Sampling Episode Report 

Mirant Mid-Atlantic, LLC’s 

Dickerson Generating Station 

Dickerson, MD 

Sampling Episode 6562

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

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

2.2.2 Biological Sequencing Batch Reactors....................................................2-4

2.2.3 Sampling Points .......................................................................................2-5

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

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

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

3.1.2 Influent to the SBR ..................................................................................3-3

3.1.3 Effluent from the SBR .............................................................................3-6

3.2 List of Analytes and Sample Preservation...........................................................3-9

3.3 Plant Operational Data.......................................................................................3-10

3.4 Deviations from the Sampling and Analysis Plan .............................................3-10

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

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

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

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

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

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

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

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

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

Appendix A: ANALYTICAL RESULTS

Appendix B: DATA REVIEW NARRATIVES

Appendix C: PICTURES FROM THE SAMPLING EPISODE

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, Dickerson.............................................................. 3-12

Table 3-2. Sample Collection at Dickerson Steam Station........................................................ 3-14

Table 3-3. Field Measurements, Dickerson ............................................................................... 3-15

Table 3-4. Crosswalk of Sample Number to Sampling Point and Day, Dickerson................... 3-17

Table 3-5. Analytical Methods, Dickerson................................................................................ 3-18

Table 3-6. Summary of Sample Container and Planned Preservation, Dickerson .................... 3-19

Table 3-7. Sample Preservation Summary, Dickerson .............................................................. 3-20

Table 3-8. Generating Unit Operating Characteristics during Sample Collection, Dickerson.. 3-23

Table 3-9. FGD Scrubber System Operating Characteristics, Dickerson.................................. 3-24

Table 3-10. Coal Usage during Sample Collection, Dickerson................................................. 3-25

Table 3-11. Scrubber Slurry Information during Sample Collection, Dickerson...................... 3-25

Table 3-12. FGD Wastewater Treatment System Operation Information, Dickerson .............. 3-26

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

Table 4-2. Influent to the SBR System, Dickerson..................................................................... 4-7

Table 4-3. Effluent from the SBR System, Dickerson.............................................................. 4-11

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

Treatment System, Dickerson........................................................................................ 4-14

Table 4-5. Metal Pollutants 4-Day Average Data Summary for FGD Wastewater Treatment 

System, Dickerson ......................................................................................................... 4-15

Table 5-1. Field Blank Analytical Results, Dickerson ............................................................... 5-5

Table 5-2. Field Duplicate Results – Influent to SBR System, Dickerson................................. 5-6

Table 5-3. Field Duplicate Results – Effluent from SBR System, Dickerson............................ 5-9

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

Dickerson ........................................................................................................................ A-1

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

Dickerson ........................................................................................................................ A-4
LIST OF TABLES (Continued) 

Page 

iii

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

Dickerson ........................................................................................................................ A-7

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

Dickerson ...................................................................................................................... A-10

Table A-5. Influent to SBR System, Day 1 Analytical Results, Dickerson............................. A-13

Table A-6. Influent to SBR System, Day 2 Analytical Results, Dickerson............................. A-16

Table A-7. Influent to SBR System, Day 3 Analytical Results, Dickerson............................. A-19

Table A-8. Influent to SBR System, Day 4 Analytical Results, Dickerson............................. A-22

Table A-9. Effluent from SBR System, Day 1 Analytical Results, Dickerson ....................... A-25

Table A-10. Effluent from SBR System, Day 2 Analytical Results, Dickerson ..................... A-28

Table A-11. Effluent from SBR System, Day 3 Analytical Results, Dickerson ..................... A-31

Table A-12. Effluent from SBR System, Day 4 Analytical Results, Dickerson ..................... A-34

Table A-13. Duplicate of Influent to SBR System, Day 3 Analytical Results, Dickerson...... A-37

Table A-14. Duplicate of Effluent from SBR System, Day 2 Analytical Results, 

Dickerson ...................................................................................................................... A-40

Table A-15. Bottle Blank and Equipment Blank Analytical Data, Dickerson ......................... A-43

Table A-16. Influent to FGD Wastewater Treatment System Field Blank, Day 1 Analytical 

Results, Dickerson ........................................................................................................ A-48

Table A-17. Influent to SBR System Field Blank, Day 1 Analytical Results, Dickerson....... A-50

Table A-18. Influent to SBR System Field Blank, Day 2 Analytical Results, Dickerson....... A-52

Table A-19. Influent to SBR System Field Blank, Day 3 Analytical Results, Dickerson....... A-53

Table A-20. Influent to SBR System Field Blank, Day 4 Analytical Results, Dickerson....... A-54

Table A-21. Effluent from SBR System Field Blank, Day 1 Analytical Results, Dickerson.. A-55

Table A-22. Effluent from SBR System Field Blank, Day 2 Analytical Results, Dickerson.. A-57

Table A-23. Effluent from SBR System Field Blank, Day 3 Analytical Results, Dickerson.. A-58

Table A-24. Effluent from SBR System Field Blank, Day 4 Analytical Results, Dickerson.. A-59
iv

LIST OF FIGURES 

Page 

Figure 2-1. Simplified Diagram of the FGD Wastewater Treatment System, Dickerson 

Generating Station ........................................................................................................... 2-7

Figure 2-2. Physical/Chemical Separation and Biological Reactor Portion of FGD 

Wastewater Treatment System, Dickerson Generating Station....................................... 2-8

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

Figure C-2. Sample Set Up at the Influent to the FGD Wastewater Treatment System..............C-2

Figure C-3. Composite Sample Collection Set Up at the Influent to the SBR System ...............C-3

Figure C-4. Composite Sample Collection Set Up at the Effluent from the SBR System ..........C-4
1-1

1. INTRODUCTION

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

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

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

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

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

place August 22 - 27, 2010, at Mirant Mid-Atlantic, LLC’s Dickerson Generating Station 

(Dickerson), located in Dickerson, Maryland (Sampling Episode 6562). The focus of Episode 

6562 was to characterize the purge stream entering the flue gas desulfurization (FGD) 

wastewater treatment system and the influent to and effluent from the sequencing batch reactor 

(SBR) system. The influent to the SBR also represents the effluent from the chemical 

precipitation system. 

1.1 Background of Detailed Study

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

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

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

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

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

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

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

wastewater. 

1.2 Power Plant Site Selection

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

configurations and characteristics of the plants. 

Dickerson 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 all three units; 

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

includes the following steps: 

— Equalization, 

— pH adjustment (lime addition), 

— Ferric chloride addition, 

— Polymer addition, 

— Clarification, 

— Filtration, 

— Biological treatment (nitrogen removal); 
1-2

 The plant operates selective non-catalytic reduction (SNCR) systems on all three 

units; and 

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

1.3 Sampling Episode Overview

EPA and its technical contractor, Eastern Research Group, Inc. (ERG) conducted a oneday pre-sampling site visit at Dickerson on March 9, 2010 as part of the detailed study. The 

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

Mirant Mid-Atlantic, LLC’s Dickerson Generating Station (Sampling Plan) [1], which describes 

the sample collection procedures used during the sampling episode. 

On Sunday, August 22, 2010, EPA arrived at Dickerson 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 (August 23 – 27, 2010). The following personnel participated in EPA’s 

sample collection activities: 

 Ron Jordan, EPA/EAD; 

 Jezebele Alicea, EPA/EAD; 

 Meghan Camp, ERG; 

 Holly Cannon, ERG; 

 TJ Finseth, ERG; 

 Kavya Kasturi, ERG; and 

 Elizabeth Sabol, 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 Dickerson’s representative and collected 

samples on behalf of the plant. 
2-1

2. FACILITY OVERVIEW

Dickerson operates three steam electric generating units and each has a coal-fired boiler. 

Units 1, 2, and 3, which came on line in 1959, 1960, and 1962, respectively, each have a capacity 

of 182 megawatts (MW). All three generating units burn eastern bituminous coal. Dickerson also 

has two combustion turbines on site that are 167 MW each. The Dickerson plant and supporting 

facilities are located on approximately 1,000 acres in Dickerson, MD, near the Potomac River. 

Mirant owns 800 acres for the plant and the other 200 acres are owned by Pepco for switch 

yards, right-of-ways, etc. 

In December 2009, Dickerson retrofitted all three units with a common wet FGD 

scrubber system to control the sulfur dioxide (SO2) releases from the plant. The wet FGD 

scrubber is designed to remove more than 95 percent of SO2 from the flue gas. With the addition 

of the FGD scrubber system, Dickerson also installed an FGD wastewater treatment system to 

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

Sections 2.1 and 2.2 further discuss the FGD scrubber system and the FGD wastewater treatment 

system, respectively. 

Dickerson retrofitted Units 1, 2, and 3 with SNCR systems in July 2009, to control 

nitrogen oxide (NOx) releases from the plant. Dickerson only operates the SNCR systems during 

ozone season, May 1 through September 30. 

The three electrostatic precipitators (ESPs) and one common baghouse at Dickerson are 

particulate control devices that are designed to remove 99.5 and 99.8 percent of the fly ash and 

other particulates from the flue gas, respectively. Dickerson utilizes ESPs and the baghouse to 

remove the fly ash from all three units. Forty percent of the flue gas from each unit goes to the 

individual unit’s ESP, while the remaining 60 percent is routed to the common baghouse. The fly 

ash and other particulates are collected in hoppers and are pneumatically transferred to fly ash 

silos. 

Units 1, 2, and 3 have the following configuration: 

 Boiler (ammonia injection for SNCR system); 

 Air preheater; 

 ESP (unit-specific) and baghouse (common); and 

 FGD scrubber system (common). 

Between 0134 and 0326 on Tuesday morning, which is prior to the end of the day 1 24-

hour sample compositing period, Dickerson shut down all three generating units due to lack of 

electricity demand1

. The station continued to operate the FGD wastewater treatment system at 

reduced flow rates and EPA continued to collect samples as planned through the end of the 

sampling episode. Additionally, the FGD system was shut down, but the plant occasionally blew 

down from the scrubber and operated the dewatering equipment to allow EPA to collect the 

influent samples. The sampling team monitored flow rates during the remainder of the sampling 

episode. The generating station and FGD scrubber did not resume operation until after the end of 

the sampling episode. 

