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 April 2012 

EPA Contract No. 68-C-02-095 

Work Assignment 9-29 
i

CONTENTS 

Page 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

4.1 Measured and Calculated Results for Influent to FGD Wastewater Treatment 

System Samples ...................................................................................................4-2

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

5. DATA QUALITY...............................................................................................................5-19

5.1 Analytical Quality Control.................................................................................5-19

5.2 Field Quality Control .........................................................................................5-19

5.2.1 Bottle Blanks..........................................................................................5-19

5.2.2 Equipment Blanks..................................................................................5-20

5.2.3 Field Blanks ...........................................................................................5-20

5.2.4 Field Duplicates .....................................................................................5-22

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

Appendix A: ANALYTICAL RESULTS

Appendix B: DATA REVIEW NARRATIVES 

Appendix C: PICTURES FROM THE SAMPLING EPISODE 

Appendix D: FGD ICP/MS SOP: INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY FOR 

TRACE ELEMENT ANALYSIS IN FLUE GAS DESULFURIZATION WASTEWATERS
ii

LIST OF TABLES 

Page 

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

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

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

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

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

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

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

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

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

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

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

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

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

Table 4-1. Influent to FGD Wastewater Treatment System, Miami Fort................................... 4-6

Table 4-2. Effluent from the FGD Wastewater Treatment System, Miami Fort...................... 4-12

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

Treatment System, Miami Fort...................................................................................... 4-16

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

System, Miami Fort ....................................................................................................... 4-17

Table 5-1. Field Blank Analytical Results, Miami Fort............................................................ 5-23

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

Miami Fort ..................................................................................................................... 5-24

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

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

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

Wastewater Treatment System, Day 2 Analytical Results, Miami Fort......................... A-4
LIST OF TABLES (Continued) 

Page 

iii

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

Wastewater Treatment System, Day 3 Analytical Results, Miami Fort......................... A-6

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

Wastewater Treatment System, Day 4 Analytical Results, Miami Fort......................... A-8

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

Miami Fort .................................................................................................................... A-10

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

Miami Fort .................................................................................................................... A-18

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

Miami Fort .................................................................................................................... A-25

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

Miami Fort .................................................................................................................... A-32

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

Miami Fort .................................................................................................................... A-39

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

Miami Fort .................................................................................................................... A-42

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

Miami Fort .................................................................................................................... A-46

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

Miami Fort .................................................................................................................... A-49

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

Analytical Results, Miami Fort..................................................................................... A-52

Table A-14. Bottle Blank and Equipment Blank Analytical Data, Miami Fort ....................... A-55

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

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

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

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

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

Analytical Results, Miami Fort..................................................................................... A-64

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

Miami Fort .................................................................................................................... A-65
LIST OF TABLES (Continued) 

Page 

iv

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

Miami Fort .................................................................................................................... A-66
v

LIST OF FIGURES 

Page 

Figure 2-1. Chemical Precipitation 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 Influent to the FGD Wastewater Treatment 

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

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

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

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

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

1. INTRODUCTION

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

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

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

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

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

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

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

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

from the chemical precipitation system. 

1.1 Background of Detailed Study

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

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

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

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

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

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

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

1.2 Power Plant Site Selection

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

configurations and characteristics of the plants. 

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

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

its three generating units; 

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

three generating units; 

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

includes the following steps: 

— Equalization and pH adjustment (lime addition), 

— Organosulfide addition, 

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

— Polymer addition, 

— Clarification; 

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

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

 The plant produces a commercial-grade gypsum by-product. 
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 March 1, 2010 as part of the detailed study. The 

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

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

procedures used during the sampling episode. 

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

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

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

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

sample collection activities: 

 Ron Jordan, EPA/EAD; 

 Jezebele Alicea, EPA/EAD; 

 Holly Cannon, ERG; 

 TJ Finseth, ERG; 

 Lydia Lambert, ERG; 

 Jennifer Lewis, ERG; and 

 Jessica Wolford, ERG. 

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

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

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

collected samples on behalf of the plant. 
2-1

2. FACILITY OVERVIEW

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

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

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

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

Ohio River. 

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

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

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

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

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

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

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

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

from the plant, year round. 

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

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

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

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

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

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

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

Miami Fort injects lime into the flue gas between the air heater and the ESP to control the 

sulfur trioxide emissions. 

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

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

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

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

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

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

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

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

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

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

the Ohio River via Outfall 002. 

Unit 6 at Miami Fort has the following configuration: 

 Boiler; 

 Air heater; and 

 ESP. 
2-2

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

 Boiler; 

 SCR system; 

 Air heater; 

 Lime injection; 

 ESP; and 

 FGD scrubber system. 

 

2.1 FGD Scrubber Systems

[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. SAMPLE COLLECTION

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

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

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

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

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

activities. 

3.1 Sampling Points, Sample Collection Methods, and Field Measurements

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

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

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

sampling point locations. 

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

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

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

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

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

sample identification and the sample points for each day. 

The sampling points for this episode were: 

 SP-1 Influent to FGD Wastewater Treatment System; 

 SP-2 Effluent from FGD Wastewater Treatment System; 

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

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

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

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

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

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

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

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

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

with one filling the bottle immediately after the other. 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

protocols. 

3.1.1 Influent to FGD Wastewater Treatment System 

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

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

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

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

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

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

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

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

split samples using composite sampling techniques. 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

from rain during the sample collection. 

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

3.1: 
3-3

 Total and dissolved mercury; 

 Total metals by 200.8; and 

 Total metals by 200.7. 

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

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

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

untouched to allow the solids in the wastewater to settle. 

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

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

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

FGD wastewater treatment system. 

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

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

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

samples were immediately placed on ice after sample collection. 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

FGD wastewater treatment system. 

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

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

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

100 minutes. Approximately 0.5- 2 liters1

 of sample were pumped through the tubing/filter to 

purge the line before collecting samples. 

 

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

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

Section 3.1: 

 Dissolved metals by 200.8; 

 Dissolved metals by 200.7; and 

 Dissolved hexavalent chromium. 

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

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

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

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

 Day 1 – Unit 8; 

 Day 2 – Unit 7; 

 Day 3 – Unit 8; and 

 Day 4 – Unit 7. 

3.1.2 Effluent from FGD Wastewater Treatment System 

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

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

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

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

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

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

collection. 

ERG collected the effluent from FGD wastewater treatment system composite samples 

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

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

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

off the specific sample volumes into the individual sample containers. 

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

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

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

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

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

grab sample for cyanide during each compositing period. 

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

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

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

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

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

wastewater treatment system. 
3-5

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

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

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

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

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

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

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

automatic compositors were calibrated such that they collected 870 mL2

 every hour, so that the 

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

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

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

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

through the sample tap between each individual sample aliquot. 

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

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

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

set-up at the effluent from the bioreactor system. 

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

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

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

procedures at the effluent from FGD wastewater treatment system. 

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

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

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

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

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

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

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

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

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

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

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

for the effluent from FGD wastewater treatment system. 

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

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

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

 

2

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

concentrations in the dissolved metals fractions. 

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

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

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

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

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

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

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

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

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

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

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

from FGD wastewater treatment system. 

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

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

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

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

3.1: 

 Dissolved metals by 200.8; 

 Dissolved metals by 200.7; and 

 Dissolved hexavalent chromium. 

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

After the dissolved metals had been collected, the filter was removed. Once the tubing was 
3-7

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

described in Section 3.1: 

 Total metals by 200.8; and 

 Total metals by 200.7. 

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

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

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

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

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

immediately placed on ice after sample collection. 

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

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

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

sampling episode. 

3.2 List of Analytes and Sample Preservation

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

 Classicals: 

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

— Chemical oxygen demand (COD), 

— Total suspended solids (TSS), 

— Total dissolved solids (TDS), 

— Sulfate, 

— Chloride, 

— Total Kjeldahl nitrogen (TKN), 

— Ammonia as nitrogen, 

— Nitrate/nitrite as nitrogen, 

— Total phosphorus, 

— Total cyanide; 

 Total Metals3

: 

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

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

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

titanium, vanadium, and zinc. 

 Dissolved Metals: 

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

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

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

 

3

 In this report, EPA uses the terms “total metals” and “total recoverable metals” interchangeably. 
3-8

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

concentrations. 

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

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

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

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

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

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

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

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

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

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

hexavalent chromium samples were preserved with ammonium sulfate buffer solution and 

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

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

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

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

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

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

3.3 Plant Operational Data

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

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

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

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

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

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

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

3.4 Deviations from the Sampling and Analysis Plan

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

described below: 

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

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

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

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

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

to reach the desired pH. 

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

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

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

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

FGD scrubber purge to the equalization tank. 
3-9

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

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

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

because the thermometer was misplaced. 

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

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

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

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

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

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

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

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

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

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

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

the bottle. 

 Filtering and purging the influent to FGD wastewater treatment system 

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

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

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

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

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

filter.

 Calibrating the automatic compositors at the effluent from FGD wastewater 

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

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

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

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

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

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

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

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

operating. 

 Influent to FGD wastewater treatment system dissolved metals samples 

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

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

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

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

the Sampling Plan suggested. 
3-10

Table 3-1. Sample Collection Information, Miami Fort

Sampling 

Point 

Number Sampling Point Description 

Type of 

Sample 

Sample 

Collection Date 

Sample Collection Time

Influent to FGD Wastewater Treatment 

System – Day 1 

Grab 7/12/10 0924a and 1149b

Influent to FGD Wastewater Treatment 

System – Day 2 

Grab 7/13/10 1034a and 1247b

Influent to FGD Wastewater Treatment 

System – Day 3 

Grab 7/14/10 0912a and 1143b

SP-1 

Influent to FGD Wastewater Treatment 

System – Day 4 

Grab 7/15/10 0927a and 1137b

Composite 7/12/10 

 7/13/10

0731c 

0841d

Effluent from FGD Wastewater 

Treatment System – Day 1 

Grab 7/12/10 

 7/13/10 

0752e

, 1353f , and 1956 g 

0147 h 

Composite 7/13/10 

 7/14/10 

0730c 

0806d 

Effluent from FGD Wastewater 

Treatment System – Day 2 

Grab 7/13/10 

7/14/10 

0745e

, 1346f , and 1947 g 

0147 h 

Composite 7/14/10 

 7/15/10 

0730c 

0813d 

Effluent from FGD Wastewater 

Treatment System – Day 3 

Grab 7/14/10 

 7/15/10 

0744e

, 1346f , and 1948 g 

0150 h 

Composite 7/15/10 

 7/16/10 

0730c 

0658d 

SP-2 

Effluent from FGD Wastewater 

Treatment System – Day 4 

Grab 7/15/10 

 7/16/10 

0747e

, 1357f , and 1945 g 

0145 h 

Composite 7/13/10 

 7/14/10 

0731c 

0841d

SP-3 Duplicate of Effluent from FGD 

Wastewater Treatment System – Day 2 

Grab 7/13/10 

 7/14/10 

0746e

, 1348f , and 1947 g 

0149 h 

SP-4 Influent to FGD Wastewater Treatment 

System Field Blank 

Grab 7/12/10 0910i and 1138j

Composite 7/12/10 

7/13/10

0640k

0829l

Effluent from FGD Wastewater 

Treatment System Field Blank – Day 1

Grab 7/12/10 0748m

Effluent from FGD Wastewater 

Treatment System Field Blank – Day 2

Grab 7/13/10 0739m

Effluent from FGD Wastewater 

Treatment System Field Blank – Day 3

Grab 7/14/10 0739m

SP-5 

Effluent from FGD Wastewater 

Treatment System Field Blank – Day 4

Grab 7/15/10 0743m

a

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

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

b

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

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

c Started compositor. 
3-11

d

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

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

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

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

f

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

g

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

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

i

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

blank samples. 

j

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

field blank samples. 

k

 Filled 20-L field blank carboy 

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

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

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

Table 3-2. Sample Collection at Miami Fort

Sampling 

Point 

Number Sampling Point Name 

Total Metals 

(EPA Method 200.8 with 

collision cell)

Total Metals 

(EPA Method 200.7) 

Dissolved Metals 

(EPA Method 200.8 with 

collision cell) 

Dissolved Metals 

(EPA Method 200.7) 

Total Mercury 

Dissolved Mercury 

Hexavalent Chromium 

BOD

5

SP-1 Influent to the FGD Wastewater 

Treatment System 

4 4 4 4 4 4 4 4 

SP-2 Effluent from the FGD Wastewater 

Treatment System 

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

SP-3 Duplicate of Effluent from the FGD 

Wastewater Treatment System 

1 1 1 1 1 1 1 1 

SP-4 Field Blank for Influent to the FGD 

Wastewater Treatment System 

1 1 1 1 1 1 

SP-5 Field Blank for Effluent from the 

FGD Wastewater Treatment System 

1 1 1 1 4 1 

Total Number of Samples 11+1QC 11+1QC 11+1QC 11+1QC 14+1QC 9+1QC 11+1QC 9+1QC 9+a Group I includes total suspended solids (TSS), total dissolved solids (TDS), sulfate, and chloride. b Group II includes ammonia as nitrogen, nitrate/nitrite as nitrogen, total Kjeldahl nitrogen (TKN), chemical oxygen demand (COD), and total phosph
3-13 

Table 3-3. Field Measurements, Miami Fort

Temperature (°C) pH (S.U.) 

Sampling 

Point 

Number 

Sampling Point 

Description Date Time Thermometer Probe Meter a Strips 

Waste Stream 

Flow Rate 

(GPM)b 

Influent to FGD Wastewater Treatment System – Day 1

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

yellow color and solids. No detectetotal cyanide grab

Influent to FGD Wastewater Treatment System – Day 2 

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

yellow color. No oxidants in total c

Influent to FGD Wastewater Treatment System – Day 3 

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

yellow color. No oxidants in total c

SP-1 

Influent to FGD Wastewater Treatment System – Day 4 

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

cyanide grab. 

7/12/10 0755 43 41.7 8.7 9.5 246.77/12/10 1355 43 41 8.63 9 0.0 7/12/10 1956 42 39.9 8.44 9 243.9 

Effluent from FGD Wastewater Treatment System – Day 1

7/13/10 0151 44 42.2 8.56 9 0.0 

Samples were clecolor and did not No detected sulficyanide grab.

7/13/10 0750 44 8.56 9 0.0 7/13/10 1350 44 42 8.62 9 248.2 7/13/10 2005 45 42.5 8.46 9 0.0 

Effluent from FGD Wastewater Treatment System – Day 2 

7/14/10 0154 42 39.2 8.62 9 244.5 

Samplers noted thyellow color. No oxidants in total c

7/14/10 0746 43 40.1 8.55 9 0.0 7/14/10 1347 44.5 42.5 8.26 9 0.0 7/14/10 1953 44 42.2 8.66 9 0.0 

Effluent from FGD Wastewater Treatment System – Day 3 

7/15/10 0154 43 40.9 8.38 9 0.0 

Samples were cledid not have any detected sulfides cyanide grab.

7/15/10 0749 42 40 8.61 9 0.0 7/15/10 1358 44 42 8.49 9 251.3 7/15/10 1950 45 42.3 8.53 9 0.0 

SP-2 

Effluent from FGD Wastewater Treatment System – Day 4 

7/16/10 0150 45 42.4 8.55 9 250.0 

Samples were cledid not have any detected sulfides cyanide grab.
3-14 

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

and 10.0. 

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

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

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

rate of the FGD scrubber purge entering the Equalization tank. 
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 Wastewater Treatment System Field Blank - Day 1 

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

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

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

71754 SP-5, Day 4 Effluent to FGD Wastewater Treatment System Field Blank - Day 4 
3-16

Table 3-5. Analytical Methods, Miami Fort

Parameter Method Number 

Classicals

Biochemical oxygen demand (BOD5) SM 5210 B 

Chemical oxygen demand (COD) EPA 410.4 

Total suspended solids (TSS) SM 2540 D 

Total dissolved solids (TDS) SM 2540 C 

Sulfate EPA 300.0 

Chloride EPA 300.0 

Ammonia as nitrogen EPA 350.1 

Nitrate/nitrate as nitrogen EPA 353.2 

Total Kjeldahl nitrogen (TKN) EPA 351.2 

Total phosphorus EPA 365.1 

Total cyanide SM 4500 CN E 

Total and Dissolved Metals

Mercury EPA 1631E 

Hexavalent chromium (dissolved only) EPA 218.6 

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

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

EPA 200.8 with collision cell1

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

molybdenum, sodium, tin, and titanium 

EPA 200.7 

1

 EPA used an SOP developed specifically for analyzing FGD wastewater (see Appendix D).
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 

BOD5 One 1-L plastic 

bottle 

One 1-L plastic 

bottle 

≤6C 

Group I a One 1-L plastic 

bottles 

One 1-L plastic 

bottles 

≤6C 

Group II b Two 1-L plastic 

bottles 

Two 1-L plastic 

bottles 

H2SO4 to pH <2 S.U., ≤6C 

Total cyanide One 1-L plastic 

bottle 

One 1-L plastic 

bottles 

Dilution until sulfide is not detected, 

NaAsO2 until total chlorine is not 

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

≤6C 

Metals 

Total metals (EPA Method 200.8 with 

collision cell) 

One 500-mL 

plastic bottle 

No additional 

volume needed 

None 

(acid preserve at laboratory) 

Total metals (EPA Method 200.7) One 500-mL 

plastic bottle 

No additional 

volume needed 

None 

(acid preserve at laboratory) 

Dissolved metals (EPA Method 200.8 

with collision cell) 

One 500-mL 

plastic bottle 

No additional 

volume needed 

0.45-μm filter (performed in field) 

(acid preserve at laboratory) 

Dissolved metals (EPA Method 200.7) One 500-mL 

plastic bottle 

No additional 

volume needed 

0.45-μm filter (performed in field) 

(acid preserve at laboratory) 

Total mercury: 

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 

None 

(acid preserve at laboratory) 

Dissolved mercury: 

Manual composite grab samples Four 125-mL 

glass bottle 

No additional 

volume needed 

Influent samples One 250-mL 

glass bottle 

No additional 

volume needed 

None 

(filter and acid preserve at 

laboratory) 

Hexavalent chromium One 250-mL 

plastic bottle 

No additional 

volume needed 

0.45-μm filter (performed in field) 

Ammonium sulfate buffer to 

pH 9.3 – 9.7 S.U., ≤6C 

a

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

 Group II includes ammonia as nitrogen, COD, nitrate/nitrite as nitrogen, TKN, and total phosphorus.
3-18 

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 H2SO4 7 <2 250 

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

(NH4)2SO4

Buffer 

71741 Hexavalent Chromium 7/12/10 6.5 6.8 100 

NH4OH 6.8 9.5 25 

(NH4)2SO4

Buffer 

71750 Hexavalent Chromium 7/12/10 6.5 8.5 100 

NH4OH 8.5 9.5 4 

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

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

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

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

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

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

(NH4)2SO4

Buffer 

71742 Hexavalent Chromium 7/13/10 6.5 7.1 100 

NH4OH 7.1 9.7 67 

(NH4)2SO4

Buffer 

71745 Hexavalent Chromium 7/13/10 8.7 8.7 100 

NH4OH 8.7 9.3 10 

(NH4)2SO4

Buffer 

71751 Hexavalent Chromium 7/13/10 6.5 8.5 50 

NH4OH 8.5 9.7 20 

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

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

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

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

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

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

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

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

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

(NH4)2SO4

Buffer 

71743 Hexavalent Chromium 7/14/10 6.5 7.1 100 

NH4OH 7.1 9.7 60 

(NH4)2SO4

Buffer 

71746 Hexavalent Chromium 7/14/10 8.7 8.7 100 

NH4OH 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) 

(NH4)2SO4

Buffer 

71749 Hexavalent Chromium 7/14/10 8.7 8.7 100 

NH4OH 8.7 9.7 15 

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

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

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

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

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

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

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

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

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

(NH4)2SO4

Buffer 

71744 Hexavalent Chromium 7/15/10 6.5 7.1 100 

NH4OH 7.1 9.5 120 

(NH4)2SO4

Buffer 

71747 Hexavalent Chromium - QC 7/15/10 8.7 8.7 100 

NH4OH 8.7 9.7 30 

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

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

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

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

(NH4)2SO4

Buffer 

71748 Hexavalent Chromium 7/16/10 8.7 8.7 100 

NH4OH 8.7 9.5 30 
3-20 

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

Unit ID Boiler Type 

Capacity 

(MW) 

Electricity Production 

(MW) 

(or Percent Capacity %)

SCR 

(No, On, Off) 

Particulate Control System 

(HS/CS ESP, or BH) 

7 Opposed Firing 550 538 MW On CS ESP 

8 Opposed Firing 550 545 MW On CS ESP 

CS ESP – Cold-side electrostatic precipitator. 
3-21 

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

Unit ID 

Wet FGD 

System (Yes/No) 

Type of 

Scrubber 

Forced 

Oxidation 

(Yes/No) Sorbent 

Additives (DBA, 

formic acid, 

etc.) 

FGD Make-up 

Water Source 

SO2 Rem

Percen

7 Yes Spray Yes Limestone None Ohio River 97.4 8 Yes Spray Yes Limestone None Ohio River 96.9 
3-22

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

Day of 

Sampling Unit ID Coal Type 

Amount of Coal 

Used During Day 

of Sampling 

(tpd) 

Source of Coal 

(Coal Region 

and/or State) 

Percent 

Sulfur in 

Coal 

(%) 

Chlorine Content of 

Coal 

(ppm) 

7 Bituminous 3635 Tons 

Northern 

Appalachian/ 

Illinois Basin 

3.36% 

(Dry) 1070 ppm (Dry) 

1 

8 Bituminous 5331 Tons Northern 

Appalachian 

4.05% 

(Dry) 574 ppm (dry) 

7 Bituminous 4865 Tons 

Northern 

Appalachian/ 

Illinois Basin 

3.44% 

(Dry) 635 ppm (Dry) 

2 

8 Bituminous 3678 Tons Northern 

Appalachian 

4.04% 

(Dry) 582 ppm (Dry) 

7 Bituminous 5417 Tons 

Northern 

Appalachian/ 

Illinois Basin 

3.77% 

(Dry) 354 ppm (Dry) 

3 

8 Bituminous 5165 Tons Northern 

Appalachian 

4.10% 

(Dry) 569 ppm (Dry) 

7 Bituminous 6937 Tons 

Northern 

Appalachian/ 

Illinois Basin 

3.48% 

(Dry) 584 ppm (Dry) 

4 

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

Scrubber Slurry 

Blowdown Flow Rate 

Day of 

Sampling 

FGD 

System ID 

Associated 

Unit IDs 

Flow Rate 

(gpm) Duration 

Scrubber 

Slurry 

Percent 

Solids 

Time of 

Dewatering 

During 

Sampling Day 

Percent 

Filtrate 

Recycled 

Back to 

Scrubber 

7 7 CBI CBI CBI CBI CBI 

1 

8 8 CBI CBI CBI CBI CBI 

7 7 CBI CBI CBI CBI CBI 

2 

8 8 CBI CBI CBI CBI CBI 

7 7 CBI CBI CBI CBI CBI 

3 

8 8 CBI CBI CBI CBI CBI 

7 7 CBI CBI CBI CBI CBI 

4 

8 8 CBI CBI CBI CBI CBI 
3-24 

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

Scrubber Purge Chemical Usage 

Day of Sampling Flow Rate (gpm) b Duration Lime a Ferric Chloride 

Organosulfide: 

Nalmet 1689 c

Polyme

776

1 CBI CBI CBI CBI CBI C2 CBI CBI CBI CBI CBI C3 CBI CBI CBI CBI CBI C4 CBI CBI CBI CBI CBI C

a Lime usage is approximately [CBI information has been removed] lbs/day. b Scrubber purge flow is a calculated value based on pump discharge pressure. c Organosulfide and polymer usage are calculated values based on dosing set points. 
4-1 

4. LABORATORY ANALYTICAL RESULTS AND DISCUSSION

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

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

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

SP-1. Section 4.2 presents the laboratory analytical data for the influent to and effluent from the 

FGD wastewater treatment system. 

The total and dissolved mercury samples were analyzed by Frontier Global Sciences 

(Frontier). The dissolved mercury samples were vacuum filtered through acid-cleaned cellulose 

nitrate membrane filters contained in disposable polystyrene filtration units at the Frontier 

laboratory under clean room conditions on the day of sample receipt. Samples with elevated 

solids were filtered through multiple filtration units until the entire sample was filtered. The 

mercury samples were subjected to a room temperature bromine monochloride digestion prior to 

analysis using a method-compliant bubbler system. 

For the total and dissolved mercury samples from SP-2 and SP-3, EPA collected four 

individual grab samples that were composited by Frontier and analyzed as one sample. Frontier 

composited these samples by combining the entire sample bottle for each of four individual grab 

samples prior to digestion and analysis; however, if one or more of the grab samples were 

received with limited volume, equal volumes from each individual grab sample were combined 

for the composite analysis. 

The total and dissolved metals by EPA Method 200.7 were analyzed by TestAmerica 

Laboratories – Denver (TestAmerica). As described in Section 3, the dissolved metals samples 

were filtered in the field. The dissolved metals samples were preserved to a pH <2 at least 24 

hours prior to being subjected to a heated nitric acid digestion according to SW846 Method 

3005A. The total metals samples were preserved to a pH <2 at least 24 hours prior to being 

subjected to a heated nitric acid digestion according to SW846 Method 3010A. 

The total and dissolved metals by EPA Method 200.8 were also analyzed by 

TestAmerica. Similar to the metals analyzed by EPA Method 200.7, the dissolved metals 

analyzed by EPA Method 200.8 were also filtered in the field. The total and dissolved metals 

samples were preserved to a pH <2 at least 24 hours prior to being subjected to a closed vessel, 

heated nitric acid and hydrochloric acid digestion according to EPA Method 1638. 

The classical analytes were analyzed by TestAmerica and were digested, prepared, and 

analyzed according to the methods specified in Table 3-5. 

Appendix A provides all analytical results for all samples collected at Miami Fort, 

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

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

For EPA Method 200.7, some of the quantitation limits provided are TestAmerica’s 

standard routine quantitation limits; these limits are used for most of TestAmerica’s projects and 

were not optimized for FGD wastewater or the EPA sampling program. The quantitation limits 

are established using not only the results of the MDL studies, but also are based on the results of 

TestAmerica’s long term blank studies. If the typical background blank levels for a given 

element are variable or frequently elevated, then the quantitation limit may be raised to prevent 
4-2 

the reporting of false positives. This resulted in some analytes (e.g., manganese, sodium) having 

a QL/MDL ratio greater than five, where three to five is the normal range. 

