND (2.00)ND (2.00)Magnesiumug/L200.79,470,0009,050,0005,590,0005,710,000Manganeseug/L200.7113,000120,000160147Mercuryng/L1631E147,0001,63013066.8Molybdenumug/L200.7523113188181Nickelug/L200.82,9301,980NQ (4.00)NQ (4.00)Seleniumug/L200.83,330313594556Silverug/L200.8NQ (6.42)ND (2.00)ND (2.00)ND (2.00)Sodiumug/L200.7422,000405,000364,000353,000Thalliumug/L200.862.231.513.513.3Tinug/L200.7NQ (426)NQ (200)ND (200)ND (200)

# 4-13< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).NA – Not analyzed.ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 at least one result is a Jvalue.Table 4-4.Metal Pollutants 4-Day Average Data Summary for FGD Wastewater Treatment System, Miami FortAnalyteUnitsMethodInfluent to FGDWastewater TreatmentSystem (SP-1)4-Day AverageEffluent fromFGD Wastewater TreatmentSystem (SP-2)4-Day AverageTotalDissolvedTotalDissolvedTitaniumug/L200.72,510NQ (20.0)NQ (20.0)NQ (37.5)Vanadiumug/L200.83,99015.316.915.5Zincug/L200.816,2007,780ND (10.0)ND (10.0)

# 5-14 5. D ATA 

# Q UALITY



# Quality assurance/quality control (QA/QC) pr ocedures 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 pr ocedures 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 labor atories for the analysis of samples collected

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

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

prepared written data review narr atives describing any qualifications of the analytical data from

this episode. The data review narrat ives 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 Samp ling Plan discusses fiel d QC specifications.

5.2.1 Bottle Blanks

ERG collects bottle blanks to evaluate possibl e 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 precleane d bottles, Frontier Global Sciences.

Frontier Global Sciences collected the bottl e blanks for the metals sample bottles by

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

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

Frontier Global Sciences collected the bottl e blanks for the mercury sample bottles by

filling the precleaned bottle with reagent wa ter, preserving the sample with bromine

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

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

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

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

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

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

poured a representative sample into a preclean ed 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 lim it used for the sample analyses (i.e., 200

ug/L); therefore, this contamination did not aff ect 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 (a s described in Section

5.2.3) include the sampling equipment and ther efore would identify whether the sampling

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

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

precleaned equipment supp lied for the episode.

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

fabricated tubing sets by pumping reagent wa ter 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 e quipment blanks, indicating that there was no

contamination from the sampling equipment. Appe ndix 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, samp ling equipment decontamination procedures,

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

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

dissolved mercury samples 3



# .

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

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

ASTM Type 1 water through a precle aned funnel attached to the si licone 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 filli ng 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 samp le 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 fo r the dissolved mercury sample. Mercury was detected at

a concentration of 0.25 ng/L in the filtration blank perf ormed 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 syst em (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 Miam i Fort’s representative, using the same procedure discussed in

the sample collection de scription (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 wastew ater treatment system (SP-4)

were collected by pouring ASTM Type 1 water th rough the funnel and tubi ng 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 bl ank water. The sample bottles were placed in

a “cleanbox” and the ASTM Type 1 water was pump ed through the tubing, capsule filter, and

“Y” splitter, and into the sample bottles. EPA co llected the field blank samples as “true” split

samples with Miami Fort’s representative, using the same procedure discussed in the sample

collection descripti on (Section 3.1).

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

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

clear plastic bag. Before purging the sample tap, ASTM Type 1 wa ter 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 Ty pe 1 water. The same T-splitter tubing used to fill the metals

composite container was used with a pump to f ill 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 th e tubing was attached to the vented cap on top

of the 20-liter field blank composite containe r. After enough volume was pumped into the 20-

liter field blank composite contai ner, the vented cap was repla ced with a closed cap and the

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

blank collection was the same cap that was late r 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 throug h the tubing and “Y” splitter, and into the

sample bottles. EPA collected the field blank samp les as “true” split samples with Miami Fort’s

representative, using the same procedure discusse d in the sample collect ion description (Section

3.1). Prior to filling the sample bottles, the tubing was purged w ith approximately one liter of

ASTM Type 1 water. First the samplers collec ted 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 T ype 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 analyt ical 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 dupl icate samples are separate samp les 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 be tween 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 D S D S (%) 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) durin g 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 a nd A-13 present all the

analytical results for the efflue nt from FGD wastewater treatmen t system (SP-2) Day 2 and the

duplicate of the effluent from FGD wastewater treatment syst em (SP-3) sample analyses,

including all qualified results a nd all results that were measur ed above the method detection

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

# 5-18Table 5-1.Field Blank Analytical Results, Miami FortAnalyteSample DescriptionMethodUnitsConcentrationTotal MetalsMagnesiumEffluent from FGD Wastewater Treatment System Field Blank - Day 1200.7ug/L410MercuryInfluent to FGD Wastewater Treatment System Field Blank - Day 11631Eng/L15.4

# 5-19< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).NC – Not calculated.ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 at least one result is a Jvalue.4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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 limitsTable 5-2. Field Duplicate Results – Effluent from FGD Wastewater Treatment System, Miami FortAnalyteMethodUnitsOriginalEffluent fromFGD WastewaterTreatment System, Day2 Concentration (SP-2)DuplicateEffluent from FGDWastewaterTreatment SystemConcentration(SP-3)AverageResultRelativePercentDifferenceClassicalsAmmonia350.1mg/L5.305.505.403.70Nitrate Nitrite as N353.2mg/L2903002953.39Nitrogen, Total Kjeldahl351.2mg/L21.0B23.0B22.09.09Biochemical Oxygen Demand5210Bmg/L8.409.609.0013.3Chemical Oxygen Demand410.4mg/L40056048033.3Chloride300.0mg/L7,5007,5007,5000.00Sulfate300.0mg/L13,00013,00013,0000.00Cyanide, Total4500 CN Emg/L2.40BNQ (0.100)B< 1.23NCTotal Dissolved Solids2540Cmg/L32,00027,00029,50016.9Total Suspended Solids2540Dmg/L10.07.608.8027.3Phosphorus, Total365.1mg/L0.180B0.0650B0.12393.9Total MetalsAluminum200.7ug/L260NQ (200)< 180NCAntimony200.8ug/L6.907.006.951.44Arsenic200.8ug/L5.604.104.8530.9Barium200.7ug/L1501601556.45Beryllium200.7ug/LND (2.00)ND (2.00)ND (2.00)NCBoron200.7ug/L320,000B,F,4320,000B320,0000.00Cadmium200.8ug/LND (4.00)ND (4.00)ND (4.00)NC

# 5-20< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).NC – Not calculated.ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 at least one result is a Jvalue.4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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 limitsTable 5-2. Field Duplicate Results – Effluent from FGD Wastewater Treatment System, Miami FortAnalyteMethodUnitsOriginalEffluent fromFGD WastewaterTreatment System, Day2 Concentration (SP-2)DuplicateEffluent from FGDWastewaterTreatment SystemConcentration(SP-3)AverageResultRelativePercentDifferenceCalcium200.7ug/L840,0004860,000850,0002.35Chromium200.8ug/L16.017.016.56.06Cobalt200.7ug/LND (20.0)ND (20.0)ND (20.0)NCCopper200.8ug/LND (4.00)ND (4.00)ND (4.00)NCIron200.7ug/LNQ (200)NQ (200)NQ (200)NCLead200.8ug/LND (2.00)ND (2.00)ND (2.00)NCMagnesium200.7ug/L5,500,000B,F,45,600,000B5,550,0001.80Manganese200.7ug/L88.0B90.0B89.02.25Mercury1631Eng/L99.81101059.72Molybdenum200.7ug/L2002002000.00Nickel200.8ug/LNQ (4.00)NQ (4.00)NQ (4.00)NCSelenium200.8ug/L540V,4,MI5305351.87Silver200.8ug/LND (2.00)F,MinND (2.00)ND (2.00)NCSodium200.7ug/L360,0004370,000365,0002.74Thallium200.8ug/L14.014.014.00.00Tin200.7ug/LND (200)ND (200)ND (200)NCTitanium200.7ug/LND (20.0)NQ (20.0)NQ (20.0)NCVanadium200.8ug/L17.018.017.55.71Zinc200.8ug/LND (10.0)ND (10.0)ND (10.0)NCDissolved Metals