 

1

 Unit 3 was shut down at 0134, Unit 1 was shut down at 0312, and Unit 2 was shut down at 0326 on August 24, 

2010. 
2-2

2.1 FGD Scrubber Systems

Dickerson operates one wet FGD scrubber system that treats the flue gas from all three 

coal-fired generating units. The plant uses limestone slurry as the sorbent for sulfur dioxide 

absorption. Limestone and service water are fed to on-site ball mills, which pulverize the 

limestone to create the slurry. From the ball mills, the slurry is transferred to classifiers to collect 

limestone particles that are too large for use in the FGD system. The underflow from the 

classifiers is sent back to the ball mill for additional processing. The overflow from the 

classifiers, which is approximately 28 percent solids (by weight), is transferred to the limestone 

slurry storage tank and then used as fresh limestone slurry in the absorber. 

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

is pumped to the various levels of the FGD scrubber with the recycle pumps. The FGD system 

has three levels of flooding headers. The flooding headers supply the slurry to the dual flow 

tray. As the slurry falls downward in the scrubber vessel, the flue gas flows countercurrent to the 

limestone slurry. The droplets of the slurry contact the flue gas and absorb the SO2, which reacts 

with the limestone particles and produces calcium sulfite. The droplets continue to flow 

downward in the scrubber until they settle on the dual flow tray, forming a layer of slurry that the 

flue gas must pass through to exit the FGD system. The spray droplets continue to flow 

downward in the scrubber until they reach the reaction tank. Dickerson bubbles air through the 

reaction tank to oxidize the calcium sulfite to calcium sulfate (i.e., gypsum). 

Dickerson controls the chlorides concentration in the scrubber to less than 20,000 parts 

per million (ppm). Typically, the chlorides concentration in the scrubber is about 15,000 ppm. 

The solids concentration in the scrubber ranges from 18 to 22 percent solids. Dickerson transfers 

the blowdown from the scrubber to the gypsum dewatering operations. 

The scrubber blowdown is pumped to the primary hydrocyclones where the solid gypsum 

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

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

The gypsum from the primary hydrocyclones is transferred to the vacuum filter belts. The 

overflow from the primary hydrocyclones is pumped to the secondary hydrocyclones. The 

underflow from the secondary hydrocyclones is sent to the FGD filtrate tank for recycle back to 

the absorber. The overflow from the secondary hydrocyclones is sent to the purge tank and then 

pumped to the FGD wastewater treatment system. 

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

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

approximately 10 percent. Dickerson has a 20-year contract to sell gypsum that is 94 to 99 

percent pure, has a moisture content of less than 9 percent, and has less than 100 ppm chlorides. 

Off-specification (“off-spec”) gypsum and other solids are sent to a waste management site in 

Virginia. Dickerson generated 2 or 3 days of off-specification gypsum at the beginning of the 

FGD start up, but has always met the specifications since that time. Dickerson expects to 

generate approximately 150,000 tons of gypsum per year.

2.2 FGD Wastewater Treatment System

The FGD wastewater treatment system is designed to receive intermittent transfers of 

FGD wastewater from the purge tank, which contains secondary hydrocyclone overflow, at a 
2-3

typical flow rate of 75 gallons per minute (gpm) and a design maximum flow rate of 110 gpm. 

The plant typically transfers FGD purge to the wastewater treatment system four to six times per 

day, depending on the unit loading. The average total daily flow rate is approximately 84,000 

gallons per day (gpd) and the maximum daily flow rate is 158,000 gpd. 

The plant operates the FGD wastewater treatment system 24 hours per day. Dickerson 

installed the wastewater treatment system to treat the FGD scrubber purge wastewater to meet its 

permit limits, which include limits for total suspended solids (TSS) and nitrogen. The Dickerson 

FGD wastewater treatment system contains the following treatment operations: 

 Physical/Chemical Separation; 

— Equalization, 

— pH adjustment (lime addition), 

— Organosulfide addition, 

— Ferric chloride addition, 

— Polymer addition, 

— Clarification; 

— Hydrochloric acid addition; and 

 Biological Reactors; 

— Influent equalization, 

— Cooling (heat extraction), 

— Carbon source addition, 

— Hypochloric acid addition, 

— SBR process, 

— Effluent equalization, and 

— Filtration. 

Figures 2-1 and 2-2, located at the end of this section, present process flow diagrams of 

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

episode. Figure 2-1 is a simplified diagram of the FGD wastewater treatment system, showing 

different portions of the system. Figure 2-2 is a diagram of the chemical precipitation and 

biological reactor portions of the treatment system. 

The secondary hydrocyclone overflow from the scrubbers is transferred to the purge tank 

and then sent to the equalization tank at the start of the wastewater treatment system. During the 

sampling episode, the FGD influent wastewater was found to contain between 0.3 and 1.1 

percent solids, had a pH of 6.5 to 7.5 S.U. and a temperature between 29 and 44 °C. The 

equalization tank also receives water from the filtrate sump (which includes filter press filtrate, 

backwash reject from the continuous backwash gravity filters, building trench drains, and tank 

overflow). 

2.2.1 Physical/Chemical Separation 

From the equalization tank, the wastewater enters reaction tank 1 in which lime slurry is 

added to increase the pH to 8.3 S.U. to precipitate the soluble metals as insoluble hydroxides and 

oxyhydroxides. The plant also adds organosulfide (i.e., TMT-15) to reaction tank 1 to form 

sulfide complexes which have very low solubility products. Wastewater then cascades by gravity 
2-4

into reaction tank 2 in which ferric chloride is added to form a dense flocculant, enhance the 

settling characteristics of the precipitate, and promote iron coprecipitation. 

The plant adds an anionic polymer as the wastewater flows from reaction tank 2 to the 

solids contact clarifier. The polymer is introduced at the inlet of the clarifier. The solids contact 

clarifier contains a sludge bed that facilitates removal of the solids in the wastewater. In the 

afternoon of day 3 of the sampling episode, the clarifier sludge bed overturned. The condition 

was identified by turbidity measurements and wastewater treatment operators added polymer to 

counteract the situation. At 1630 on August 25, the wastewater treatment operator stated that 

turbidity levels were still elevated, although the polymer addition had reduced the turbidity. The 

operator said that SP-2 day 1 and 2 samples should be unaffected, but day 3 and 4 samples would 

be affected. The sampling team monitored sample color and turbidity of the samples during the 

remainder of the sampling episode. 

As the clarifier overflow is transferred to the sequencing batch reactor (SBR) influent 

equalization tank, the plant injects hydrochloric acid into the wastewater to adjust the pH to 7 

prior to the biological treatment system. After the hydrochloric acid addition, the wastewater 

flows to the SBR influent equalization tank. The hydraulic residence time for the chemical 

precipitation portion of the FGD wastewater treatment system is approximately 16 hours, based 

on operating level conditions. 

The majority of the sludge from the clarifier is transferred to a sludge holding tank; 

however, the plant recycles approximately 50 to 60 gpm of clarifier sludge back to reaction tank 

1 to act as seed crystals for gypsum nucleation. The plant maintains a TSS concentration of 5 

percent solids in the outlet from reaction tank 1. The sludge in the sludge holding tank is pumped 

to a filter press for dewatering. The filter press filtrate is sent to the filtrate sump. The filter press 

cake is transferred to the waste management site in Virginia, where the FGD solids and off-spec 

gypsum are sent. Dickerson performs approximately 5 filter press operations per day. 

2.2.2 Biological Sequencing Batch Reactors 

Water from the clarifier as well as the SBR decant flush and backwash reject from the 

tertiary continuous backwash filters is transferred to the SBR influent equalization tank where it 

is then pumped through heat exchangers. After the heat exchangers have reduced the temperature 

of the water to approximately 95 degrees Fahrenheit, the wastewater is recycled back to the SBR 

influent equalization tank. Hypochloric acid (to reduce the pH of the water) and a carbon source 

(i.e., glycerin, to promote cell growth in the biological treatment process) are also added to the 

SBR influent equalization tank. The food to mass ratio in the SBR system ranges from 4:1 to 8:1 

depending on the desired mixed liquor volatile suspended solids concentration. Water is then 

batch transferred to two 178,705 gallon SBR tanks operating in parallel. 

Dickerson uses an SBR to biologically treat the wastewater to remove nitrogen by 

nitrification and denitrification. Currently, the SBR tanks are open to the atmosphere, but the 

plant has erected tarps to cover the tanks. Dickerson plans to construct a building that will 

enclose the SBR by the winter of 2010/2011. The purpose of the tarps/building is to reduce the 

heat loss that occurs during cold weather. 

Each batch of the SBR consists of the following five cycles: 
2-5

 Fill 

o Anoxic: Food is loaded into the basin and soluble BOD is absorbed and 

stored by the facultative biomass until air is received to metabolize the 

food. Good settling, facultative organisms predominate. 

o Aerated: Air is pumped in and mixed to initiate metabolism. During the 

initial stages of Aerated Fill, both nitrification and denitrification occur.

The ammonia is converted to nitrates within the highly aerated plume of the 

jet. The nitrates are converted to nitrogen gas in the low dissolved oxygen 

areas of the basin. The denitrifying organisms use the BOD as a food 

source and the oxygen off the nitrates converting the nitrates to nitrogen 

gas. A secondary denitrification phase can be inserted at any point during 

the aerated cycle (Aerated Fill & React cycles). During this step, the 

blowers are turned off and the jet pump continues to mix, providing anoxic 

mixing to drive denitrification. 

 React: No additional flow or food is added forcing the organisms to scour for any 

remaining BOD. Aeration continues until complete biodegradation is achieved. 

The cycle continues until the biomass enters its “famine” state at which time the 

residual dissolved oxygen levels begin to rise quickly. 

 Settle: No influent is introduced and no effluent is decanted allowing the biomass 

to settle in quiescent conditions. 

 Decant: An automatic valve is opened and the upper one-third of the basin is 

discharged. 

 Idle: While waiting to receive flow settled sludge is wasted. 