4.1 Measured and Calculated Results for Influent to FGD Wastewater Treatment 

System Samples

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

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

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

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

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

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

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

results. This biphasic approach provides EPA with measured or calculated pollutant 

concentrations for the following phases of the sample: 

 Aqueous phase; 

 Solid phase; and 

 Total sample. 

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

and the mercury laboratory, Frontier, used two different approaches for the biphasic analysis. 

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

analyses. 

Metals and Classicals Analyses 

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

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

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

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

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

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

Once the FGD influent samples were separated into solid and aqueous phases, the 

aqueous portion was analyzed using EPA Method 200.7 or Method 200.8, depending on the 

analyte. The solid portion of the samples associated with the 200.7 analysis were prepared and 

analyzed according to SW846 Method 6010B, while the solid portion of the samples associated 

with the 200.8 analysis were prepared and analyzed according to SW846 Method 6020. 

For solid phase analyses of nitrate/nitrite and ammonia, the analytical methods (i.e., EPA 

Method 353.2 and EPA Method 350.1, respectively) do not include procedures for analyzing 

solid solids. Therefore, TestAmerica determined the concentration of nitrate/nitrite and 

ammonia in the FGD influent solid samples by performing a deionized leach of the solid sample. 

TestAmerica achieved this by placing a specified amount of the solid sample with an amount of 

deionized water and shaking the mixture for one hour. TestAmerica than separated the leachate 

from the solids using a centrifuge and then preserved the leachate to a pH <2 S.U. and analyzed 

the leachate according the specified methods. 
4-3 

TestAmerica also dried the solids prior to analysis, so the solid concentration is on a dryweight basis. To calculate the total sample concentration from the solid and aqueous phase 

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

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

concentrations for the sample. 

Sample

Filtrate Filtrate Solid Solid

V

(C V ) (C Wt ) TotalSampleConcentration     (4-1) 

where: 

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

VFiltrate = volume of the filtrate; 

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

WtSolid = weight of the solids in the sample; and 

VSample = volume of the original sample. 

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

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

Kjeldahl nitrogen (TKN), and total phosphorus. 

Mercury Analyses 

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

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

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

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

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

solid and aqueous phases separately. 

Once the FGD influent samples were separated into solid and aqueous phases, the 

aqueous portion was analyzed using EPA Method 1631E, just like all the other mercury samples. 

The solid portion was analyzed according to the Appendix to 1631: Total Mercury in Tissue, 

Sludge, Sediment, and Soil by Acid Digestion and BrCl Oxidation, which was associated with 

EPA Method 1631B. Frontier digested the samples with aqua regia (HCl/HNO3) and then 

analyzed the samples using EPA Method 1631E. 

Frontier did not dry the solids prior to analysis, so the solid concentration is on a wetweight basis. To calculate the total sample concentration from the solid and aqueous phase 

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

and filtrate volume. EPA used Equation 4-1 to calculate the individual total mercury 

concentrations for the sample. 

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

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

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

rounded to three significant figures. 
4-4 

4.2 FGD Wastewater Treatment System

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

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

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

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

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

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

(SP-2). 

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

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

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

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

sample-specific quantitation limit in parentheses. 

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

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

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

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

difference (RPD). 

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

averages, ERG used the following methodology: 

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

together; 

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

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

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

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

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

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

the average of the sample-specific quantitation limits; and 

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

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

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

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

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

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

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

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

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

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

system. 
4-5 

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

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

system (SP-2), and the duplicate of the effluent from the FGD wastewater treatment system (SP3) sample analyses, including J-values. 
4-6 

Note: The total metals results and the results for certain classical analytes (i.e., ammonia as nitrogen, chloride, nitrate/nitrite, sulfate, total cyanide, TKrepresent the total result that was calculated based on the results of the solid and aqueous phase of the samples. See Section 4.1 for more details. Samp

‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘S( )’ are qualifiers associated with the soli

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

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

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

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

B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. Min – Minimum value P – Sample was not preserved immediately following collection. V – Serial dilution is not within control limits. 

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

Influent to FGD Wastewater Treatment System (SP-1) 

Analyte Units Method Day 1 Day 2 Day 3 

Classicals Ammonia mg/L 350.1 5.21 

F(H, P, Est) – 

S(H, P, Est) 6.12 

F(P, Est) – 

S(H, P, Est) 7.90 

F(P, Est) – S(P, 

Est) 6.06 

Nitrate Nitrite as N mg/L 353.2 71.7 

F(H, P, Est) – 

S(H, P, Est) 86.6 

F(P, Est) – 

S(H, P, Est) 74.9 

F(P, Est) – S(P, 

Est) 82.8 

Nitrogen, Total Kjeldahl mg/L 351.2 40.5 

F(H, P, Est) – 

S(H, P, Est) 52.6 

F(H, P, Est) – 

S(H, P, Est) 47.6 

F(P, Est) – 

S(P, Est) 40.8 

Biochemical Oxygen Demand mg/L 5210B NQ (2.50) NQ (2.50) 3.30 ND (2.00Chemical Oxygen Demand mg/L 410.4 620 670 910 720 Chloride mg/L 300.0 9,000 9,800 9,600 9,600 Sulfate mg/L 300.0 18,000 21,000 32,000 24,000 Cyanide, Total mg/L 

4500 

CN E 0.255 

F(B, H, P, Est) – 

S(B, H, P) 0.644 

F(B, H, P, Est) – 

S(B, H, P) 2.05 

F(B, H, P, Est) – 

S(B, H, P) 0.198 

F

Total Dissolved Solids mg/L 2540C 56,000 68,000 59,000 50,000 Total Suspended Solids mg/L 2540D 16,000 30,000 20,000 19,000 Phosphorus, Total mg/L 365.1 0.476 

F(B, H, P) – S(H, 

P, Est) 7.68 

F(B, H, P) – S(H, 

P, Est) 

NQ 

(0.191) 

F(B, P) – 

S(P) 6.52 
4-7 

Note: The total metals results and the results for certain classical analytes (i.e., ammonia as nitrogen, chloride, nitrate/nitrite, sulfate, total cyanide, TKrepresent the total result that was calculated based on the results of the solid and aqueous phase of the samples. See Section 4.1 for more details. Samp

‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘S( )’ are qualifiers associated with the soli

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

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

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

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

B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. Min – Minimum value P – Sample was not preserved immediately following collection. V – Serial dilution is not within control limits. 

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

Influent to FGD Wastewater Treatment System (SP-1) 

Analyte Units Method Day 1 Day 2 Day 3 

Total Metals Aluminum ug/L 

200.7, 

6010B 561,000 626,000 F(B) 687,000 F(B) – S(4) 497,000 

Antimony ug/L 

200.8, 

6020 NQ (10.3) NQ (11.0) NQ (13.4) S(4, Min) NQ (9.47

Arsenic ug/L 

200.8, 

6020 937 896 1,310 695 

Barium ug/L 

200.7, 

6010B 7,640 

F(F, Min) – 

S(B) 7,510 S(B) 10,400 S(B) 6,410 

Beryllium ug/L 

200.7, 

6010B 27.6 28.3 41.8 22.4 

Boron ug/L 

200.7, 

6010B 624,000 F(B, 4) – S(B) 803,000 F(B) – S(B) 844,000 

F(B) – S(B, 

4) 762,000 

Cadmium ug/L 

200.8, 

6020 342 426 522 396 

Calcium ug/L 

200.7, 

6010B 1,340,000 S(B) 1,350,000 

F(B) – 

S(B) 2,060,000 

F(B) – 

S(B, 4) 1,140,00

Chromium ug/L 

200.8, 

6020 4,000 S(^) 4,460 S(^) 4,430 S(4, ^) 3,640 

Cobalt ug/L 

200.7, 

6010B 425 503 632 459 
4-8 

Note: The total metals results and the results for certain classical analytes (i.e., ammonia as nitrogen, chloride, nitrate/nitrite, sulfate, total cyanide, TKrepresent the total result that was calculated based on the results of the solid and aqueous phase of the samples. See Section 4.1 for more details. Samp

‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘S( )’ are qualifiers associated with the soli

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

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

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

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

B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. Min – Minimum value P – Sample was not preserved immediately following collection. V – Serial dilution is not within control limits. 

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

Influent to FGD Wastewater Treatment System (SP-1) 

Analyte Units Method Day 1 Day 2 Day 3 

Copper ug/L 

200.8, 

6020 1,350 1,520 1,670 1,210 

Iron ug/L 

200.7, 

6010B 911,000 965,000 1,030,000 S(4) 766,000 

Lead ug/L 

200.8, 

6020 756 842 887 651 

Magnesium ug/L 

200.7, 

6010B 7,870,000 F(4) 9,210,000 11,800,000 9,010,00

Manganese ug/L 

200.7, 

6010B 93,100 F(B, 4) 105,000 F(B) 157,000 F(B) 96,000 

Mercury ng/L 

1631E, 

FGS069 166,000 148,000 231,000 44,000 

Molybdenum ug/L 

200.7, 

6010B 506 540 641 406 

Nickel ug/L 

200.8, 

6020 2,580 F(4) 2,980 3,610 2,560 

Selenium ug/L 

200.8, 

6020 3,400 F(V, 4, MI) 3,650 3,330 2,920 

Silver ug/L 

200.8, 

6020 NQ (6.06) F(F, Min) NQ (6.50) NQ (7.47) S(F, Min) NQ (5.64
4-9 

Note: The total metals results and the results for certain classical analytes (i.e., ammonia as nitrogen, chloride, nitrate/nitrite, sulfate, total cyanide, TKrepresent the total result that was calculated based on the results of the solid and aqueous phase of the samples. See Section 4.1 for more details. Samp

‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘S( )’ are qualifiers associated with the soli

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

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

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

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

B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. Min – Minimum value P – Sample was not preserved immediately following collection. V – Serial dilution is not within control limits. 

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

Influent to FGD Wastewater Treatment System (SP-1) 

Analyte Units Method Day 1 Day 2 Day 3 

Sodium ug/L 

200.7, 

6010B 355,000 427,000 502,000 404,000 

Thallium ug/L 

200.8, 

6020 52.8 S(B) 56.4 S(B) 93.5 S(B) 46.2 

Tin ug/L 

200.7, 

6010B NQ (403) NQ (430) NQ (460) NQ (411

Titanium ug/L 

200.7, 

6010B 2,020 2,050 4,140 S(F Max) 1,820 

Vanadium ug/L 

200.8, 

6020 4,010 4,220 4,440 S(4) 3,270 

Zinc ug/L 

200.8, 

6020 13,900 F(B, 4) 16,300 F(B) 20,200 F(B) – S(4) 14,500 

Dissolved Metals Aluminum ug/L 200.7 4,200 B 2,400 B 29,000 B 2,800 Antimony ug/L 200.8 3.40 3.30 3.70 2.80 Arsenic ug/L 200.8 4.40 4.90 6.60 5.50 Barium ug/L 200.7 140 140 180 150 Beryllium ug/L 200.7 4.70 4.10 12.0 4.60 Boron ug/L 200.7 650,000 B 690,000 B 820,000 730,000 Cadmium ug/L 200.8 340 390 510 420 Calcium ug/L 200.7 690,000 670,000 620,000 640,000 
4-10 

Note: The total metals results and the results for certain classical analytes (i.e., ammonia as nitrogen, chloride, nitrate/nitrite, sulfate, total cyanide, TKrepresent the total result that was calculated based on the results of the solid and aqueous phase of the samples. See Section 4.1 for more details. Samp

‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘S( )’ are qualifiers associated with the soli

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

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

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

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

B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. Min – Minimum value P – Sample was not preserved immediately following collection. V – Serial dilution is not within control limits. 

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

Influent to FGD Wastewater Treatment System (SP-1) 

Analyte Units Method Day 1 Day 2 Day 3 

Chromium ug/L 200.8 

ND 

(8.00) ND (8.00) ND (8.00) ND (8.00

Chromium (VI) ug/L 218.6 

ND 

(10.0) ND (10.0) ND (10.0) ND (10.0

Cobalt ug/L 200.7 340 360 490 380 Copper ug/L 200.8 54.0 50.0 110 55.0 Iron ug/L 200.7 NQ (200) ND (200) NQ (200) ND (200Lead ug/L 200.8 

ND 

(2.00) ND (2.00) ND (2.00) ND (2.00

Magnesium ug/L 200.7 7,900,000 8,400,000 11,000,000 8,900,00Manganese ug/L 200.7 100,000 100,000 170,000 110,000 Mercury ng/L 1631E 1,110 1,830 1,600 1,990 Molybdenum ug/L 200.7 120 110 130 90.0 Nickel ug/L 200.8 1,700 1,700 2,500 2,000 Selenium ug/L 200.8 290 330 330 300 Silver ug/L 200.8 

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 Thallium ug/L 200.8 25.0 26.0 49.0 26.0 Tin ug/L 200.7 NQ (200) ND (200) ND (200) ND (200
4-11 

Note: The total metals results and the results for certain classical analytes (i.e., ammonia as nitrogen, chloride, nitrate/nitrite, sulfate, total cyanide, TKrepresent the total result that was calculated based on the results of the solid and aqueous phase of the samples. See Section 4.1 for more details. Samp

‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘S( )’ are qualifiers associated with the soli

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

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

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

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

B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. Min – Minimum value P – Sample was not preserved immediately following collection. V – Serial dilution is not within control limits. 

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

Influent to FGD Wastewater Treatment System (SP-1) 

Analyte Units Method Day 1 Day 2 Day 3 

Titanium ug/L 200.7 

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 Zinc ug/L 200.8 6,300 6,200 11,000 7,600 
4-12 

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

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

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

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

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

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

Effluent from the FGD Wastewater System 

Analyte Units Method Day 1 Day 2 Day 3 Day 4 

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

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

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

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

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

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

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

Effluent from the FGD Wastewater System 

Analyte Units Method Day 1 Day 2 Day 3 Day 4 

Calcium ug/L 200.7 890,000 850,000 840,000 800,000 Chromium ug/L 200.8 17.0 16.5 14.0 16.0 Cobalt ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND (20.0) Copper ug/L 200.8 ND (4.00) ND (4.00) ND (4.00) ND (4.00) Iron ug/L 200.7 NQ (200) NQ (200) 260 NQ (200) Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.00) Magnesium ug/L 200.7 5,600,000 B 5,550,000 5,500,000 B,F,4 5,700,000 Manganese ug/L 200.7 170 B 89.0 280 B 100 Mercury ng/L 1631E 101 105 148 165 Molybdenum ug/L 200.7 220 200 180 150 Nickel ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.00) Selenium ug/L 200.8 560 535 800 4 480 Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) F,Min ND (2.00) Sodium ug/L 200.7 370,000 365,000 360,000 4 360,000 Thallium ug/L 200.8 14.0 14.0 14.0 12.0 Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (200) Titanium ug/L 200.7 ND (20.0) NQ (20.0) NQ (20.0) NQ (20.0) Vanadium ug/L 200.8 16.0 17.5 16.0 18.0 Zinc ug/L 200.8 ND (10.0) ND (10.0) ND (10.0) ND (10.0) Dissolved Metals
4-14 

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

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

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

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

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

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

Effluent from the FGD Wastewater System 

Analyte Units Method Day 1 Day 2 Day 3 Day 4 

Aluminum ug/L 200.7 ND (200) NQ (200) ND (200) ND (200) Antimony ug/L 200.8 7.80 6.80 6.60 5.80 Arsenic ug/L 200.8 4.80 < 3.00 4.80 4.70 Barium ug/L 200.7 140 145 150 150 Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.00) Boron ug/L 200.7 300,000 B 325,000 320,000 F,4 330,000 Cadmium ug/L 200.8 ND (4.00) ND (4.00) ND (4.00) ND (4.00) Calcium ug/L 200.7 880,000 835,000 840,000 4 820,000 Chromium ug/L 200.8 14.0 14.0 15.0 ^ 15.0 Chromium (VI) ug/L 218.6 7.04 7.34 7.61 6.71 Cobalt ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND (20.0) Copper ug/L 200.8 NQ (4.00) NQ (4.00) ND (4.00) ND (4.00) Iron ug/L 200.7 ND (200) ND (200) ND (200) ND (200) Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.00) Magnesium ug/L 200.7 5,500,000 5,750,000 5,600,000 F,4 6,000,000 Manganese ug/L 200.7 160 B 84.0 250 B 93.0 Mercury ng/L 1631E 49.7 61.5 71.3 84.5 Molybdenum ug/L 200.7 210 195 170 150 Nickel ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.00) Selenium ug/L 200.8 560 495 640 4 530 
4-15 

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

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

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

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

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

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

Effluent from the FGD Wastewater System 

Analyte Units Method Day 1 Day 2 Day 3 Day 4 

Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) F,Min ND (2.00) Sodium ug/L 200.7 350,000 350,000 350,000 360,000 Thallium ug/L 200.8 14.0 14.0 13.0 12.0 Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (200) Titanium ug/L 200.7 ND (50.0) NQ (60.0) NQ (20.0) NQ (20.0) Vanadium ug/L 200.8 16.0 17.0 14.0 ^ 15.0 Zinc ug/L 200.8 ND (10.0) ND (10.0) ND (10.0) ND (10.0) 
4-16 

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

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

Analyte Units Method

Influent to FGD 

Wastewater Treatment 

System (SP-1)

4-Day Average

Effl

FGD Waste

Syst

4-Da

ClassicalsAmmonia mg/L 350.1 6.32 Nitrate Nitrite as N mg/L 353.2 79.0 Nitrogen, Total Kjeldahl mg/L 351.2 45.4 Biochemical Oxygen Demand mg/L 5210B < 1.70 Chemical Oxygen Demand mg/L 410.4 730 Chloride mg/L 300.0 9,500 Sulfate mg/L 300.0 23,800 Cyanide, Total mg/L 4500 CN E 0.787 < Total Dissolved Solids mg/L 2540C 58,300 Total Suspended Solids mg/L 2540D 21,300 Phosphorus, Total mg/L 365.1 < 3.69 
4-17 

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

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

value. 

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

Influent to FGD 

Wastewater Treatment

System (SP-1)

4-Day Average

Efflu

FGD Waste

Syst

4-Da

Analyte Units Method Total Dissolved Total 

MetalsAluminum ug/L 200.7 593,000 9,600 < 178 Antimony ug/L 200.8 NQ (11.0) 3.30 6.31 Arsenic ug/L 200.8 960 5.35 4.61 Barium ug/L 200.7 7,990 153 154 Beryllium ug/L 200.7 30.0 6.35 ND (2.00) Boron ug/L 200.7 758,000 723,000 318,000 Cadmium ug/L 200.8 422 415 ND (4.00) Calcium ug/L 200.7 1,470,000 655,000 845,000 Chromium ug/L 200.8 4,130 ND (8.00) 15.9 Chromium (VI) ug/L 218.6 NA ND (10.0) NA Cobalt ug/L 200.7 505 393 ND (20.0) Copper ug/L 200.8 1,440 67.3 ND (4.00) Iron ug/L 200.7 918,000 NQ (200) < 140 Lead ug/L 200.8 784 ND (2.00) ND (2.00) Magnesium ug/L 200.7 9,470,000 9,050,000 5,590,000 Manganese ug/L 200.7 113,000 120,000 160 Mercury ng/L 1631E 147,000 1,630 130 Molybdenum ug/L 200.7 523 113 188 Nickel ug/L 200.8 2,930 1,980 NQ (4.00) Selenium ug/L 200.8 3,330 313 594 Silver ug/L 200.8 NQ (6.42) ND (2.00) ND (2.00) Sodium ug/L 200.7 422,000 405,000 364,000 Thallium ug/L 200.8 62.2 31.5 13.5 Tin ug/L 200.7 NQ (426) NQ (200) ND (200) 
4-18 

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

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

value. 

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

Influent to FGD 

Wastewater Treatment

System (SP-1)

4-Day Average

Efflu

FGD Waste

Syst

4-Da

Analyte Units Method Total Dissolved Total 

Titanium ug/L 200.7 2,510 NQ (20.0) NQ (20.0) Vanadium ug/L 200.8 3,990 15.3 16.9 Zinc ug/L 200.8 16,200 7,780 ND (10.0) 
5-19 

5. DATA QUALITY

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

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

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

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

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

QC standard checks. 

5.1 Analytical Quality Control

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

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

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

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

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

5.2 Field Quality Control

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

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

5.2.1 Bottle Blanks 

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

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

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

Frontier collected the bottle blanks for the metals sample bottles by filling the precleaned 

bottle with reagent water, preserving the sample with nitric acid to a pH <2 S.U. Frontier then 

analyzed the samples using EPA Method 1638. 

Frontier collected the bottle blanks for the mercury sample bottles by filling the 

precleaned bottle with reagent water, preserving the sample with bromine monochloride. Frontier 

then analyzed the samples using EPA Method 1631E. 

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

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

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

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

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

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

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

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

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

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

ug/L); therefore, this contamination did not affect the results of the sampling episode. Appendix 
5-20 

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

used to collect the metals and mercury samples. 

5.2.2 Equipment Blanks 

EPA collects equipment blanks to evaluate possible contamination from the equipment 

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

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

equipment was introducing contamination. In addition, Frontier collected and analyzed 

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

equipment supplied for the episode. 

Frontier collected the equipment blanks for the capsule filters and fabricated tubing sets 

by pumping reagent water through the cleaned and fully assembled equipment sets (with the 

filter attached) into a cleaned bottle (an HDPE bottle for metals and a glass bottle for mercury). 

The blank samples were then preserved and analyzed according to the analytical methods (EPA 

Method 1638 and 1631E), as described in Section 5.2.1 for the bottle blank samples. 

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

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

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

collection of metals and mercury samples. 

5.2.3 Field Blanks 

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

contamination from sampling equipment, sampling equipment decontamination procedures, 

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

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

dissolved mercury samples4

. 

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

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

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

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

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

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

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

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

as “true” split samples with Miami Fort’s representative, using the same procedure discussed in 

the sample collection description (Section 3.1). 

 

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

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

filtering the sample, which is assessed as the field blank for the dissolved mercury sample. Mercury was detected at 

a concentration of 0.25 ng/L in the filtration blank performed for the fourth day of samples, which includes the 

influent to the FGD wastewater treatment system (Day 4), the third and fourth grab sample for the effluent from 

FGD wastewater treatment system (Day 3), and the first and second grab samples for effluent from FGD wastewater 

treatment system (Day 4). Mercury was not detected above the method detection limit (0.24 ng/L) in the filtration 

blanks performed for the first, second, third, or fifth day of samples.
5-21 

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

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

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

composite container. After approximately 100 minutes, the sampling team began pumping off 

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

the tubing and filter were purged with 750 mL of blank water. The sample bottles were placed in 

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

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

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

collection description (Section 3.1). 

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

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

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

the sample bottles under the clear plastic bag. 

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

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

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

composite container was used with a pump to fill the field blank composite container. Prior to 

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

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

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

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

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

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

After 24 hours, the ASTM Type 1 water in the field blank composite container was 

pumped off into the individual sample bottles. The sample bottles were placed in a “cleanbox” 

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

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

representative, using the same procedure discussed in the sample collection description (Section 

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

ASTM Type 1 water. First the samplers collected the total metals by 200.8 and total metals by 

200.7 field blank samples. Then the sampling team attached a filter to the tubing set and purged 

the tubing with approximately 0.75 liter of ASTM Type 1 water. The samplers then collected the 

dissolved metals by 200.8, dissolved metals by 200.7, and dissolved hexavalent chromium field 

blank samples. 

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

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

included in the table. Results are rounded to three significant digits. Appendix Tables A-15 

through A-19 present all the analytical results for the field blanks from each of the sampling 

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

detection limit, but below the quantitation limit (i.e., J-values). 
5-22 

5.2.4 Field Duplicates 

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

precision for the episode. Field duplicate samples are separate samples collected from the same 

location as the original sample. The duplicate is filled immediately after the original sample and 

is stored and analyzed independently. The RPD between the two sample results is examined to 

determine the precision of the data. EPA used the following equation to calculate the RPD for 

the duplicate sample results. 

100

2

S D

S D

RPD (%) 





 



 

  (5-1) 

where: 

S = concentration of the analyte from original sample analysis; 

D = concentration of the analyte from the duplicate sample analysis; and 

RPD = relative percent difference between the original and duplicate sample 

result. 