# 5-21< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).NC – Not calculated.ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 at least one result is a Jvalue.4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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 limitsTable 5-2. Field Duplicate Results – Effluent from FGD Wastewater Treatment System, Miami FortAnalyteMethodUnitsOriginalEffluent fromFGD WastewaterTreatment System, Day2 Concentration (SP-2)DuplicateEffluent from FGDWastewaterTreatment SystemConcentration(SP-3)AverageResultRelativePercentDifferenceAluminum200.7ug/LNQ (200)BND (200)NQ (200)NCAntimony200.8ug/L6.806.806.800.00Arsenic200.8ug/LNQ (4.00)4.00< 3.00NCBarium200.7ug/L1501401456.90Beryllium200.7ug/LND (2.00)ND (2.00)ND (2.00)NCBoron200.7ug/L330,000F,4320,000325,0003.08Cadmium200.8ug/LND (4.00)ND (4.00)ND (4.00)NCCalcium200.7ug/L860,000810,000835,0005.99Chromium200.8ug/L14.014.014.00.00Chromium (VI)218.6ug/L7.327.357.340.409Cobalt200.7ug/LND (20.0)ND (20.0)ND (20.0)NCCopper200.8ug/LND (4.00)NQ (4.00)NQ (4.00)NCIron200.7ug/LND (200)ND (200)ND (200)NCLead200.8ug/LND (2.00)ND (2.00)ND (2.00)NCMagnesium200.7ug/L5,900,000F,45,600,0005,750,0005.22Manganese200.7ug/L87.0B81.0B84.07.14Mercury1631Eng/L63.159.961.55.20Molybdenum200.7ug/L2001901955.13Nickel200.8ug/LNQ (4.00)NQ (4.00)NQ (4.00)NCSelenium200.8ug/L520V,4,MI47049510.1

# 5-22< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).NC – Not calculated.ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 at least one result is a Jvalue.4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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 limitsTable 5-2. Field Duplicate Results – Effluent from FGD Wastewater Treatment System, Miami FortAnalyteMethodUnitsOriginalEffluent fromFGD WastewaterTreatment System, Day2 Concentration (SP-2)DuplicateEffluent from FGDWastewaterTreatment SystemConcentration(SP-3)AverageResultRelativePercentDifferenceSilver200.8ug/LND (2.00)F,MinND (2.00)ND (2.00)NCSodium200.7ug/L360,000340,000350,0005.71Thallium200.8ug/L14.014.014.00.00Tin200.7ug/LND (200)ND (200)ND (200)NCTitanium200.7ug/LNQ (20.0)ND (100.0)NQ (60.0)NCVanadium200.8ug/L16.018.017.011.8Zinc200.8ug/LND (10.0)ND (10.0)ND (10.0)NC

# 6-1 6. R EFERENCES



# 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 C oupled 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-1ND – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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 FGDWastewater Treatment System, Day 1Analytical Results, Miami FortAnalyteAqueous Phase Result(mg/L)Solid Phase Result(mg/kg)Calculated TotalResult (mg/L)ClassicalsAmmonia5.1H,P,Est24H,P,Est5.21Nitrate Nitrite as N77H,P,Est49H,P,Est71.7Nitrogen, Total Kjeldahl24H,P,Est830H,P,Est40.5Cyanide, Total0.27B,H,P,Est0.35J,B,H,P0.255Phosphorus, Total0.01J,B,H,P21H,P,Est0.476Total MetalsAluminum6,00025,000561,000Antimony3.10.16J6.4Arsenic4.142937Barium88F,Min340B7,640Beryllium3.41.127.6Boron660,000B,4860B624,000Cadmium3202.2342Calcium610,00035,000B1,340,000ChromiumND (8)U180^4,000Cobalt3205.9425Copper42591,350IronND (200)U41,000911,000

# A-2ND – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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 FGDWastewater Treatment System, Day 1Analytical Results, Miami FortAnalyteAqueous Phase Result(mg/L)Solid Phase Result(mg/kg)Calculated TotalResult (mg/L)LeadND (2)U34756Magnesium8,100,000420,0007,870,000Manganese95,000B,427093,100Mercury2,9207,570166,000Molybdenum14017506Nickel1,5004542,580Selenium320V,4,MI1403,400SilverND (2)U,F,Min0.14J3.11Sodium360,0001,100355,000Thallium141.8B52.8Tin11J2.3J61.2TitaniumND (20)U912,020Vanadium8.7J1804,010Zinc5,200B,441013,900

# A-3ND – 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 Classicalsand Total Metals, Influent to FGD WastewaterTreatment System, Day 2 Analytical Results, Miami FortAnalyteAqueous Phase Result(mg/L)Solid Phase Result(mg/kg)Calculated TotalResult (mg/L)ClassicalsAmmonia5.3P,Est28H,P,Est6.12Nitrate Nitrite as N83P,Est64H,P,Est86.6Nitrogen, Total Kjeldahl31H,P,Est840H,P,Est52.6Cyanide, Total0.62B,H,P,Est0.33J,B,H,P0.644Phosphorus, Total0.008J,B,H,P310H,P,Est7.68Total MetalsAluminum6,600B25,000626,000Antimony2.70.15J6.48Arsenic4.436896Barium83300B7,510Beryllium3.5128.3Boron760,000B980B803,000Cadmium3602.3426Calcium590,000B30,000B1,350,000ChromiumND (8)U180^4,460Cobalt3605.4503Copper59591,520IronND (200)U39,000965,000Lead0.82J34842Magnesium8,500,00020,0009,210,000Manganese96,000B260105,000Mercury2,9907,330148,000Molybdenum14016540

# A-4ND – 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 Classicalsand Total Metals, Influent to FGD WastewaterTreatment System, Day 2 Analytical Results, Miami FortAnalyteAqueous Phase Result(mg/L)Solid Phase Result(mg/kg)Calculated TotalResult (mg/L)Nickel1,600542,980Selenium4201303,650SilverND (2)U0.14J3.47Sodium390,0001,100427,000Thallium141.7B56.4Tin6.1J2.2J60.7TitaniumND (20)U832,050Vanadium9.9J1704,220Zinc6,000B41016,300

# A-5ND – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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 Classicalsand Total Metals, Influent to FGD WastewaterTreatment System, Day 3 Analytical Results, Miami FortAnalyteAqueous Phase Result(mg/L)Solid Phase Result(mg/kg)Calculated TotalResult (mg/L)ClassicalsAmmonia7.7P,Est26P,Est7.9Nitrate Nitrite as N79P,Est56P,Est74.9Nitrogen, Total Kjeldahl29P,Est700P,Est47.6Cyanide, Total2.2B,H,P,Est0.37J,B,H,P2.05Phosphorus, Total0.013J,B,P1.9J,P0.068Total MetalsAluminum40,000B22,0004687,000Antimony3.60.16J,F,Min8.06Arsenic7.2441,310Barium80350B10,400Beryllium101.141.8Boron880,000B950B,4844,000Cadmium5002522Calcium570,000B52,000B,42,060,000ChromiumND (8)U1504,^4,430Cobalt5005.7632Copper86541,670IronND (200)U35,00041,030,000Lead0.82J30887Magnesium12,000,00023,00011,800,000Manganese160,000B300157,000

# A-6ND – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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 Classicalsand Total Metals, Influent to FGD WastewaterTreatment System, Day 3 Analytical Results, Miami FortAnalyteAqueous Phase Result(mg/L)Solid Phase Result(mg/kg)Calculated TotalResult (mg/L)Mercury3,6405,990231,000Molybdenum15017641Nickel2,400473,610Selenium4101003,330SilverND (2)U0.14J,F,Min4.14Sodium500,0001,300502,000Thallium342.1B93.5TinND (200)U2.4J70.9TitaniumND (20)U140F Max4,140Vanadium1415044,440Zinc11,000B340420,200