During the decant cycle, the water is transferred from the SBR to the SBR effluent 

equalization tank. The hydraulic residence time of the biological portion of the wastewater 

treatment system, including the equalization tanks, is approximately 16 hours. The hydraulic 

residence time of the SBR itself is a minimum of four hours. From the SBR effluent equalization 

tank, the wastewater is then pumped to continuous backwash gravity filters. Backwash reject 

returns to the SBR influent equalization tank for reprocessing. The filtered effluent is conveyed 

via gravity to the treated water storage tank. 

Water in the treated water storage tank is monitored for NPDES compliance prior to 

commingling with the main cooling water discharge. The commingled water then discharges 

through a canal that carries it approximately 1⁄4 mile downstream where it is discharged through 

Outfall 001 to the Potomac River. 

2.2.3 Sampling Points 

Figure 2-2 shows the sampling points for the Dickerson sampling episode; they are 

summarized below: 

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

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

sample was collected prior to any chemical addition or treatment system 

recirculation flow streams); 
2-6

 An in-process sample of the influent to the SBR, at the heat exchanger tank pump 

discharge sample tap (after HCl addition); and 

 A sample of the effluent from the SBR, downstream of the continuous backwash 

gravity filters and upstream of treated water storage tank. 
2-7 Figure 2-1. Simplified Diagram of the FGD Wastewater Treatment System, Dickerson Generating 
2-8 

Figure 2-2. Physical/Chemical Separation and Biological Reactor Portion of FGD Wastewater Treatment Sy

Generating Station 

FGD Scrubber Purge 

(from Purge Tank)

Lime

Polymer

Equalization 

Tank Reaction Tank 1 Reaction 

Tank 2

SP-1

SP-2

Indicates a Sampling Point

Ferric 

Chloride

Solids 

Contact Clarifier

Sludge 

Storage 

Tank

Filter Press

Sump

Solids to Waste 

Management Site

Wastewater Flow

Sludge Flow

Intermittent Wastewater Flow

Clarifier 

Sludge

Hydrochloric 

Acid

SP-3

Organosulfide

SBR Influent 

Equalization 

Tank

Cooling Water

Cooling Water 

Return

Carbon Source

Sequencing 

Batch Reactors 

(2)

SBR Effluent 

Equalization 

Tank

Decant Flush

Tertiary 

Continuous 

Backwash 

Gravity 

Filters (2)

Treated Water 

Storage Tank

Backwash Reject
3-1

3. SAMPLE COLLECTION

During the Dickerson 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. Figures 2-1 

and 2-2 of this report present flow diagrams 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 Influent to the SBR; 

 SP-3 Effluent from the SBR; 

 SP-4 Duplicate of Influent to the SBR (SP-2); 

 SP-5 Duplicate of Effluent from the SBR (SP-3); 

 SP-6 Influent to FGD Wastewater Treatment System (SP-1) Field Blank; 

 SP-7 Influent to the SBR (SP-2) Field Blank; and 

 SP-8 Effluent from the SBR (SP-3) Field Blank. 

For all the sampling points, EPA collected split samples with Dickerson’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 Dickerson’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 
3-2

“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 

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 drain of the pump that transfers the FGD wastewater from the purge tank to the 

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

collected as a grab sample. Due to the relatively high concentration of suspended solids, the FGD 

purge was not amenable to collecting representative split samples using composite sampling 

techniques. The sampling point was located inside the FGD gypsum transfer building. Because 

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

collection. 

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

treatment system (SP-1), the sampling team collected field blanks (SP-6) for total mercury, total 

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

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

system. 

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

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

wastewater pump drain. 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 sample 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). 

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

3.1: 

 Total and dissolved mercury; 

 Total metals by 200.8; and 

 Total metals by 200.7. 

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 
3-3

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 Dickerson’s representatives. 

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 80 to 90 minutes. Approximately 1- 

1.5 liters2

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

samples. 

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

Section 3.1: 

 Dissolved metals by 200.8; 

 Dissolved metals by 200.7; and 

 Dissolved hexavalent chromium; 

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

3.1.2 Influent to the SBR 

The influent to the SBR (SP-2) was collected at the sample tap located at the heat 

exchanger tank pump discharge to the SBR influent equalization tank. Dickerson installed a 

three-way splitter on the sample tap, which had three separate taps to collect samples from the 

 

2

 On days 1, 2, and 3, the filter/tubing was purged for 1 liter. On day 4, the filter/tubing was purged for 1.5 liters. 

There was no need to change the filter on any of the days. 
3-4

sampling point. The sample tap was located outside (see Figure 2-2 for the sampling location for 

SP-2). The sampling team set up a tent to cover the samplers/samples from rain and/or wind. 

ERG collected the influent from the SBR composite samples using two automatic 

compositors which were programmed to collect individual sample volumes into two 20-liter 

containers. The compositors were programmed to collect 830 mL every hour during the 24-hour 

composite period. Following the composite period, ERG pumped off the specific sample 

volumes into the individual sample containers. 

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

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

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

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

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

grab sample for cyanide during each compositing period. 

On day 1 only, ERG collected field blank samples (SP-7) for hexavalent chromium, total 

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

description of the field blank sample collection procedures at the influent to the SBR. 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

each individual sample aliquot. 

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

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

to minimize contamination. Figure C-3, in Appendix C, is a picture of the composite sampling 

set-up at the influent to the SBR. 

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 influent to the SBR. 

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 
3-5

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 Dickerson’s representatives; 

therefore, duplicate samples were collected. ERG collected another set of total and dissolved 

mercury samples every six hours thereafter over the 24-hour period. The plastic shroud was 

replaced for each set of mercury grab samples. After collecting each set of mercury grabs, ERG 

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

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

SBR. 

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

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

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

split samples with Dickerson’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 the sampling episode at the influent to the SBR. 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. 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 Dickerson’s representative. 

On Day 1 only, prior to collecting any samples of the influent to the SBR, the samplers 

collected a field blank sample (SP-7) for dissolved and total metals. See Section 5.2.3 for a 

description of the dissolved metals field blank sample collection at the influent to the SBR. 
3-6

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 influent to 

the SBR. After the tubing and filter were purged with 2 liters of sample, samplers collected the 

following samples using a “cleanbox,” as described in Section 3.1: 

 Dissolved metals by 200.8; 

 Dissolved metals by 200.7; and 

 Dissolved hexavalent chromium. 

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

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

purged with 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. Once the tubing was purged 

with 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 influent to the SBR (SP-2) on Day 4 of 

the sampling episode. In addition, for all analytes, ERG collected a duplicate sample of the 

influent from bioreactor system (SP-4) on Day 3 of the sampling episode. 

3.1.3 Effluent from the SBR 

The effluent from the SBR (SP-3) was collected downstream of the continuous backwash 

gravity filters and upstream of the treated water storage tank. Dickerson 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 outside (see Figure 2-2 for the sampling location for SP-3). The 

sampling team set up a tent to cover the samplers/samples from rain and/or wind. 

ERG collected the effluent from the SBR composite samples using two automatic 

compositors which were programmed to collect individual sample volumes into two 20-liter 

containers. The compositors were programmed to collect 830 mL every hour during the 24-hour 

composite period. Following the composite period, ERG pumped off the specific sample 

volumes into the individual sample containers. 

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

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

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

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

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

grab sample for cyanide during each compositing period. 
3-7

On day 1 only, ERG collected field blank samples (SP-8) for hexavalent chromium, total 

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

description of the field blank sample collection procedures at the effluent from the SBR. 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

individual sample aliquot. 

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

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

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

set-up at the effluent from the SBR. 

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

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

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

procedures at the effluent from the SBR. 

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 Dickerson’s representatives; 

therefore, duplicate samples were collected. ERG collected another set of total and dissolved 

mercury samples every six hours thereafter over the 24-hour period. The plastic shroud was 

replaced for each set of mercury grab samples. After collecting each set of mercury grabs, ERG 

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

meter, and a thermometer. Table 3-3 presents the field measurement data for the effluent from 

the SBR. 

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

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

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

split samples with Dickerson’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 
3-8

oxidants were detected during this sampling episode at the effluent from the SBR. 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. 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 Dickerson’s representatives. 

On Day 1 only, prior to collecting any samples of the effluent from the SBR, the samplers 

collected a field blank sample (SP-8) for dissolved and total metals. See Section 5.2.3 for a 

description of the dissolved metals field blank sample collection at the effluent from the SBR. 

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

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

the SBR. After the tubing and filter were purged with 1.5-2 liters of sample, samplers collected 

the following samples using a “cleanbox,” as described in Section 3.1: 

 Dissolved metals by 200.8; 

 Dissolved metals by 200.7; and 

 Dissolved hexavalent chromium. 

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

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

purged with 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. 
3-9

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 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 the SBR (SP-3) on Day 

3 of the sampling episode. In addition, for all analytes, ERG collected a duplicate sample of the 

effluent from the SBR (SP-5) on Day 2 of the sampling episode. 

3.2 List of Analytes and Sample Preservation

Samples collected at Dickerson 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 

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

concentrations. 

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

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

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

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

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

 

3

 In this report, EPA uses the terms “total metals” and “total recoverable metals” interchangeably. 
3-10

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, Dickerson 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: 

 Plant Shutdown. Between 0134 and 0326 on Tuesday morning, which is prior to 

the end of the day 1 24-hour sample compositing period, Dickerson shut down all 

three generating units due to lack of electricity demand. The station continued to 

operate the FGD wastewater treatment system at reduced flow rates and EPA 

continued to collect samples as planned through the end of the sampling episode. 

Additionally, the FGD system was shut down, but the plant occasionally blew 

down from the scrubber and operated the dewatering equipment to allow EPA to 

collect the influent samples. The sampling team monitored flow rates during the 

remainder of the sampling episode. The generating station and FGD scrubber did 

not resume operation until after the end of the sampling episode. 

 Clarifier Bed Turnover. In the afternoon of day 3 of the sampling episode, the 

clarifier sludge bed overturned. The condition was identified by turbidity 

measurements and wastewater treatment operators added polymer to counteract 

the situation. At 1630 on August 25, the wastewater treatment operator stated that 

turbidity levels were still elevated, although the polymer addition had reduced the 

turbidity. The operator said that SP-2 day 1 and 2 samples should be unaffected, 

but day 3 and 4 samples would be affected.
3-11

 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. 