During this sampling episode, EPA collected duplicate samples for the effluent from 

FGD wastewater treatment system (SP-3) during Day 2 of the sampling episode. The duplicate 

samples were analyzed for all analytes. Table 5-2 presents analytical results and the RPD for SP3. Results are rounded to three significant digits. Appendix Tables A-10 and A-13 present all the 

analytical results for the effluent from FGD wastewater treatment system (SP-2) Day 2 and the 

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

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

limit, but below the quantitation limit (i.e., J-values). 
5-23 

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

Analyte Sample Description Method Units 

Total MetalsMagnesium Effluent from FGD Wastewater Treatment System Field Blank - Day 1 200.7 ug/L Mercury Influent to FGD Wastewater Treatment System Field Blank - Day 1 1631E ng/L 
5-24 

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

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

value. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. MI – Matrix interferences present. Min – Minimum value. V – Serial dilution is not within control limits

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

Analyte Method Units

Original Effluent from 

FGD Wastewater 

Treatment System, Day 

2 Concentration (SP-2) 

Duplicate

Effluent from FGD 

Wastewater 

Treatment System 

Concentration 

(SP-3)

Aver

Resu

ClassicalsAmmonia 350.1 mg/L 5.30 5.50 5.4Nitrate Nitrite as N 353.2 mg/L 290 300 29Nitrogen, Total Kjeldahl 351.2 mg/L 21.0 B 23.0 B 22.Biochemical Oxygen Demand 5210B mg/L 8.40 9.60 9.0Chemical Oxygen Demand 410.4 mg/L 400 560 48Chloride 300.0 mg/L 7,500 7,500 7,50Sulfate 300.0 mg/L 13,000 13,000 13,0Cyanide, Total 4500 CN E mg/L 2.40 B NQ (0.100) B < 1.Total Dissolved Solids 2540C mg/L 32,000 27,000 29,5Total Suspended Solids 2540D mg/L 10.0 7.60 8.8Phosphorus, Total 365.1 mg/L 0.180 B 0.0650 B 0.12Total MetalsAluminum 200.7 ug/L 260 NQ (200) < 18Antimony 200.8 ug/L 6.90 7.00 6.9Arsenic 200.8 ug/L 5.60 4.10 4.8Barium 200.7 ug/L 150 160 15Beryllium 200.7 ug/L ND (2.00) ND (2.00) ND (2
5-25 

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

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

value. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. MI – Matrix interferences present. Min – Minimum value. V – Serial dilution is not within control limits

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

Analyte Method Units

Original Effluent from 

FGD Wastewater 

Treatment System, Day 

2 Concentration (SP-2) 

Duplicate

Effluent from FGD 

Wastewater 

Treatment System 

Concentration 

(SP-3)

Aver

Resu

Boron 200.7 ug/L 320,000 B,F,4 320,000 B 320,0Cadmium 200.8 ug/L ND (4.00) ND (4.00) ND (4Calcium 200.7 ug/L 840,000 4 860,000 850,0Chromium 200.8 ug/L 16.0 17.0 16.Cobalt 200.7 ug/L ND (20.0) ND (20.0) ND (2Copper 200.8 ug/L ND (4.00) ND (4.00) ND (4Iron 200.7 ug/L NQ (200) NQ (200) NQ (2Lead 200.8 ug/L ND (2.00) ND (2.00) ND (2Magnesium 200.7 ug/L 5,500,000 B,F,4 5,600,000 B 5,550Manganese 200.7 ug/L 88.0 B 90.0 B 89.Mercury 1631E ng/L 99.8 110 10Molybdenum 200.7 ug/L 200 200 20Nickel 200.8 ug/L NQ (4.00) NQ (4.00) NQ (4Selenium 200.8 ug/L 540 V,4,MI 530 53Silver 200.8 ug/L ND (2.00) F,Min ND (2.00) ND (2Sodium 200.7 ug/L 360,000 4 370,000 365,0Thallium 200.8 ug/L 14.0 14.0 14.Tin 200.7 ug/L ND (200) ND (200) ND (2
5-26 

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

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

value. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. MI – Matrix interferences present. Min – Minimum value. V – Serial dilution is not within control limits

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

Analyte Method Units

Original Effluent from 

FGD Wastewater 

Treatment System, Day 

2 Concentration (SP-2) 

Duplicate

Effluent from FGD 

Wastewater 

Treatment System 

Concentration 

(SP-3)

Aver

Resu

Titanium 200.7 ug/L ND (20.0) NQ (20.0) NQ (2Vanadium 200.8 ug/L 17.0 18.0 17.Zinc 200.8 ug/L ND (10.0) ND (10.0) ND (1Dissolved MetalsAluminum 200.7 ug/L NQ (200) B ND (200) NQ (2Antimony 200.8 ug/L 6.80 6.80 6.8Arsenic 200.8 ug/L NQ (4.00) 4.00 < 3.Barium 200.7 ug/L 150 140 14Beryllium 200.7 ug/L ND (2.00) ND (2.00) ND (2Boron 200.7 ug/L 330,000 F,4 320,000 325,0Cadmium 200.8 ug/L ND (4.00) ND (4.00) ND (4Calcium 200.7 ug/L 860,000 810,000 835,0Chromium 200.8 ug/L 14.0 14.0 14.Chromium (VI) 218.6 ug/L 7.32 7.35 7.3Cobalt 200.7 ug/L ND (20.0) ND (20.0) ND (2Copper 200.8 ug/L ND (4.00) NQ (4.00) NQ (4Iron 200.7 ug/L ND (200) ND (200) ND (2Lead 200.8 ug/L ND (2.00) ND (2.00) ND (2
5-27 

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

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

value. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. MI – Matrix interferences present. Min – Minimum value. V – Serial dilution is not within control limits

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

Analyte Method Units

Original Effluent from 

FGD Wastewater 

Treatment System, Day 

2 Concentration (SP-2) 

Duplicate

Effluent from FGD 

Wastewater 

Treatment System 

Concentration 

(SP-3)

Aver

Resu

Magnesium 200.7 ug/L 5,900,000 F,4 5,600,000 5,750Manganese 200.7 ug/L 87.0 B 81.0 B 84.Mercury 1631E ng/L 63.1 59.9 61.Molybdenum 200.7 ug/L 200 190 19Nickel 200.8 ug/L NQ (4.00) NQ (4.00) NQ (4Selenium 200.8 ug/L 520 V,4,MI 470 49Silver 200.8 ug/L ND (2.00) F,Min ND (2.00) ND (2Sodium 200.7 ug/L 360,000 340,000 350,0Thallium 200.8 ug/L 14.0 14.0 14.Tin 200.7 ug/L ND (200) ND (200) ND (2Titanium 200.7 ug/L NQ (20.0) ND (100.0) NQ (6Vanadium 200.8 ug/L 16.0 18.0 17.Zinc 200.8 ug/L ND (10.0) ND (10.0) ND (1
6-1

6. REFERENCES

1. Eastern Research Group, Inc., 2010. Sampling Plan, Duke Energy’s Miami Fort Station. 

July 1. DCN SE00501. 

2. Eastern Research Group, Inc., 2010. Quality Assurance Project Plan for the Steam 

Electric Effluent Guidelines Rulemaking. (October). DCN SE00058. 

3. U.S. EPA. 2001. Method 200.7: Determination of Metals and Trace Elements in Water 

and Wastes by Inductively Coupled Plasma – Atomic Emission Spectrometry. Revision 

4.4. 

4. U.S. EPA. 1994. Method 200.7: Determination of Trace Elements in Waters and Wastes 

by Inductively Coupled Plasma - Mass Spectrometry. Revision 5.4. 
Appendix A 

ANALYTICAL RESULTS 
A-1 

Note: Sample qualifiers denoted with an ‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘Swith the solid portion of the sample. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). V – Serial dilution is not within control limits. 

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

Day 1 Analytical Results, Miami Fort 

Analyte

Aqueous Phase Result 

(mg/L for Classicals; 

ug/L for Metals; and 

ng/L for Mercury)

Solid Phase Result 

(mg/kg for Classicals 

and Metals and ng/g for 

Mercury)

Calculated Total Result (mg/L 

ug/L for Metals; and ng/L 

ClassicalsAmmonia 5.1 H,P,Est 24 H,P,Est 5.21 F(H, P, ENitrate Nitrite as N 77 H,P,Est 49 H,P,Est 71.7 F(H, P, ENitrogen, Total Kjeldahl 24 H,P,Est 830 H,P,Est 40.5 F(H, P, ECyanide, Total 0.27 B,H,P,Est 0.35 J,B,H,P 0.255 F(B, H, P, EPhosphorus, Total 0.01 J,B,H,P 21 H,P,Est 0.476 F(J, B, H, Total MetalsAluminum 6,000 25,000 561,000Antimony 3.1 0.16 J 6.4 Arsenic 4.1 42 937Barium 88 F,Min 340 B 7,640 F(F, Beryllium 3.4 1.1 27.6Boron 660,000 B,4 860 B 624,000 F(BCadmium 320 2.2 342Calcium 610,000 35,000 B 1,340,000 
A-2 

Note: Sample qualifiers denoted with an ‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘Swith the solid portion of the sample. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). V – Serial dilution is not within control limits. 

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

Day 1 Analytical Results, Miami Fort 

Analyte

Aqueous Phase Result 

(mg/L for Classicals; 

ug/L for Metals; and 

ng/L for Mercury)

Solid Phase Result 

(mg/kg for Classicals 

and Metals and ng/g for 

Mercury)

Calculated Total Result (mg/L 

ug/L for Metals; and ng/L 

Chromium ND (8) U 180 ^ 4,000 F(Cobalt 320 5.9 425Copper 42 59 1,350Iron ND (200) U 41,000 911,000 Lead ND (2) U 34 756 Magnesium 8,100,000 4 20,000 7,870,000 Manganese 95,000 B,4 270 93,100 Mercury 2,920 7,570 166,000Molybdenum 140 17 506Nickel 1,500 4 54 2,580 Selenium 320 V,4,MI 140 3,400 F(Silver ND (2) U,F,Min 0.14 J 3.11 F(U, FSodium 360,000 1,100 355,000Thallium 14 1.8 B 52.8 Tin 11 J 2.3 J 61.2 FTitanium ND (20) U 91 2,020 
A-3 

Note: Sample qualifiers denoted with an ‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘Swith the solid portion of the sample. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). V – Serial dilution is not within control limits. 

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

Day 1 Analytical Results, Miami Fort 

Analyte

Aqueous Phase Result 

(mg/L for Classicals; 

ug/L for Metals; and 

ng/L for Mercury)

Solid Phase Result 

(mg/kg for Classicals 

and Metals and ng/g for 

Mercury)

Calculated Total Result (mg/L 

ug/L for Metals; and ng/L 

Vanadium 8.7 J 180 4,010 Zinc 5,200 B,4 410 13,900 
A-4 

Note: Sample qualifiers denoted with an ‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘Swith the solid portion of the sample. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analytical Results, Miami Fort 

Analyte

Aqueous Phase Result 

(mg/L for Classicals; ug/L 

for Metals; and ng/L for 

Mercury)

Solid Phase Result 

(mg/kg for Classicals and 

Metals and ng/g for 

Mercury)

Calculated Total Result 

ug/L for Metals; and 

ClassicalsAmmonia 5.3 P,Est 28 H,P,Est 6.12 F(Nitrate Nitrite as N 83 P,Est 64 H,P,Est 86.6 F(Nitrogen, Total Kjeldahl 31 H,P,Est 840 H,P,Est 52.6 F(HCyanide, Total 0.62 B,H,P,Est 0.33 J,B,H,P 0.644 F(B, HPhosphorus, Total 0.008 J,B,H,P 310 H,P,Est 7.68 F(J, Total MetalsAluminum 6,600 B 25,000 626,000 Antimony 2.7 0.15 J 6.48 Arsenic 4.4 36 896Barium 83 300 B 7,510 Beryllium 3.5 1 28.3Boron 760,000 B 980 B 803,000 Cadmium 360 2.3 426Calcium 590,000 B 30,000 B 1,350,000 Chromium ND (8) U 180 ^ 4,460 Cobalt 360 5.4 503Copper 59 59 1,520Iron ND (200) U 39,000 965,000 Lead 0.82 J 34 842 
A-5 

Note: Sample qualifiers denoted with an ‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘Swith the solid portion of the sample. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analytical Results, Miami Fort 

Analyte

Aqueous Phase Result 

(mg/L for Classicals; ug/L 

for Metals; and ng/L for 

Mercury)

Solid Phase Result 

(mg/kg for Classicals and 

Metals and ng/g for 

Mercury)

Calculated Total Result 

ug/L for Metals; and 

Magnesium 8,500,000 20,000 9,210,000Manganese 96,000 B 260 105,000 Mercury 2,990 7,330 148,000Molybdenum 140 16 540Nickel 1,600 54 2,980Selenium 420 130 3,650Silver ND (2) U 0.14 J 3.47 Sodium 390,000 1,100 427,000Thallium 14 1.7 B 56.4 Tin 6.1 J 2.2 J 60.7 Titanium ND (20) U 83 2,050 Vanadium 9.9 J 170 4,220 Zinc 6,000 B 410 16,300 
A-6 

Note: Sample qualifiers denoted with an ‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘Swith the solid portion of the sample. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Day 3 Analytical Results, Miami Fort 

Analyte

Aqueous Phase Result 

(mg/L for Classicals; ug/L 

for Metals; and ng/L for 

Mercury)

Solid Phase Result 

(mg/kg for Classicals and 

Metals and ng/g for 

Mercury)

Calculated Total Result (m

ug/L for Metals; and ng

ClassicalsAmmonia 7.7 P,Est 26 P,Est 7.9 F(P, Nitrate Nitrite as N 79 P,Est 56 P,Est 74.9 F(P, Nitrogen, Total Kjeldahl 29 P,Est 700 P,Est 47.6 F(P, Cyanide, Total 2.2 B,H,P,Est 0.37 J,B,H,P 2.05 F(B, H, PPhosphorus, Total 0.013 J,B,P 1.9 J,P 0.068 F(J, Total MetalsAluminum 40,000 B 22,000 4 687,000 FAntimony 3.6 0.16 J,F,Min 8.06 SArsenic 7.2 44 1,310Barium 80 350 B 10,400 Beryllium 10 1.1 41.8Boron 880,000 B 950 B,4 844,000 F(Cadmium 500 2 522Calcium 570,000 B 52,000 B,4 2,060,000 F(Chromium ND (8) U 150 4,^ 4,430 FCobalt 500 5.7 632Copper 86 54 1,670
A-7 

Note: Sample qualifiers denoted with an ‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘Swith the solid portion of the sample. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Day 3 Analytical Results, Miami Fort 

Analyte

Aqueous Phase Result 

(mg/L for Classicals; ug/L 

for Metals; and ng/L for 

Mercury)

Solid Phase Result 

(mg/kg for Classicals and 

Metals and ng/g for 

Mercury)

Calculated Total Result (m

ug/L for Metals; and ng

Iron ND (200) U 35,000 4 1,030,000 FLead 0.82 J 30 887 Magnesium 12,000,000 23,000 11,800,000Manganese 160,000 B 300 157,000 Mercury 3,640 5,990 231,000Molybdenum 150 17 641Nickel 2,400 47 3,610Selenium 410 100 3,330Silver ND (2) U 0.14 J,F,Min 4.14 F(U) Sodium 500,000 1,300 502,000Thallium 34 2.1 B 93.5 Tin ND (200) U 2.4 J 70.9 FTitanium ND (20) U 140 F Max 4,140 F(UVanadium 14 150 4 4,440 Zinc 11,000 B 340 4 20,200 F
A-8 

Note: Sample qualifiers denoted with an ‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘Swith the solid portion of the sample. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analytical Results, Miami Fort

Analyte

Aqueous Phase Result 

(mg/L for Classicals; ug/L 

for Metals; and ng/L for 

Mercury)

Solid Phase Result 

(mg/kg for Classicals 

and Metals and ng/g for 

Mercury)

Calculated Total Result (mg/L 

for Metals; and ng/L fo

ClassicalsAmmonia 6.2 P,Est 23 P,Est 6.06 F(PNitrate Nitrite as N 90 P,Est 65 P,Est 82.8 F(PNitrogen, Total Kjeldahl 26 P,Est 900 P,Est 40.8 F(PCyanide, Total 0.21 B,H,P,Est 0.42 J,B,H,P 0.198 F(B, H, Phosphorus, Total 0.012 J,B,P 340 P,Est 6.52 F(J, Total MetalsAluminum 20,000 B 25,000 497,000 Antimony 2.5 0.14 J 4.95 Arsenic 5.9 36 695Barium 100 330 B 6,410 Beryllium 3.6 1 22.4Boron 820,000 B 990 B 762,000 Cadmium 380 2.7 396Calcium 600,000 B 31,000 B 1,140,000 Chromium ND (8) U 190 ^ 3,640 Cobalt 390 5.5 459Copper 72 60 1,210Iron ND (200) U 40,000 766,000 Lead ND (2) U 34 651 
A-9 

Note: Sample qualifiers denoted with an ‘F( )’ are qualifiers associated with the filtrate portion of the sample and sample qualifiers denoted with an ‘Swith the solid portion of the sample. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analytical Results, Miami Fort

Analyte

Aqueous Phase Result 

(mg/L for Classicals; ug/L 

for Metals; and ng/L for 

Mercury)

Solid Phase Result 

(mg/kg for Classicals 

and Metals and ng/g for 

Mercury)