# A-7ND – 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 WastewaterTreatment System, Day 4 Analytical Results, Miami FortAnalyteAqueous Phase Result(mg/L)Solid Phase Result(mg/kg)Calculated TotalResult (mg/L)ClassicalsAmmonia6.2P,Est23P,Est6.06Nitrate Nitrite as N90P,Est65P,Est82.8Nitrogen, Total Kjeldahl26P,Est900P,Est40.8Cyanide, Total0.21B,H,P,Est0.42J,B,H,P0.198Phosphorus, Total0.012J,B,P340P,Est6.52Total MetalsAluminum20,000B25,000497,000Antimony2.50.14J4.95Arsenic5.936695Barium100330B6,410Beryllium3.6122.4Boron820,000B990B762,000Cadmium3802.7396Calcium600,000B31,000B1,140,000ChromiumND (8)U190^3,640Cobalt3905.5459Copper72601,210IronND (200)U40,000766,000LeadND (2)U34651Magnesium9,500,00021,0009,010,000Manganese100,000B28096,000Mercury4,3704,99044,000Molybdenum11016406

# A-8ND – 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 WastewaterTreatment System, Day 4 Analytical Results, Miami FortAnalyteAqueous Phase Result(mg/L)Solid Phase Result(mg/kg)Calculated TotalResult (mg/L)Nickel1,700532,560Selenium4701302,920SilverND (2)U0.12J2.3Sodium420,0001,200404,000Thallium151.7B46.2TinND (200)U2.3J44.1TitaniumND (20)U951,820Vanadium141703,270Zinc6,700B44014,500

# A-9NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassical Pollutants - TotalAmmonia350.1mg/lNA0.1922.055.21Nitrate Nitrite as N353.2mg/lNA0.1821.1471.7Nitrogen, Total Kjeldahl351.2mg/lNA3.0215.940.5Biochemical Oxygen Demand5210Bmg/L10.32.52JChemical Oxygen Demand410.4mg/L1041200620Chloride300.0mg/L5001301,5009,000Sulfate300.0mg/L5001202,50018,000Cyanide, Total4500 CN Emg/lNA0.02050.1020.255Total Dissolved Solids2540Cmg/L14701,00056,000Total Suspended Solids2540Dmg/L15520016,000Phosphorus, Total365.1mg/lNA0.02240.1530.476Classicals Pollutants - Solid (dry weight)Ammonia350.1mg/Kg14.19.924H,P,EstNitrate Nitrite as N353.2mg/Kg10.361049H,P,EstNitrogen, Total Kjeldahl351.2mg/Kg10120510830H,P,EstCyanide, Total4500 CN Emg/Kg10.0950.460.35J,B,H,P

# A-10NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationPhosphorus, Total365.1mg/Kg10.84.821H,P,EstClassicals Pollutants -Filtered AqueousAmmonia350.1mg/L10.1125.1H,P,EstNitrate Nitrite as N353.2mg/L100.19177H,P,EstNitrogen, Total Kjeldahl351.2mg/L20.38524H,P,EstCyanide, Total4500 CN Emg/L10.020.10.27B,H,P,EstPhosphorus, Total365.1mg/L10.0050.050.01J,B,H,PMetals - Calculated TotalAluminum200.7, 6010Bug/LNA42403561,000Antimony200.8, 6020ug/LNA1.2610.36.4Arsenic200.8, 6020ug/LNA27.8315937Barium200.7, 6010Bug/LNA3.9640.37,640Beryllium200.7, 6010Bug/LNA1.3812.927.6Boron200.7, 6010Bug/LNA2655,700624,000Cadmium200.8, 6020ug/LNA1.57.89342Calcium200.7, 6010Bug/LNA3741,4801,340,000Chromium200.8, 6020ug/LNA431144,000

# A-11NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationCobalt200.7, 6010Bug/LNA3.2140.3425Copper200.8, 6020ug/LNA38.71371,350Iron200.7, 6010Bug/LNA114517911,000Lead200.8, 6020ug/LNA10.281.8756Magnesium200.7, 6010Bug/LNA5779,6207,870,000Manganese200.7, 6010Bug/LNA14.148193,100Mercury1631E, FGS-069ng/LNA1,6704,530166,000Molybdenum200.7, 6010Bug/LNA7.2581.1506Nickel200.8, 6020ug/LNA1.8810.12,580Selenium200.8, 6020ug/LNA6.1224.83,400Silver200.8, 6020ug/LNA1.416.063.11Sodium200.7, 6010Bug/LNA1,45020,300355,000Thallium200.8, 6020ug/LNA0.586.0652.8Tin200.7, 6010Bug/LNA24.440361.2Titanium200.7, 6010Bug/LNA4.5840.32,020Vanadium200.8, 6020ug/LNA222764,010Zinc200.8, 6020ug/LNA20462513,900

# A-12NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationMetals - DissolvedAluminum200.7ug/L29.42004,200BAntimony200.8ug/L20.7223.4Arsenic200.8ug/L21.244.4Barium200.7ug/L22.520140Beryllium200.7ug/L20.7124.7Boron200.7ug/L5001,70050,000650,000BCadmium200.8ug/L52.910340Calcium200.7ug/L269400690,000Chromium200.8ug/L23.38ND (8)UChromium (VI)218.6ug/L51.9610ND (10)UCobalt200.7ug/L21.120340Copper200.8ug/L20.96454Iron200.7ug/L23220047JLead200.8ug/L20.732ND (2)UMagnesium200.7ug/L5005,400100,0007,900,000Manganese200.7ug/L5001305,000100,000

# A-13NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationMercury1631Eng/L5001242601,110Molybdenum200.7ug/L21.640120Nickel200.8ug/L2511501,700Selenium200.8ug/L51.610290Silver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000360,000Thallium200.8ug/L20.47225Tin200.7ug/L24.82008.7JTitanium200.7ug/L21.6203.2JVanadium200.8ug/L21.71012Zinc200.8ug/L1002005006,300Metals - Filtered AqueousAluminum200.7ug/L29.42006,000Antimony200.8ug/L20.7223.1Arsenic200.8ug/L21.244.1Barium200.7ug/L22.52088F,MinBeryllium200.7ug/L20.7123.4

# A-14NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationBoron200.7ug/L501705,000660,000B,4Cadmium200.8ug/L21.24320Calcium200.7ug/L269400610,000Chromium200.8ug/L23.38ND (8)UCobalt200.7ug/L21.120320Copper200.8ug/L20.96442Iron200.7ug/L232200ND (200)ULead200.8ug/L20.732ND (2)UMagnesium200.7ug/L5054010,0008,100,0004Manganese200.7ug/L501350095,000B,4Mercury1631Eng/L5001242602,920Molybdenum200.7ug/L21.640140Nickel200.8ug/L20.8941,5004Selenium200.8ug/L20.624320V,4,MISilver200.8ug/L20.592ND (2)U,F,MinSodium200.7ug/L218010,000360,000Thallium200.8ug/L20.47214

# A-15NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationTin200.7ug/L24.820011JTitanium200.7ug/L21.620ND (20)UVanadium200.8ug/L21.7108.7JZinc200.8ug/L20411005,200B,4Metals - Solid (dry weight)Aluminum6010Bmg/kg11.59.925,000Antimony6020mg/kg20.0270.380.16JArsenic6020mg/kg251.21442Barium6010Bmg/kg10.0750.99340BBeryllium6010Bmg/kg10.0330.51.1Boron6010Bmg/kg54.950860BCadmium6020mg/kg20.0180.192.2Calcium6010Bmg/kg1145035,000BChromium6020mg/kg251.84.8180^Cobalt6010Bmg/kg10.0990.995.9Copper6020mg/kg251.7659Iron6010Bmg/kg13.81541,000