 Total mercury grab sample at SP-1 (Day 3): On day 3 of sample collection at 

the influent to FGD wastewater treatment system (SP-1), the sampling team 

dropped the total mercury volume 2 grab sample bottle inside the clean box. A 

portion of the contents spilled into the clean box. Since the majority of the sample 

volume remained in the sample bottle, additional sample volume was not 

collected. 

 Total mercury field blank at SP-2 (Day 2): On day 2 of sample collection at the 

influent to the SBR (SP-2), the total mercury field blank volume 1 bottle was 

taken out from under the plastic bag shrouding the sampling tap prior to closing 

the inner bag; however, the lid to the bottle was closed prior to the bottle leaving 

the plastic bag shroud. 

 Classicals compositor set up at SP-3 (Day 1): On day 1 of sample collection at 

the effluent to the SBR (SP-3), the valve for the classical compositor was 

inadvertently adjusted while collecting total mercury grab 1. The sampling team 

readjusted the valve to its approximate position. The sampling team noted that 

the classicals compositor collected 20 liters of sample during the day. 

 Total cyanide QC sample at SP-3 (Day 3): On day 3 of sample collection at the 

effluent to the SBR (SP-3), the sampling team collected the field test jar volume 

prior to collecting the total cyanide QC sample. The “clean hands” sampler 

changed her gloves prior to collecting the total cyanide QC sample. 

 Analytical method for zinc analyses: ERG had planned to analyze zinc using 

EPA Method 200.8 with collision cell; however, after discussions with the 

laboratory, EPA decided to analyzed zinc using EPA Method 200.7. 
3-12

Table 3-1. Sample Collection Information, Dickerson

Sampling 

Point 

Number Sampling Point Description 

Type of 

Sample 

Sample 

Collection Date 

Sample Collection 

Time 

Influent to FGD Wastewater Treatment 

System – Day 1 

Grab 08/23/10 1012a and 1146b

Influent to FGD Wastewater Treatment 

System – Day 2 

Grab 08/24/10 1126a and 1305 b

Influent to FGD Wastewater Treatment 

System – Day 3 

Grab 08/25/10 1135a and 1311b

SP-1 

Influent to FGD Wastewater Treatment 

System – Day 4 

Grab 08/26/10 1111a and 1300b

Composite 08/23/10 

08/24/10 

0901c 

1039d

Influent to the SBR – Day 1 

Grab 08/23/10 

08/24/10 

0913e

, 1514f , and 2113 g 

0314 h 

Composite 08/24/10 

08/25/10 

0900c 

1031d 

Influent to the SBR – Day 2 

Grab 08/24/10 

08/25/10 

0911e

, 1518f , and 2113 g 

0312 h 

Composite 08/25/10 

08/26/10 

0900c 

1014d 

Influent to the SBR – Day 3 

Grab 08/25/10 

08/26/10 

0912e

, 1517f , and 2114 g 

0314 h 

Composite 08/26/10 

08/27/10 

0900c 

0825d 

SP-2 

Influent to the SBR – Day 4 

Grab 08/26/10 

08/27/10 

0911e

, 1516f , and 2107 g 

0310 h 

Composite 08/23/10 

08/24/10 

0731c 

0955d 

Effluent from the SBR – Day 1 

Grab 08/23/10 

08/24/10 

0745e

, 1345f , and 1946 g 

0152 h 

Composite 08/24/10 

08/25/10 

0730c 

0945d 

Effluent from the SBR – Day 2 

Grab 08/24/10 

08/25/10 

0743e

, 1346f , and 1948 g 

0145h 

Composite 08/25/10 

08/26/10 

0730c 

0939d 

Effluent from the SBR – Day 3 

Grab 08/25/10 

08/26/10 

0744e

, 1345f , and 1944 g 

0143h 

Composite 08/26/10 

08/27/10 

0731c 

0657d 

SP-3 

Effluent from the SBR – Day 4 

Grab 08/26/10 

08/27/10 

0743e

, 1345f , and 1942 g 

0142h 
3-13

Table 3-1. Sample Collection Information, Dickerson

Sampling 

Point 

Number Sampling Point Description 

Type of 

Sample 

Sample 

Collection Date 

Sample Collection 

Time 

Composite 08/25/10 

08/26/10 

0900c 

1014d 

SP-4 Duplicate of Influent to the SBR – Day 3 

Grab 08/25/10 

08/26/10 

0914e

, 1518f , and 2116 g 

0315 h 

Composite 08/24/10 

08/25/10 

0730c 

0945d 

SP-5 Duplicate of Effluent from the SBR – 

Day 2 

Grab 08/24/10 

08/25/10 

0745e

, 1348f , and 1950 g 

0146 h 

SP-6 Influent to FGD Wastewater Treatment 

System Field Blank 

Grab 08/23/10 0958i and 1139j

Composite 08/23/10 

08/24/10 

0823k

1028l

Influent to the SBR Field Blank – Day 1 

Grab 08/23/10 0906m

Influent to the SBR Field Blank – Day 2 Grab 08/24/10 0907m

Influent to the SBR Field Blank – Day 3 Grab 08/25/10 0907m

SP-7 

Influent to the SBR Field Blank – Day 4 Grab 08/26/10 0906m

Composite 08/23/10 

08/24/10 

0650k

0942l

Effluent from the SBR Field Blank – 

Day 1 

Grab 08/23/10 0741m

Effluent from the SBR Field Blank – 

Day 2 

Grab 08/24/10 0739m

Effluent from the SBR Field Blank – 

Day 3 

Grab 08/25/10 0739m

SP-8 

Effluent from the SBR Field Blank – 

Day 4 

Grab 08/26/10 0738m

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. 

d

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

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

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

f

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

g

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

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

i

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

blank samples. 

j

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

field blank samples. 

k

 Filled 20L field blank carboy 

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

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

m Start time for the collection of total mercury field blank samples. 
3-14 

Table 3-2. Sample Collection at Dickerson Steam Station

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 FGD Wastewater Treatment 

System 

4 4 4 4 4 4 4 4 

SP-2 Influent to the SBR 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4SP-3 Effluent from the SBR 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4SP-4 Duplicate of Influent to the SBR 1 1 1 1 1 1 1 1 SP-5 Duplicate of Effluent from the SBR 1 1 1 1 1 1 1 1 SP-6 Field Blank for Influent to FGD Wastewater 

Treatment System 

1 1 1 1 1 1 

SP-7 Field Blank for Influent to the SBR 1 1 1 1 4 1 SP-8 Field Blank for Effluent from the SBR 1 1 1 1 4 1 Total Number of Samples 17+2QC 17+2QC 17+2QC 17+2QC 23+2QC 14+2QC 17+2QC 14+2QC 1
3-15 

Table 3-3. Field Measurements, Dickerson

Temperature (°C) pH 

Sampling 

Point 

Number 

Sampling Point 

Description Date Time Thermometer Probe Metera Strips

Waste 

Stream Flow 

Rate (GPM) N

Influent to FGD Wastewater Treatment System – Day 1

8/23/10 1024 44 39 6.61 7 82.1b No detected sulfides or 

grab. 

Influent to FGD Wastewater Treatment System – Day 2 

8/24/10 1138 33 30 7 7.5 66.5b No detected sulfides or 

grab. 

Influent to FGD Wastewater Treatment System – Day 3 

8/25/10 1149 31 29.2 7.18 7 49.6b Samples collected were 

sulfides or oxidants in t

SP-1 

Influent to FGD Wastewater Treatment System – Day 4 

8/26/10 1123 33 30.1 7.01 7 60.2b No detected sulfides or 

grab. 

8/23/10 0915 38 36.1 7.03 7.5 112.18/23/10 1518 39 34.9 7.13 7 111.88/23/10 2120 38 35.6 7.12 7 109.4 

Influent to SBR – Day 1

8/24/10 0320 36 33.9 7.09 7 99.9 

No detected sulfides or grab.

8/24/10 0914 36 33 6.98 7 96.6 8/24/10 1520 36 32.5 6.92 7 96.0 8/24/10 2118 34 31.3 6.95 6.5 87.1 

Influent to the SBR – Day 2 

8/25/10 0320 32 29.3 6.92 6.5 81.6 

No detected sulfides or grab.

8/25/10 0917 31 28.5 6.9 7 81.1 8/25/10 1521 31 28.5 6.9 7 83.9 8/25/10 2132 31 28.7 6.87 6.5 78.6 

SP-2 

Influent to the SBR – Day 3 

8/26/10 0319 30 28.7 6.88 7.0 78.5 

Clarifier bed overturneby turbidity measuremewere grey and Grab 3 hfrom previous sampling sulfides or oxidants in t
3-16 

Table 3-3. Field Measurements, Dickerson

Temperature (°C) pH 

Sampling 

Point 

Number 

Sampling Point 

Description Date Time Thermometer Probe Metera Strips

Waste 

Stream Flow 

Rate (GPM) N

8/26/10 0913 30.5 29 6.84 7 77.8 8/26/10 1518 32 30.3 6.63 7 83.4 8/26/10 2113 30 28.7 6.70 6.5 84.4 

SP-2 Influent to the SBR – 

Day 4 

8/27/10 0320 30 27.6 6.77 6.5 79.2 

The samples collected wgrey/brownish. No detin total cyanide grab.

8/23/10 0748 31 29 7.12 7 97.38/23/10 1349 32 29.4 7.06 7 95.38/23/10 1950 31 29.5 7.07 7 95.3

Effluent from the SBR – Day 1

8/24/10 0158 31 29 7.11 7 88.3

The samples collected wsulfides or oxidants in t

8/24/10 0748 30.5 27.9 7.01 7 86.38/24/10 1351 30 28.5 7.04 7.5 88.18/24/10 2005 30 28.3 7.01 7 88.1

Effluent from the SBR – Day 2 

8/25/10 0154 30 27.3 7.07 7.5 86.7

The samples collected wsulfides or oxidants in t

8/25/10 0746 30 27.8 7.01 7 86.38/25/10 1347 30 28.3 7.01 7 66.68/25/10 1949 30.5 29.3 6.93 7.5 66.6

Effluent from the SBR – Day 3 

8/26/10 0148 30 27.9 6.95 7.5 66.6

No detected sulfides or grab.