Calculated Total Result (mg/L 

for Metals; and ng/L fo

Magnesium 9,500,000 21,000 9,010,000Manganese 100,000 B 280 96,000 Mercury 4,370 4,990 44,000Molybdenum 110 16 406Nickel 1,700 53 2,560Selenium 470 130 2,920Silver ND (2) U 0.12 J 2.3 Sodium 420,000 1,200 404,000Thallium 15 1.7 B 46.2 Tin ND (200) U 2.3 J 44.1 Titanium ND (20) U 95 1,820 Vanadium 14 170 3,270Zinc 6,700 B 440 14,500 
A-10 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Classical Pollutants - TotalAmmonia 350.1 mg/l NA 0.192 2.05 5.21Nitrate Nitrite as N 353.2 mg/l NA 0.182 1.14 71.7Nitrogen, Total Kjeldahl 351.2 mg/l NA 3.02 15.9 40.5Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 2 Chemical Oxygen Demand 410.4 mg/L 10 41 200 620Chloride 300.0 mg/L 500 130 1,500 9,000Sulfate 300.0 mg/L 500 120 2,500 18,000Cyanide, Total 4500 CN E mg/l NA 0.0205 0.102 0.255Total Dissolved Solids 2540C mg/L 1 470 1,000 56,000Total Suspended Solids 2540D mg/L 1 55 200 16,000Phosphorus, Total 365.1 mg/l NA 0.0224 0.153 0.476Classicals Pollutants - Solid (dry weight)Ammonia 350.1 mg/Kg 1 4.1 9.9 24 Nitrate Nitrite as N 353.2 mg/Kg 1 0.36 10 49 Nitrogen, Total Kjeldahl 351.2 mg/Kg 10 120 510 830 Cyanide, Total 4500 CN E mg/Kg 1 0.095 0.46 0.35 
A-11 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Phosphorus, Total 365.1 mg/Kg 1 0.8 4.8 21 Classicals Pollutants -Filtered AqueousAmmonia 350.1 mg/L 1 0.11 2 5.1 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 77 Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.38 5 24 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.27 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.01 Metals - Calculated TotalAluminum 200.7, 6010B ug/L NA 42 403 561,000Antimony 200.8, 6020 ug/L NA 1.26 10.3 6.4Arsenic 200.8, 6020 ug/L NA 27.8 315 937Barium 200.7, 6010B ug/L NA 3.96 40.3 7,640Beryllium 200.7, 6010B ug/L NA 1.38 12.9 27.6Boron 200.7, 6010B ug/L NA 265 5,700 624,000Cadmium 200.8, 6020 ug/L NA 1.5 7.89 342Calcium 200.7, 6010B ug/L NA 374 1,480 1,340,000Chromium 200.8, 6020 ug/L NA 43 114 4,000
A-12 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Cobalt 200.7, 6010B ug/L NA 3.21 40.3 425Copper 200.8, 6020 ug/L NA 38.7 137 1,350Iron 200.7, 6010B ug/L NA 114 517 911,000Lead 200.8, 6020 ug/L NA 10.2 81.8 756Magnesium 200.7, 6010B ug/L NA 577 9,620 7,870,000Manganese 200.7, 6010B ug/L NA 14.1 481 93,100Mercury 1631E, FGS-069 ng/L NA 1,670 4,530 166,000Molybdenum 200.7, 6010B ug/L NA 7.25 81.1 506Nickel 200.8, 6020 ug/L NA 1.88 10.1 2,580Selenium 200.8, 6020 ug/L NA 6.12 24.8 3,400Silver 200.8, 6020 ug/L NA 1.41 6.06 3.11Sodium 200.7, 6010B ug/L NA 1,450 20,300 355,000Thallium 200.8, 6020 ug/L NA 0.58 6.06 52.8Tin 200.7, 6010B ug/L NA 24.4 403 61.2Titanium 200.7, 6010B ug/L NA 4.58 40.3 2,020Vanadium 200.8, 6020 ug/L NA 22 276 4,010Zinc 200.8, 6020 ug/L NA 204 625 13,900
A-13 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Metals - DissolvedAluminum 200.7 ug/L 2 9.4 200 4,200 Antimony 200.8 ug/L 2 0.72 2 3.4Arsenic 200.8 ug/L 2 1.2 4 4.4Barium 200.7 ug/L 2 2.5 20 140Beryllium 200.7 ug/L 2 0.71 2 4.7Boron 200.7 ug/L 500 1,700 50,000 650,000 Cadmium 200.8 ug/L 5 2.9 10 340Calcium 200.7 ug/L 2 69 400 690,000Chromium 200.8 ug/L 2 3.3 8 ND (8) Chromium (VI) 218.6 ug/L 5 1.96 10 ND (10) Cobalt 200.7 ug/L 2 1.1 20 340Copper 200.8 ug/L 2 0.96 4 54Iron 200.7 ug/L 2 32 200 47 Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 500 5,400 100,000 7,900,000Manganese 200.7 ug/L 500 130 5,000 100,000
A-14 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Mercury 1631E ng/L 500 124 260 1,110Molybdenum 200.7 ug/L 2 1.6 40 120Nickel 200.8 ug/L 25 11 50 1,700Selenium 200.8 ug/L 5 1.6 10 290Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 360,000Thallium 200.8 ug/L 2 0.47 2 25Tin 200.7 ug/L 2 4.8 200 8.7 Titanium 200.7 ug/L 2 1.6 20 3.2 Vanadium 200.8 ug/L 2 1.7 10 12Zinc 200.8 ug/L 100 200 500 6,300Metals - Filtered AqueousAluminum 200.7 ug/L 2 9.4 200 6,000Antimony 200.8 ug/L 2 0.72 2 3.1Arsenic 200.8 ug/L 2 1.2 4 4.1Barium 200.7 ug/L 2 2.5 20 88 Beryllium 200.7 ug/L 2 0.71 2 3.4
A-15 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Boron 200.7 ug/L 50 170 5,000 660,000 Cadmium 200.8 ug/L 2 1.2 4 320Calcium 200.7 ug/L 2 69 400 610,000Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 320Copper 200.8 ug/L 2 0.96 4 42Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 50 540 10,000 8,100,000 Manganese 200.7 ug/L 50 13 500 95,000 Mercury 1631E ng/L 500 124 260 2,920Molybdenum 200.7 ug/L 2 1.6 40 140Nickel 200.8 ug/L 2 0.89 4 1,500 Selenium 200.8 ug/L 2 0.62 4 320 Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 360,000Thallium 200.8 ug/L 2 0.47 2 14
A-16 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Tin 200.7 ug/L 2 4.8 200 11 Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 8.7 Zinc 200.8 ug/L 20 41 100 5,200 Metals - Solid (dry weight)Aluminum 6010B mg/kg 1 1.5 9.9 25,000Antimony 6020 mg/kg 2 0.027 0.38 0.16 Arsenic 6020 mg/kg 25 1.2 14 42Barium 6010B mg/kg 1 0.075 0.99 340 Beryllium 6010B mg/kg 1 0.033 0.5 1.1Boron 6010B mg/kg 5 4.9 50 860 Cadmium 6020 mg/kg 2 0.018 0.19 2.2Calcium 6010B mg/kg 1 14 50 35,000 Chromium 6020 mg/kg 25 1.8 4.8 180 Cobalt 6010B mg/kg 1 0.099 0.99 5.9Copper 6020 mg/kg 25 1.7 6 59Iron 6010B mg/kg 1 3.8 15 41,000
A-17 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Lead 6020 mg/kg 25 0.43 3.6 34Magnesium 6010B mg/kg 1 3.7 20 20,000Manganese 6010B mg/kg 1 0.099 0.99 270Mercury FGS-069 ng/g 4,000 71.9 198 7,570Molybdenum 6010B mg/kg 1 0.26 2 17Nickel 6020 mg/kg 2 0.048 0.29 54Selenium 6020 mg/kg 2 0.25 0.95 140Silver 6020 mg/kg 2 0.039 0.19 0.14 Sodium 6010B mg/kg 1 58 500 1,100Thallium 6020 mg/kg 2 0.0067 0.19 1.8 Tin 6010B mg/kg 1 0.9 9.9 2.3 Titanium 6010B mg/kg 1 0.14 0.99 91Vanadium 6020 mg/kg 25 0.92 12 180Zinc 6020 mg/kg 25 7.5 24 410
A-18 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Classical Pollutants - TotalAmmonia 350.1 mg/l NA 0.214 2.3 6.12Nitrate Nitrite as N 353.2 mg/l NA 0.203 1.27 86.6Nitrogen, Total Kjeldahl 351.2 mg/l NA 3.36 18 52.6Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 1.9 Chemical Oxygen Demand 410.4 mg/L 10 41 200 670Chloride 300.0 mg/L 500 130 1,500 9,800Sulfate 300.0 mg/L 500 120 2,500 21,000Cyanide, Total 4500 CN E mg/l NA 0.0232 0.116 0.644Total Dissolved Solids 2540C mg/L 1 470 1,000 68,000Total Suspended Solids 2540D mg/L 1 55 200 30,000Phosphorus, Total 365.1 mg/l NA 0.208 1.29 7.68Classicals Pollutants - Solid (dry weight)Ammonia 350.1 mg/Kg 1 4.1 10 28 Nitrate Nitrite as N 353.2 mg/Kg 1 0.35 9.9 64 Nitrogen, Total Kjeldahl 351.2 mg/Kg 10 120 520 840 Cyanide, Total 4500 CN E mg/Kg 1 0.11 0.53 0.33 Phosphorus, Total 365.1 mg/Kg 10 8.2 50 310 Classicals Pollutants -Filtered AqueousAmmonia 350.1 mg/L 1 0.11 2 5.3 
A-19 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 83 Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.38 5 31 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.62 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.008 Metals - Calculated TotalAluminum 200.7, 6010B ug/L NA 44.3 430 626,000Antimony 200.8, 6020 ug/L NA 1.36 11 6.48Arsenic 200.8, 6020 ug/L NA 28.5 351 896Barium 200.7, 6010B ug/L NA 4.27 43 7,510Beryllium 200.7, 6010B ug/L NA 1.47 13.2 28.3Boron 200.7, 6010B ug/L NA 286 6,240 803,000Cadmium 200.8, 6020 ug/L NA 1.65 8.55 426Calcium 200.7, 6010B ug/L NA 392 1,520 1,350,000Chromium 200.8, 6020 ug/L NA 45.5 120 4,460Cobalt 200.7, 6010B ug/L NA 3.38 43 503Copper 200.8, 6020 ug/L NA 40.6 143 1,520Iron 200.7, 6010B ug/L NA 119 551 965,000Lead 200.8, 6020 ug/L NA 10.9 86.2 842Magnesium 200.7, 6010B ug/L NA 638 10,700 9,210,000Manganese 200.7, 6010B ug/L NA 15.6 535 105,000
A-20 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Mercury 1631E, FGS-069 ng/L NA 1,520 4,120 148,000Molybdenum 200.7, 6010B ug/L NA 7.58 85.5 540Nickel 200.8, 6020 ug/L NA 2.05 10.8 2,980Selenium 200.8, 6020 ug/L NA 6.58 26.4 3,650Silver 200.8, 6020 ug/L NA 1.52 6.5 3.47Sodium 200.7, 6010B ug/L NA 1,520 21,400 427,000Thallium 200.8, 6020 ug/L NA 0.638 6.5 56.4Tin 200.7, 6010B ug/L NA 25.5 430 60.7Titanium 200.7, 6010B ug/L NA 4.86 43 2,050Vanadium 200.8, 6020 ug/L NA 23.3 283 4,220Zinc 200.8, 6020 ug/L NA 196 621 16,300Metals - DissolvedAluminum 200.7 ug/L 2 9.4 200 2,400 Antimony 200.8 ug/L 2 0.72 2 3.3Arsenic 200.8 ug/L 2 1.2 4 4.9Barium 200.7 ug/L 2 2.5 20 140Beryllium 200.7 ug/L 2 0.71 2 4.1Boron 200.7 ug/L 500 1,700 50,000 690,000 Cadmium 200.8 ug/L 5 2.9 10 390Calcium 200.7 ug/L 2 69 400 670,000
A-21 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Chromium 200.8 ug/L 2 3.3 8 ND (8) Chromium (VI) 218.6 ug/L 5 1.96 10 ND (10) Cobalt 200.7 ug/L 2 1.1 20 360Copper 200.8 ug/L 2 0.96 4 50Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 500 5,400 100,000 8,400,000Manganese 200.7 ug/L 500 130 5,000 100,000Mercury 1631E ng/L 500 124 260 1,830Molybdenum 200.7 ug/L 2 1.6 40 110Nickel 200.8 ug/L 25 11 50 1,700Selenium 200.8 ug/L 5 1.6 10 330Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 380,000Thallium 200.8 ug/L 2 0.47 2 26Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 2.1 Vanadium 200.8 ug/L 2 1.7 10 13Zinc 200.8 ug/L 100 200 500 6,200
A-22 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Metals - Filtered AqueousAluminum 200.7 ug/L 2 9.4 200 6,600 Antimony 200.8 ug/L 2 0.72 2 2.7Arsenic 200.8 ug/L 2 1.2 4 4.4Barium 200.7 ug/L 2 2.5 20 83Beryllium 200.7 ug/L 2 0.71 2 3.5Boron 200.7 ug/L 50 170 5,000 760,000 Cadmium 200.8 ug/L 2 1.2 4 360Calcium 200.7 ug/L 2 69 400 590,000 Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 360Copper 200.8 ug/L 2 0.96 4 59Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 0.82 Magnesium 200.7 ug/L 50 540 10,000 8,500,000Manganese 200.7 ug/L 50 13 500 96,000 Mercury 1631E ng/L 500 124 260 2,990Molybdenum 200.7 ug/L 2 1.6 40 140Nickel 200.8 ug/L 2 0.89 4 1,600Selenium 200.8 ug/L 2 0.62 4 420
A-23 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 390,000Thallium 200.8 ug/L 2 0.47 2 14Tin 200.7 ug/L 2 4.8 200 6.1 Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 9.9 Zinc 200.8 ug/L 10 20 50 6,000 Metals - Solid (dry weight)Aluminum 6010B mg/kg 1 1.4 9.1 25,000Antimony 6020 mg/kg 2 0.025 0.36 0.15 Arsenic 6020 mg/kg 25 1.1 14 36Barium 6010B mg/kg 1 0.069 0.91 300 Beryllium 6010B mg/kg 1 0.03 0.45 1Boron 6010B mg/kg 5 4.5 45 980 Cadmium 6020 mg/kg 2 0.017 0.18 2.3Calcium 6010B mg/kg 1 13 45 30,000 Chromium 6020 mg/kg 25 1.7 4.5 180 Cobalt 6010B mg/kg 1 0.091 0.91 5.4Copper 6020 mg/kg 25 1.6 5.6 59Iron 6010B mg/kg 1 3.5 14 39,000
A-24 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Lead 6020 mg/kg 25 0.41 3.4 34Magnesium 6010B mg/kg 1 3.4 18 20,000Manganese 6010B mg/kg 1 0.091 0.91 260Mercury FGS-069 ng/g 4,000 71.1 196 7,330Molybdenum 6010B mg/kg 1 0.24 1.8 16Nickel 6020 mg/kg 2 0.046 0.27 54Selenium 6020 mg/kg 2 0.24 0.9 130Silver 6020 mg/kg 2 0.037 0.18 0.14 Sodium 6010B mg/kg 1 54 450 1,100Thallium 6020 mg/kg 2 0.0063 0.18 1.7 Tin 6010B mg/kg 1 0.83 9.1 2.2 Titanium 6010B mg/kg 1 0.13 0.91 83Vanadium 6020 mg/kg 25 0.87 11 170Zinc 6020 mg/kg 25 7.1 23 410
A-25 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Classical Pollutants – TotalAmmonia 350.1 mg/l NA 0.223 2.15 7.9Nitrate Nitrite as N 353.2 mg/l NA 0.186 1.22 74.9Nitrogen, Total Kjeldahl 351.2 mg/l NA 3.9 19.4 47.6Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 3.3Chemical Oxygen Demand 410.4 mg/L 10 41 200 910Chloride 300.0 mg/L 500 130 1,500 9,60Sulfate 300.0 mg/L 1,000 230 5,000 32,00Cyanide, Total 4500 CN E mg/l NA 0.0218 0.109 2.05Total Dissolved Solids 2540C mg/L 1 470 1,000 59,00Total Suspended Solids 2540D mg/L 1 55 200 20,00Phosphorus, Total 365.1 mg/l NA 0.0286 0.191 0.06Classicals Pollutants - Solid (dry weight)Ammonia 350.1 mg/Kg 1 4.1 10 26 Nitrate Nitrite as N 353.2 mg/Kg 1 0.35 9.9 56 Nitrogen, Total Kjeldahl 351.2 mg/Kg 10 120 500 700 Cyanide, Total 4500 CN E mg/Kg 1 0.11 0.55 0.37 Phosphorus, Total 365.1 mg/Kg 1 0.81 4.9 1.9 Classicals Pollutants -Filtered AqueousAmmonia 350.1 mg/L 1 0.11 2 7.7 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 79 Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.38 5 29 
A-26 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 2.2 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.01Metals - Calculated TotalAluminum 200.7, 6010B ug/L NA 50.1 460 687,0Antimony 200.8, 6020 ug/L NA 1.46 13.4 8.06Arsenic 200.8, 6020 ug/L NA 30.1 358 1,31Barium 200.7, 6010B ug/L NA 4.41 46 10,40Beryllium 200.7, 6010B ug/L NA 1.57 15.7 41.8Boron 200.7, 6010B ug/L NA 293 6,020 844,0Cadmium 200.8, 6020 ug/L NA 1.64 9.32 522Calcium 200.7, 6010B ug/L NA 2,010 7,170 2,060,0Chromium 200.8, 6020 ug/L NA 47.4 123 4,43Cobalt 200.7, 6010B ug/L NA 3.77 46 632Copper 200.8, 6020 ug/L NA 42.2 148 1,67Iron 200.7, 6010B ug/L NA 136 599 1,030,0Lead 200.8, 6020 ug/L NA 11 87.5 887Magnesium 200.7, 6010B ug/L NA 604 9,830 11,800,Manganese 200.7, 6010B ug/L NA 14.8 491 157,0Mercury 1631E, FGS-069 ng/L NA 2,860 7,810 231,0Molybdenum 200.7, 6010B ug/L NA 8.57 93.2 641Nickel 200.8, 6020 ug/L NA 2.27 12.3 3,61
A-27 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Selenium 200.8, 6020 ug/L NA 10.6 47.2 3,33Silver 200.8, 6020 ug/L NA 1.7 7.47 4.14Sodium 200.7, 6010B ug/L NA 1,790 23,200 502,0Thallium 200.8, 6020 ug/L NA 0.636 7.47 93.5Tin 200.7, 6010B ug/L NA 29.6 460 70.9Titanium 200.7, 6010B ug/L NA 5.32 46 4,14Vanadium 200.8, 6020 ug/L NA 23.7 296 4,44Zinc 200.8, 6020 ug/L NA 36.6 102 20,20Metals - DissolvedAluminum 200.7 ug/L 10 47 1,000 29,00Antimony 200.8 ug/L 2 0.72 2 3.7Arsenic 200.8 ug/L 2 1.2 4 6.6Barium 200.7 ug/L 2 2.5 20 180Beryllium 200.7 ug/L 2 0.71 2 12Boron 200.7 ug/L 500 1,700 50,000 820,0Cadmium 200.8 ug/L 50 29 100 510Calcium 200.7 ug/L 2 69 400 620,0Chromium 200.8 ug/L 2 3.3 8 ND (Chromium (VI) 218.6 ug/L 5 1.96 10 ND (1Cobalt 200.7 ug/L 2 1.1 20 490Copper 200.8 ug/L 2 0.96 4 110
A-28 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Iron 200.7 ug/L 2 32 200 42 Lead 200.8 ug/L 2 0.73 2 ND (Magnesium 200.7 ug/L 500 5,400 100,000 11,000,Manganese 200.7 ug/L 500 130 5,000 170,0Mercury 1631E ng/L 500 124 260 1,60Molybdenum 200.7 ug/L 2 1.6 40 130Nickel 200.8 ug/L 50 22 100 2,50Selenium 200.8 ug/L 5 1.6 10 330Silver 200.8 ug/L 2 0.59 2 ND (Sodium 200.7 ug/L 2 180 10,000 480,0Thallium 200.8 ug/L 2 0.47 2 49Tin 200.7 ug/L 2 4.8 200 ND (2Titanium 200.7 ug/L 2 1.6 20 1.8 Vanadium 200.8 ug/L 2 1.7 10 20Zinc 200.8 ug/L 200 410 1,000 11,00Metals - Filtered AqueousAluminum 200.7 ug/L 2 9.4 200 40,00Antimony 200.8 ug/L 2 0.72 2 3.6Arsenic 200.8 ug/L 2 1.2 4 7.2Barium 200.7 ug/L 2 2.5 20 80Beryllium 200.7 ug/L 2 0.71 2 10
A-29 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Boron 200.7 ug/L 50 170 5,000 880,0Cadmium 200.8 ug/L 2 1.2 4 500Calcium 200.7 ug/L 2 69 400 570,0Chromium 200.8 ug/L 2 3.3 8 ND (Cobalt 200.7 ug/L 2 1.1 20 500Copper 200.8 ug/L 2 0.96 4 86Iron 200.7 ug/L 2 32 200 ND (2Lead 200.8 ug/L 2 0.73 2 0.82 Magnesium 200.7 ug/L 50 540 10,000 12,000,Manganese 200.7 ug/L 50 13 500 160,0Mercury 1631E ng/L 500 124 260 3,64Molybdenum 200.7 ug/L 2 1.6 40 150Nickel 200.8 ug/L 2 0.89 4 2,40Selenium 200.8 ug/L 10 3.1 20 410Silver 200.8 ug/L 2 0.59 2 ND (Sodium 200.7 ug/L 2 180 10,000 500,0Thallium 200.8 ug/L 2 0.47 2 34Tin 200.7 ug/L 2 4.8 200 ND (2Titanium 200.7 ug/L 2 1.6 20 ND (2Vanadium 200.8 ug/L 2 1.7 10 14Zinc 200.8 ug/L 10 20 50 11,00Metals - Solid (dry weight)
A-30 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Aluminum 6010B mg/kg 1 1.4 9.3 22,00Antimony 6020 mg/kg 2 0.027 0.39 0.16 Arsenic 6020 mg/kg 20 0.98 12 44Barium 6010B mg/kg 1 0.071 0.93 350 Beryllium 6010B mg/kg 1 0.031 0.47 1.1Boron 6010B mg/kg 5 4.6 47 950 Cadmium 6020 mg/kg 2 0.018 0.19 2Calcium 6010B mg/kg 5 66 230 52,00Chromium 6020 mg/kg 20 1.5 3.9 150 Cobalt 6010B mg/kg 1 0.093 0.93 5.7Copper 6020 mg/kg 20 1.4 4.9 54Iron 6010B mg/kg 1 3.6 14 35,00Lead 6020 mg/kg 20 0.35 2.9 30Magnesium 6010B mg/kg 1 3.5 19 23,00Manganese 6010B mg/kg 1 0.093 0.93 300Mercury FGS-069 ng/g 4,000 72.1 199 5,99Molybdenum 6010B mg/kg 1 0.24 1.9 17Nickel 6020 mg/kg 2 0.049 0.29 47Selenium 6020 mg/kg 2 0.26 0.97 100Silver 6020 mg/kg 2 0.039 0.19 0.14 Sodium 6010B mg/kg 1 55 470 1,30
A-31 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. Max – Maximum value. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Thallium 6020 mg/kg 2 0.0068 0.19 2.1 Tin 6010B mg/kg 1 0.85 9.3 2.4 Titanium 6010B mg/kg 1 0.13 0.93 140 Vanadium 6020 mg/kg 20 0.75 9.7 150 Zinc 6020 mg/kg 2 0.61 1.9 340 
A-32 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Classical Pollutants - TotalAmmonia 350.1 mg/l NA 0.178 2 6.06Nitrate Nitrite as N 353.2 mg/l NA 0.179 1.1 82.8Nitrogen, Total Kjeldahl 351.2 mg/l NA 2.64 14.5 40.8Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) Chemical Oxygen Demand 410.4 mg/L 10 41 200 720Chloride 300.0 mg/L 500 130 1,500 9,600Sulfate 300.0 mg/L 500 120 2,500 24,000Cyanide, Total 4500 CN E mg/l NA 0.0202 0.101 0.198Total Dissolved Solids 2540C mg/L 1 470 1,000 50,000Total Suspended Solids 2540D mg/L 1 92 330 19,000Phosphorus, Total 365.1 mg/l NA 0.163 1 6.52Classicals Pollutants - Solid (dry weight)Ammonia 350.1 mg/Kg 1 4.1 10 23 Nitrate Nitrite as N 353.2 mg/Kg 1 0.35 9.9 65 Nitrogen, Total Kjeldahl 351.2 mg/Kg 10 120 520 900 Cyanide, Total 4500 CN E mg/Kg 1 0.11 0.54 0.42 Phosphorus, Total 365.1 mg/Kg 10 8.3 50 340 Classicals Pollutants -Filtered AqueousAmmonia 350.1 mg/L 1 0.11 2 6.2 
A-33 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 90 Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.38 5 26 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.21 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.012 Metals - Calculated TotalAluminum 200.7, 6010B ug/L NA 44.9 411 497,000Antimony 200.8, 6020 ug/L NA 1.19 9.47 4.95Arsenic 200.8, 6020 ug/L NA 26 291 695Barium 200.7, 6010B ug/L NA 4.09 41.1 6,410Beryllium 200.7, 6010B ug/L NA 1.43 13.7 22.4Boron 200.7, 6010B ug/L NA 271 5,720 762,000Cadmium 200.8, 6020 ug/L NA 1.45 7.46 396Calcium 200.7, 6010B ug/L NA 407 1,550 1,140,000Chromium 200.8, 6020 ug/L NA 39.4 103 3,640Cobalt 200.7, 6010B ug/L NA 3.3 41.1 459Copper 200.8, 6020 ug/L NA 35.3 122 1,210Iron 200.7, 6010B ug/L NA 121 545 766,000Lead 200.8, 6020 ug/L NA 9.28 72.7 651Magnesium 200.7, 6010B ug/L NA 578 9,540 9,010,000Manganese 200.7, 6010B ug/L NA 14.1 476 96,000
A-34 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Mercury 1631E, FGS-069 ng/L NA 691 1,830 44,000Molybdenum 200.7, 6010B ug/L NA 7.58 84.1 406Nickel 200.8, 6020 ug/L NA 1.76 9.37 2,560Selenium 200.8, 6020 ug/L NA 5.54 22.6 2,920Silver 200.8, 6020 ug/L NA 1.3 5.64 2.3Sodium 200.7, 6010B ug/L NA 1,580 20,900 404,000Thallium 200.8, 6020 ug/L NA 0.56 5.64 46.2Tin 200.7, 6010B ug/L NA 25.4 411 44.1Titanium 200.7, 6010B ug/L NA 4.9 41.1 1,820Vanadium 200.8, 6020 ug/L NA 19.7 239 3,270Zinc 200.8, 6020 ug/L NA 168 524 14,500Metals - DissolvedAluminum 200.7 ug/L 2 9.4 200 2,800 Antimony 200.8 ug/L 2 0.72 2 2.8Arsenic 200.8 ug/L 2 1.2 4 5.5Barium 200.7 ug/L 2 2.5 20 150Beryllium 200.7 ug/L 2 0.71 2 4.6Boron 200.7 ug/L 500 1,700 50,000 730,000Cadmium 200.8 ug/L 5 2.9 10 420Calcium 200.7 ug/L 2 69 400 640,000
A-35 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Chromium 200.8 ug/L 2 3.3 8 ND (8) Chromium (VI) 218.6 ug/L 5 1.96 10 ND (10) Cobalt 200.7 ug/L 2 1.1 20 380Copper 200.8 ug/L 2 0.96 4 55Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 500 5,400 100,000 8,900,000Manganese 200.7 ug/L 500 130 5,000 110,000Mercury 1631E ng/L 500 124 260 1,990Molybdenum 200.7 ug/L 2 1.6 40 90Nickel 200.8 ug/L 25 11 50 2,000Selenium 200.8 ug/L 5 1.6 10 300Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 400,000Thallium 200.8 ug/L 2 0.47 2 26Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 2 Vanadium 200.8 ug/L 2 1.7 10 16 Zinc 200.8 ug/L 25 51 120 7,600Metals - Filtered Aqueous
A-36 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Aluminum 200.7 ug/L 2 9.4 200 20,000 Antimony 200.8 ug/L 2 0.72 2 2.5Arsenic 200.8 ug/L 2 1.2 4 5.9Barium 200.7 ug/L 2 2.5 20 100Beryllium 200.7 ug/L 2 0.71 2 3.6Boron 200.7 ug/L 50 170 5,000 820,000 Cadmium 200.8 ug/L 2 1.2 4 380Calcium 200.7 ug/L 2 69 400 600,000 Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 390Copper 200.8 ug/L 2 0.96 4 72Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 50 540 10,000 9,500,000Manganese 200.7 ug/L 50 13 500 100,000 Mercury 1631E ng/L 500 124 260 4,370Molybdenum 200.7 ug/L 2 1.6 40 110Nickel 200.8 ug/L 2 0.89 4 1,700Selenium 200.8 ug/L 2 0.62 4 470Silver 200.8 ug/L 2 0.59 2 ND (2) 
A-37 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Sodium 200.7 ug/L 2 180 10,000 420,000Thallium 200.8 ug/L 2 0.47 2 15Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 14Zinc 200.8 ug/L 10 20 50 6,700 Metals - Solid (dry weight)Aluminum 6010B mg/kg 1 1.9 12 25,000Antimony 6020 mg/kg 2 0.028 0.4 0.14 Arsenic 6020 mg/kg 25 1.3 15 36Barium 6010B mg/kg 1 0.095 1.2 330 Beryllium 6010B mg/kg 1 0.041 0.62 1Boron 6010B mg/kg 5 6.1 62 990 Cadmium 6020 mg/kg 2 0.019 0.2 2.7Calcium 6010B mg/kg 1 18 62 31,000 Chromium 6020 mg/kg 25 1.9 5 190 Cobalt 6010B mg/kg 1 0.12 1.2 5.5Copper 6020 mg/kg 25 1.8 6.2 60Iron 6010B mg/kg 1 4.8 19 40,000Lead 6020 mg/kg 25 0.45 3.7 34
A-38 

NA – Not applicable. Total results is based on calculated result from solid and aqueous phases. ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. H – Sample was prepared/analyzed beyond the specified holding time. J – Result measured above the MDL, but less than the quantitation limit. P – Sample was not preserved immediately following collection. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentr

Magnesium 6010B mg/kg 1 4.6 25 21,000Manganese 6010B mg/kg 1 0.12 1.2 280Mercury FGS-069 ng/g 4,000 71.9 198 4,990Molybdenum 6010B mg/kg 1 0.32 2.5 16Nickel 6020 mg/kg 2 0.05 0.3 53Selenium 6020 mg/kg 2 0.26 0.99 130Silver 6020 mg/kg 2 0.04 0.2 0.12 Sodium 6010B mg/kg 1 74 620 1,200Thallium 6020 mg/kg 2 0.007 0.2 1.7 Tin 6010B mg/kg 1 1.1 12 2.3 Titanium 6010B mg/kg 1 0.18 1.2 95Vanadium 6020 mg/kg 25 0.95 12 170Zinc 6020 mg/kg 25 7.8 25 440
A-39 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentratio

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 4.8Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 55Nitrogen, Total Kjeldahl 351.2 mg/L 4 0.31 4 21 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 6.7Chemical Oxygen Demand 410.4 mg/L 10 41 200 570Chloride 300.0 mg/L 500 130 1,500 5,300Sulfate 300.0 mg/L 500 120 2,500 8,400Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.21 Total Dissolved Solids 2540C mg/L 1 47 100 29,000Total Suspended Solids 2540D mg/L 1 1.1 4 17Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.096 Total MetalsAluminum 200.7 ug/L 2 9.4 200 180 Antimony 200.8 ug/L 2 0.72 2 6.8Arsenic 200.8 ug/L 2 1.2 4 4.3Barium 200.7 ug/L 2 2.5 20 150Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 500 1,700 50,000 300,000 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 890,000Chromium 200.8 ug/L 2 3.3 8 17Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 ND (4) 
A-40 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentratio

Iron 200.7 ug/L 2 32 200 110 Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 50 540 10,000 5,600,000 Manganese 200.7 ug/L 2 0.51 20 170 Mercury 1631E ng/L 20 4.87 10.2 101Molybdenum 200.7 ug/L 2 1.6 40 220Nickel 200.8 ug/L 2 0.89 4 3.4 Selenium 200.8 ug/L 2 0.62 4 560Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 370,000Thallium 200.8 ug/L 2 0.47 2 14Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 16Zinc 200.8 ug/L 2 4.1 10 ND (10) Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) Antimony 200.8 ug/L 2 0.72 2 7.8Arsenic 200.8 ug/L 2 1.2 4 4.8Barium 200.7 ug/L 2 2.5 20 140Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 50 170 5,000 300,000 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 880,000
A-41 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Concentratio

Chromium 200.8 ug/L 2 3.3 8 14Chromium (VI) 218.6 ug/L 1 0.39 2 7.04Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 1.4 Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 50 540 10,000 5,500,000Manganese 200.7 ug/L 2 0.51 20 160 Mercury 1631E ng/L 20 4.87 10.2 49.7Molybdenum 200.7 ug/L 2 1.6 40 210Nickel 200.8 ug/L 2 0.89 4 2.2 Selenium 200.8 ug/L 2 0.62 4 560Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 350,000Thallium 200.8 ug/L 2 0.47 2 14Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 5 4.1 50 ND (50) Vanadium 200.8 ug/L 2 1.7 10 16Zinc 200.8 ug/L 2 4.1 10 ND (10) 
A-42 

ND – Not detected (number in parentheses is the quantitation limit). 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). V – Serial dilution is not within control limits. 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Conce

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 5.3Nitrate Nitrite as N 353.2 mg/L 50 0.95 5 290Nitrogen, Total Kjeldahl 351.2 mg/L 4 0.31 4 21 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 8.4Chemical Oxygen Demand 410.4 mg/L 10 41 200 400Chloride 300.0 mg/L 500 130 1,500 7,500Sulfate 300.0 mg/L 500 120 2,500 13,000Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 2.4 Total Dissolved Solids 2540C mg/L 1 47 100 32,000Total Suspended Solids 2540D mg/L 1 1.1 4 10Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.18 Total MetalsAluminum 200.7 ug/L 2 9.4 200 260Antimony 200.8 ug/L 2 0.72 2 6.9Arsenic 200.8 ug/L 2 1.2 4 5.6Barium 200.7 ug/L 2 2.5 20 150Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 100 330 10,000 320,000 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 840,000 
A-43 

ND – Not detected (number in parentheses is the quantitation limit). 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). V – Serial dilution is not within control limits. 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Conce

Chromium 200.8 ug/L 2 3.3 8 16Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 ND (4) Iron 200.7 ug/L 2 32 200 110 Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 100 1,100 20,000 5,500,000 Manganese 200.7 ug/L 2 0.51 20 88 Mercury 1631E ng/L 20 4.87 10.2 99.8Molybdenum 200.7 ug/L 2 1.6 40 200Nickel 200.8 ug/L 2 0.89 4 3.3 Selenium 200.8 ug/L 2 0.62 4 540 Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 360,000 Thallium 200.8 ug/L 2 0.47 2 14Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 17Zinc 200.8 ug/L 2 4.1 10 ND (10) Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 24 Antimony 200.8 ug/L 2 0.72 2 6.8
A-44 

ND – Not detected (number in parentheses is the quantitation limit). 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). V – Serial dilution is not within control limits. 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Conce

Arsenic 200.8 ug/L 2 1.2 4 3.8 Barium 200.7 ug/L 2 2.5 20 150Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 50 170 5,000 330,000 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 860,000Chromium 200.8 ug/L 2 3.3 8 14Chromium (VI) 218.6 ug/L 1 0.39 2 7.32Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 ND (4) Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 50 540 10,000 5,900,000 Manganese 200.7 ug/L 2 0.51 20 87 Mercury 1631E ng/L 20 4.97 10.4 63.1Molybdenum 200.7 ug/L 2 1.6 40 200Nickel 200.8 ug/L 2 0.89 4 2.2 Selenium 200.8 ug/L 2 0.62 4 520 Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 360,000Thallium 200.8 ug/L 2 0.47 2 14
A-45 

ND – Not detected (number in parentheses is the quantitation limit). 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. MI – Matrix interferences present. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). V – Serial dilution is not within control limits. 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific 

MDL

SampleSpecific 

QL Conce

Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 4.5 Vanadium 200.8 ug/L 2 1.7 10 16Zinc 200.8 ug/L 2 4.1 10 ND (10) 
A-46 

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

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 5.5Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 58Nitrogen, Total Kjeldahl 351.2 mg/L 4 0.31 4 21 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 6.9 Chemical Oxygen Demand 410.4 mg/L 10 41 200 56Chloride 300.0 mg/L 500 130 1,500 7,30Sulfate 300.0 mg/L 500 120 2,500 13,0Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.6 Total Dissolved Solids 2540C mg/L 1 47 100 28,0Total Suspended Solids 2540D mg/L 1 1.1 4 8.4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.1Total MetalsAluminum 200.7 ug/L 2 9.4 200 33Antimony 200.8 ug/L 2 0.72 2 5.7Arsenic 200.8 ug/L 2 1.2 4 4.9Barium 200.7 ug/L 2 2.5 20 16Beryllium 200.7 ug/L 2 0.71 2 ND Boron 200.7 ug/L 100 330 10,000 320,0Cadmium 200.8 ug/L 2 1.2 4 ND Calcium 200.7 ug/L 2 69 400 840,0Chromium 200.8 ug/L 2 3.3 8 14Cobalt 200.7 ug/L 2 1.1 20 ND (Copper 200.8 ug/L 2 0.96 4 ND Iron 200.7 ug/L 2 32 200 26
A-47 