# A-16NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationLead6020mg/kg250.433.634Magnesium6010Bmg/kg13.72020,000Manganese6010Bmg/kg10.0990.99270MercuryFGS-069ng/g4,00071.91987,570Molybdenum6010Bmg/kg10.26217Nickel6020mg/kg20.0480.2954Selenium6020mg/kg20.250.95140Silver6020mg/kg20.0390.190.14JSodium6010Bmg/kg1585001,100Thallium6020mg/kg20.00670.191.8BTin6010Bmg/kg10.99.92.3JTitanium6010Bmg/kg10.140.9991Vanadium6020mg/kg250.9212180Zinc6020mg/kg257.524410

# A-17NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassical Pollutants - TotalAmmonia350.1mg/lNA0.2142.36.12Nitrate Nitrite as N353.2mg/lNA0.2031.2786.6Nitrogen, Total Kjeldahl351.2mg/lNA3.361852.6Biochemical Oxygen Demand5210Bmg/L10.32.51.9JChemical Oxygen Demand410.4mg/L1041200670Chloride300.0mg/L5001301,5009,800Sulfate300.0mg/L5001202,50021,000Cyanide, Total4500 CN Emg/lNA0.02320.1160.644Total Dissolved Solids2540Cmg/L14701,00068,000Total Suspended Solids2540Dmg/L15520030,000Phosphorus, Total365.1mg/lNA0.2081.297.68Classicals Pollutants - Solid (dry weight)Ammonia350.1mg/Kg14.11028H,P,EstNitrate Nitrite as N353.2mg/Kg10.359.964H,P,EstNitrogen, Total Kjeldahl351.2mg/Kg10120520840H,P,EstCyanide, Total4500 CN Emg/Kg10.110.530.33J,B,H,PPhosphorus, Total365.1mg/Kg108.250310H,P,EstClassicals Pollutants -Filtered AqueousAmmonia350.1mg/L10.1125.3P,Est

# A-18NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationNitrate Nitrite as N353.2mg/L100.19183P,EstNitrogen, Total Kjeldahl351.2mg/L20.38531H,P,EstCyanide, Total4500 CN Emg/L10.020.10.62B,H,P,EstPhosphorus, Total365.1mg/L10.0050.050.008J,B,H,PMetals - Calculated TotalAluminum200.7, 6010Bug/LNA44.3430626,000Antimony200.8, 6020ug/LNA1.36116.48Arsenic200.8, 6020ug/LNA28.5351896Barium200.7, 6010Bug/LNA4.27437,510Beryllium200.7, 6010Bug/LNA1.4713.228.3Boron200.7, 6010Bug/LNA2866,240803,000Cadmium200.8, 6020ug/LNA1.658.55426Calcium200.7, 6010Bug/LNA3921,5201,350,000Chromium200.8, 6020ug/LNA45.51204,460Cobalt200.7, 6010Bug/LNA3.3843503Copper200.8, 6020ug/LNA40.61431,520Iron200.7, 6010Bug/LNA119551965,000Lead200.8, 6020ug/LNA10.986.2842Magnesium200.7, 6010Bug/LNA63810,7009,210,000Manganese200.7, 6010Bug/LNA15.6535105,000

# A-19NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationMercury1631E, FGS-069ng/LNA1,5204,120148,000Molybdenum200.7, 6010Bug/LNA7.5885.5540Nickel200.8, 6020ug/LNA2.0510.82,980Selenium200.8, 6020ug/LNA6.5826.43,650Silver200.8, 6020ug/LNA1.526.53.47Sodium200.7, 6010Bug/LNA1,52021,400427,000Thallium200.8, 6020ug/LNA0.6386.556.4Tin200.7, 6010Bug/LNA25.543060.7Titanium200.7, 6010Bug/LNA4.86432,050Vanadium200.8, 6020ug/LNA23.32834,220Zinc200.8, 6020ug/LNA19662116,300Metals - DissolvedAluminum200.7ug/L29.42002,400BAntimony200.8ug/L20.7223.3Arsenic200.8ug/L21.244.9Barium200.7ug/L22.520140Beryllium200.7ug/L20.7124.1Boron200.7ug/L5001,70050,000690,000BCadmium200.8ug/L52.910390Calcium200.7ug/L269400670,000

# A-20NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationChromium200.8ug/L23.38ND (8)UChromium (VI)218.6ug/L51.9610ND (10)UCobalt200.7ug/L21.120360Copper200.8ug/L20.96450Iron200.7ug/L232200ND (200)ULead200.8ug/L20.732ND (2)UMagnesium200.7ug/L5005,400100,0008,400,000Manganese200.7ug/L5001305,000100,000Mercury1631Eng/L5001242601,830Molybdenum200.7ug/L21.640110Nickel200.8ug/L2511501,700Selenium200.8ug/L51.610330Silver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000380,000Thallium200.8ug/L20.47226Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.6202.1JVanadium200.8ug/L21.71013Zinc200.8ug/L1002005006,200

# A-21NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationMetals - Filtered AqueousAluminum200.7ug/L29.42006,600BAntimony200.8ug/L20.7222.7Arsenic200.8ug/L21.244.4Barium200.7ug/L22.52083Beryllium200.7ug/L20.7123.5Boron200.7ug/L501705,000760,000BCadmium200.8ug/L21.24360Calcium200.7ug/L269400590,000BChromium200.8ug/L23.38ND (8)UCobalt200.7ug/L21.120360Copper200.8ug/L20.96459Iron200.7ug/L232200ND (200)ULead200.8ug/L20.7320.82JMagnesium200.7ug/L5054010,0008,500,000Manganese200.7ug/L501350096,000BMercury1631Eng/L5001242602,990Molybdenum200.7ug/L21.640140Nickel200.8ug/L20.8941,600Selenium200.8ug/L20.624420

# A-22NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationSilver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000390,000Thallium200.8ug/L20.47214Tin200.7ug/L24.82006.1JTitanium200.7ug/L21.620ND (20)UVanadium200.8ug/L21.7109.9JZinc200.8ug/L1020506,000BMetals - Solid (dry weight)Aluminum6010Bmg/kg11.49.125,000Antimony6020mg/kg20.0250.360.15JArsenic6020mg/kg251.11436Barium6010Bmg/kg10.0690.91300BBeryllium6010Bmg/kg10.030.451Boron6010Bmg/kg54.545980BCadmium6020mg/kg20.0170.182.3Calcium6010Bmg/kg1134530,000BChromium6020mg/kg251.74.5180^Cobalt6010Bmg/kg10.0910.915.4Copper6020mg/kg251.65.659Iron6010Bmg/kg13.51439,000

# A-23NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationLead6020mg/kg250.413.434Magnesium6010Bmg/kg13.41820,000Manganese6010Bmg/kg10.0910.91260MercuryFGS-069ng/g4,00071.11967,330Molybdenum6010Bmg/kg10.241.816Nickel6020mg/kg20.0460.2754Selenium6020mg/kg20.240.9130Silver6020mg/kg20.0370.180.14JSodium6010Bmg/kg1544501,100Thallium6020mg/kg20.00630.181.7BTin6010Bmg/kg10.839.12.2JTitanium6010Bmg/kg10.130.9183Vanadium6020mg/kg250.8711170Zinc6020mg/kg257.123410