8/26/10 0745 30 27.5 6.91 7.5 66.88/26/10 1348 31 29.3 6.92 7.5 67.88/26/10 1949 31 29.9 6.95 7 61.7

SP-3 

Effluent from the SBR – Day 4 

8/27/10 0149 30 26.8 6.94 6.5 61.7

Water color was light ydetected sulfides or oxigrab.

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 Based on average flow rate, in gpm, for the entire day of sampling. The flow rate does not represent the flow rate at the time of samp
3-17

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

Sample Number Sample Point Sample Description 

71841 SP-1, Day 1 Influent to FGD Wastewater Treatment System - Day 1 

71842 SP-1, Day 2 Influent to FGD Wastewater Treatment System - Day 2 

71843 SP-1, Day 3 Influent to FGD Wastewater Treatment System - Day 3 

71844 SP-1, Day 4 Influent to FGD Wastewater Treatment System - Day 4 

71845 SP-2, Day 1 Influent to SBR System - Day 1 

71846 SP-2, Day 2 Influent to SBR System - Day 2 

71847 SP-2, Day 3 Influent to SBR System - Day 3 

71848 SP-2, Day 4 Influent to SBR System - Day 4 

71849 SP-3, Day 1 Effluent from SBR System - Day 1 

71850 SP-3, Day 2 Effluent from SBR System - Day 2 

71851 SP-3, Day 3 Effluent from SBR System - Day 3 

71852 SP-3, Day 4 Effluent from SBR System - Day 4 

71853 SP-4, Day 3 Duplicate of Influent to SBR System - Day 3 

71854 SP-5, Day 2 Duplicate of Effluent from SBR System - Day 2 

71855 SP-6, Day 1 Influent to FGD Wastewater Treatment System Field Blank - Day 1 

71856 SP-7, Day 1 Influent to SBR System Field Blank - Day 1 

71857 SP-7, Day 2 Influent to SBR System Field Blank - Day 2 

71858 SP-7, Day 3 Influent to SBR System Field Blank - Day 3 

71859 SP-7, Day 4 Influent to SBR System Field Blank - Day 4 

71860 SP-8, Day 1 Effluent from SBR System Field Blank - Day 1 

71861 SP-8, Day 2 Effluent from SBR System Field Blank - Day 2 

71862 SP-8, Day 3 Effluent from SBR System Field Blank - Day 3 

71863 SP-8, Day 4 Effluent from SBR System Field Blank - Day 4 
3-18

Table 3-5. Analytical Methods, Dickerson

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, nickel, selenium, 

silver, thallium, and vanadium 

EPA 200.8 with collision cell1

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

manganese, molybdenum, sodium, tin, titanium, and zinc 

EPA 200.7 

1

 EPA used an SOP developed specifically for analyzing FGD wastewater (see Appendix D).
3-19

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

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.
3-20 

Table 3-7. Sample Preservation Summary, Dickerson

Sampling Point 

Number Analysis Date 

Chemical 

Added Initial pH Final pH 

Amount 

Added 

(drops) 

71841 Group II Volume 1 8/23/10 H2SO4 7 2 100 

71841 Group II Volume 2 8/23/10 H2SO4 7 2 100 

(NH4)2SO4

Buffer 

71841 Hexavalent Chromium 7 7.9 100 8/23/10

NH4OH 7.9 9.5 54 

(NH4)2SO4

Buffer 

71855 Hexavalent Chromium – 5.5 8.5 100 

Field Blank 

8/23/10

NH4OH 8.5 9.5 29 

71841 Total Cyanide 8/23/10 NaOH 7 10 30 

71845 Total Cyanide 8/23/10 NaOH 7 10 15 

71849 Total Cyanide 8/23/10 NaOH 7 10 20 

71842 Group II Volume 1 8/24/10 H2SO4 7 2 100 

71842 Group II Volume 2 8/24/10 H2SO4 7 2 100 

71845 Group II Volume 1 8/24/10 H2SO4 7 1.5 100 

71845 Group II Volume 2 8/24/10 H2SO4 7 1.5 100 

71849 Group II Volume 1 8/24/10 H2SO4 7 1 100 

71849 Group II Volume 2 8/24/10 H2SO4 7 1 100 

(NH4)2SO4

Buffer 

71842 Hexavalent Chromium 8/24/10 7 8.1 100 

NH4OH 8.1 9.5 55 

(NH4)2SO4

Buffer 

71845 Hexavalent Chromium 8/24/10 7.5 8.3 100 

NH4OH 8.3 9.5 30 

(NH4)2SO4

Buffer 

71849 Hexavalent Chromium 7.5 8.3 100 8/24/10

NH4OH 8.3 9.5 23 

(NH4)2SO4

Buffer 

71856 Hexavalent Chromium – 6.5 8.5 100 

Field Blank 

8/24/10

NH4OH 8.5 9.5 40 

(NH4)2SO4

Buffer 

71860 Hexavalent Chromium – 6 8.5 100 

Field Blank 8/24/10

NH4OH 8.5 9.5 40 

71842 Total Cyanide 8/24/10 NaOH 7 >10 125 

71846 Total Cyanide 8/24/10 NaOH 7 >10 20 

71850 Total Cyanide 8/24/10 NaOH 7 >10 20 

71854 Total Cyanide 8/24/10 NaOH 7 >10 20 

71843 Group II Volume 1 8/25/10 H2SO4 7 2 100 

71843 Group II Volume 2 8/25/10 H2SO4 7 2 100 

71846 Group II Volume 1 8/25/10 H2SO4 7 2 100 
3-21 

Table 3-7. Sample Preservation Summary, Dickerson

Sampling Point 

Number Analysis Date 

Chemical 

Added Initial pH Final pH 

Amount 

Added 

(drops) 

71846 Group II Volume 2 8/25/10 H2SO4 7 2 100 

71850 Group II Volume 1 8/25/10 H2SO4 7 2 100 

71850 Group II Volume 2 8/25/10 H2SO4 7 2 100 

71854 Group II Volume 1 8/25/10 H2SO4 7 2 100 

71854 Group II Volume 2 8/25/10 H2SO4 7 2 100 

(NH4)2SO4

Buffer 

71843 Hexavalent Chromium 8/25/10 7 8.5 100 

NH4OH 8.5 9.5 35 

(NH4)2SO4

Buffer 

71846 Hexavalent Chromium 8/25/10 7 8.1 100 

NH4OH 8.1 9.5 35 

(NH4)2SO4

Buffer 

71850 Hexavalent Chromium 8/25/10 7 8.1 100 

NH4OH 8.1 9.5 40 

(NH4)2SO4

Buffer 

71854 Hexavalent Chromium 8/25/10 7 8.1 100 

NH4OH 8.1 9.5 35 

71843 Total Cyanide 8/25/10 NaOH 7 10 150 

71847 Total Cyanide 8/25/10 NaOH 6.5 10 20 

71851 Total Cyanide 8/25/10 NaOH 7.5 10 20 

71851 Total Cyanide - QC 8/25/10 NaOH 7.5 10 20 

71853 Total Cyanide 8/25/10 NaOH 6.5 10 20 

71844 Group II Volume 1 8/26/10 H2SO4 7 2 100 

71844 Group II Volume 2 8/26/10 H2SO4 7 2 100 

71847 Group II Volume 1 8/26/10 H2SO4 7 1 100 

71847 Group II Volume 2 8/26/10 H2SO4 7 1 100 

71851 Group II Volume 1 8/26/10 H2SO4 7 2 100 

71851 Group II Volume 2 8/26/10 H2SO4 7 2 100 

71851 Group II Volume 1 - QC 8/26/10 H2SO4 7 2 100 

71851 Group II Volume 2 - QC 8/26/10 H2SO4 7 2 100 

71853 Group II Volume 1 8/26/10 H2SO4 7 1 100 

71853 Group II Volume 2 8/26/10 H2SO4 7 1 100 

(NH4)2SO4

Buffer 

71844 Hexavalent Chromium 8/26/10 7 8.1 100 

NH4OH 8.1 9.5 45 

(NH4)2SO4

Buffer 

71847 Hexavalent Chromium 8/26/10 7 8.3 100 

NH4OH 8.3 9.5 32 
3-22 

Table 3-7. Sample Preservation Summary, Dickerson

Sampling Point 

Number Analysis Date 

Chemical 

Added Initial pH Final pH 

Amount 

Added 

(drops) 

(NH4)2SO4

Buffer 

71851 Hexavalent Chromium 8/26/10 7 8.3 100 

NH4OH 8.3 9.5 20 

(NH4)2SO4

Buffer 

71853 Hexavalent Chromium 8/26/10 7 8.3 100 

NH4OH 8.3 9.5 30 

71844 Total Cyanide 8/26/10 NaOH 7 10 200 

71848 Total Cyanide 8/26/10 NaOH 6.5 >10 20 

71848 Total Cyanide - QC 8/26/10 NaOH 6.5 >10 20 

71852 Total Cyanide 8/26/10 NaOH 7.5 >10 20 

71848 Group II Volume 1 8/27/10 H2SO4 7 2 100 

71848 Group II Volume 2 8/27/10 H2SO4 7 2 120 

71848 Group II Volume 1 - QC 8/27/10 H2SO4 7 2 100 

71848 Group II Volume 2 - QC 8/27/10 H2SO4 7 2 100 

71852 Group II Volume 1 8/27/10 H2SO4 7 2 100 

71852 Group II Volume 2 8/27/10 H2SO4 7 2 100 

(NH4)2SO4

Buffer 

71848 Hexavalent Chromium 8/27/10 7 8.3 100 

NH4OH 8.3 9.5 25 

(NH4)2SO4

Buffer 

71852 Hexavalent Chromium 8/27/10 7 8.3 100 

NH4OH 8.3 9.5 22 
3-23 

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

Unit ID Boiler Type 

Capacity 

(MW) 

Electricity Production 

(MW) 

(or Percent Capacity %)a 

SCR 

(No, On, Off) 

Particulate Control System 

(HS/CS ESP, or BH) 

1 Coal 191 20% Off ESP/BH 

2 Coal 191 20% Off ESP/BH 

3 Coal 191 20% Off ESP/BH 

a

 The percent capacity was measured on a daily basis from midnight on August 24 to midnight on August 27. 