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

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Lead 200.8 ug/L 2 0.73 2 ND Magnesium 200.7 ug/L 100 1,100 20,000 5,500Manganese 200.7 ug/L 2 0.51 20 28Mercury 1631E ng/L 100 24.4 51 14Molybdenum 200.7 ug/L 2 1.6 40 18Nickel 200.8 ug/L 2 0.89 4 2.9 Selenium 200.8 ug/L 10 3.1 20 80Silver 200.8 ug/L 2 0.59 2 ND Sodium 200.7 ug/L 2 180 10,000 360,0Thallium 200.8 ug/L 2 0.47 2 14Tin 200.7 ug/L 2 4.8 200 ND (2Titanium 200.7 ug/L 2 1.6 20 7.5 Vanadium 200.8 ug/L 2 1.7 10 16Zinc 200.8 ug/L 2 4.1 10 ND (Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 ND (2Antimony 200.8 ug/L 2 0.72 2 6.6Arsenic 200.8 ug/L 2 1.2 4 4.8Barium 200.7 ug/L 2 2.5 20 15Beryllium 200.7 ug/L 2 0.71 2 ND Boron 200.7 ug/L 50 170 5,000 320,0Cadmium 200.8 ug/L 2 1.2 4 ND Calcium 200.7 ug/L 2 69 400 840,0Chromium 200.8 ug/L 2 3.3 8 15 Chromium (VI) 218.6 ug/L 1 0.39 2 7.6
A-48 

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

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Cobalt 200.7 ug/L 2 1.1 20 ND (Copper 200.8 ug/L 2 0.96 4 ND Iron 200.7 ug/L 2 32 200 ND (2Lead 200.8 ug/L 2 0.73 2 ND Magnesium 200.7 ug/L 50 540 10,000 5,600Manganese 200.7 ug/L 2 0.51 20 25Mercury 1631E ng/L 20 4.87 10.2 71.Molybdenum 200.7 ug/L 2 1.6 40 17Nickel 200.8 ug/L 2 0.89 4 2.3 Selenium 200.8 ug/L 10 3.1 20 64Silver 200.8 ug/L 2 0.59 2 ND Sodium 200.7 ug/L 2 180 10,000 350,0Thallium 200.8 ug/L 2 0.47 2 13Tin 200.7 ug/L 2 4.8 200 ND (2Titanium 200.7 ug/L 2 1.6 20 4.6 Vanadium 200.8 ug/L 2 1.7 10 14 Zinc 200.8 ug/L 2 4.1 10 ND (
A-49 

ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. S – Seed correction blank recovery low. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 5.Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 6Nitrogen, Total Kjeldahl 351.2 mg/L 4 0.31 4 24 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 4.Chemical Oxygen Demand 410.4 mg/L 10 41 200 51Chloride 300.0 mg/L 500 130 1,500 7,4Sulfate 300.0 mg/L 500 120 2,500 14,0Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 1.Total Dissolved Solids 2540C mg/L 1 47 100 33,0Total Suspended Solids 2540D mg/L 1 2.2 8 22Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.0Total MetalsAluminum 200.7 ug/L 2 9.4 200 53 Antimony 200.8 ug/L 2 0.72 2 5.Arsenic 200.8 ug/L 2 1.2 4 4.Barium 200.7 ug/L 2 2.5 20 15Beryllium 200.7 ug/L 2 0.71 2 ND Boron 200.7 ug/L 100 330 10,000 330,Cadmium 200.8 ug/L 2 1.2 4 ND Calcium 200.7 ug/L 2 69 400 800,Chromium 200.8 ug/L 2 3.3 8 16Cobalt 200.7 ug/L 2 1.1 20 ND (Copper 200.8 ug/L 2 0.96 4 ND Iron 200.7 ug/L 2 32 200 13Lead 200.8 ug/L 2 0.73 2 ND 
A-50 

ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. S – Seed correction blank recovery low. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Magnesium 200.7 ug/L 100 1,100 20,000 5,700Manganese 200.7 ug/L 2 0.51 20 10Mercury 1631E ng/L 100 24.1 50.5 16Molybdenum 200.7 ug/L 2 1.6 40 15Nickel 200.8 ug/L 2 0.89 4 2.Selenium 200.8 ug/L 2 0.62 4 48Silver 200.8 ug/L 2 0.59 2 ND Sodium 200.7 ug/L 2 180 10,000 360,Thallium 200.8 ug/L 2 0.47 2 12Tin 200.7 ug/L 2 4.8 200 ND (Titanium 200.7 ug/L 2 1.6 20 6.Vanadium 200.8 ug/L 2 1.7 10 18Zinc 200.8 ug/L 2 4.1 10 ND (Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 ND (Antimony 200.8 ug/L 2 0.72 2 5.Arsenic 200.8 ug/L 2 1.2 4 4.Barium 200.7 ug/L 2 2.5 20 15Beryllium 200.7 ug/L 2 0.71 2 ND Boron 200.7 ug/L 50 170 5,000 330,Cadmium 200.8 ug/L 2 1.2 4 ND Calcium 200.7 ug/L 2 69 400 820,Chromium 200.8 ug/L 2 3.3 8 15 Chromium (VI) 218.6 ug/L 1 0.39 2 6.7Cobalt 200.7 ug/L 2 1.1 20 ND (Copper 200.8 ug/L 2 0.96 4 ND 
A-51 

ND – Not detected (number in parentheses is the quantitation limit). * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. S – Seed correction blank recovery low. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL Co

Iron 200.7 ug/L 2 32 200 ND (Lead 200.8 ug/L 2 0.73 2 ND Magnesium 200.7 ug/L 50 540 10,000 6,000Manganese 200.7 ug/L 2 0.51 20 93 Mercury 1631E ng/L 20 4.83 10.1 84Molybdenum 200.7 ug/L 2 1.6 40 15Nickel 200.8 ug/L 2 0.89 4 1.Selenium 200.8 ug/L 2 0.62 4 53Silver 200.8 ug/L 2 0.59 2 ND Sodium 200.7 ug/L 2 180 10,000 360,Thallium 200.8 ug/L 2 0.47 2 12Tin 200.7 ug/L 2 4.8 200 ND (Titanium 200.7 ug/L 2 1.6 20 4.Vanadium 200.8 ug/L 2 1.7 10 15 Zinc 200.8 ug/L 2 4.1 10 ND (
A-52 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 50 0.95 5 Nitrogen, Total Kjeldahl 351.2 mg/L 4 0.31 4 Biochemical Oxygen Demand 5210B mg/L 1 0.59 5 Chemical Oxygen Demand 410.4 mg/L 10 41 200 Chloride 300.0 mg/L 500 130 1,500 Sulfate 300.0 mg/L 500 120 2,500 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 100 330 10,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 100 1,100 20,000 Manganese 200.7 ug/L 2 0.51 20 
A-53 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL 

Mercury 1631E ng/L 20 4.87 10.2 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 0.39 2 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 
A-54 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution 

Factor

SampleSpecific MDL Sample- Specific QL 

Mercury 1631E ng/L 20 4.87 10.2 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 5 1.6 10 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 10 8.2 100 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

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

A-55 

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-56 

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

Analyte Method Process Units Concentration 

Iron EPA 1638 Total Recoverable ug/L ND (10) 

Lead EPA 1638 Total Recoverable ug/L ND (0.040) 

Magnesium EPA 1638 Total Recoverable ug/L ND (2.5) 

Manganese EPA 1638 Total Recoverable ug/L ND (0.10) 

Molybdenum EPA 1638 Total Recoverable ug/L ND (0.060) 

Nickel EPA 1638 Total Recoverable ug/L ND (0.10) 

Selenium EPA 1638 Total Recoverable ug/L ND (0.60) 

Silver EPA 1638 Total Recoverable ug/L ND (0.020) 

Sodium EPA 1638 Total Recoverable ug/L ND (20) 

Thallium EPA 1638 Total Recoverable ug/L ND (0.0050) 

Tin EPA 1638 Total Recoverable ug/L ND (0.10) 

Titanium EPA 1638 Total Recoverable ug/L ND (0.50) 

Vanadium EPA 1638 Total Recoverable ug/L ND (0.10) 

Zinc EPA 1638 Total Recoverable ug/L ND (0.20) 

125 ml Glass Bottles – Bottle Blank (for mercury composite samples)

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

250 ml Glass Bottles – Bottle Blank (for mercury grab samples)

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

LDPE 10 L Composite Bottles – Bottle Blank (sample composite bottle for dissolved/filtration pump-off)

Aluminuma EPA 1638 Dissolved ug/L 4.71 

Antimony EPA 1638 Dissolved ug/L ND (0.50) 

Arsenic EPA 1638 Dissolved ug/L ND (0.50) 

Barium EPA 1638 Dissolved ug/L ND (0.10) 

Beryllium EPA 1638 Dissolved ug/L ND (0.10) 

Cadmium EPA 1638 Dissolved ug/L ND (0.10) 

Chromium EPA 1638 Dissolved ug/L ND (1.0) 

Cobalt EPA 1638 Dissolved ug/L ND (0.10) 

Copper EPA 1638 Dissolved ug/L ND (0.30) 

Lead EPA 1638 Dissolved ug/L ND (0.050) 

Manganese EPA 1638 Dissolved ug/L ND (0.50) 

Molybdenum EPA 1638 Dissolved ug/L ND (0.50) 

Nickel EPA 1638 Dissolved ug/L ND (0.50) 

Selenium EPA 1638 Dissolved ug/L ND (2.0) 

Silver EPA 1638 Dissolved ug/L ND (0.10) 

Thallium EPA 1638 Dissolved ug/L ND (0.050) 

Vanadium EPA 1638 Dissolved ug/L ND (1.0) 

Zinc EPA 1638 Dissolved ug/L ND (0.50) 

LDPE 20 L Composite Bottles – Bottle Blank (sample composite bottle for dissolved/filtration pump-off)

Aluminum EPA 1638 Dissolved ug/L ND (2.0) 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

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

A-57 

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

Analyte Method Process Units Concentration 

Antimony EPA 1638 Dissolved ug/L ND (0.50) 

Arsenic EPA 1638 Dissolved ug/L ND (0.50) 

Barium EPA 1638 Dissolved ug/L ND (0.10) 

Beryllium EPA 1638 Dissolved ug/L ND (0.10) 

Cadmium EPA 1638 Dissolved ug/L ND (0.10) 

Chromium EPA 1638 Dissolved ug/L ND (1.0) 

Cobalt EPA 1638 Dissolved ug/L ND (0.10) 

Copper EPA 1638 Dissolved ug/L ND (0.30) 

Lead EPA 1638 Dissolved ug/L ND (0.050) 

Manganese EPA 1638 Dissolved ug/L ND (0.50) 

Molybdenum EPA 1638 Dissolved ug/L ND (0.50) 

Nickel EPA 1638 Dissolved ug/L ND (0.50) 

Selenium EPA 1638 Dissolved ug/L ND (2.0) 

Silver EPA 1638 Dissolved ug/L ND (0.10) 

Thallium EPA 1638 Dissolved ug/L ND (0.050) 

Vanadium EPA 1638 Dissolved ug/L ND (1.0) 

Zinc EPA 1638 Dissolved ug/L ND (0.50) 

Sample Tap Tubing Set – Equipment Blank (seven feet of #73 silicone tubing, Y-splitter, and two pieces of 5 

feet of #24 silicone tubing for sample collection for mercury and metals from sample taps) 

Aluminum EPA 1638 Total Recoverable ug/L ND (4.0) 

Antimony EPA 1638 Total Recoverable ug/L ND (0.020) 

Arsenic EPA 1638 Total Recoverable ug/L ND (0.15) 

Barium EPA 1638 Total Recoverable ug/L ND (0.20) 

Beryllium EPA 1638 Total Recoverable ug/L ND (0.060) 

Boron EPA 1638 Total Recoverable ug/L ND (3.0) 

Cadmium EPA 1638 Total Recoverable ug/L ND (0.020) 

Calcium EPA 1638 Total Recoverable ug/L ND (40) 

Chromium EPA 1638 Total Recoverable ug/L ND (0.10) 

Cobalt EPA 1638 Total Recoverable ug/L ND (0.10) 

Copper EPA 1638 Total Recoverable ug/L ND (0.10) 

Iron EPA 1638 Total Recoverable ug/L ND (10) 

Lead EPA 1638 Total Recoverable ug/L ND (0.040) 

Magnesium EPA 1638 Total Recoverable ug/L ND (2.5) 

Manganese EPA 1638 Total Recoverable ug/L ND (0.10) 

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

Molybdenum EPA 1638 Total Recoverable ug/L ND (0.060) 

Nickel EPA 1638 Total Recoverable ug/L ND (0.10) 

Selenium EPA 1638 Total Recoverable ug/L ND (0.60) 

Silver EPA 1638 Total Recoverable ug/L ND (0.020) 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

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

A-58 

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

Analyte Method Process Units Concentration 

Sodium EPA 1638 Total Recoverable ug/L ND (20) 

Thallium EPA 1638 Total Recoverable ug/L ND (0.0050) 

Tin EPA 1638 Total Recoverable ug/L ND (0.10) 

Titanium EPA 1638 Total Recoverable ug/L ND (0.50) 

Vanadium EPA 1638 Total Recoverable ug/L ND (0.10) 

Zinc EPA 1638 Total Recoverable ug/L ND (0.20) 

Pump-Off Tubing Set – Equipment Blank (Three feet of Teflon® tubing, 10 feet of #73 silicone tubing, Ysplitter, and two pieces of 5 feet of #24 silicone tubing for total and dissolved sample collection for metals)

Aluminum EPA 1638 Total Recoverable ug/L ND (4.0) 

Antimony EPA 1638 Total Recoverable ug/L ND (0.020) 

Arsenic EPA 1638 Total Recoverable ug/L ND (0.15) 

Barium EPA 1638 Total Recoverable ug/L ND (0.20) 

Beryllium EPA 1638 Total Recoverable ug/L ND (0.060) 

Boron EPA 1638 Total Recoverable ug/L ND (3.0) 

Cadmium EPA 1638 Total Recoverable ug/L ND (0.020) 

Calcium EPA 1638 Total Recoverable ug/L ND (40) 

Chromium EPA 1638 Total Recoverable ug/L ND (0.10) 

Cobalt EPA 1638 Total Recoverable ug/L ND (0.10) 

Copper EPA 1638 Total Recoverable ug/L ND (0.10) 

Iron EPA 1638 Total Recoverable ug/L ND (10) 

Lead EPA 1638 Total Recoverable ug/L ND (0.040) 

Magnesium EPA 1638 Total Recoverable ug/L ND (2.5) 

Manganese EPA 1638 Total Recoverable ug/L ND (0.10) 

Mercury EPA 1631E Total Recoverable ug/L ND (0.00050) 

Molybdenum EPA 1638 Total Recoverable ug/L ND (0.060) 

Nickel EPA 1638 Total Recoverable ug/L ND (0.10) 

Selenium EPA 1638 Total Recoverable ug/L ND (0.60) 

Silver EPA 1638 Total Recoverable ug/L ND (0.020) 

Sodium EPA 1638 Total Recoverable ug/L ND (20) 

Thallium EPA 1638 Total Recoverable ug/L ND (0.0050) 

Tin EPA 1638 Total Recoverable ug/L ND (0.10) 

Titanium EPA 1638 Total Recoverable ug/L ND (0.50) 

Vanadium EPA 1638 Total Recoverable ug/L ND (0.10) 

Zinc EPA 1638 Total Recoverable ug/L ND (0.20) 

T-Splitter Tubing Set – Equipment Blank (Ten feet of #73 silicone tubing, T-splitter, six feet of #73 silicone 

tubing, and 15 feet of #73 silicone tubing for total and dissolved sample collection for metal composites)

Aluminum EPA 1638 Total Recoverable ug/L ND (4.0) 

Antimony EPA 1638 Total Recoverable ug/L ND (0.020) 

Arsenic EPA 1638 Total Recoverable ug/L ND (0.15) 
a

 Aluminum was detected in two equipment blanks for the 10-liter composite container at 2.53 ug/L and 4.71 ug/L. 

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

A-59 

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-60 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL C

Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 NBeryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 NCopper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 Molybdenum 200.7 ug/L 2 1.6 40 NNickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 ND Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 NTitanium 200.7 ug/L 2 1.6 20 NVanadium 200.8 ug/L 2 1.7 10 NZinc 200.8 ug/L 2 4.1 10 NDissolved MetalsAluminum 200.7 ug/L 2 9.4 200 NAntimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 
A-61 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL C

Barium 200.7 ug/L 2 2.5 20 NBeryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 0.39 2 Cobalt 200.7 ug/L 2 1.1 20 NCopper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 NLead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Molybdenum 200.7 ug/L 2 1.6 40 NNickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 NTitanium 200.7 ug/L 2 1.6 20 NVanadium 200.8 ug/L 2 1.7 10 NZinc 200.8 ug/L 2 4.1 10 N
A-62 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. Est – Estimated value. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL 

Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 
A-63 

ND – Not detected (number in parentheses is the quantitation limit). B – Analyte was found in the blank and sample. Est – Estimated value. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL 

Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 1 0.39 2 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.8 ug/L 2 4.1 10 
A-64 

ND – Not detected (number in parentheses is the quantitation limit). U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL 

Total MetalsMercury 1631E ng/L 1 0.24 0.5 
A-65 

ND – Not detected (number in parentheses is the quantitation limit). U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL C

Total MetalsMercury 1631E ng/L 1 0.24 0.5 N
A-66 

ND – Not detected (number in parentheses is the quantitation limit). U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units Dilution Factor Sample-Specific MDL Sample-Specific QL C

Total MetalsMercury 1631E ng/L 1 0.24 0.5 N
Appendix B

DATA REVIEW NARRATIVES
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

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

Deb Bartram, ERG

TJ Finseth, ERG

From: Randy Mercurio, ERG

Donna Tedder, ERG

Date: 9/1/2011

Subject: FGS Data Review Narrative for Total and Dissolved Mercury – Episode 6560

Frontier Global Sciences (FGS) generated analytical data for total and dissolved mercury. 

FGS analyzed the samples according to EPA Method 1631E for mercury by Cold Vapor 

Atomic Fluorescence Spectrometry (CVAFS) analysis.

Table 1 summarizes the 27 samples (excluding laboratory filter blanks) FGS extracted 

and analyzed for total and dissolved mercury.

Table 1. EPA Episode 6560 Total & Dissolved Mercury – Sample Identification

EPA 

Sample #

Lab Sample 

ID #

Sample 

Matrix Sample Description

Sampling 

Date

71741 1007078-01 Aqueous FGD Influent Day 1 7/12/2010

71741 1007078-08 Solid FGD Influent, Day 1 (Solids) 7/12/2010

71741 1007078-06 Aqueous Dissolved FGD Influent, Day 1 7/12/2010

71742 1007095-01 Aqueous FGD Influent, Day 2 7/13/2010

71742 1007095-11 Solid FGD Influent, Day 2 (Solids) 7/13/2010

71742 1007095-02 Aqueous Dissolved FGD Influent, Day 2 7/13/2010

71743 1007105-04 Aqueous FGD Influent, Day 3 7/14/2010

71743 1007105-11 Solid FGD Influent, Day 3 (Solids) 7/14/2010

71743 1007105-05 Aqueous Dissolved FGD Influent, Day 3 7/14/2010

71744 1007121-01 Aqueous FGD Influent, Day 4 7/15/2010

71744 1007121-09 Solid FGD Influent, Day 4 (Solids) 7/15/2010

71744 1007121-02 Aqueous Dissolved FGD Influent, Day 4 7/15/2010

71745 1007095-03 Aqueous FGD Effluent, Day 1 7/13/2010

71745 1007095-04 Aqueous Dissolved FGD Effluent, Day 1 7/13/2010

71746 1007105-06 Aqueous FGD Effluent, Day 2 7/14/2010

71746 1007105-07 Aqueous Dissolved FGD Effluent, Day 2 7/14/2010

71747 1007121-03 Aqueous FGD Effluent, Day 3 7/15/2010

71747 1007121-04 Aqueous Dissolved FGD Effluent, Day 3 7/15/2010

71748 1007131-02 Aqueous FGD Effluent, Day 4 7/16/2010
2

Table 1. EPA Episode 6560 Total & Dissolved Mercury – Sample Identification

EPA 

Sample #

Lab Sample 

ID #

Sample 

Matrix Sample Description

Sampling 

Date

71748 1007131-03 Aqueous Dissolved FGD Effluent, Day 4 7/16/2010

71749 1007105-08 Aqueous FGD Effluent Duplicate, Day 2 7/14/2010

71749 1007105-09 Aqueous Dissolved FGD Effluent Duplicate, Day 2 7/14/2010

71750 1007078-02 Aqueous FGD Influent Field Blank, Day 1 7/12/2010

71751 1007078-04 Aqueous FGD Effluent Field Blank Day 1 7/12/2010

71752 1007095-05 Aqueous FGD Effluent Field Blank, Day 2 7/13/2010

71753 1007105-03 Aqueous FGD Effluent Field Blank, Day 3 7/14/2010

71754 1007121-05 Aqueous FGD Effluent Field Blank, Day 4 7/15/2010

SUMMARY

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

There were no issues requiring qualifiers with the mercury data in this episode. ERG 

noted the following during the data review:

• An ongoing precision and recovery (OPR) sample was not analyzed at the 

beginning and end of the solid fraction sample analysis.

• A matrix spike (MS) and matrix spike duplicate (MSD) were not performed on a

solid sample fraction from this episode.

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES

There were no sample receipt issues in this data package.

INITIAL CALIBRATION

FGS performed the initial calibrations on each analysis day. The initial calibration for 

the CVAFS analysis consisted of a blank and five calibration standards with a correlation 

coefficient ≥0.995. All method specified criteria were met.

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

All initial and continuing calibration verifications (ICVs, CCVs) met method-specified

criteria.

BLANKS

All preparation blanks or laboratory reagent blanks (LRBs) and the continuing calibration 

blanks (CCBs) met method-specified criteria. 
3

DUPLICATES

Field duplicates, sample 71749, were collected on sample 71746. The 71746/71749 total 

mercury relative percent difference (RPD) was 9.72% and the dissolved mercury RPD

was 5.20%. The method-suggested RPD criterion between field duplicates is 20%.

Laboratory duplicates were performed on samples 71742, 71747, and 71748. All RPDs 

were less than 20% (the method-suggested RPD criterion between field duplicates; the 

method does not require the analysis of laboratory duplicates).

A laboratory duplicate was not performed on the solid sample fraction from this episode; 

however, FGS analyzed another client’s sample as the duplicate for this batch, which 

passed the method-specified criteria.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

MS and MSDs were performed on samples 71742, 71743, 71747, and 71748 for the total 

mercury analyses. MS and MSDs were performed on samples 71742 and 71747 for the 

dissolved mercury analyses. All aqueous MS/MSD recoveries were within method 

specifications of 71-125%. All RPDs met method-specified criteria.

An MS/MSD was not performed on a solid sample fraction from this episode. FGS 

performed an MS/MSD on another client’s sample that was not part of this episode, 

which met method-specified criteria.

DETECTION LIMITS

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

were reported as not detected (ND).
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

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

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Randy Mercurio, ERG 

Date: 9/1/2011

Subject: TestAmerica Data Review Narrative for Total and Dissolved Metals by 200.8 – 

Episode 6560

TestAmerica generated analytical data for total and dissolved metals (antimony, arsenic, 

cadmium, chromium, copper, lead, nickel, selenium, silver, thallium, vanadium and zinc). 

The samples were analyzed according to EPA Method 200.8. 

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

dissolved metals by EPA Method 200.8. 

Table 1. EPA Episode 6560 Total and Dissolved Metals – Sample Identification 

EPA 

Sample # 

EPA Sample Description Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71741 FGD Influent, Day 1 280-5257-1 Aqueous 7/12/2010 7/13/2010

71741 FGD Influent, Day 1 - Filtrate 280-5257-3 Aqueous 7/12/2010 7/13/2010

71741 FGD Influent, Day 1 - Solids 280-5257-4 Solid 7/12/2010 7/13/2010

71742 FGD Influent, Day 2 280-5302-1 Aqueous 7/13/2010 7/14/2010

71742 FGD Influent, Day 2 - Filtrate 280-5302-4 Aqueous 7/13/2010 7/14/2010

71742 FGD Influent, Day 2 - Solids 280-5302-5 Solid 7/13/2010 7/14/2010

71743 FGD Influent, Day 3 280-5343-1 Aqueous 7/14/2010 7/15/2010

71743 FGD Influent, Day 3 - Filtrate 280-5343-4 Aqueous 7/14/2010 7/15/2010

71743 FGD Influent, Day 3 - Solids 280-5343-5 Solid 7/14/2010 7/15/2010

71744 FGD Influent, Day 4 280-5398-1 Aqueous 7/15/2010 7/16/2010

71744 FGD Influent, Day 4 - Filtrate 280-5398-3 Aqueous 7/15/2010 7/16/2010

71744 FGD Influent, Day 4 - Solids 280-5398-4 Solid 7/15/2010 7/16/2010

71745 FGD Effluent, Day 2 280-5302-2 Aqueous 7/13/2010 7/14/2010

71746 FGD Effluent, Day 2 280-5343-2 Aqueous 7/14/2010 7/15/2010

71747 FGD Effluent, Day 3 280-5398-2 Aqueous 7/15/2010 7/16/2010

71748 FGD Effluent, Day 4 280-5438-1 Aqueous 7/16/2010 7/17/2010

71749 FGD Effluent Duplicate 280-5343-3 Aqueous 7/14/2010 7/15/2010

71750 FGD Influent Field Blank, 

Day 1 

280-5257-2 Aqueous 7/12/2010 7/13/2010
2

Table 1. EPA Episode 6560 Total and Dissolved Metals – Sample Identification 

EPA 

Sample # 

EPA Sample Description Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71751 FGD Effluent Field Blank, 

Day 1 

280-5302-3 Aqueous 7/13/2010 7/14/2010

SUMMARY 

The samples were prepared for total and dissolved metals analysis according to 

TestAmerica’s “FGD ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for 

Trace Elements Analysis in Flue Gas Desulfurization Wastewaters,” dated October 6, 

2010, based on EPA Method 200.8, by ICP/MS analysis. 

Any significant findings are summarized below. Specific results that required additional 

qualifiers appear in Table 2. 

• The dissolved selenium result of 530 μg/L for sample 71748 FGD Effluent Day 4 

(280-5438-1) is greater than the total Selenium value of 480 μg/L reported for the 

same sample. 

• The serial dilution analysis for total selenium for sample 71741 did not meet 

TestAmerica’s requirement of ±10%. 

• The matrix spike (MS) and matrix spike duplicate (MSD) analyses performed for 

this sampling episode had several silver and one antimony result failed the 70-

130% control limits with poor recoveries. 

INTERNAL STANDARDIZATION 

All internal standards used by TestAmerica were within the method criteria. 

INITIAL CALIBRATION 

TestAmerica performed the initial calibrations on each analysis day or before each 

analysis if more than one analysis was performed in one day. The initial calibration for 

the ICP-MS analysis consisted of a blank and four calibration standards. 