# A-24NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassical Pollutants – TotalAmmonia350.1mg/lNA 0.2232.157.9Nitrate Nitrite as N353.2mg/lNA 0.1861.2274.9Nitrogen, Total Kjeldahl351.2mg/lNA 3.919.447.6Biochemical Oxygen Demand5210Bmg/L10.32.53.3Chemical Oxygen Demand410.4mg/L1041200910Chloride300.0mg/L5001301,5009,600Sulfate300.0mg/L1,0002305,00032,000Cyanide, Total4500 CN Emg/lNA0.02180.1092.05Total Dissolved Solids2540Cmg/L14701,00059,000Total Suspended Solids2540Dmg/L15520020,000Phosphorus, Total365.1mg/lNA0.02860.1910.068Classicals Pollutants - Solid (dry weight)Ammonia350.1mg/Kg14.11026P,EstNitrate Nitrite as N353.2mg/Kg10.359.956P,EstNitrogen, Total Kjeldahl351.2mg/Kg10120500700P,EstCyanide, Total4500 CN Emg/Kg10.110.550.37J,B,H,PPhosphorus, Total365.1mg/Kg10.814.91.9J,PClassicals Pollutants -Filtered AqueousAmmonia350.1mg/L10.1127.7P,EstNitrate Nitrite as N353.2mg/L100.19179P,EstNitrogen, Total Kjeldahl351.2mg/L20.38529P,EstCyanide, Total4500 CN Emg/L10.020.12.2B,H,P,Est

# A-25NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationPhosphorus, Total365.1mg/L10.0050.050.013J,B,PMetals - Calculated TotalAluminum200.7, 6010Bug/LNA50.1460687,000Antimony200.8, 6020ug/LNA1.4613.48.06Arsenic200.8, 6020ug/LNA30.13581,310Barium200.7, 6010Bug/LNA4.414610,400Beryllium200.7, 6010Bug/LNA1.5715.741.8Boron200.7, 6010Bug/LNA2936,020844,000Cadmium200.8, 6020ug/LNA1.649.32522Calcium200.7, 6010Bug/LNA2,0107,1702,060,000Chromium200.8, 6020ug/LNA47.41234,430Cobalt200.7, 6010Bug/LNA3.7746632Copper200.8, 6020ug/LNA42.21481,670Iron200.7, 6010Bug/LNA1365991,030,000Lead200.8, 6020ug/LNA1187.5887Magnesium200.7, 6010Bug/LNA6049,83011,800,000Manganese200.7, 6010Bug/LNA14.8491157,000Mercury1631E, FGS-069ng/LNA2,8607,810231,000Molybdenum200.7, 6010Bug/LNA8.5793.2641Nickel200.8, 6020ug/LNA2.2712.33,610Selenium200.8, 6020ug/LNA10.647.23,330Silver200.8, 6020ug/LNA1.77.474.14Sodium200.7, 6010Bug/LNA1,79023,200502,000

# A-26NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationThallium200.8, 6020ug/LNA0.6367.4793.5Tin200.7, 6010Bug/LNA29.646070.9Titanium200.7, 6010Bug/LNA5.32464,140Vanadium200.8, 6020ug/LNA23.72964,440Zinc200.8, 6020ug/LNA36.610220,200Metals - DissolvedAluminum200.7ug/L10471,00029,000BAntimony200.8ug/L20.7223.7Arsenic200.8ug/L21.246.6Barium200.7ug/L22.520180Beryllium200.7ug/L20.71212Boron200.7ug/L5001,70050,000820,000Cadmium200.8ug/L5029100510Calcium200.7ug/L269400620,000Chromium200.8ug/L23.38ND (8)UChromium (VI)218.6ug/L51.9610ND (10)UCobalt200.7ug/L21.120490Copper200.8ug/L20.964110Iron200.7ug/L23220042JLead200.8ug/L20.732ND (2)UMagnesium200.7ug/L5005,400100,00011,000,000Manganese200.7ug/L5001305,000170,000Mercury1631Eng/L5001242601,600

# A-27NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationMolybdenum200.7ug/L21.640130Nickel200.8ug/L50221002,500Selenium200.8ug/L51.610330Silver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000480,000Thallium200.8ug/L20.47249Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.6201.8JVanadium200.8ug/L21.71020Zinc200.8ug/L2004101,00011,000Metals - Filtered AqueousAluminum200.7ug/L29.420040,000BAntimony200.8ug/L20.7223.6Arsenic200.8ug/L21.247.2Barium200.7ug/L22.52080Beryllium200.7ug/L20.71210Boron200.7ug/L501705,000880,000BCadmium200.8ug/L21.24500Calcium200.7ug/L269400570,000BChromium200.8ug/L23.38ND (8)UCobalt200.7ug/L21.120500Copper200.8ug/L20.96486Iron200.7ug/L232200ND (200)U

# A-28NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationLead200.8ug/L20.7320.82JMagnesium200.7ug/L5054010,00012,000,000Manganese200.7ug/L5013500160,000BMercury1631Eng/L5001242603,640Molybdenum200.7ug/L21.640150Nickel200.8ug/L20.8942,400Selenium200.8ug/L103.120410Silver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000500,000Thallium200.8ug/L20.47234Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.620ND (20)UVanadium200.8ug/L21.71014Zinc200.8ug/L10205011,000BMetals - Solid (dry weight)Aluminum6010Bmg/kg11.49.322,0004Antimony6020mg/kg20.0270.390.16J,F,MinArsenic6020mg/kg200.981244Barium6010Bmg/kg10.0710.93350BBeryllium6010Bmg/kg10.0310.471.1Boron6010Bmg/kg54.647950B,4Cadmium6020mg/kg20.0180.192Calcium6010Bmg/kg56623052,000B,4

# A-29NA – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.B – Analyte was found in the blank and sample.Est – Estimated value.F – MS and/or MSD not within laboratory control limits.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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationChromium6020mg/kg201.53.91504,^Cobalt6010Bmg/kg10.0930.935.7Copper6020mg/kg201.44.954Iron6010Bmg/kg13.61435,0004Lead6020mg/kg200.352.930Magnesium6010Bmg/kg13.51923,000Manganese6010Bmg/kg10.0930.93300MercuryFGS-069ng/g4,00072.11995,990Molybdenum6010Bmg/kg10.241.917Nickel6020mg/kg20.0490.2947Selenium6020mg/kg20.260.97100Silver6020mg/kg20.0390.190.14J,F,MinSodium6010Bmg/kg1554701,300Thallium6020mg/kg20.00680.192.1BTin6010Bmg/kg10.859.32.4JTitanium6010Bmg/kg10.130.93140F MaxVanadium6020mg/kg200.759.71504Zinc6020mg/kg20.611.93404

# A-30NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassical Pollutants - TotalAmmonia350.1mg/lNA 0.17826.06Nitrate Nitrite as N353.2mg/lNA0.1791.182.8Nitrogen, Total Kjeldahl351.2mg/lNA2.6414.540.8Biochemical Oxygen Demand5210Bmg/L10.242ND (2)U,*Chemical Oxygen Demand410.4mg/L1041200720Chloride300.0mg/L5001301,5009,600Sulfate300.0mg/L5001202,50024,000Cyanide, Total4500 CN Emg/lNA0.02020.1010.198Total Dissolved Solids2540Cmg/L14701,00050,000Total Suspended Solids2540Dmg/L19233019,000Phosphorus, Total365.1mg/lNA0.16316.52Classicals Pollutants - Solid (dry weight)Ammonia350.1mg/Kg14.11023P,EstNitrate Nitrite as N353.2mg/Kg10.359.965P,EstNitrogen, Total Kjeldahl351.2mg/Kg10120520900P,EstCyanide, Total4500 CN Emg/Kg10.110.540.42J,B,H,PPhosphorus, Total365.1mg/Kg108.350340P,EstClassicals Pollutants -Filtered AqueousAmmonia350.1mg/L10.1126.2P,Est

# A-31NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationNitrate Nitrite as N353.2mg/L100.19190P,EstNitrogen, Total Kjeldahl351.2mg/L20.38526P,EstCyanide, Total4500 CN Emg/L10.020.10.21B,H,P,EstPhosphorus, Total365.1mg/L10.0050.050.012J,B,PMetals - Calculated TotalAluminum200.7, 6010Bug/LNA44.9411497,000Antimony200.8, 6020ug/LNA1.199.474.95Arsenic200.8, 6020ug/LNA26291695Barium200.7, 6010Bug/LNA4.0941.16,410Beryllium200.7, 6010Bug/LNA1.4313.722.4Boron200.7, 6010Bug/LNA2715,720762,000Cadmium200.8, 6020ug/LNA1.457.46396Calcium200.7, 6010Bug/LNA4071,5501,140,000Chromium200.8, 6020ug/LNA39.41033,640Cobalt200.7, 6010Bug/LNA3.341.1459Copper200.8, 6020ug/LNA35.31221,210Iron200.7, 6010Bug/LNA121545766,000Lead200.8, 6020ug/LNA9.2872.7651Magnesium200.7, 6010Bug/LNA5789,5409,010,000Manganese200.7, 6010Bug/LNA14.147696,000