ESP/BH – Electrostatic precipitator and baghouse. 
3-24 

Table 3-9. FGD Scrubber System Operating Characteristics, Dickerson 

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 Re

Percen

1, 2, 3 Yes Tray Yes Limestone None Industrial WWTP – River water 96.2

Note: One FGD system services all three generating units.
3-25

Table 3-10. Coal Usage during Sample Collection, Dickerson 

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 

(%) 

1 Fed 2 a

/Brooks 

Run 900b PA 

WV 

5.1 

1.7 

0.07 

0.12 

2 Fed 2 a /Brooks 

Run 825 PA WV 

5.1 

1.7 

0.07 

0.12 1 

3 Fed 2 a /Brooks 

Run 704 PA 

WV 

5.1 

1.7 

0.07 

0.12 

1 Fed 2 a /Storage 655 PA 

WV 

4.9 

1.7 

0.07 

0.102 

2 Fed 2 a 833 PA 4.9 0.07 2 

3 Fed 2 a 715 PA 4.9 0.07 

1 NAc NAc NAc NAc NAc

2 NAc NAc NAc NAc NAc 3 

3 NAc NAc

 NAc NAc NAc

1 NAc NAc NAc NAc NAc

2 NAc NAc NAc NAc NAc 4 

3 NAc NAc

 NAc NAc NAc

a

 Fed 2 coal is sourced from the Federal Mining Complex in Northern West Virginia from a single mine, Federal 2. 

b

 Estimated value. 

c

 All three generating units were shut down on days 3 and 4 due to low electricity demand. 

 

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

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 

1 1 1, 2, 3 896 10.3 hrs 19-21% Note 1 85% 

2 1 1, 2, 3 696 2 hrs 19-21% Note 1 85% 

3 1 1, 2, 3 880 2.3 hrs 18.9-19.2% Note 1 85% 

4 1 1, 2, 3 884 2.6 hrs 18.9-19.0% Note 1 85% 

Note 1: Once the bleed stream from the absorber starts, it may take up to 30-minutes for gypsum slurry to flow to 

the slurry tank. At that point it takes up to 1-minute to dewater depending on the slurry density.
3-26 

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

Chemical Usage 

Day of Sampling 

Scrubber Purge 

Flow Rate 

(gpd) 

Lime 

(tons/day) 

Ferric Chloride 

(liters/day) 

Organosulfide 

(liters/day)a 

Polymer 

(liters/day) 

1 118,217 7.3 (8.70 S.U.) 115 (47 ppm) NA 19.5 (20 ppm) 2 95,775 15.5 (8.70 S.U.) 110 (47 ppm) NA 19.3 (20 ppm) 3 71,394 15.1 (8.70 S.U.) 108 (47 ppm) NA 18 (20 ppm) 4 86,689 15.1 (8.70 S.U.) 107 (47 ppm) NA 17.5 (20 ppm) 

a Dickerson was not adding organosulfide to the wastewater treatment system during the sampling episode. 

Note: Values in parentheses are the set points for the system.
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 influent to and effluent from the SBR 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 heated bromine monochloride digestion (i.e., sealed bottles 

in oven at 50 degrees C for six hours) 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 Dickerson, 

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. 

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. Tables 4-2 and 4-3 

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

the influent to the SBR (SP-2) and the effluent from the SBR (SP-3), respectively. 

Tables 4-1 through 4-3 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 sample-specific 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 (Influent to the SBR), a duplicate sample was collected on Day 3 of the 

sampling episode. The Day 3 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). For Table 4-3 (Effluent 

from the SBR), a duplicate sample was collected on Day 2 of the sampling episode. The Day 2 

results presented in Table 4-3 represent the average of the original and the duplicate sample 

results. Table 5-3 presents the analytical results for the original and duplicate results and the 

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

the FGD wastewater treatment system (SP-1), the influent to the SBR (SP-2), and the effluent 

from the SBR (SP-3). Table 4-5 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), the influent to the SBR (SP-2), and the effluent from the SBR (SP-3). The results 

presented in this report are not paired results, meaning that the sample collection across the 
4-3 

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

through the system. 

Appendix Tables A-1 through A-14 present all the analytical results from the influent to 

the FGD wastewater treatment system (SP-1), the influent to the SBR (SP-2), the effluent from 

the SBR (SP-3), the duplicate of the influent to the SBR (SP-4), and the duplicate of the effluent 

from the SBR (SP-5) sample analyses, including J-values. 
4-4 

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

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

value. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. ** - The accuracy of the Day 1 total dissolved solid result seems questionable based on the results from the other sampling days. If the Day 1 total dis

included in the calculated average, the 4-day average would be 52,000 mg/L. B – Analyte was found in the blank and sample. C – pH upon receipt was less than 10 S.U. D – Laboratory duplicate RPD greater than method-specified criteria. L – LFB or LCS percent recovery not within method-specified criteria, but is within laboratory-specified criteria. 

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

Influent to FGD Wastewater Treatment System 

Analyte Units Method Day 1 Day 2 Day 3 D

Classicals Ammonia mg/L 350.1 5.90 5.40 4.00 4.9Nitrate Nitrite as N mg/L 353.2 67.0 67.0 47.0 62.Nitrogen, Total Kjeldahl mg/L 351.2 130 L 23.0 B 12.0 B 21.Biochemical Oxygen Demand mg/L 5210B NQ (2.50) 3.70 6.30 8.0Chemical Oxygen Demand mg/L 410.4 110 150 110 15Chloride mg/L 300.0 9,200 8,400 5,700 7,40Sulfate mg/L 300.0 1,800 1,800 1,700 1,80Cyanide, Total mg/L 4500 CN E 1.20 C 1.10 B 0.740 0.76Total Dissolved Solids mg/L 2540C 170,000** B 15,000 12,000 11,0Total Suspended Solids mg/L 2540D 3,900 11,000 3,900 3,70Phosphorus, Total mg/L 365.1 3.70 NQ (0.0500) 3.20 4.3Total Metals Aluminum ug/L 200.7 130,000 110,000 91,000 110,0Antimony ug/L 200.8 23.0 18.0 15.0 19.Arsenic ug/L 200.8 280 220 190 23Barium ug/L 200.7 700 720 590 79Beryllium ug/L 200.7 15.0 12.0 10.0 13.Boron ug/L 200.7 220,000 B 200,000 B 150,000 B 200,0Cadmium ug/L 200.8 31.0 27.0 21.0 27.Calcium ug/L 200.7 2,900,000 2,700,000 2,600,000 2,600Chromium ug/L 200.8 690 ^ 570 ^ 450 ^ 57Cobalt ug/L 200.7 130 120 99.0 12Copper ug/L 200.8 660 530 440 54Iron ug/L 200.7 180,000 160,000 130,000 160,0
4-5 

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

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

value. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. ** - The accuracy of the Day 1 total dissolved solid result seems questionable based on the results from the other sampling days. If the Day 1 total dis

included in the calculated average, the 4-day average would be 52,000 mg/L. B – Analyte was found in the blank and sample. C – pH upon receipt was less than 10 S.U. D – Laboratory duplicate RPD greater than method-specified criteria. L – LFB or LCS percent recovery not within method-specified criteria, but is within laboratory-specified criteria. 

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

Influent to FGD Wastewater Treatment System 

Analyte Units Method Day 1 Day 2 Day 3 D

Lead ug/L 200.8 220 170 140 18Magnesium ug/L 200.7 1,700,000 1,600,000 1,200,000 1,600Manganese ug/L 200.7 11,000 9,800 7,800 9,90Mercury ng/L 1631E 8,550 4,830 4,030 5,63Molybdenum ug/L 200.7 520 440 360 44Nickel ug/L 200.8 660 580 450 57Selenium ug/L 200.8 1,500 1,200 920 1,20Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2Sodium ug/L 200.7 200,000 190,000 160,000 190,0Thallium ug/L 200.8 NQ (2.00) NQ (2.00) 2.90 NQ (2Tin ug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (2Titanium ug/L 200.7 6,200 5,400 4,500 5,60Vanadium ug/L 200.8 580 470 390 49Zinc ug/L 200.7 2,500 2,000 1,500 2,00Dissolved Metals Aluminum ug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (2Antimony ug/L 200.8 3.70 3.80 2.80 3.5Arsenic ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4Barium ug/L 200.7 250 210 130 14Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2Boron ug/L 200.7 210,000 B 190,000 B 150,000 B 200,0Cadmium ug/L 200.8 28.0 24.0 17.0 22.Calcium ug/L 200.7 2,300,000 2,100,000 1,600,000 2,100Chromium ug/L 200.8 ND (8.00) ^ ND (8.00) ^ ND (8.00) ^ ND (8Chromium (VI) ug/L 218.6 ND (10.0) ND (10.0) ND (10.0) ND (1
4-6 

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

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

value. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. ** - The accuracy of the Day 1 total dissolved solid result seems questionable based on the results from the other sampling days. If the Day 1 total dis

included in the calculated average, the 4-day average would be 52,000 mg/L. B – Analyte was found in the blank and sample. C – pH upon receipt was less than 10 S.U. D – Laboratory duplicate RPD greater than method-specified criteria. L – LFB or LCS percent recovery not within method-specified criteria, but is within laboratory-specified criteria. 