INITIAL AND CONTINUING CALIBRATION VERIFICATION 

The initial calibration verifications (ICV) and continuing calibration verifications (CCV) 

performed by TestAmerica all had recoveries within the method criteria. 
3

METHOD/INSTRUMENT BLANKS 

All the method blanks were less than the reporting limit (RL); however, some elements 

were found above the method detection limit (MDL) and were flagged with the “J” 

qualifier indicating the concentrations were an estimated value. No additional data 

qualifiers were required for method blanks. 

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

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

flagged with the “J” qualifier. 

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

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

LABORATORY CONTROL SAMPLES (LCS) 

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

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION 

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

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

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

ICS. 

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

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

The ICSA solution for the method 200.8 analysis exceeded the acceptance limits for 

Chromium in analytical batches 280-24259 and 280-27200. The lab has confirmed with 

the vendor that Chromium is a trace impurity in the ICSA solution. Therefore, corrective 

action was deemed unnecessary; the associated data have been flagged “^”. 

SERIAL DILUTION 

Serial dilutions were performed for each batch of total and dissolved samples. The serial 

dilution on sample 71741 (280-5257-3) passed TestAmerica’s requirement of ±10% for 

all analytes except total selenium at 14%. The total selenium result is flagged with a “V” 

qualifier. 

FIELD DUPLICATES 

The RPD of the field duplicates 71746/71749 were less than 20% for all values above the 

reporting limit, with the exception of total arsenic, which had an RPD of 30.9%. Even 
4

though the RPD was greater than 20%, the total arsenic result was not qualified because 

there are no specific control limits for field duplicates specified in EPA Method 200.8. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES 

MS and MSDs were performed on samples 71741, 71743, 71746, and 71747. Many 

spike recoveries were outside the method contrl limits of 70–130% when sample 

concentrations exceeded the spike concentration by a factor of four or more, which have 

been flagged “4,” indicating concentrations in the parent samples were greater than four 

times the spike amounts. All MS/MSDs for total and dissolved silver failed the 70–130% 

control limits. The poor recoveries for silver are probably due to high sulfates in the 

samples that could form insoluble silver sulfide and/or silver sulfate. Otherwise, the 

MS/MSD spike recoveries were within the control limits of 70-130%, with the exception 

of the following: 

• The MS/MSD performed on sample 71741 FGD Influent, Day 1 (280-5257-3) 

failed the 70–130% control limits for total silver. 

• The MS/MSD performed on solid sample 71743 FGD Influent, Day 3 (280-5343-

5) failed the 70–130% control limits for antimony and silver. 

• The MS/MSD performed on sample 71746 FGD Effluent, Day 2 (280-5343-2) 

failed the 70–130% control limits for total and dissolved silver. The RPD for the 

total silver MS/MSD also failed at 58%. 

• The MS/MSD performed on sample 71747 FGD Effluent, Day 3 (280-5398-2) 

failed the 70–130% control limits for total and dissolved silver. Additionally, the 

RPD between the total and dissolved silver MS/MSD for this sample failed the 

method control limits. 

The RPD for all MS/MSD passed the method-specified criteria of 20 percent. 

POST DIGESITON SPIKES 

The post digestion spike (PDS) performed on sample 71747 FGD Effluent, Day 3 (280-

5398-2) failed TestAmerica’s control limits of 85–115% recovery for total selenium and 

total silver, with recoveries of 69% and 80%, respectively. The selenium result was 

flagged by the laboratory; however, the silver result was not flagged by the laboratory 

and therefore, has been included in Table 2 below. 

DETECTION LIMITS 

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water. 
5

Table 2. Data Review Summary 

Sample Analyte Qualifier/Action Reason Level Detected 

71741 Selenium 

(filtrate, 

total) 

Matrix 

Interference 

SRD Failed ±10% 

Difference 

320 μg/L 

71741 Silver (total) Minimum value MS/MSD Failed 

70–130% recovery 

ND 

71743 Antimony 

(solid) 

Minimum value MS/MSD Failed 

70–130% recovery 

160 μg/kg 

71743 Silver 

(solid) 

Minimum value MS/MSD Failed 

70–130% recovery 

140 μg/kg 

71746 Silver (total) Minimum value MS/MSD Failed 

70–130% recovery 

ND 

71746 Silver 

(dissolved) 

Minimum value MS/MSD Failed 

70–130% recovery 

ND 

71747 Silver (total) Minimum value MS/MSD Failed 

70–130% recovery 

ND 

71747 Silver 

(dissolved) 

Minimum value MS/MSD Failed 

70–130% recovery 

ND 

71747 Silver (total) Minimum value PDS Failed 85–

115% recovery 

ND 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

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

Deb Bartram, ERG

TJ Finseth, ERG

From: Randy Mercurio, ERG

Date: 9/1/2011

Subject: TestAmerica Data Review Narrative for Total and Dissolved Metals by 200.7 –

Episode 6560

TestAmerica generated analytical data for total and dissolved metals (aluminum, boron, 

barium, beryllium, calcium, cobalt, iron, magnesium, manganese, molybdenum, sodium, 

tin and titanium) for Sample Episode 6560. The samples were analyzed according to EPA 

Method 200.7.

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

dissolved metals by EPA Method 200.7

Table 1. EPA Episode 6560 Total and Dissolved Metals – Sample Identification

EPA 

Sample # EPA Sample Description

Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71741 FGD Influent, Day 1 280-5257-1 Aqueous 7/12/2010 7/13/2010

71741 FGD Influent, Day 1 - Filtrate 280-5257-3 Aqueous 7/12/2010 7/13/2010

71741 FGD Influent, Day 1 - Solids 280-5257-4 Solid 7/12/2010 7/13/2010

71742 FGD Influent, Day 2 280-5302-1 Aqueous 7/13/2010 7/14/2010

71742 FGD Influent, Day 2 - Filtrate 280-5302-4 Aqueous 7/13/2010 7/14/2010

71742 FGD Influent, Day 2 - Solids 280-5302-5 Solid 7/13/2010 7/14/2010

71743 FGD Influent, Day 3 280-5343-1 Aqueous 7/14/2010 7/15/2010

71743 FGD Influent, Day 3 - Filtrate 280-5343-4 Aqueous 7/14/2010 7/15/2010

71743 FGD Influent, Day 3 - Solids 280-5343-5 Solid 7/14/2010 7/15/2010

71744 FGD Influent, Day 4 280-5398-1 Aqueous 7/15/2010 7/16/2010

71744 FGD Influent, Day 4 - Filtrate 280-5398-3 Aqueous 7/15/2010 7/16/2010

71744 FGD Influent, Day 4 - Solids 280-5398-4 Solid 7/15/2010 7/16/2010

71745 FGD Effluent, Day 2 280-5302-2 Aqueous 7/13/2010 7/14/2010

71746 FGD Effluent, Day 2 280-5343-2 Aqueous 7/14/2010 7/15/2010

71747 FGD Effluent, Day 3 280-5398-2 Aqueous 7/15/2010 7/16/2010

71748 FGD Effluent, Day 4 280-5438-1 Aqueous 7/16/2010 7/17/2010

71749 FGD Effluent Duplicate 280-5343-3 Aqueous 7/14/2010 7/15/2010
2

Table 1. EPA Episode 6560 Total and Dissolved Metals – Sample Identification

EPA 

Sample # EPA Sample Description

Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71750 FGD Influent Field Blank, Day 1 280-5257-2 Aqueous 7/12/2010 7/13/2010

71751 FGD Effluent Field Blank, Day 1 280-5302-3 Aqueous 7/13/2010 7/14/2010

SUMMARY

The samples were prepared for total and dissolved metals analysis according to 

TestAmerica’s SOP for ICP Analysis of Trace Metals by Method 200.7. Due to the total 

suspended solids being in excess of 1% in the influent samples a phase separation was 

performed creating four solid samples. Any significant findings are summarized below. 

Specific sample or QC results that required additional data qualifiers appear in Table 2.

• The relative percent difference (RPD) for total aluminum for the field duplicate 

samples 71746 and 71749 161%; however, the duplicate sample was less than the 

reporting limit; therefore, the RPD could not be accurately calculated. 

• The serial dilution analysis for cobalt for sample 71741 did not meet 

TestAmerica’s requirement of ±10% difference.

• The MS and MSD recoveries for titanium in the solid phase of sample 71743 

failed the 70-130% control limits.

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES

There were no sample receipt issues in this data package.

INTERNAL STANDARDIZATION

While the internal standard (ISTD) Yttrium was used for these analyses, no checks on the 

ISTD recoveries in the ±30% criterion of the calibration blank as per Section 9.11 of the 

SOP were seen. All ISTD were within the control limits. 

INITIAL CALIBRATION

TestAmerica performed the initial calibrations on each analysis day. The initial 

calibration for the ICP analysis consisted of a blank and one calibration standard.

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

All initial calibration verifications (ICV) and continuing valibration verifications (CCV)

had recoveries within the method criteria.

METHOD/INSTRUMENT BLANKS
3

All the Method Blanks were less than the reporting limit (RL); however, some elements

had levels above the method detection limit (MDL) and were flagged with the “J” 

qualifier.

All instrument blanks (ICB and CCB) were less than the RL; however, some elements 

were above the MDL and were flagged with the “J” qualifier.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

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

LABORATORY CONTROL SAMPLES (LCS)

All LCSs passed the method control limits of 85-115%.

SYNTHETIC FGD INTERFERENCE CHECK SOLUTIONS

Interference checks were performed using the synthetic matrix as the check solution. All 

recoveries met the method-specified criteria.

SERIAL DILUTION

Serial dilutions were performed for each batch of total and dissolved samples. Sample 

71741 failed the method required ±10% difference for cobalt (11%), which was flagged 

“V” as failing the QC criteria. Otherwise, all serial dilution percent differences were less 

than 10%.

FIELD DUPLICATES

The RPD of the field duplicates 71746/71749 were less than 20% for all values equal to 

or greater than the RL, except for total aluminum, which had an RPD of 161%. The 

parent sample value (260 ug/L) was greater than the RL, but the duplicate value (28 ug/L) 

was less than the RL; therefore, the RPD could not be accurately calculated. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

MS and MSD were performed on samples 71741 (total), 71743 (total solid), 71746 (total 

and dissolved) and 71747 (total and dissolved). Many elements with high concentrations 

frequently failed the spike recovery but were flagged with a “4” qualifier indicating that 

the concentration in the parent sample was greater than four times the spike and could not 

be reliably calculated. Otherwise, the MS/MSD spike recoveries were within the control 

limits of 70–130% with the exception of the following:

• The MS and MSD recoveries for titanium in the solid phase of sample 71743 

were 131% and 137%, respectively.
4

The RPDs between the MS and MSD samples were always within ± 20% except for the 

following:

• The RPD between the MS and MSD for boron for sample 71746 was 165% for 

both total and dissolved analyses.

• The RPD between the MS and MSD for magnesium for sample 71746 was 165% 

for both total and dissolved analyses.

• The RPD between the MS and MSD for total boron and total magnesium for 

sample 71747 was 162%.

• The RPD between the MS and MSD for dissolved boron and dissolved 

magnesium for sample 71747 was 163%.

POST DIGESTION SPIKE

The post digestion spike (PDS) performed on sample 71741 FGD Influent, Day 1 passed

TestAmerica’s control limits of 85-115% recovery for all total and dissolved analytes 

except for total aluminum and total titanium. The post digestion spike performed on 

sample 71746 FGD Effluent, Day 2 passed TestAmerica’s control limits of 85-115% 

recovery for all total and dissolved analytes except for total aluminum, total titanium, and 

dissolved titanium. 

DETECTION LIMITS

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water.

Table 2. Data Review Summary

Sample Analyte Qualifier/Action Reason Level Detected

71743 Titanium 

(solid) Maximum value MS/MSD recovery > 130% 140 mg/kg
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

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

Deb Bartram, ERG

TJ Finseth, ERG

From: Donna Tedder, ERG

Date: 9/1/2011

Subject: FGS Data Review Narrative for Dissolved Hexavalent Chromium – Episode 

6560

Frontier Global Sciences (FGS) generated analytical data for dissolved hexavalent 

chromium for Sample Episode 6560. FGS analyzed the samples according to a modified 

EPA Method 218.6 for dissolved hexavalent chromium by Liquid Chromatography –

Inductively Coupled Plasma Mass Spectrometry (LC-ICP-MS).

Table 1 summarizes the samples FGS extracted and analyzed for dissolved hexavalent 

chromium.

Table 1. EPA Episode 6560 Dissolved Hexavalent Chromium – Sample Identification

EPA 

Sample 

#

Sample 

Matrix Sample Description

Sampling 

Date Analysis Date

71741 Aqueous FGD Influent Day 1 7/12/10 8/9/10

71742 Aqueous FGD Influent Day 2 7/14/10 8/9/10

71743 Aqueous FGD Influent Day 3 7/14/10 8/9/10

71744 Aqueous FGD Influent Day 4 7/15/10 8/9/10

71745 Aqueous FGD Effluent Day 1 7/14/10 8/9/10

71746 Aqueous FGD Effluent Day 2 7/14/10 8/9/10

71747 Aqueous FGD Effluent Day 3 7/15/10 8/9/10

71748 Aqueous FGD Effluent Day 4 7/16/10 8/9/10

71749 Aqueous FGD Effluent Day 2 Duplicate 7/14/10 8/9/10

71750 Aqueous FGD Influent Field Blank Day 1 7/12/10 8/9/10

71751 Aqueous FGD Effluent Field Blank Day 1 7/14/10 8/9/10

SUMMARY

The samples were prepared for dissolved hexavalent chromium analysis according to 

FGS-129.01 Standard Operating Procedure (SOP), a modified EPA Method 218.6.
2

Several samples (71741, 71742, 71743, and 71744) were diluted prior to analysis due to 

the presence of high levels of non-target chloride interferences.

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES

The pH for sample 71751 (FGD Effluent Field Blank) was 9.98 S.U. upon receipt at the 

laboratory, which is outside the appropriate range of 9.0-9.5 S.U.; therefore, the 

laboratory adjusted the pH. The final sample pH was 9.68 S.U. Because this sample was 

not at the method-specified pH, this sample was qualified as an estimated value. 

INITIAL PRECISION AND ACCURACY/RECOVERY

The initial precision and recovery (IPR) performed by FGS had recoveries within the 

method criteria.

ON-GOING PRECISION AND ACCURACY/RECOVERY

The analytical method did not require the analysis of an on-going precision and recovery 

(OPR).

INITIAL CALIBRATION

FGS performed the initial calibrations on each analysis day. The initial calibration for 

the LC-ICP-MS analysis consisted of a blank and eight calibration standards with a 

correlation factor ≥0.995 as required by the method.

A secondary source initial calibration verification (ICV) was analyzed and passed ± 10% 

of true value required by the method.

CONTINUING CALIBRATION VERIFICATION

All CCVs met method-specified criteria, ± 10% of true value with recoveries ranging 

from 98.5 to 109%.

BLANK

All of the preparation blanks/laboratory reagent blanks (LRBs) and the continuing 

calibration blanks (CCBs) met method-specified requirements.

OTHER CHECKS

The laboratory control sample/duplicate (LCS/LCSD) or laboratory fortified 

blank/duplicate (LFB/LFBD) passed method criteria of ± 10% of true value with 

recoveries of 102% and 102%. The laboratory SOP indicated that a second source 

quality control sample (QCS) must be analyzed by the laboratory at least once a quarter. 
3

The data for the QCS was not included in the data package for review. However, the 

ICV was a second source standard.

DETECTION LIMITS

The laboratory method detection limit (MDL) in the synthetic matrix was 0.392 ug/L. 

Results below this MDL were reported as not detected.

DUPLICATES

There were no laboratory duplicates performed in this episode other than a duplicate of 

the LCSD and a duplicate of the matrix spike (MS). 

One field duplicate was collected and analyzed. Sample 71749, with a result of 7.35 

μg/L, was a duplicate of sample 71746, which had 7.32 μg/L hexavalent chromium. 

These duplicate samples had an RPD of 0.41%, which meets the method-suggested 

criteria.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

The MS and matrix spike duplicate (MSD) was performed using a secondary source 

spike on sample 71747. The MS and MSD recoveries were 101% and 99.5%,

respectively, with an RPD of 1.07%. A second set of MS and MSDs were prepared on 

the diluted sample and had recoveries of 95.3% and 96.0%, respectively, with an RPD of 

0.64%.

Table 2. Data Review Summary Table

Sample Analyte Qualifier Reason Level Detected

71751 Chromium (VI) Estimated value

pH outside of 

method-specified 

range.

ND

ND - Not detected.
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

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

Deb Bartram, ERG

TJ Finseth, ERG

From: Donna Tedder, ERG

Date: 9/1/2011

Subject: TestAmerica Data Review Narrative for Classicals Analyses – Episode 6560

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for Sample Episode 6560. All samples were tested for the following analytes: 

• Ammonia by EPA method 350.1, 

• Biochemical Oxygen Demand – 5 day (BOD5) by SM 5210B, 

• Chloride and Sulfate by EPA method 300.0, 

• Chemical Oxygen Demand (COD) by EPA method 410.4, 

• Cyanide (total) by SM 4500 CN- E, 

• Nitrate/Nitrite by EPA method 353.2

• Phosphorus (total) by EPA method 365.1, 

• Total Dissolved Solids (TDS) by SM 2540C, 

• Total Kjeldakl Nitrogen (TKN) by EPA method 351.2, and 

• Total Suspended Solids (TSS) by SM 2540D.

The TSS concentration of the influent samples was greater than one percent, so as 

requested, the laboratory separated the solid and liquid portions of the samples and 

analyzed both portions separately for the following analytes:

• Ammonia, 

• Cyanide, 

• Nitrate/Nitrite, 

• Phosphorus, and

• TKN. 

TestAmerica was also required to analyze chloride and sulfate using this phase separation

technique, but they mistakenly only analyzed the solids fraction and not the filtrate 

fraction. Therefore, TestAmerica instead analyzed and reported the results for the raw 

sample without phase separation for chloride and sulfate.

Table 1 summarizes the nine field samples analyzed by TestAmerica, including how the

laboratory split and analyzed the influent samples.
2

Table 1. EPA Episode 6560 Classical Analytes – Sample Identification

EPA

Sample #

Sample 

Description

Sampling

Date

Sample

Matrix

Portion of 

Sample

Analytes 

71741 FGD Influent, 

Day 1 7/12/10

Water Entire 

Fraction

BOD5, COD, Chloride, 

Sulfate, TDS, and TSS

Water Filtrate

Ammonia, Cyanide, 

Nitrate/Nitrite, 

Phosphorus, and TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

71742 FGD Influent, 

Day 2 7/13/10

Water Entire 

Fraction

BOD5, COD, Chloride, 

Sulfate, TDS, and TSS

Water Filtrate

Ammonia, Cyanide, 

Nitrate/Nitrite, 

Phosphorus, and TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

71743 FGD Influent, 

Day 3 7/14/10

Water Entire 

Fraction

BOD5, COD, Chloride, 

Sulfate, TDS, and TSS

Water Filtrate

Ammonia, Cyanide, 

Nitrate/Nitrite, 

Phosphorus, and TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

71744 FGD Influent, 

Day 4 7/15/10

Water Entire 

Fraction

BOD5, COD, Chloride, 

Sulfate, TDS, and TSS

Water Filtrate

Ammonia, Cyanide, 

Nitrate/Nitrite, 

Phosphorus, and TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Phosphorus, Sulfate, and 

TKN

71745 FGD Effluent, 

Day 1 7/13/10 Water Entire Fraction All analytes

71746 FGD Effluent, 

Day 2 7/14/10 Water Entire Fraction All analytes

71747 FGD Effluent, 

Day 3 7/15/10 Water Entire Fraction All analytes
3

Table 1. EPA Episode 6560 Classical Analytes – Sample Identification

EPA

Sample #

Sample 

Description

Sampling

Date

Sample

Matrix

Portion of 

Sample

Analytes 

71748 FGD Effluent, 

Day 4 7/16/10 Water Entire Fraction All analytes

71749 FGD Effluent 

- Duplicate 7/14/10 Water Entire Fraction All analytes

SUMMARY

All samples were analyzed within the holding time specified in 40 CFR 136 Table II

unless otherwise noted below.

TestAmerica could not perform the phase separation of the preserved Group II influent 

samples; therefore, the laboratory used some of the extra volume from the unpreserved 

metals sample volume for the analyses. After phase separation, TestAmerica preserved 

the samples accordingly. Because of this process, the ammonia, nitrate/nitrite, TKN, 

phosphorus, and cyanide influent samples used for the analyses were not preserved 

immediately following sample collection as required by the method. 

One field duplicate sample was collected and analyzed for each analyte. The relative 

percent difference (RPD) between the sample and its duplicate was less than 20% unless 

otherwise noted below. 

If applicable, the appropriate number of standards was used to create a calibration curve. 

If sample results were above the highest standard used to create the curve, the sample was 

diluted and reanalyzed. All sample results were between the lowest and highest standards

unless noted below. Additionally, all calibration blanks and calibration verification 

samples met the criteria specified in the method.

If required by the method, the quality control sample (QCS), a secondary source standard 

used to verify calibration, was always within the control limits specified by the method. 

As described below, the analyte of interest was detected above the method detection limit 

(MDL) in some laboratory reagent blanks (LRB). However, the analyte of interest was 

never detected above the reporting limit (RL) in the LRBs. If required by the method, all 

laboratory fortified blanks (LFB) met the criteria specified in the method.

If required by the method, a matrix spike (MS) analysis was run on sample 71747 (FGD 

effluent) for each analyte to check for matrix interferences. For some analytes, 

TestAmerica spiked more samples than required. All MS samples analyzed met the 

criteria specified in the method unless described below. 
4

DATA NOTES/ISSUES

Ammonia

As stated above, filtrate and solid aliquots of samples 71741 - 71744 were not preserved 

immediately after sample collection. Instead, TestAmerica preserved the sample after 

phase separation. Because these samples were not preserved immediately as required by 

the method, these samples were qualified as estimated values.

The filtrate of sample 71741 and the solids portion of 71742 were analyzed one day after 

the 28-day hold time. The solids portion of sample 71741 was analyzed two days after the 

28-day hold time. These samples were already qualified as estimated values because they 

were not preserved immediately following sample collection, so no further action was 

necessary.

The results for the MS/MSD samples for 71747 were above the highest calibration 

standard. The laboratory did not dilute and reanalyze these samples because the MS/MSD 

percent recoveries were within the control limits specified by EPA method 350.1. 

Therefore, if the MS/MSD results for sample 71747 are reported, they will be qualified as

estimated values. The result for sample 71747 was within the calibration range, so this 

sample does not need to be qualified. The LFB associated with sample 71747 met the 

method criteria.

BOD5

TestAmerica analyzed five dilutions, but no dilutions had a dissolved oxygen (DO) 

depletion greater than 2.0 mg/L for sample 71744. Therefore, BOD5 was reported as not 

detected for this sample. The rest of the samples had at least one dilution with a DO 

depletion greater than 2.0 mg/L. As required in the method, the final result was calculated 

by taking the average of the results for all dilutions with a DO depletion greater than 2.0 

mg/L and a final DO greater than 1.0 mg/L. 

The glucose-glutamic acid (GGA) standards associated with samples 71744 and 71747 

had percent recoveries of 80% and 78%. The GGA standards associated with sample

71748 had percent recoveries of 79% and 81%. These percent recoveries were below the

method and laboratory criteria of 85-115%. TestAmerica flagged these samples with a 

“*” meaning the laboratory control sample was not within laboratory control limits. BOD 

was not detected in sample 71744, so no further qualification was necessary for this 

sample. Samples 71747 and 71748 were additionally qualified as minimum values.

The seed correction factor associated with sample 71748 was 0.5328 mg/L, which is less 

than the method and laboratory control limits of 0.6-1.0 mg/L. The result for this sample 

could be biased low. This sample was qualified by TestAmerica with an “s” meaning the 

seed control blank (SCB) recovery was low. Since this sample was already qualified as a 

minimum value because the GGA percent recovery was low, no further action was taken. 
5

All laboratory duplicates and water blanks were analyzed appropriately and met method 

criteria.

Chloride and Sulfate

The laboratory diluted the MSD sample for 71747 by 500 fold, but the diluted result for 

sulfate was still above the highest calibration standard. The laboratory did not reanalyze 

this sample with a higher dilution factor, because the MSD percent recovery was within 

the control limits specified by EPA method 300.0. Therefore, if the MSD result for 

sample 71747 for sulfate is reported, it will be qualified as an estimated value. 

COD

The RPD between sample 71746 and its field duplicate 71749 for COD was 33.3%. Even 

though the RPD was greater than 20%, the sample was not qualified because there are no 

control limits for field duplicates specified in EPA Method 410.4.

The percent recoveries for the MS and MSD samples associated with 71747 were 87% 

and 93% respectively. The MS percent recovery did not meet the method control limits 

of 90-110%. Because the percent recovery for the MS sample was below the method

control limits, sample 71747 was flagged as a minimum value.

Cyanide 

As stated above, filtrate and solid aliquots of samples 71741 - 71744 were not preserved 

immediately after sample collection. Instead, TestAmerica preserved the sample after 

phase separation. Solid aliquots of samples 71741 - 71744 were all qualified by the 

laboratory with a “J” meaning the sample result was an estimated value because it was 

less than the RL, so there was no need to further qualify these samples. Because the 

filtrate aliquots of samples 71741 - 71744 were not preserved immediately as required by 

the method, these samples were qualified as estimated values.

Sample 71747 was preserved to pH 10 with NaOH immediately after sample collection, 

but the pH was neutral when the sample was received by the laboratory. The laboratory 

added more NaOH to correct the pH upon receipt. This sample was flagged as an 

estimated value.

Both the filtrate and solids fraction of samples 71741, 71742, 71743, and 71744 were 

analyzed 16, 15, 14, and 13 days respectively past the 14-day hold time. Since all of these 

samples were already qualified as estimated values because the sample was not preserved 

appropriately or because the sample result was greater than the MDL but less than the RL 

(i.e., a J-value), no further action was necessary. 

Cyanide was detected at 0.00240 mg/L in the LRB associated with the filtrate fraction of 

samples 71741 - 71744. Additionally, cyanide was detected at 0.141 mg/kg in the LRB

associated with the solids fraction of samples 71741 - 71744. Cyanide was also detected 
6

at 0.00499 mg/L in the LRB associated with the samples 71745 - 71749. Because all of 

these blank results were less than the RL, no samples were qualified based on these LRB 

results. 

All samples were diluted prior to distillation by a factor of 10 due to matrix interferences.

The diluted result for sample 71749 was less than the lowest calibration standard. The 

solid fraction results for samples 71741 - 71744 were also all below the lowest calibration 

standard. These sample results were already qualified by the laboratory with a “J” 

meaning the sample result was an estimated value because it was less than the RL, so 

there was no need to further qualify these samples.

The RPD between sample 71746 and its field duplicate 71749 for cyanide was 193%. 