# A-32NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationMercury1631E, FGS-069ng/LNA6911,83044,000Molybdenum200.7, 6010Bug/LNA7.5884.1406Nickel200.8, 6020ug/LNA1.769.372,560Selenium200.8, 6020ug/LNA5.5422.62,920Silver200.8, 6020ug/LNA1.35.642.3Sodium200.7, 6010Bug/LNA1,58020,900404,000Thallium200.8, 6020ug/LNA0.565.6446.2Tin200.7, 6010Bug/LNA25.441144.1Titanium200.7, 6010Bug/LNA4.941.11,820Vanadium200.8, 6020ug/LNA19.72393,270Zinc200.8, 6020ug/LNA16852414,500Metals - DissolvedAluminum200.7ug/L29.42002,800BAntimony200.8ug/L20.7222.8Arsenic200.8ug/L21.245.5Barium200.7ug/L22.520150Beryllium200.7ug/L20.7124.6Boron200.7ug/L5001,70050,000730,000Cadmium200.8ug/L52.910420Calcium200.7ug/L269400640,000

# A-33NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationChromium200.8ug/L23.38ND (8)U,^Chromium (VI)218.6ug/L51.9610ND (10)UCobalt200.7ug/L21.120380Copper200.8ug/L20.96455Iron200.7ug/L232200ND (200)ULead200.8ug/L20.732ND (2)UMagnesium200.7ug/L5005,400100,0008,900,000Manganese200.7ug/L5001305,000110,000Mercury1631Eng/L5001242601,990Molybdenum200.7ug/L21.64090Nickel200.8ug/L2511502,000Selenium200.8ug/L51.610300Silver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000400,000Thallium200.8ug/L20.47226Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.6202JVanadium200.8ug/L21.71016^Zinc200.8ug/L25511207,600Metals - Filtered Aqueous

# A-34NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationAluminum200.7ug/L29.420020,000BAntimony200.8ug/L20.7222.5Arsenic200.8ug/L21.245.9Barium200.7ug/L22.520100Beryllium200.7ug/L20.7123.6Boron200.7ug/L501705,000820,000BCadmium200.8ug/L21.24380Calcium200.7ug/L269400600,000BChromium200.8ug/L23.38ND (8)UCobalt200.7ug/L21.120390Copper200.8ug/L20.96472Iron200.7ug/L232200ND (200)ULead200.8ug/L20.732ND (2)UMagnesium200.7ug/L5054010,0009,500,000Manganese200.7ug/L5013500100,000BMercury1631Eng/L5001242604,370Molybdenum200.7ug/L21.640110Nickel200.8ug/L20.8941,700Selenium200.8ug/L20.624470Silver200.8ug/L20.592ND (2)U

# A-35NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationSodium200.7ug/L218010,000420,000Thallium200.8ug/L20.47215Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.620ND (20)UVanadium200.8ug/L21.71014Zinc200.8ug/L1020506,700BMetals - Solid (dry weight)Aluminum6010Bmg/kg11.91225,000Antimony6020mg/kg20.0280.40.14JArsenic6020mg/kg251.31536Barium6010Bmg/kg10.0951.2330BBeryllium6010Bmg/kg10.0410.621Boron6010Bmg/kg56.162990BCadmium6020mg/kg20.0190.22.7Calcium6010Bmg/kg1186231,000BChromium6020mg/kg251.95190^Cobalt6010Bmg/kg10.121.25.5Copper6020mg/kg251.86.260Iron6010Bmg/kg14.81940,000Lead6020mg/kg250.453.734

# A-36NA – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationMagnesium6010Bmg/kg14.62521,000Manganese6010Bmg/kg10.121.2280MercuryFGS-069ng/g4,00071.91984,990Molybdenum6010Bmg/kg10.322.516Nickel6020mg/kg20.050.353Selenium6020mg/kg20.260.99130Silver6020mg/kg20.040.20.12JSodium6010Bmg/kg1746201,200Thallium6020mg/kg20.0070.21.7BTin6010Bmg/kg11.1122.3JTitanium6010Bmg/kg10.181.295Vanadium6020mg/kg250.9512170Zinc6020mg/kg257.825440

# A-37ND – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia350.1mg/L10.05514.8Nitrate Nitrite as N353.2mg/L100.19155Nitrogen, Total Kjeldahl351.2mg/L40.31421BBiochemical Oxygen Demand5210Bmg/L10.32.56.7Chemical Oxygen Demand410.4mg/L1041200570Chloride300.0mg/L5001301,5005,300Sulfate300.0mg/L5001202,5008,400Cyanide, Total4500 CN Emg/L10.020.10.21BTotal Dissolved Solids2540Cmg/L14710029,000Total Suspended Solids2540Dmg/L11.1417Phosphorus, Total365.1mg/L10.0050.050.096BTotal MetalsAluminum200.7ug/L29.4200180JAntimony200.8ug/L20.7226.8Arsenic200.8ug/L21.244.3Barium200.7ug/L22.520150Beryllium200.7ug/L20.712ND (2)UBoron200.7ug/L5001,70050,000300,000BCadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L269400890,000Chromium200.8ug/L23.3817Cobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.964ND (4)U

# A-38ND – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationIron200.7ug/L232200110JLead200.8ug/L20.732ND (2)UMagnesium200.7ug/L5054010,0005,600,000BManganese200.7ug/L20.5120170BMercury1631Eng/L204.8710.2101Molybdenum200.7ug/L21.640220Nickel200.8ug/L20.8943.4JSelenium200.8ug/L20.624560Silver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000370,000Thallium200.8ug/L20.47214Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.620ND (20)UVanadium200.8ug/L21.71016Zinc200.8ug/L24.110ND (10)UDissolved MetalsAluminum200.7ug/L29.4200ND (200)UAntimony200.8ug/L20.7227.8Arsenic200.8ug/L21.244.8Barium200.7ug/L22.520140Beryllium200.7ug/L20.712ND (2)UBoron200.7ug/L501705,000300,000BCadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L269400880,000

# A-39ND – 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 FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationChromium200.8ug/L23.3814Chromium (VI)218.6ug/L10.3927.04Cobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.9641.4JIron200.7ug/L232200ND (200)ULead200.8ug/L20.732ND (2)UMagnesium200.7ug/L5054010,0005,500,000Manganese200.7ug/L20.5120160BMercury1631Eng/L204.8710.249.7Molybdenum200.7ug/L21.640210Nickel200.8ug/L20.8942.2JSelenium200.8ug/L20.624560Silver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000350,000Thallium200.8ug/L20.47214Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L54.150ND (50)UVanadium200.8ug/L21.71016Zinc200.8ug/L24.110ND (10)U

# A-40ND – Not detected (number in parentheses is the quantitation limit).4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationClassicalsAmmonia350.1mg/L10.05515.3Nitrate Nitrite as N353.2mg/L500.955290Nitrogen, Total Kjeldahl351.2mg/L40.31421BBiochemical Oxygen Demand5210Bmg/L10.32.58.4Chemical Oxygen Demand410.4mg/L1041200400Chloride300.0mg/L5001301,5007,500Sulfate300.0mg/L5001202,50013,000Cyanide, Total4500 CN Emg/L10.020.12.4BTotal Dissolved Solids2540Cmg/L14710032,000Total Suspended Solids2540Dmg/L11.1410Phosphorus, Total365.1mg/L10.0050.050.18BTotal MetalsAluminum200.7ug/L29.4200260Antimony200.8ug/L20.7226.9Arsenic200.8ug/L21.245.6Barium200.7ug/L22.520150Beryllium200.7ug/L20.712ND (2)UBoron200.7ug/L10033010,000320,000B,F,4Cadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L269400840,0004