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

Influent to FGD Wastewater Treatment System 

Analyte Units Method Day 1 Day 2 Day 3 D

Cobalt ug/L 200.7 81.0 77.0 58.0 71.Copper ug/L 200.8 26.0 12.0 8.30 9.2Iron ug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (2Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2Magnesium ug/L 200.7 1,600,000 1,500,000 1,200,000 1,500Manganese ug/L 200.7 11,000 10,000 8,100 10,0Mercury ng/L 1631E 177 49.7 193 24.Molybdenum ug/L 200.7 250 210 180 22Nickel ug/L 200.8 460 420 310 38Selenium ug/L 200.8 150 210 150 18Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2Sodium ug/L 200.7 210,000 200,000 160,000 200,0Thallium ug/L 200.8 2.40 NQ (2.00) NQ (2.00) NQ (2Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (2Titanium ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND (2Vanadium ug/L 200.8 NQ (10.0) NQ (10.0) NQ (10.0) NQ (1Zinc ug/L 200.7 1,300 700 370 45
4-7 

Note: The Day 3 results represent the average of the original sample and the field duplicate (SP-4). 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. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. ** - The Day 3 influent to the SBR system was detected at a concentration of 42.8 ng/L, which seems like an erroneous result compared to the Day 3 d

concentration and the other three sample days. For presentation purposes in this table, the original sample result has been removed from the average othe calculation of the 4-day average result. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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

Table 4-2. Influent to the SBR System, Dickerson 

Influent to the SBR System (SP-2)

Analyte Units Method Day 1 Day 2 Day 3 Da

ClassicalsAmmonia mg/L 350.1 4.40 4.10 3.10 3.20 Nitrate Nitrite as N mg/L 353.2 48.0 43.0 38.0 37.0 Nitrogen, Total Kjeldahl mg/L 351.2 10.0 B NQ (10.0) B 10.5 NQ (10.Biochemical Oxygen Demand mg/L 5210B 4.00 3.00 NQ (2.50) 2.80 Chemical Oxygen Demand mg/L 410.4 160 81.0 135 130 Chloride mg/L 300.0 8,600 7,800 6,700 6,700 Sulfate mg/L 300.0 1,800 1,600 1,750 1,700 Cyanide, Total mg/L 4500 CN E 0.220 B 0.130 B 0.0520 0.0500 Total Dissolved Solids mg/L 2540C 14,000 14,000 12,500 12,000 Total Suspended Solids mg/L 2540D 38.0 37.0 70.5 42.0 Phosphorus, Total mg/L 365.1 NQ (0.0500) NQ (0.0500) < 0.0375 NQ (0.05Total MetalsAluminum ug/L 200.7 600 450 1,450 1,500 Antimony ug/L 200.8 5.50 4.40 4.60 3.90 Arsenic ug/L 200.8 NQ (4.00) NQ (4.00) 4.95 5.50 Barium ug/L 200.7 300 260 250 230 Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.0Boron ug/L 200.7 170,000 B 170,000 B 160,000 150,00Cadmium ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.0
4-8 

Note: The Day 3 results represent the average of the original sample and the field duplicate (SP-4). 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. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. ** - The Day 3 influent to the SBR system was detected at a concentration of 42.8 ng/L, which seems like an erroneous result compared to the Day 3 d

concentration and the other three sample days. For presentation purposes in this table, the original sample result has been removed from the average othe calculation of the 4-day average result. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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

Table 4-2. Influent to the SBR System, Dickerson 

Influent to the SBR System (SP-2)

Analyte Units Method Day 1 Day 2 Day 3 Da

Calcium ug/L 200.7 2,600,000 2,400,000 2,250,000 2,100,00Chromium ug/L 200.8 NQ (8.00) ^ NQ (8.00) ^ NQ (8.00) NQ (8.0Cobalt ug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.Copper ug/L 200.8 43.0 46.0 55.5 98.0 Iron ug/L 200.7 740 570 1,700 1,800 Lead ug/L 200.8 2.70 NQ (2.00) 3.65 5.00 Magnesium ug/L 200.7 1,200,000 1,200,000 1,200,000 1,100,00Manganese ug/L 200.7 90.0 110 265 300 Mercury ng/L 1631E 222 200 446 416 Molybdenum ug/L 200.7 300 260 245 230 Nickel ug/L 200.8 60.0 51.0 50.5 50.0 Selenium ug/L 200.8 130 110 105 100 Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.0Sodium ug/L 200.7 200,000 200,000 185,000 180,00Thallium ug/L 200.8 NQ (2.00) NQ (2.00) NQ (2.00) NQ (2.0Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (20Titanium ug/L 200.7 46.0 35.0 99.5 100 Vanadium ug/L 200.8 NQ (10.0) NQ (10.0) 10.5 11.0 Zinc ug/L 200.7 NQ (40.0) NQ (40.0) 53.0 65.0 Dissolved Metals
4-9 

Note: The Day 3 results represent the average of the original sample and the field duplicate (SP-4). 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. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. ** - The Day 3 influent to the SBR system was detected at a concentration of 42.8 ng/L, which seems like an erroneous result compared to the Day 3 d

concentration and the other three sample days. For presentation purposes in this table, the original sample result has been removed from the average othe calculation of the 4-day average result. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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

Table 4-2. Influent to the SBR System, Dickerson 

Influent to the SBR System (SP-2)

Analyte Units Method Day 1 Day 2 Day 3 Da

Aluminum ug/L 200.7 ND (200) NQ (200) NQ (200) NQ (20Antimony ug/L 200.8 4.80 4.80 3.60 4.10 Arsenic ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.0Barium ug/L 200.7 280 250 190 170 Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.0Boron ug/L 200.7 180,000 B 170,000 B 160,000 160,00Cadmium ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.0Calcium ug/L 200.7 2,600,000 2,500,000 2,300,000 2,200,00Chromium ug/L 200.8 ND (8.00) ^ ND (8.00) ^ ND (8.00) ND (8.0Chromium (VI) ug/L 218.6 ND (10.0) ND (10.0) ND (10.0) ND (10.Cobalt ug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.Copper ug/L 200.8 40.0 45.0 45.0 69.0 Iron ug/L 200.7 ND (200) ND (200) ND (200) ND (20Lead ug/L 200.8 NQ (2.00) NQ (2.00) ND (2.00) ND (2.0Magnesium ug/L 200.7 1,200,000 1,300,000 1,200,000 1,200,00Manganese ug/L 200.7 70.0 100 210 250 Mercury ng/L 1631E 5.97 6.78 5.56** 5.81 Molybdenum ug/L 200.7 290 260 240 230 Nickel ug/L 200.8 54.0 51.0 49.5 50.0 Selenium ug/L 200.8 120 110 97.0 95.0 
4-10 

Note: The Day 3 results represent the average of the original sample and the field duplicate (SP-4). 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. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. ** - The Day 3 influent to the SBR system was detected at a concentration of 42.8 ng/L, which seems like an erroneous result compared to the Day 3 d

concentration and the other three sample days. For presentation purposes in this table, the original sample result has been removed from the average othe calculation of the 4-day average result. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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

Table 4-2. Influent to the SBR System, Dickerson 

Influent to the SBR System (SP-2)

Analyte Units Method Day 1 Day 2 Day 3 Da

Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.0Sodium ug/L 200.7 190,000 190,000 180,000 180,00Thallium ug/L 200.8 NQ (2.00) NQ (2.00) NQ (2.00) NQ (2.0Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (20Titanium ug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20.Vanadium ug/L 200.8 NQ (10.0) NQ (10.0) NQ (10.0) NQ (10.Zinc ug/L 200.7 NQ (40.0) NQ (40.0) NQ (40.0) 45.0 
4-11 

Note: The Day 2 results represent the average of the original sample and the field duplicate (SP-5). 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. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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

Table 4-3. Effluent from the SBR System, Dickerson 

Effluent from the SBR System (SP-3) 

Analyte Units Method Day 1 Day 2 Day 3 Day 

Classicals Ammonia mg/L 350.1 NQ (1.00) NQ (1.00) NQ (1.00) NQ (1.0Nitrate Nitrite as N mg/L 353.2 NQ (0.100) 0.110 0.140 0.150 Nitrogen, Total Kjeldahl mg/L 351.2 13.0 B 13.0 13.0 B,4 13.0 Biochemical Oxygen Demand mg/L 5210B 3.90 4.70 5.70 4.50 Chemical Oxygen Demand mg/L 410.4 150 185 140 F 84.0 Chloride mg/L 300.0 9,700 8,000 7,800 7,600 Sulfate mg/L 300.0 1,800 1,700 1,700 1,700 Cyanide, Total mg/L 4500 CN E 0.100 B NQ (0.0100) NQ (0.0100) B,F NQ (0.01Total Dissolved Solids mg/L 2540C 15,000 13,500 14,000 13,000 Total Suspended Solids mg/L 2540D 8.80 14.0 8.00 14.0 Phosphorus, Total mg/L 365.1 NQ (0.0500) NQ (0.0500) NQ (0.0500) NQ (0.05Total Metals Aluminum ug/L 200.7 660 710 870 920 Antimony ug/L 200.8 5.00 5.50 5.10 4.60 Arsenic ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.0Barium ug/L 200.7 310 305 280 230 Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.0Boron ug/L 200.7 180,000 B 185,000 180,000 B,4 170,00Cadmium ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.0Calcium ug/L 200.7 2,700,000 2,750,000 2,700,000 4 2,400,0Chromium ug/L 200.8 ND (8.00) ^ ND (8.00) ND (8.00) ^ ND (8.0Cobalt ug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20Copper ug/L 200.8 21.0 22.0 21.0 32.0 Iron ug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (20Lead ug/L 200.8 NQ (2.00) NQ (2.00) NQ (2.00) NQ (2.0Magnesium ug/L 200.7 1,300,000 1,250,000 1,300,000 4 1,200,0
4-12 

Note: The Day 2 results represent the average of the original sample and the field duplicate (SP-5). 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. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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

Table 4-3. Effluent from the SBR System, Dickerson 

Effluent from the SBR System (SP-3) 

Analyte Units Method Day 1 Day 2 Day 3 Day 

Manganese ug/L 200.7 81.0 84.5 100 160 Mercury ng/L 1631E 7.27 9.65 10.9 8.59 Molybdenum ug/L 200.7 320 315 300 260 Nickel ug/L 200.8 78.0 64.0 58.0 50.0 Selenium ug/L 200.8 110 110 110 100 Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) F ND (2.0Sodium ug/L 200.7 220,000 225,000 230,000 4 220,00Thallium ug/L 200.8 NQ (2.00) NQ (2.00) NQ (2.00) NQ (2.0Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (20Titanium ug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20Vanadium ug/L 200.8 NQ (10.0) NQ (10.0) NQ (10.0) NQ (10Zinc ug/L 200.7 43.0 42.5 NQ (40.0) NQ (40Dissolved Metals Aluminum ug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (20Antimony ug/L 200.8 5.70 5.10 4.50 4.80 Arsenic ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.0Barium ug/L 200.7 320 300 270 230 Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.0Boron ug/L 200.7 190,000 B 180,000 180,000 B,4 170,00Cadmium ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.0Calcium ug/L 200.7 2,800,000 2,750,000 2,700,000 4 2,400,0Chromium ug/L 200.8 ND (8.00) ^ ND (8.00) ND (8.00) ^ ND (8.0Chromium (VI) ug/L 218.6 ND (10.0) ND (10.0) ND (10.0) ND (10Cobalt ug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20Copper ug/L 200.8 16.0 17.5 13.0 20.0 Iron ug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (20Lead ug/L 200.8 NQ (2.00) NQ (2.00) ND (2.00) ND (2.0
4-13 