Even though the RPD was greater than 20%, the sample was not qualified because there 

are no control limits for field duplicates specified in SM 4500 CN- E.

Nitrate/Nitrite

As stated above, filtrate and solid aliquots of samples 71741 - 71744 were not preserved 

immediately after sample collection. Instead, TestAmerica preserved the sample after 

phase separation. Because these samples were not preserved immediately as required by 

the method, these samples were qualified as estimated values.

The 28-day hold time was exceeded by one day for the filtrate fraction of sample 71741 

and for the solids fraction of sample 71742. The solids fraction of sample 71741 was 

analyzed two days past the holding time. These samples were already qualified as 

estimated values because they were not preserved immediately following sample 

collection, so no further action was necessary.

Phosphorus 

As stated above, filtrate and solid aliquots of samples 71741 - 71744 were not preserved 

immediately after sample collection. Instead, TestAmerica preserved the sample after 

phase separation. Filtrate samples 71741 - 71744 and solid sample 71743 were already 

qualified by the laboratory with a “J” meaning the sample result was an estimated value 

because it was less than the RL, so there was no need to further qualify these samples. 

Solid samples 71741, 71742, and 71744 were qualified as estimated values because they 

were not preserved immediately following sample collection, as required by the method.

The filtrate and solids fractions from sample 71741 were analyzed two days after the 28-

day hold time and the filtrate and solids fractions from sample 71742 were analyzed one

day outside of the hold time. TestAmerica did not flag these results; therefore, ERG 

qualified these samples with an “H”. These samples were already qualified as estimated 

values because they were not preserved immediately following sample collection.

Phosphorus was detected at 0.00837 mg/L in the laboratory reagent blank associated with 

samples 71745 - 71749. Phosphorus was also detected at 0.00977 mg/L in the laboratory 
7

reagent blank associated with the filtrate of samples 71741 - 71744. Because all of these 

blank results were less than the RL, no samples were qualified based on these LRB 

results.

The filtrate results for samples 71741 - 71744 were all below the lowest calibration 

standard. These samples were already qualified by the laboratory with a “J” meaning the 

sample result was an estimated value because it was less than the RL, so there was no 

need to further qualify these samples.

The RPD between sample 71746 and its field duplicate 71749 for phosphorus was 93.9%. 

Even though the RPD was greater than 20%, the sample was not qualified because there 

are no control limits for field duplicates specified in the method.

The percent recoveries for the MS and MSD analyses for sample 71747, 55% and 57%, 

respectively, were not within the method control limits of 90-110% or within the 

laboratory control limits of 71-128%. Results for samples with a similar matrix (i.e., FGD 

effluent) could be biased low because of matrix interferences. Sample 71747 was

qualified as a minimum value because the MS percent recovery was less than the control 

limits specified in the method.

TDS

Two laboratory duplicates were analyzed. The RPDs for these laboratory duplicates were

less than 10%, which is required by the method. 

Samples 71743, 71746, 71748, and 71749 did not achieve a constant weight after three 

drying cycles. SM 2540C warns that samples that contain high levels of calcium, 

magnesium, chloride, and sulfate may be hygroscopic, meaning they absorb moisture 

from the air. FGD wastewater contains high concentrations of all of these species, so this 

may be the cause for the inconsistent weight calculations. These samples were not 

qualified, but results may be biased high.

TKN

As stated above, filtrate and solid aliquots of samples 71741 - 71744 were not preserved 

immediately after sample collection. Instead, TestAmerica preserved the sample after 

phase separation. Because these samples were not preserved immediately as required by 

the method, these samples were qualified as estimated values.

The solids and filtrate fraction of samples 71741 and 71742 were analyzed two days and 

one day after the 28-day hold time, respectively. These samples were already qualified as 

estimated values because they were not preserved immediately following sample 

collection, so no further action was necessary. 
8

TKN was detected at 0.234 mg/L in the laboratory reagent blank associated with samples 

71745 - 71749. Because this blank result was less than the RL, no samples were qualified 

based on the LRB result.

TestAmerica performed MS and MSD analyses on sample 71747. The percent recoveries

for the MS and MSD samples were 88% and 116% and the results were 23.2 and 24.0 

mg/L. The samples did not meet the method control limits of 90-110%, but did meet the 

laboratory control limits of 54-131%. The sample concentration was greater than 4 times 

the spike amount in the MS and MSD samples, so TestAmerica stated that the percent 

recoveries and RPDs could not be reliably calculated. Considering that the MS percent 

recovery was below the control limits and the MSD percent recovery was above the 

limits, this was likely the case. Sample 71747 was not qualified because it is not possible 

to determine if the MS/MSD failure was a result of matrix interferences or caused by the 

low spiking level.

TSS 

Four laboratory duplicates were analyzed. The RPDs for these laboratory duplicates were 

less than or equal to 10% as required by the method. 

TSS was detected at 1.60 mg/L in the method blank (MB) associated with sample 71747. 

Because this blank result was less than the RL, no samples were qualified based on the 

MB result

The RPD between sample 71746 and its field duplicate 71749 for TSS was 27.3%. Even 

though the RPD was greater than 20%, the sample was not qualified because there are no 

specific control limits for field duplicates specified in the SM 2540D.

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71741 

(filtrate)

Ammonia Estimated value Sample not preserved 

immediately following 

collection. Analyzed one 

day past holding time

5.1 mg/L

71741 

(solid)

Ammonia Estimated value Sample not preserved 

immediately following 

collection. Analyzed two 

days past holding time

24 mg/kg

71742 

(filtrate)

Ammonia Estimated value Sample not preserved 

immediately following 

collection

5.3 mg/L
9

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71742 

(solid)

Ammonia Estimated value Sample not preserved 

immediately following 

collection. Analyzed one 

day past holding time

28 mg/kg

71743 

(filtrate)

Ammonia Estimated value Sample not preserved 

immediately following 

collection

7.7 mg/L

71743 

(solid)

Ammonia Estimated value Sample not preserved 

immediately following 

collection

26 mg/kg

71744 

(filtrate)

Ammonia Estimated value Sample not preserved 

immediately following 

collection

6.2 mg/L

71744 

(solid)

Ammonia Estimated value Sample not preserved 

immediately following 

collection

23 mg/kg

71747 BOD5 Minimum value GGA % recovery below 

method-specified criteria

6.9 mg/L

71748 BOD5 Minimum value GGA % recovery and 

SCB recovery below 

method-specified criteria

4.6 mg/L

71747 COD Minimum value MS % recovery below 

method-specified criteria

560 mg/L

71741 

(filtrate)

Total Cyanide H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed 16 

days past holding time

0.27 mg/L

71742 

(filtrate)

Total Cyanide H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed 15 

days past holding time

0.62 mg/L

71743 

(filtrate)

Total Cyanide H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed 14 

days past holding time

2.2 mg/L

71744 

(filtrate)

Total Cyanide H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed 13 

days past holding time

0.21 mg/L

71747 Total Cyanide Estimated value pH upon receipt < 10 0.60 mg/L
10

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71741 

(filtrate)

Nitrate/nitrite H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed 1 

day past holding time

77 mg/L

71741 

(solids)

Nitrate/nitrite H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed two

days past holding time

49 mg/kg

71742 

(filtrate)

Nitrate/nitrite Estimated value Sample not preserved 

immediately following 

collection.

83 mg/L

71742 

(solids)

Nitrate/nitrite H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed one

day past holding time

64 mg/kg

71743 

(filtrate)

Nitrate/nitrite Estimated value Sample not preserved 

immediately following 

collection.

79 mg/L

71743 

(solids)

Nitrate/nitrite Estimated value Sample not preserved 

immediately following 

collection.

56 mg/kg

71744 

(filtrate)

Nitrate/nitrite Estimated value Sample not preserved 

immediately following 

collection.

90 mg/L

71744 

(solids)

Nitrate/nitrite Estimated value Sample not preserved 

immediately following 

collection.

65 mg/kg

71741 

(filtrate)

Total 

Phosphorus

H Analyzed two days past 

holding time

0.0096 

mg/L

71741 

(solids)

Total 

Phosphorus

H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed two

days past holding time

21 mg/kg

71742 

(filtrate)

Total

Phosphorus

H Analyzed one day past 

holding time

0.0081 

mg/L

71742 

(solids)

Total 

Phosphorus

H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed one

day past holding time

310 mg/kg

71744 

(solids)

Total 

Phosphorus

Estimated value Sample not preserved 

immediately following 

collection.

340 mg/kg
11

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71747 Total 

Phosphorus

Minimum value MS % recovery below 

method-specified criteria

0.18 mg/L

71741 

(filtrate)

TKN H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed two

days past holding time

24 mg/L

71741 

(solids)

TKN H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed two

days past holding time

830 mg/kg

71742 

(filtrate)

TKN H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed one

day past holding time

31 mg/L

71742 

(solids)

TKN H, Estimated 

value

Sample not preserved 

immediately following 

collection. Analyzed one

day past holding time

840 mg/kg

71743 

(filtrate)

TKN Estimated value Sample not preserved 

immediately following 

collection.

29 mg/L

71743 

(solids)

TKN Estimated value Sample not preserved 

immediately following 

collection.

700 mg/kg

71744 

(filtrate)

TKN Estimated value Sample not preserved 

immediately following 

collection.

26 mg/L

71744 

(solids)

TKN Estimated value Sample not preserved 

immediately following 

collection.

900 mg/kg
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
Appendix D 

FGD ICP/MS SOP: INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY FOR TRACE 

ELEMENT ANALYSIS IN FLUE GAS DESULFURIZATION WASTEWATERS
D-1 

FGD ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for 

Trace Element Analysis in Flue Gas Desulfurization Wastewaters 

1.0 Scope and Application

1.1 This document describes procedures used to measure elements in Flue Gas 

Desulfurization, FGD, wastewaters. Inductively coupled plasma-mass 

spectrometry (ICP/MS), as described in EPA Methods 200.8 and 1638, was used 

with a collision cell to mitigate the effects of interferences in the samples. These 

procedures are intended for use by analysts experienced with applying ICP/MS 

to complex wastewater samples. 

1.2 These procedures are applicable to the analysis of acid digested FGD 

wastewater, and have been evaluated for the analysis of 13 elements of interest. 

These are Al, As, Cd, Cr, Cu, Pb, Mn, Ni, Se, Ag, Tl, V and Zn. Additional 

elements may be included provided that the performance criteria presented in 

Sections 9 and 12 are met. 

1.3 Flue Gas Desulfurization wastewaters frequently have very high levels of 

calcium, sodium, magnesium, manganese, chloride and sulfate (up to thousands 

of ppm). The use of instrument configurations and/or accessories designed to 

accommodate samples with high dissolved solids levels is highly recommended. 

2.0 Summary

2.1 Aqueous samples, digestates, or leachates are nebulized into a spray chamber 

where a stream of argon carries the sample aerosol through the quartz torch and 

injects it into an RF plasma. There the sample is decomposed and desolvated. 

2.2 The ions produced are entrained in the plasma gas and by means of a watercooled, differentially pumped interface, introduced into a high-vacuum chamber 

that houses a quadrupole mass spectrometer capable of providing a resolution 

better than or equal to 0.9 amu peak width at 10% of the peak height. The ions 

are separated according to their mass-to-charge ratio and measured with a 

detector, such as an electron multiplier. 

2.3 A collision/reaction cell utilizing He and (optionally) H2 gases is used to remove 

molecular interferences. 

2.4 Interferences not eliminated by the collision/reaction cell must be assessed and 

valid corrections applied, or the data flagged to indicate problems. Interference 

correction must include compensation for interferences not removed by the 

collision / reaction cell. Recommended elemental equations are listed in 

Attachment 1. Use of the internal standard technique is required to compensate 

for suppressions and enhancements caused by sample matrices. 

3.0 Definitions

3.1 Batch – A group of samples which behave similarly with respect to the sampling 

or the testing procedures being employed and which are processed as a unit. 

For QC purposes, if the number of samples in a group is greater than 20, then 

each group of 20 samples or less will all be handled as a separate batch 
D-2 

3.2 Dissolved Metals - Those elements which pass through a 0.45-m membrane 

filter (sample is acidified after filtration). 

3.3 Suspended Metals - Those elements which are retained by a 0.45-m 

membrane filter. 

3.4 Total Recoverable Metals - The concentration determined on an unfiltered 

sample following treatment with hot, diluted mineral acids, as described in this 

procedure 

3.5 Instrument Detection Limit (IDL) - See Section 12.2 

3.6 Sensitivity - The slope of the analytical curve (i.e., the functional relationship 

between raw instrument signal and the concentration). 

3.7 Tuning Solution - This is a multi-element solution containing analytes which are 

representative of the entire mass range capable of being scanned by the 

instrument. It is used to optimize the sensitivity of the instrument and to verify 

the mass resolution meets method criteria. 

3.8 Initial Calibration Verification / Quality Control Standard (ICV/QCS) - A multielement standard of known concentrations prepared to verify instrument 

calibration. This solution must be an independent standard prepared near the 

mid-point of the calibration curve, and at a concentration other than that used for 

instrument calibration. 

3.9 Continuing Calibration Verification (CCV) - A multi-element standard of known 

concentrations prepared to monitor and verify the instrument daily continuing 

performance. 

3.10 Laboratory Control Sample / Laboratory Fortified Blank (LCS/LFB) - A multielement standard of known concentrations that is carried through the entire 

sample preparation and analysis procedure. This solution is used to verify 

method performance in an ideal sample matrix. 

3.11 Reagent Blank - High purity (> 18 megohm-cm) water containing the same acid 

matrix as the calibration standards that is carried through the entire digestion 

process. The reagent blank is used to determine the concentrations of trace 

metals in the reagents used to prepare and analyze the samples. 

3.12 Calibration Blank - High purity (> 18 megohm- cm) water acidified with the 

same acid concentrations present in the standards and samples. Also referred to 

as the Initial Calibration Blank (ICB) and Continuing Calibration Blank (CCB). 

3.13 Method Detection Limit (MDL) – Refers to the instructions in Appendix B to 40 

CFR Part 136. Also see Section 12.1 of this document. The MDL is determined 

from analysis of a sample in a given matrix containing the analyte. 

3.14 Individual FGD Interference Check solutions – Single element solutions at 

concentrations similar to those found in flue gas desulfurization wastewaters. 

3.15 Synthetic FGD wastewater – A mixed solution of elements at typical 

concentrations found in flue gas desulfurization wastewaters. 

4.0 Interferences

4.1 Isobaric Interferences 

Isobaric interferences in the ICP/MS are caused by isotopes of different elements 

forming ions with the same nominal mass-to-charge ratio (m/z). The 
D-3 

recommended ions used for the elements in this procedure do not have 

elemental isobaric interferences, except for a very small interference from 

krypton on 78Se, which can be avoided by using argon free of krypton. 

4.2 Isobaric Molecular 

Isobaric molecular interferences are caused by ions consisting of more than one 

atom. These molecular interferences are minimized by use of the collision cell 

utilizing He and/or H2 gases. Common examples are potential interferences from 

40Ar35Cl or 40Ca35Cl on 75As, or 35Cl16O on 51V, or 40Ar12C on 52Cr. Collision cell 

interference removal works both by causing the interfering molecular ion to 

dissociate and by reducing the kinetic energy of the ion. The latter is termed 

Kinetic Energy Discrimination (KED), and is the primary mechanism for 

interference removal. Polyatomic ions are larger than elemental ions and so 

collide with the helium atoms in the collision cell more frequently than the smaller 

elemental ions. Each collision reduces the energy of the ion, so the molecular 

ions lose energy more quickly. At the end of the collision cell a positive voltage 

plate prevents passage of the now low energy molecular ions. Thus, the 

interference is eliminated because the molecular ions do not reach the detector. 

4.3 Doubly Charged Ion Interferences 

Doubly charged elemental ions are possible in cases where the second 

ionization potential of the element is significantly below the fist ionization 

potential for argon (15.7eV). If a doubly charged ion is formed, it will cause a 

response at half of its elemental mass, potentially causing an interference. 

Fortunately, most elements have high enough second ionization potentials that 

formation of doubly charged ions is not an issue. For the target analytes in this 

procedure, a significant potential for interference is from 150Nd and 150Dy 

(potential interference on 75As and from 156Gd (potential interference on 78Se). To 

check for these potential interferences, monitor the response for mass 150 and 

156. If the cps for these masses is > 5 times the cps for the quantitation limit for 

arsenic (in the case of mass 150) or selenium (in the case of mass 156) an 

interference is possible. In this case analyze a 100ppb standard of Nd and Dy (if 

mass 150 is observed) or Gd (if mass 156 is observed) and measure the 

response at 150 and 75 (or 156 and 78). This ratio can then be used to create an 

interference correction equation. For example, if the response for a 100ppb Gd 

standard at mass 156 is 10,000 cps, and the observed response for the same 

standard at mass 78 is 1,000 counts, then the equation for 78Se would be: 

78Se = 78Se – (156Gd/10) 

4.4 Physical Interferences 

 Physical interferences are associated with the transport and nebulization 

process. Internal standards are used to compensate for these types of 

interferences. 

 Internal standards should be added at a level to give approximately 

50,000 - 800,000 counts of raw signal intensity. The mass of the internal 

standard should ideally be within 50 amu of the mass of the measured 

analyte. Consideration should also be given to matching internal 

standards to analytes with similar ionization potentials. 

 Matrix effects are monitored by comparing the internal standard intensity 

in the sample to the internal standard intensity of the calibration blank. 

The internal standards must be between 60% and 125% of the calibration 
D-4 

blank. If they are outside this window the sample is diluted by a factor of 

2 (1:1) and is reanalyzed. 

 Memory effects are dependent on the relative concentration differences 

between samples and/or standards which are analyzed sequentially. The 

rinse period between samples must be long enough to eliminate 

significant memory interference (see section 10.3.6). 

5.0 Safety 

This procedure may involve hazardous material, operations and equipment. This 

procedure does not purport to address all of the safety problems associated with its use. 

It is the responsibility of the user of the method to follow appropriate safety, waste 

disposal and health practices under the assumption that all samples and reagents are 

potentially hazardous. Safety glasses, gloves, lab coats and closed-toe, nonabsorbent 

shoes are required. 

5.1 Specific Safety Concerns or Requirements 

5.1.1 Eye protection that satisfies ANSI Z87.1, laboratory coat, and 

nonpowdered nitrile or latex gloves must be worn while handling 

samples, standards, solvents, and reagents. Disposable gloves that 

have been contaminated must be removed and discarded; nondisposable gloves must be cleaned immediately. 

5.1.2 The ICP plasma emits strong UV light and is harmful to vision. All 

analysts must avoid looking directly at the plasma. The RF Generator 

produces strong radio frequency waves, most of which are unshielded. 

People with pacemakers should not go near the instrument while in 

operation. 

5.2 Primary Materials Used 

The following is a list of the materials used in this method, which have a serious 

or significant hazard rating. Note: This list does not include all materials 

used in the method. The table contains a summary of the primary hazards 

listed in the MSDS for each of the materials listed in the table. 
D-5 

Material (1) Hazards Exposure 

Limit (2) Signs and Symptoms of Exposure 

Nitric Acid Corrosive 

Oxidizer 

Poison 

2 ppmTWA 

4 ppmSTEL 

Nitric acid is extremely hazardous; it is corrosive, reactive, 

an oxidizer, and a poison. Inhalation of vapors can cause 

breathing difficulties and lead to pneumonia and pulmonary 

edema, which may be fatal. Other symptoms may include 

coughing, choking, and irritation of the nose, throat, and 

respiratory tract. Can cause redness, pain, and severe skin 

burns. Concentrated solutions cause deep ulcers and stain 

skin a yellow or yellow-brown color. Vapors are irritating and 

may cause damage to the eyes. Contact may cause severe 

burns and permanent eye damage. 

Material (1) 

Hazards 

Exposure 

Limit (2) Signs and Symptoms of Exposure 

Hydrochloric 

Acid 

Corrosive 

Poison 

5 ppmCeiling Inhalation of vapors can cause coughing, choking, 

inflammation of the nose, throat, and upper respiratory tract, 

and in severe cases, pulmonary edema, circulatory failure, 

and death. Can cause redness, pain, and severe skin burns. 

Vapors are irritating and may cause damage to the eyes. 

Contact may cause severe burns and permanent eye 

damage. 

1 – Always add acid to water to prevent violent reactions. 

2 – Exposure limit refers to the OSHA regulatory exposure limit. 

6.0 Equipment and Supplies

6.1 Instrumentation 

 Inductively Coupled Plasma Mass Spectrometer (ICP/MS) capable of providing 

resolution, less than or equal to 0.9 amu at 10% peak height from 6-253 amu 

and 1.0 amu at 5% peak height from 6-253 amu with a data system that allows 

corrections for isobaric interferences and the application of the internal standard 

technique. The ICP/MS must be equipped with a collision cell for the removal of 

molecular interferences. This procedure was developed using an Agilent 7500 

or 7700 instrument equipped with a high matrix interface. The interface extends 

the amounts of total dissolved solids that may be measured into the percent 

concentration range. Any collision cell instrumentation that meets the 

specifications in this procedure may be used. 

 A discrete sample introduction system enables the use of only the exact amount 

of sample volume required for data acquisition. 

 Accessories and configuration that are designed to accommodate samples with 

high levels of dissolved solids should be used. 

 This sampling system results in less matrix being deposited in the system 

during analysis and minimizes the rinse times normally needed for difficult 

matrices. 

 Autosampler with autosampler tubes. 

 Appropriate water cooling device. 

 Block digester with tubes. 

6.2 Supplies 
D-6 

 Argon gas: High purity grade (99.99%). 

 Helium gas: High purity grade (99.99%). 

 Hydrogen gas: High purity grade (99.99%). 

 Calibrated automatic pipettes or Class A glass volumetric pipettes. 

7.0 Reagents and Standards

7.1 Storage and Shelf-Life 

7.1.1 All standards must be stored in glass, FEP fluorocarbon or previously 

unused polyethylene or polypropylene bottles. Standards stored at 

concentrations as received from the vendor and mid-level dilutions must 

be replaced prior to the expiration date assigned by the vendor. If no 

expiration date is provided, the stocks and mid-level standards may be 

stored for up to one year. They must be replaced sooner if verification 

from an independent source indicates a problem (See section 10.3.5 for 

initial calibration verification acceptance criteria). 

7.1.2 Working standards, i.e., all standards at concentrations ready to 

analyze on the ICP/MS (all except tuning mixes, ICSA and ICSAB 

mixes, which are received at ready-to-use concentrations), are prepared 

fresh daily. 

7.2 Standards

7.2.1 Tuning Solution, 10 ppb 

The tuning solution stock is purchased as a custom multi-element mix. 

The concentrations of the constituents are shown in Attachment 5. 

Prepare the Tuning Solution as detailed below. 

 Obtain a clean 100 mL volumetric flask. 

 Place 50 mL of reagent water and 2 mL of conc. HNO3 and 0.5 

mL of conc. HCl in the flask. 

 Swirl to mix. 

 Pipet 0.1mL of the Tuning Solution Stock into the flask. 

 Dilute to volume with reagent water. Stopper and mix. 

7.2.2 PA Tuning Solution 

The dual detector solution may be commercially purchased as a custom 

multi-element mix. 

Prepare the PA Tuning Solution as detailed below. 

 Add approximately 50 mL of the 2% HNO3 / 0.5% HCl to a 100 

mL volumetric flask. 

 Prepare at a concentration recommended by the instrument 

manufacturer. 

7.2.3 Calibration Standards 

Stock calibration standards are purchased as custom multi-element 

mixes or as single element solutions. Each day of analysis, the 

standards are diluted to working levels using 2% nitric acid and 0.5% 

HCl acid matrix. Suggested concentrations are given in Attachment 8, 
D-7 

but the laboratory may adjust calibration standard concentrations as 

appropriate for the instrument and samples. At a minimum, a 3 point 

curve must be used. 

7.2.4 Individual FGD Interference check solutions. 

7.2.4.1 All individual FGD interference check solutions should be 

made up in the same acid matrix as the calibration standards. 

7.2.4.2 Chloride, 10,000 mg/L 

7.2.4.3 Calcium, 5,000 mg/L 

7.2.4.4 Sulfate, 4,000 mg/L 

7.2.4.5 Magnesium, 3,000 mg/L 

7.2.4.6 Sodium, 2,000 mg/L 

7.2.4.7 Boron, 500 mg/L 

7.2.4.8 Iron, 500 mg/L

7.2.4.9 Nitrate, 250 mg/L 

7.2.4.10 Manganese, 200 mg/L 

7.2.4.11 Bromide, 100 mg/L 

7.2.4.12 Fluoride, 100 mg/L 

7.2.4.13 Selenium, 20 mg/L

7.2.4.14 Vanadium, 10 mg/L

7.2.4.15 Zinc, 2 mg/L

7.2.4.16 Chromium, 1 mg/L

7.2.4.17 Copper, 1 mg/L

7.2.5 Mixed Interference Check Solution (Synthetic FGD Wastewater) 

7.2.5.1 Chloride, 5,000 mg/L 

7.2.5.2 Calcium, 2,000 mg/L 

7.2.5.3 Magnesium, 1,000 mg/L 

7.2.5.4 Sulfate, 2,000 mg/L 

7.2.5.5 Sodium, 1,000 mg/L 

7.2.5.6 Butanol, 2000ppm 

7.2.6 Initial Calibration Verification (ICV) Standard 

The ICV stock is from a source different than the source for the 

calibration standards. Each day of analysis, the ICV standard is 

prepared in 2% HNO3 and 0.5 % HCl acid to the concentrations shown 

in Attachment 8. 
D-8 

7.2.7 Continuing Calibration Verification (CCV) Standard 

The CCV is prepared from the same source as the calibration 

standards. The CCV standards are prepared fresh each day of analysis 

in 2% HNO3/0.5% HCl. The concentrations are shown in Attachment 8. 

Prepare the Working CCV as detailed below. 

 Dilute by 2X a known volume of the Working Calibration 

Standard in the 2% HNO3 / 0.5% HCl acid matrix. 

7.2.8 Spiking Stock Solution 

The spike stock solution is prepared from the same stocks as the 

calibration standards using the 2% HNO3 / 0.5% HCl acid matrix. Spike 

concentrations are listed in Attachment 8. 

7.3 Reagents

7.3.1 Reagent Water - ASTM Type I or equivalent for the elements of 

interest, generated using an ion-exchange water polishing system 

capable of achieving 18.0 megohm-cm.

7.3.2 Blank Matrix 2% HNO3 and 0.5% HCl. 

8.0 Sample Collection, Preservation, Shipment and Storage

Sample container, preservation techniques and holding times may vary and are 

dependent on sample matrix, method of choice, regulatory compliance, and/or specific 

contract or client requests. Listed below are the holding times and the references that 

include preservation requirements. 