# A-41ND – Not detected (number in parentheses is the quantitation limit).4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationChromium200.8ug/L23.3816Cobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.964ND (4)UIron200.7ug/L232200110JLead200.8ug/L20.732ND (2)UMagnesium200.7ug/L1001,10020,0005,500,000B,F,4Manganese200.7ug/L20.512088BMercury1631Eng/L204.8710.299.8Molybdenum200.7ug/L21.640200Nickel200.8ug/L20.8943.3JSelenium200.8ug/L20.624540V,4,MISilver200.8ug/L20.592ND (2)U,F,MinSodium200.7ug/L218010,000360,0004Thallium200.8ug/L20.47214Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.620ND (20)UVanadium200.8ug/L21.71017Zinc200.8ug/L24.110ND (10)UDissolved MetalsAluminum200.7ug/L29.420024J,BAntimony200.8ug/L20.7226.8

# A-42ND – Not detected (number in parentheses is the quantitation limit).4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationArsenic200.8ug/L21.243.8JBarium200.7ug/L22.520150Beryllium200.7ug/L20.712ND (2)UBoron200.7ug/L501705,000330,000F,4Cadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L269400860,000Chromium200.8ug/L23.3814Chromium (VI)218.6ug/L10.3927.32Cobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.964ND (4)UIron200.7ug/L232200ND (200)ULead200.8ug/L20.732ND (2)UMagnesium200.7ug/L5054010,0005,900,000F,4Manganese200.7ug/L20.512087BMercury1631Eng/L204.9710.463.1Molybdenum200.7ug/L21.640200Nickel200.8ug/L20.8942.2JSelenium200.8ug/L20.624520V,4,MISilver200.8ug/L20.592ND (2)U,F,MinSodium200.7ug/L218010,000360,000Thallium200.8ug/L20.47214

# A-43ND – Not detected (number in parentheses is the quantitation limit).4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecificMDLSampleSpecificQLConcentrationTin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.6204.5JVanadium200.8ug/L21.71016Zinc200.8ug/L24.110ND (10)U

# A-44ND – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia350.1mg/L10.05515.5Nitrate Nitrite as N353.2mg/L100.19158Nitrogen, Total Kjeldahl351.2mg/L40.31421BBiochemical Oxygen Demand5210Bmg/L10.32.56.9*,MinChemical Oxygen Demand410.4mg/L1041200560F,MinChloride300.0mg/L5001301,5007,300Sulfate300.0mg/L5001202,50013,000Cyanide, Total4500 CN Emg/L10.020.10.6B,CTotal Dissolved Solids2540Cmg/L14710028,000Total Suspended Solids2540Dmg/L11.148.4BPhosphorus, Total365.1mg/L10.0050.050.18B,F,MinTotal MetalsAluminum200.7ug/L29.4200330Antimony200.8ug/L20.7225.7Arsenic200.8ug/L21.244.9Barium200.7ug/L22.520160Beryllium200.7ug/L20.712ND (2)UBoron200.7ug/L10033010,000320,000B,F,4Cadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L269400840,000Chromium200.8ug/L23.3814Cobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.964ND (4)UIron200.7ug/L232200260Lead200.8ug/L20.732ND (2)U

# A-45ND – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationMagnesium200.7ug/L1001,10020,0005,500,000B,F,4Manganese200.7ug/L20.5120280BMercury1631Eng/L10024.451148Molybdenum200.7ug/L21.640180Nickel200.8ug/L20.8942.9JSelenium200.8ug/L103.1208004Silver200.8ug/L20.592ND (2)U,F,MinSodium200.7ug/L218010,000360,0004Thallium200.8ug/L20.47214Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.6207.5JVanadium200.8ug/L21.71016Zinc200.8ug/L24.110ND (10)UDissolved MetalsAluminum200.7ug/L29.4200ND (200)UAntimony200.8ug/L20.7226.6Arsenic200.8ug/L21.244.8Barium200.7ug/L22.520150Beryllium200.7ug/L20.712ND (2)UBoron200.7ug/L501705,000320,000F,4Cadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L269400840,0004Chromium200.8ug/L23.3815^Chromium (VI)218.6ug/L10.3927.61Cobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.964ND (4)U

# A-46ND – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationIron200.7ug/L232200ND (200)ULead200.8ug/L20.732ND (2)UMagnesium200.7ug/L5054010,0005,600,000F,4Manganese200.7ug/L20.5120250BMercury1631Eng/L204.8710.271.3Molybdenum200.7ug/L21.640170Nickel200.8ug/L20.8942.3JSelenium200.8ug/L103.1206404Silver200.8ug/L20.592ND (2)U,F,MinSodium200.7ug/L218010,000350,000Thallium200.8ug/L20.47213Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.6204.6JVanadium200.8ug/L21.71014^Zinc200.8ug/L24.110ND (10)U

# A-47ND – 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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia350.1mg/L10.05515.3Nitrate Nitrite as N353.2mg/L100.19161Nitrogen, Total Kjeldahl351.2mg/L40.31424BBiochemical Oxygen Demand5210Bmg/L10.32.54.6S,*,MinChemical Oxygen Demand410.4mg/L1041200510Chloride300.0mg/L5001301,5007,400Sulfate300.0mg/L5001202,50014,000Cyanide, Total4500 CN Emg/L10.020.11.5BTotal Dissolved Solids2540Cmg/L14710033,000Total Suspended Solids2540Dmg/L12.2822Phosphorus, Total365.1mg/L10.0050.050.075BTotal MetalsAluminum200.7ug/L29.420053JAntimony200.8ug/L20.7225.8Arsenic200.8ug/L21.244.4Barium200.7ug/L22.520150Beryllium200.7ug/L20.712ND (2)UBoron200.7ug/L10033010,000330,000BCadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L269400800,000Chromium200.8ug/L23.3816Cobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.964ND (4)UIron200.7ug/L232200130JLead200.8ug/L20.732ND (2)UMagnesium200.7ug/L1001,10020,0005,700,000B

# A-48ND – 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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationManganese200.7ug/L20.5120100BMercury1631Eng/L10024.150.5165Molybdenum200.7ug/L21.640150Nickel200.8ug/L20.8942.8JSelenium200.8ug/L20.624480Silver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000360,000Thallium200.8ug/L20.47212Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.6206.5JVanadium200.8ug/L21.71018Zinc200.8ug/L24.110ND (10)UDissolved MetalsAluminum200.7ug/L29.4200ND (200)UAntimony200.8ug/L20.7225.8Arsenic200.8ug/L21.244.7Barium200.7ug/L22.520150Beryllium200.7ug/L20.712ND (2)UBoron200.7ug/L501705,000330,000Cadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L269400820,000Chromium200.8ug/L23.3815^Chromium (VI)218.6ug/L10.3926.71Cobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.964ND (4)UIron200.7ug/L232200ND (200)ULead200.8ug/L20.732ND (2)U

# A-49ND – 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, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationMagnesium200.7ug/L5054010,0006,000,000Manganese200.7ug/L20.512093BMercury1631Eng/L204.8310.184.5Molybdenum200.7ug/L21.640150Nickel200.8ug/L20.8941.8JSelenium200.8ug/L20.624530Silver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000360,000Thallium200.8ug/L20.47212Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.6204.5JVanadium200.8ug/L21.71015^Zinc200.8ug/L24.110ND (10)U