Matrix Sample 

Container 

Min. Sample 

Size Preservation Holding Time Reference 

Waters HDPE 50 mLs HNO3, pH < 2 180 Days 40 CFR Part 136.3

Soils Glass or 

HDPE 

4 oz Cool 4 + 2oC 180 Days N/A 

9.0 Quality Control 

9.1 Quality control requirements are also summarized in Attachment 7. 

9.2 Ongoing data quality checks are compared with established performance criteria 

to determine if the results of analyses meet the performance characteristics of 

the method. Any QC result that fails to meet control criteria must be 

documented. 

9.3 Individual interference check solutions 

The individual interference check solutions listed in section 7.2.6 are analyzed 

prior to initiating sample analysis, and at least once per quarter while FGD 

wastewaters are being analyzed, and after any major changes to instrument 

operating conditions. Concentrations of target elements observed should be less 

than their reporting limits. In some cases it may not be possible to obtain 

interference check solutions that are completely free of contamination. In this 
D-9 

case, results up to 5X the reporting limit are acceptable if it is possible to 

demonstrate that the isotopic ratios correspond to natural abundances. For 

example, the natural abundances of zinc isotopes are Zn64 48.6%; Zn66 27.9%; 

Zn67 4.1%; Zn68 18.8%; Zn70 0.6%. The measured ratios are not expected to be 

exact, especially for low abundance isotopes, and some isotope may be masked 

by other elements in the solution, (for example Zn70 in the above example will be 

masked by Ge70) but it must be possible to explain the observed ratios. 

Because Arsenic, Manganese and Aluminum are monoisotopic, this 

demonstration is not possible and the level of interference observed must be less 

than the reporting limit. 

9.4 Synthetic FGD interference check solution 

The synthetic FGD matrix solution listed in section 7.2.7 is analyzed prior to 

initiating sample analysis, and at least once per day (immediately after 

calibration) while FGD wastewaters are being analyzed, and after any major 

changes to instrument operating conditions. Internal standard recovery must 

meet method criteria (Section 9.9) and concentrations of target elements 

observed should be less than their reporting limits. In some cases it may not be 

possible to obtain interference check solutions that are completely free of 

contamination. In this case, results up to 5X the reporting limit are acceptable if it 

is possible to demonstrate that the isotopic ratios correspond to natural 

abundances. For example, the natural abundances of zinc isotopes are Zn64

48.6%; Zn66 27.9%; Zn67 4.1%; Zn68 18.8%; Zn70 0.6%. The measured ratios are 

not expected to be exact, and some isotopes may be masked by other elements 

in the solution, (for example Zn70 in the above example will be masked by Ge70) 

but it must be possible to explain the observed ratios. Because Arsenic, 

Manganese and Aluminum are monoisotopic, this demonstration is not possible, 

and the level of interference observed must be less than the reporting limit. 

If the Synthetic FGD solution has to be diluted in order to analyze it 

effectively on the ICP/MS, then all samples and QC (including the MDL 

replicates) must be diluted by at least the same factor. 

9.4.1 Laboratory fortified Synthetic FGD solution 

The synthetic FGD solution is spiked with 40ppb of each of the target 

elements (400ppb for zinc and 4000ppb for aluminum) and analyzed 

once per day, immediately after the synthetic FGD check in section 9.4. 

All target elements must be recovered within 70-130% of the true value. 

If the Laboratory Fortified Synthetic FGD solution has to be diluted 

in order to analyze it effectively on the ICP/MS, then all samples 

and QC (including the MDL replicates) must be diluted by at least 

the same factor. 

9.5 Linear range determination 

The linear range for each element is determined prior to initiating sample 

analysis and at least once per year thereafter. The linear range must also be 

determined subsequent to changes that will have a major effect on instrument 

sensitivity, such as changing the detector. The linear range is established using a 

single element standard at the desired linear range. The result of the analysis 

must be within 10% of the true value. 
D-10 

9.6 Method Blank / Laboratory Reagent Blank (MB/LRB) 

The method blank consists of reagent water that has been processed in 

the same manner as the samples. One method blank must be processed with 

each preparation batch. 

Acceptance Criteria: Method blank results are acceptable if the concentration 

for each analyte of interest is less than the reporting limit. 

Corrective Action: If the method blank does not meet the acceptance 

criteria, the source of contamination should be 

investigated to determine if the problem can be 

minimized or eliminated. Samples associated with the 

contaminated blank shall be reprocessed for analysis, or 

under the following circumstances, may be reported as 

qualified (qualifier flags or narrative comments must be 

included on report): 

 The same analyte was not detected in the 

associated samples; 

 The method blank concentration is less than 1/10 of 

the measured concentration of any sample in the 

batch; 

 The method blank concentration is less than 1/10 

the specified regulatory limit; or 

 The analyte is a common laboratory contaminant 

(copper, iron, lead, calcium, magnesium, 

potassium, sodium, or zinc) less than 2 times the 

RL. Note that some programs do not recognize 

common lab contaminants. 

If the above criteria are not met and reanalysis is not 

possible, then the sample data must be qualified. This 

anomaly must be addressed in the project narrative 

and the client must be notified. 

9.7 Laboratory Control Sample / Laboratory Fortified Blank (LCS/LFB) 

The LCS consists of reagent water that is spiked with the analytes of 

interest as summarized in Attachment 8. One LCS must be processed (digestion 

and analysis) for each preparation batch. 

Acceptance Criteria: LCS control limits are based on three standard 

deviations of past laboratory results. These limits are not 

to exceed 85-115% recovery. The control limits are 

maintained in a LIMS or other appropriate system. 

Corrective Action: If the LCS % recovery falls outside of the control limits for 

any analyte, that analyte is judged to be out of control. 

All associated samples must be reprocessed for 

analysis. One possible exception is a recovery for a 

given element above the upper control limit with no 

detection for the same element in the samples. 

9.8 Matrix Spike / Matrix Spike Duplicate / Laboratory Fortified Sample Matrix / 

Laboratory Fortified Matrix Duplicate (MS/MSD/LFSM/LFMD) 

MS is prepared by taking a second aliquot of a selected sample and spiking it 

with the analytes of interest as summarized in Attachment 8. An MSD is 
D-11 

prepared by taking a third aliquot of a selected sample and spiking it with the 

analytes of interest as summarized in Attachment 8. The MS and MSD are 

processed in the same manner as the samples. One MS/MSD pair must be 

processed every 10 samples. 

Acceptance Criteria: Control limits are based on three standard deviations of 

past laboratory results. These limits are not to exceed 

70-130% recovery, and 20% relative percent difference 

(RPD). The control limits are maintained in the LIMS 

system. If the sample concentration for a specific analyte 

in the sample selected for spiking is greater than the 

concentration added by the spike, then recovery 

accuracy will be reduced. In this case a dilution test may 

be performed. A 1:5 dilution should agree within 20% of 

the original determination. If not, a physical or chemical 

interference is suspected, and must be discussed in the 

sample narrative. 

Corrective Action: If MS/MSD results and any applicable dilution tests do 

not meet the acceptance criteria and all other quality 

control criteria have been met, then a matrix interference 

is suspected. Failed matrix spikes are flagged, and are 

discussed in the final report case narrative. 

9.9 Internal Standards Evaluation for Samples 

The internal standards in samples must be between 60 and 125% of the intensity 

in the calibration blank. If the sample intensities fall outside this range, the 

calibration blank is reanalyzed to confirm the instrument has not drifted out of 

control. If the criteria is met, the sample is diluted by a factor of 2 (1:1) and 

reanalyzed. IS limits and corrective actions for standards and blanks are 

described in Section 10. 

10.0 Procedure

10.1 One-time procedural variations are allowed only if deemed necessary in the 

professional judgment of the supervisor to accommodate variation in sample 

matrix, radioactivity, chemistry, sample size, or other parameters. Any variation 

in procedure shall be completely documented. Any unauthorized deviations from 

this procedure must also be documented as a nonconformance, with a cause 

and corrective action described. 

10.2 Sample Preparation 

10.2.1 EPA Method 1638 was used as the reference for the digestion of the 

samples in which Section 12.2.8 describes Closed Vessel digestion. 

10.2.2 Transfer a 50mL (+/- 0.5mL) aliquot from a well mixed acid preserved 

sample to a 50mL digestion tube. 

10.2.3 Add 0.5mL of concentrated nitric acid and 0.25 mL hydrochloric acid. 

10.2.4 Spike the LCS and MS/MSD samples per spiking protocols. 
D-12 

10.2.5 The total volume of the solution in the tube is now greater than 50 mLs. 

The final volume will be 50 ml following the procedure to eliminate the 

discrepancy in the initial and final volumes. 

10.2.6 Tightly cap each digestion vessel. 

10.2.7 Place the digestion tube into a block digester adjusted to achieve a 

temperature of approximately 85o

C. 

10.2.8 Heat for 2 hours after 85o

C is obtained. 

10.2.9 Remove from the block and allow to cool. 

10.3 Calibration 

10.3.1 Instrument Start Up 

Set up the instrument according to manufacturer’s operating instructions. 

Allow the instrument to become thermally stable for at least 30 minutes 

before tuning. 

10.3.2 Instrument Tuning / Mass Calibration 

Tune the instrument with a solution containing elements representing all 

of the mass regions of interest. The relative standard deviations must be 

less than 5% for a minimum of 4 integrations of the solution. Mass 

calibration and resolution checks using the tuning solution must be 

completed at the beginning of every day. 

Mass Calibration Check – The mass calibration results must be within 

0.1 amu from the true value. If this criterion 

is not met, the mass calibration must be 

adjusted before running samples. 

Mass Resolution Check - The resolution must be verified to be less 

than 0.9 amu full width at 10% peak height. 

10.3.3 Mass 75 interference check 

The concentration determined for arsenic (mass 75) must be less than 

0.25 x the reporting limit when the blank matrix (2% nitric acid / 0.5% 

hydrochloric acid) is infused (using the collision gas mode used for 

arsenic). 

10.3.4 Initial Calibration 

The ICP/MS is calibrated each day of operation using a blank and at 

least 3 standards (see Section 7.2.3). Report the average of at least 

three integrations. 

The validity of the calibration is determined by the subsequent 

calibration verifications, which are performed at concentrations as 

described in the next sections. 

10.3.5 Second-Source Initial Calibration Verification (ICV) 

A 40 g/L / 4,000 ug/L ICV standard (see Section 7.2.8) is analyzed 

immediately after the initial calibration. This is a standard obtained from 

a different vendor than the standard used for calibration. This analysis 

also satisfies the Method 200.8 requirement for a Quality Check 

Standard (QCS). 

Acceptance Criteria: The ICV recovery must be within 90-110%. 

Additionally, the internal standard recoveries for 
D-13 

200.8 must fall between 60 and 125% of true 

values. The ICV can be reanalyzed, but must 

be successful twice in succession or corrective 

action must be taken. 

Corrective Action: If the ICV results are outside of the acceptance 

limits, investigate the accuracy of the 

standards, correct as necessary, and 

recalibrate. 

10.3.6 Calibration Blank 

Checks for the memory effects described at Section 4.4 may be 

accomplished by analysis of an initial calibration blank (ICB) after the 

ICV. Continuing calibration blanks (CCBs) are analyzed after each 

continuing calibration verification. 

Acceptance Criteria: Results for the calibration blanks must be less 

than the RL. 

Corrective Action: If the calibration blank exceeds acceptance 

limits, then the possibility of instrument 

contamination should be examined, particularly 

the possibility of carry-over from high level 

samples. The blank can be reanalyzed, and if 

successful, analysis can continue. However, 

samples tested after high-level samples should 

be retested. If the reanalysis is not successful, 

then the analysis should be terminated. After 

the problem is corrected, recalibrate and 

reanalyze all samples tested since the last 

acceptable CCB. 

10.3.7 Reporting Limit (RL) Verification Standard 

An independent standard is analyzed after the ICV to monitor the lab’s 

ability to produce reliable results at RL-level concentrations. The RL 

verification standard is analyzed after the daily ICB. 

Acceptance Criteria: For project reporting limits at or above two 

times the MDL, the results should be within 

50% of the expected value. Some programs 

may require tighter control, in which case the 

RLs will need to be three or more times the 

MDL concentration. 

Corrective Action: If the RL verification fails to meet acceptance 

limits, data for the associated samples must be 

assessed. For example, if the results are high, 

consider blank contamination, and if the results 

are low, consider MDL verifications. At a 

minimum, sample results must be qualified in 

the final report. 

10.3.8 Continuing Calibration Verification (CCV) Standard 

A 50 g/L CCV standard is analyzed after every set of ten samples and 

at the end of the analytical sequence. 
D-14 

Acceptance Criteria: The CCV recovery must be within 85-115%. In 

addition, the IS recovery must be within 60-

125%. If CCV results are not within these 

limits, the CCV can be reanalyzed, but it must 

be successful twice in succession or further 

corrective action must be taken. 

Corrective Action: If the CCV fails acceptance criteria, then the 

analysis should be terminated. Recalibrate and 

reanalyze all samples tested since the last 

acceptable CCB. 

10.4 Sample Analysis 

10.4.1 Report the average of at least three integrations for all field and QC 

samples analyzed. 

10.4.2 Flush the system with the rinse blank for at least 30 seconds between 

samples and standards during the analytical run. Evaluate the 

effectiveness of this time and increase the flush time, if needed. 

10.4.3 It may be valuable to monitor additional isotopes for elements that are 

potentially susceptible to interferences. In particular, monitoring 

additional isotopes for selenium may help data analysis. 

10.4.4 Dilute and reanalyze samples that are more concentrated than the 

highest calibration standard for an analyte or specific isotope of interest. 

No analyte may be reported from an analysis of a diluted sample in 

which the analyte concentration is less than 5 times the RL. 

The analytical run sequence should be performed as follows to meet all 

quality control criteria: 

Instrument initialization 

Warm-up 

Tune instrument 

Perform mass calibration 

Perform resolution check 

Validate tuning criteria 

Calibration blank 

Calibration standard 1 

Calibration standard 2 

Calibration standard 3 

ICV 

ICB 

RL verification standard 

Synthetic FGD matrix 

Spiked synthetic FGD matrix 

Carryover check 

CCV 

CCB 

10 Samples (which can include all sample types) 

CCV 

CCB 
D-15 

11.0 Calculations / Data Reduction

11.1 LCS percent recoveries are calculated according to the equation:

11.2 ICV percent recoveries are calculated according to the equation:

11.3 CCV percent recoveries are calculated according to the equation:

11.4 Matrix Spike Recoveries are calculated according to the following equation:

Where: 

SSR = Spike Sample Result 

SR = Sample Result 

SA = Spike Added 

NOTE: When the sample concentration is less than the detection limit, use SR = 0 

for the purpose of calculating %R. 

11.5 The relative percent difference (RPD) between sample duplicates is 

calculated according to the following equation:

Where: 

DU1 = Sample result 

DU2 = Sample duplicate result 

100%

ICV True Value

ICV Found Value % 



 



 R 

100%

CCV True Value

CCV Found Value % 



 



 R 

100%

SA

SSR - SR % 



 



 R 

  100

1 2 2

1

/ 1 2/





















  DU DUDU DU RPD

100%

LCSTrue Value

LCS Found Value - LRB Found Value % 



 



 R 
D-16 

11.6 The final concentration for an aqueous sample is calculated as follows:

2

1 Result ( g/L) V

C V  D

 

Where: 

C = Concentration from instrument readout, ppb 

D = Instrument dilution factor 

V1 = Final volume in liters after sample preparation 

V2 = Initial volume of sample digested in liters 

12.0 Method Performance 

12.1 Method Detection Limit Study (MDL) 

An initial method detection limit study must be performed on each instrument 

before samples can be analyzed. MDL studies are conducted annually as 

follows: 

 Prepare seven samples at three to five times the estimated MDL 

concentration. The MDL samples are prepared in the Synthetic FGD 

wastewater matrix and in reagent water. 

 Prepare and analyze the MDL standards as described in Section 10. 

 Calculate the average concentration found in μg/L, and the standard 

deviation of the concentration(s) in μg/L, for each analyte. 

 The MDL is calculated as Students t for the 99th percentile times the standard 

deviation of the MDL replicate results, following the procedure at 40CFR Part 

136, Appendix B. 

NOTE1: Perform the MDL study in the synthetic FGD 

wastewater matrix. Spiking this matrix provides detection 

limits that are better matched to the complex matrix 

typical of FGD wastewater. These limits can be 

significantly higher than those obtained in a reagent water 

matrix. In some cases (zinc in particular), the level of 

contamination in the synthetic FGD solution may be high 

enough to result in somewhat elevated MDLs. 

NOTE2: An FGD-MDL may be less than the MDL observed in 

method blanks. If this occurs frequently, the FGD-MDL 

should be elevated to the mean of the method blanks plus 

the Student t factor times the standard deviation of the 

method blanks. 

12.2 Instrument Detection Limit Study 

Instrument detection limit (IDL) studies are conducted quarterly for each 

instrument and each mass used for analysis. 

 Prepare ten blanks. 

 Analyze the IDL blanks on three non-consecutive days. 

 The IDL is equal to three times the standard deviation of the blank results.
D-17 

12.3 Demonstration of Capabilities

All personnel are required to perform an initial demonstration of proficiency 

(IDOC) on the instrument they will be using for analysis prior to testing samples. 

On-going proficiency must be demonstrated annually. IDOCs and on-going 

proficiency demonstrations are conducted as follows. 

Four aliquots of the ICV are analyzed using the same instrumental conditions 

and procedures used to analyze samples. The analyst must employ ICV’s from 

four distinct analytical sequences. Using these four ICV’s demonstrates the 

analyst’s ability to optimize and calibrate the instrument and to prepare analytical 

solutions. Calculate the average recovery and standard deviation of the recovery 

for each analyte of interest. 

 If any analyte does not meet the acceptance criteria, (85-115% recovery, 

unless other criteria are established) the test must be repeated. Only those 

analytes that did not meet criteria in the first test need to be evaluated. 

Repeated failure for any analyte indicates the need for the laboratory to 

evaluate the analytical procedure and take corrective action. 

12.4 Training Requirements 

12.4.1 Each analyst performing the method must complete a demonstration of 

capability (DOC) by successfully preparing and/or analyzing four 

consecutive LCSs, or a blind performance evaluation (PE) sample, or 

other acceptable QC samples. Analysts who continue to perform the 

method must successfully complete a demonstration of capability 

annually. 

13.0 Pollution Control 

13.1.1 For information about pollution prevention that may be applicable to 

laboratory operations, consult “Less is Better: Laboratory Chemical 

Management for Waste Reduction” available from the American 

Chemical Society’s Department of Government Relations and Science 

Policy, 1155 16th Street N.W., Washington, D.C., 20036, or online at 

http://www.ups.edu/x7432.xml. 

14.0 Waste Management

All waste must be disposed of in accordance with Federal, State, and local 

regulations. 

15.0 References / Cross-References

15.1 EPA Method 200.8, “Determination of Trace Elements in Waters and Wastes 

by Inductively Coupled Plasma - Mass Spectrometry”, Revision 5.4, EMMC 

Version. 

15.2 EPA Method 1638, “Determination of Trace Elements in Ambient Waters by 

Inductively Coupled Plasma – Mass Spectrometry, January 1996 
D-18 

16.0 Attachments

Attachment 1: Recommended Elemental Equations 

Attachment 2: Internal Standards and Corresponding Metals 

Attachment 3: Sample Preservation and Holding Times 

Attachment 4: Suggested Mass Choices 

Attachment 5: Tuning Solution 

Attachment 6: Suggested Tuning and Response Factor Criteria 

Attachment 7: Summary of Quality Control Requirements 

Attachment 8: Calibration, Calibration Verification, and Spike Concentrations
D-19 

Attachment 1 

Recommended Elemental Equations 

Element 

Isobaric 

Correction Mathematical Equation 

Pb None (1.0000)(208M) + (1.0000)(207M) + (1.0000)(206M) 

6Li Li (natural) (1.0000)(6M) - (0.0813)(7M) 

In Sn (1.0000)(115M) - (0.0149)(118M) 

The 6

Li correction equation is only needed if 6Li is used as an internal standard for low mass elements. 

Attachment 2: Internal Standards and Corresponding Metals 

Internal Std. Associated elements1,2

Sc Na, Mg, Al, K, Ca, V, Cr, Mn 

Ge Fe, Ni, Cu, Zn, As, Se 

In Ag, Cd 

Ho Tl, Pb 

Footnote: (1) Na, Mg, K, Ca and Fe are included in the synthetic FGD wastewater but their 

analytical determination is optional – the interferences caused by these elements are more 

important than the determination of their exact concentration. 

(2) Other internal standards may be used. For example, 6

Li, Ga, Rh, Bi, Ho and Tb may be 

considered for use as internal standards. 
D-20 

Attachment 3: Sample Preservation and Holding Times 

Measurement 

Parameter

Container (1) Preservative (2) Maximum Holding 

Time (3)

Waters: 

Metals (4) P,G HNO3 to pH < 2 6 months 

Soils/Sediments/Wastes: 

The preservation required for soil/sediment/waste samples is maintenance at 4°C ( ± 2°C) until 

digestion. 

Footnotes: (1) Polyethylene (P) or glass (G). 

 (2) Sample preservation is performed by the sampler immediately upon sample 

collection or shipped to the laboratory unpreserved for preservation at the 

laboratory. 

 (3) Samples must be analyzed as soon as possible after collection. The times listed 

are the maximum times that sample may be held before analysis and still 

considered valid. Holding times are calculated from the date when the sample 

was collected. 

 (4) Samples are filtered immediately on-site by the sampler before adding 

preservative for dissolved elements. 
D-21 

Attachment 4: Suggested Mass Choices 

Masses listed indicate the masses which have the most impact on data quality and the elemental 

equations used to collect the data. 

Mass Element of Interest Analysis mode 

27 Aluminum No gas 

75 Arsenic He 

111 Cadmium He 

52 Chromium He 

63 Copper He 

208, 207, 206 Lead No gas or He 

24 Magnesium No gas 

55 Manganese He 

60 Nickel He 

39 Potassium No gas or He 

78 Selenium He (H2) 

107 Silver He 

23 Sodium No gas or He 

205 Thallium No gas or He 

51 Vanadium He 

66 Zinc He 

NOTE: It is strongly recommended that elements other than those of interest be 

monitored to indicate other potential molecular interferences which could 

affect the data quality. 
D-22 

Attachment 5: Tuning Solution 

A tuning solution containing elements representing all of the mass regions of interest must be analyzed. 

Below are two groups of suggested solutions which cover a typical mass calibration range. 

Method 200.8 

Element Concentration (g/L) 

Mg 10 

Rh 10 

Ba 10 

Be 10 

U 10 

Ce 10 

Y 10 

Pb 10 

Li 10 

Co 10 

In 10 

Tl 10 
D-23 

Attachment 6: Suggested Tuning and Response Factor Criteria 

No Gas Mode

Li7 >2000cps 

Tl205 >3000cps 

CeO/Ce 156/140 1% 

Ce++/Ce+ 70/140 <3% 

He Mode:

ArAr 78 2-3 counts/sec 

ArCl 75 2-3 counts/sec 
D-24 

Attachment 7: Summary of Quality Control Requirements 

QC Parameter Frequency Acceptance Criteria Corrective Action 

ICV/QCS Beginning of every 

analytical run. 

90 - 110% recovery. 

200.8 IS, 60-125% rec. 

Terminate analysis; 

correct the problem; 

recalibrate. 

ICB/CCB Immediately after each 

ICV. 

The result is < RL 

200.8 IS, 60-125% rec. 

Terminate analysis; 

correct the problem; 

recalibrate. 

Synthetic FGD 

interference check 

Prior to initiating 

analysis and at least 

quarterly. 

Result for target elements 

is < RL, unless actual 

presence of target 

element can be 

demonstrated, in which 

case result is < 5X RL. 

Correct the problem prior 

to sample analysis. 

Individual element 

interference checks 

Prior to initiating 

analysis and at least 

quarterly. 

Result for target elements 

is < RL, unless actual 

presence of target 

element can be 

demonstrated, in which 

case result is < 5X RL. 

Correct the problem prior 

to sample analysis. 

CCV Beginning and end of run 

and every 10 samples OR

every 2 hours, whichever 

is more frequent. 

Beginning and end of 

each lot. 

90 - 110% recovery. 

IS, 60-125% rec. 

If unacceptable, 

terminate analysis; 

correct the problem; 

recalibrate the 

instrument, reverify 

calibration and rerun all 

samples since the last 

acceptable CCV. 

CCB Immediately following 

each CCV. 

The result must be < RL 

200.8 IS, 60-125% rec. 

If unacceptable, 

terminate analysis; 

correct the problem, 

recalibrate the 

instrument, reverify 

calibration and rerun 

all samples since the 

last acceptable CCB. 
D-25 

Attachment 7: Summary of Quality Control Requirements (continued) 

QC Parameter Frequency Acceptance Criteria Corrective Action 

Method 

Blank/Laboratory 

Reagent Blank 

One per lot of 20 field 

samples or fewer. 

The result must be less 

than the RL. 

Sample results greater 

than 10x the blank 

concentration or samples 

for which the 

contaminant is < RL, do 

not require redigestion or 

reanalysis. 

Re-run once. If > than 

the RL, Redigest and 

reanalyze samples. 

Note exceptions under 

criteria section. 

See Section 9.4 for 

additional requirements. 

Matrix Spike/Laboratory 

Fortified Matrix 

One every ten samples or 

fewer. 

Must be within 

laboratory control limits. 

See section 9.6 for 

additional requirements. 
D-26 

Attachment 8: Calibration, Calibration Verification, and Spike Concentrations 

Element 

Initial Calibration 

(g/L) 

ICV 

(g/L)

CCV 

(g/L)

LCS

(g/L)

MS/MSD 

(g/L)

Aluminum 100, 1,000, 10,000 4000 5000 4000 4000 

Arsenic 1, 10, 100 40 50 40 40 

Cadmium 1, 10, 100 40 50 40 40 

Chromium 1, 10, 100 40 50 40 40 

Copper 1, 10, 100 40 50 40 40 

Lead 1, 10, 100 40 50 40 40 

Manganese 1, 10, 100 40 50 40 40 

Nickel 1, 10, 100 40 50 40 40 

Selenium 1, 10, 100 40 50 40 40 

Silver 1, 10, 100 40 50 40 40 

Thallium 1, 10, 100 40 50 40 40 

Vanadium 1, 10, 100 40 50 40 40 

Zinc 1, 10, 100 40 50 40 40 

Additional elements may be included in the calibration solution at the above levels. Levels 

may be adjusted to meet specific requirements. 

####