# A-50ND – 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 AnalyticalResults, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia350.1mg/L10.05515.5Nitrate Nitrite as N353.2mg/L500.955300Nitrogen, Total Kjeldahl351.2mg/L40.31423BBiochemical Oxygen Demand5210Bmg/L10.5959.6Chemical Oxygen Demand410.4mg/L1041200560Chloride300.0mg/L5001301,5007,500Sulfate300.0mg/L5001202,50013,000Cyanide, Total4500 CN Emg/L10.020.10.045J,BTotal Dissolved Solids2540Cmg/L14710027,000Total Suspended Solids2540Dmg/L11.147.6Phosphorus, Total365.1mg/L10.0050.050.065BTotal MetalsAluminum200.7ug/L29.420028JAntimony200.8ug/L20.7227Arsenic200.8ug/L21.244.1Barium200.7ug/L22.520160Beryllium200.7ug/L20.712ND (2)UBoron200.7ug/L10033010,000320,000BCadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L269400860,000Chromium200.8ug/L23.3817Cobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.964ND (4)UIron200.7ug/L23220091JLead200.8ug/L20.732ND (2)UMagnesium200.7ug/L1001,10020,0005,600,000BManganese200.7ug/L20.512090BMercury1631Eng/L204.8710.2110Molybdenum200.7ug/L21.640200

# A-51ND – 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 AnalyticalResults, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationNickel200.8ug/L20.8942.7JSelenium200.8ug/L20.624530Silver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000370,000Thallium200.8ug/L20.47214Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.6205.5JVanadium200.8ug/L21.71018Zinc200.8ug/L24.110ND (10)UDissolved MetalsAluminum200.7ug/L29.4200ND (200)UAntimony200.8ug/L20.7226.8Arsenic200.8ug/L21.244Barium200.7ug/L22.520140Beryllium200.7ug/L20.712ND (2)UBoron200.7ug/L501705,000320,000Cadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L269400810,000Chromium200.8ug/L23.3814Chromium (VI)218.6ug/L10.3927.35Cobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.9641.4JIron200.7ug/L232200ND (200)ULead200.8ug/L20.732ND (2)UMagnesium200.7ug/L5054010,0005,600,000Manganese200.7ug/L20.512081BMercury1631Eng/L204.8710.259.9Molybdenum200.7ug/L21.640190Nickel200.8ug/L20.8942.5JSelenium200.8ug/L51.610470

# A-52ND – 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 AnalyticalResults, Miami FortAnalyteMethodUnitsDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationSilver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000340,000Thallium200.8ug/L20.47214Tin200.7ug/L24.8200ND (200)UTitanium200.7ug/L108.2100ND (100)UVanadium200.8ug/L21.71018Zinc200.8ug/L24.110ND (10)U

# 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 Bl ank (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)

Aluminum a 

# 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-sp litter, and two pieces of 5

feet of #24 silicone tubing for sample collect ion 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 Blan k (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 di ssolved 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 #7 3 silicone tubing, T-splitter, six feet of #73 silicone

tubing, and 15 feet of #73 silicone tubing for total and dissolved sample collect ion 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-58ND – 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, Miami FortAnalyteMethodUnitsDilution FactorSample-Specific MDLSample-Specific QLConcentrationTotal MetalsAluminum200.7ug/L29.420040JAntimony200.8ug/L20.722ND (2)UArsenic200.8ug/L21.24ND (4)UBarium200.7ug/L22.520ND (20)UBeryllium200.7ug/L20.712ND (2)UBoron200.7ug/L26.7200130JCadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L26940086JChromium200.8ug/L23.38ND (8)UCobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.964ND (4)UIron200.7ug/L23220045JLead200.8ug/L20.732ND (2)UMagnesium200.7ug/L221400310J,BManganese200.7ug/L20.51204.1J,BMercury1631Eng/L10.240.515.4Molybdenum200.7ug/L21.640ND (40)UNickel200.8ug/L20.894ND (4)USelenium200.8ug/L20.624ND (4)USilver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000ND (10,000)UThallium200.8ug/L20.472ND (2)UTin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.620ND (20)UVanadium200.8ug/L21.710ND (10)UZinc200.8ug/L24.110ND (10)UDissolved MetalsAluminum200.7ug/L29.4200ND (200)UAntimony200.8ug/L20.722ND (2)UArsenic200.8ug/L21.24ND (4)U

# A-59ND – 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, Miami FortAnalyteMethodUnitsDilution FactorSample-Specific MDLSample-Specific QLConcentrationBarium200.7ug/L22.520ND (20)UBeryllium200.7ug/L20.712ND (2)UBoron200.7ug/L26.720035JCadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L269400130JChromium200.8ug/L23.38ND (8)UChromium (VI)218.6ug/L10.392ND (2)UCobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.964ND (4)UIron200.7ug/L232200ND (200)ULead200.8ug/L20.732ND (2)UMagnesium200.7ug/L221400210J,BManganese200.7ug/L20.512011J,BMolybdenum200.7ug/L21.640ND (40)UNickel200.8ug/L20.894ND (4)USelenium200.8ug/L20.624ND (4)USilver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000190JThallium200.8ug/L20.472ND (2)UTin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.620ND (20)UVanadium200.8ug/L21.710ND (10)UZinc200.8ug/L24.110ND (10)U

# A-60ND – 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 AnalyticalResults, Miami FortAnalyteMethodUnitsDilution FactorSample-Specific MDLSample-Specific QLConcentrationTotal MetalsAluminum200.7ug/L29.420014JAntimony200.8ug/L20.722ND (2)UArsenic200.8ug/L21.24ND (4)UBarium200.7ug/L22.520ND (20)UBeryllium200.7ug/L20.712ND (2)UBoron200.7ug/L26.7200110JCadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L269400100JChromium200.8ug/L23.38ND (8)UCobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.964ND (4)UIron200.7ug/L232200ND (200)ULead200.8ug/L20.732ND (2)UMagnesium200.7ug/L221400410BManganese200.7ug/L20.51204.3J,BMercury1631Eng/L10.240.5ND (0.5)UMolybdenum200.7ug/L21.640ND (40)UNickel200.8ug/L20.894ND (4)USelenium200.8ug/L20.6240.76JSilver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000270JThallium200.8ug/L20.472ND (2)UTin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.620ND (20)UVanadium200.8ug/L21.710ND (10)UZinc200.8ug/L24.110ND (10)UDissolved MetalsAluminum200.7ug/L29.4200ND (200)UAntimony200.8ug/L20.722ND (2)U

# A-61ND – 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 AnalyticalResults, Miami FortAnalyteMethodUnitsDilution FactorSample-Specific MDLSample-Specific QLConcentrationArsenic200.8ug/L21.24ND (4)UBarium200.7ug/L22.520ND (20)UBeryllium200.7ug/L20.712ND (2)UBoron200.7ug/L26.7200150JCadmium200.8ug/L21.24ND (4)UCalcium200.7ug/L269400ND (400)UChromium200.8ug/L23.38ND (8)UChromium (VI)218.6ug/L10.392ND (2)U,EstCobalt200.7ug/L21.120ND (20)UCopper200.8ug/L20.964ND (4)UIron200.7ug/L232200ND (200)ULead200.8ug/L20.732ND (2)UMagnesium200.7ug/L221400160J,BManganese200.7ug/L20.51201.4J,BMolybdenum200.7ug/L21.640ND (40)UNickel200.8ug/L20.894ND (4)USelenium200.8ug/L20.624ND (4)USilver200.8ug/L20.592ND (2)USodium200.7ug/L218010,000230JThallium200.8ug/L20.472ND (2)UTin200.7ug/L24.8200ND (200)UTitanium200.7ug/L21.620ND (20)UVanadium200.8ug/L21.710ND (10)UZinc200.8ug/L24.110ND (10)U

# A-62ND – 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 Results, Miami FortAnalyteMethodUnitsDilution FactorSample-Specific MDLSample-Specific QLConcentrationTotal MetalsMercury1631Eng/L10.240.5ND (0.5)U

# A-63ND – 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, Miami FortAnalyteMethodUnitsDilution FactorSample-Specific MDLSample-Specific QLConcentrationTotal MetalsMercury1631Eng/L10.240.5ND (0.5)U

# A-64ND – 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, Miami FortAnalyteMethodUnitsDilution FactorSample-Specific MDLSample-Specific QLConcentrationTotal MetalsMercury1631Eng/L10.240.5ND (0.5)U

# 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