Note: The Day 2 results represent the average of the original sample and the field duplicate (SP-5). 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. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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

Table 4-3. Effluent from the SBR System, Dickerson 

Effluent from the SBR System (SP-3) 

Analyte Units Method Day 1 Day 2 Day 3 Day 

Magnesium ug/L 200.7 1,300,000 1,300,000 1,300,000 4 1,200,0Manganese ug/L 200.7 85.0 85.0 100 160 Mercury ng/L 1631E 1.69 4.28 8.61 F 1.21 Molybdenum ug/L 200.7 330 315 290 260 Nickel ug/L 200.8 78.0 66.5 57.0 51.0 Selenium ug/L 200.8 100 105 98.0 98.0 Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) F ND (2.0Sodium ug/L 200.7 220,000 220,000 220,000 4 210,00Thallium ug/L 200.8 NQ (2.00) NQ (2.00) NQ (2.00) NQ (2.0Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (20Titanium ug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20Vanadium ug/L 200.8 NQ (10.0) NQ (10.0) NQ (10.0) NQ (10Zinc ug/L 200.7 43.0 < 31.0 NQ (40.0) NQ (40
4-14 

< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu* - The 4-day average result includes an analytical result where the accuracy is questionable. If the questionable result was included from the calculatwould be 52,000 mg/L. 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. Classical Pollutants 4-Day Average Data Summary for FGD Wastewater Treatment Syst

Analyte Units Method

Influent to FGD 

Wastewater 

Treatment System (SP-1)

4-Day Average

Influent to 

SBR

System (SP-2)

4-Day Average

ClassicalsAmmonia mg/L 350.1 5.05 3.70 Nitrate Nitrite as N mg/L 353.2 60.8 41.5 Nitrogen, Total Kjeldahl mg/L 351.2 46.5 < 7.63 Biochemical Oxygen Demand mg/L 5210B < 4.81 < 2.76 Chemical Oxygen Demand mg/L 410.4 130 127 Chloride mg/L 300.0 7,680 7,450 Sulfate mg/L 300.0 1,780 1,710 Cyanide, Total mg/L 4500 CN E 0.950 0.113 Total Dissolved Solids mg/L 2540C 12,700* 13,100 Total Suspended Solids mg/L 2540D 5,630 46.9 Phosphorus, Total mg/L 365.1 < 2.81 < 0.0281 
4-15 

< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu* - The 4-day average result presented has been revised to exclude the Day 3 original sample result of 42.8 ng/L. EPA determined that this is erroneou

result of 5.56 ng/L and the other sampling days. 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 4-5. Metal Pollutants 4-Day Average Data Summary for FGD Wastewater Treatment Syste

Influent to FGD 

Wastewater Treatment 

System (SP-1)

4-Day Average

Influent to 

SBR 

System (SP-2)

4-Day Average

Analyte Units Method Total Dissolved Total Dissolved Tot

MetalsAluminum ug/L 200.7 110,000 NQ (200) 1,000 NQ (200) 79Antimony ug/L 200.8 18.8 3.45 4.60 4.33 5.0Arsenic ug/L 200.8 230 NQ (4.00) < 3.61 NQ (4.00) NQ (4Barium ug/L 200.7 700 183 260 223 28Beryllium ug/L 200.7 12.5 ND (2.00) ND (2.00) ND (2.00) ND (2Boron ug/L 200.7 193,000 188,000 163,000 168,000 179,Cadmium ug/L 200.8 26.5 22.8 NQ (4.00) NQ (4.00) NQ (4Calcium ug/L 200.7 2,700,000 2,030,000 2,340,000 2,400,000 2,640Chromium ug/L 200.8 570 ND (8.00) NQ (8.00) ND (8.00) ND (8Chromium (VI) ug/L 218.6 NA ND (10.0) NA ND (10.0) NA Cobalt ug/L 200.7 117 71.8 NQ (20.0) NQ (20.0) NQ (2Copper ug/L 200.8 543 13.9 60.6 49.8 24Iron ug/L 200.7 158,000 NQ (200) 1,200 ND (200) NQ (Lead ug/L 200.8 178 ND (2.00) < 3.09 NQ (2.00) NQ (2Magnesium ug/L 200.7 1,530,000 1,450,000 1,180,000 1,230,000 1,260Manganese ug/L 200.7 9,630 9,780 191 158 10Mercury ng/L 1631E 5,760 111 321 6.03* 9.1Molybdenum ug/L 200.7 440 215 259 255 29Nickel ug/L 200.8 565 393 52.9 51.1 62Selenium ug/L 200.8 1,210 173 111 106 10Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.00) ND (2Sodium ug/L 200.7 185,000 193,000 191,000 185,000 224,Thallium ug/L 200.8 < 1.48 < 1.35 NQ (2.00) NQ (2.00) NQ (2
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* - The 4-day average result presented has been revised to exclude the Day 3 original sample result of 42.8 ng/L. EPA determined that this is erroneou

result of 5.56 ng/L and the other sampling days. 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 4-5. Metal Pollutants 4-Day Average Data Summary for FGD Wastewater Treatment Syste

Influent to FGD 

Wastewater Treatment 

System (SP-1)

4-Day Average

Influent to 

SBR 

System (SP-2)

4-Day Average

Analyte Units Method Total Dissolved Total Dissolved Tot

Tin ug/L 200.7 NQ (200) ND (200) ND (200) ND (200) ND (Titanium ug/L 200.7 5,430 ND (20.0) 70.1 NQ (20.0) NQ (2Vanadium ug/L 200.8 483 NQ (10.0) < 7.88 NQ (10.0) NQ (1Zinc ug/L 200.7 2,000 705 < 39.5 < 26.3 < 3
5-1

5. DATA QUALITY

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

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 sample bottle. The blank samples were 

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

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

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

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

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

A-15 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-15 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-6, SP-7, and SP-8) to evaluate possible 

contamination from sampling equipment, sampling equipment decontamination procedures, 

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

samples for the total and dissolved metals and total and dissolved mercury 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-6) 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 0.5 liters 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 Dickerson’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 not 

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

days.
5-3

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-6) 

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

composite container. After around 90 minutes, the sampling team began pumping off the ASTM 

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

was purged with 1 liter 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 Dickerson’s 

representative, using the same procedure discussed in the sample collection description (Section 

3.1). 

The total mercury field blank sample for the influent to the SBR (SP-7) and for the 

effluent from the SBR (SP-8) were 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 

influent to the SBR (SP-7) and the effluent from the SBR (SP-8) 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 at each point was used with a pump to fill the 20-liter field blank 

composite container. Prior to attaching one end of the tubing to the sample tap, it was placed 

directly into the container holding ASTM Type 1 water. The other end of the tubing was 

attached to the vented cap on top of the 20-liter field blank composite container. After enough 

volume was pumped into the 20-liter field blank composite container, the vented cap was 

replaced with a closed cap and the container was placed on ice in a covered plastic trash can. 

The vented cap used for the field blank collection was the same cap that was later used for the 

metals composite container. 

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

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

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

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

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

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

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

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

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

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

hexavalent chromium field blank samples. 

Table 5-1 presents the field blank analytical results for SP-6 through SP-8. 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-16 

through A-24 present all the analytical results for the field blanks from each of the sampling 

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

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

5.2.4 Field Duplicates 

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

precision for the episode. Field duplicate samples are separate samples collected from the same 

location as the original sample. The duplicate is filled immediately after the original sample and 

is stored and analyzed independently. The RPD between the two sample results is examined to 

determine the precision of the data. EPA used the following equation to calculate the RPD for 

the duplicate sample results. 

100

2

S D

S D

RPD (%) 





 



 

  (5-1) 

where: 

S = concentration of the analyte from original sample analysis; 

D = concentration of the analyte from the duplicate sample analysis; and 

RPD = relative percent difference between the original and duplicate sample 

result. 

During this sampling episode, EPA collected duplicate samples for the influent to the 

SBR (SP-4) and the effluent from the SBR (SP-5) during day 3 and day 2 of the sampling 

episode, respectively. The duplicate samples were analyzed for all analytes. Tables 5-2 and 5-3 

present the analytical results and the RPD for SP-4 and SP-5, respectively. Results are rounded 

to three significant digits. Appendix Tables A-7 and A-13 present all the analytical results for the 

influent to the SBR (SP-2) Day 3 and the duplicate of the influent to the SBR (SP-4) 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). Appendix Tables A-10 and A-14 

present all the analytical results for the effluent from the SBR (SP-3) Day 2 and the duplicate of 

the effluent from the SBR (SP-5) sample analyses, including all qualified results and all results 

that were measured above the method detection limit, but below the quantitation limit (i.e., Jvalues). 
5-5 

Table 5-1. Field Blank Analytical Results, Dickerson 

Analyte Sample Description Method Units C

Mercury Influent to FGD Wastewater Treatment System Field Blank - Day 1 1631E ng/L 
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

* - The dissolved mercury original sample result seems erroneous based on the Day 3 duplicate sample concentration and the other three sample days. 

was excluded from the presentation of the Day 3 average result in Table 4-2. Additionally, 5.56 ng/L (instead of 24.2 ng/L) was used in the calculatiopresented in Table 4-2 and 4-5. NC – Not calculated. ND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

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

value. ^ - 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. 

5-6 5-6 

Table 5-2. Field Duplicate Results – Influent to SBR System, Dickerson 

Analyte Method Units 

Original Influent 

to SBR 

System, Day 3 

Concentration (SP-2) 

Duplicate Influent 

to SBR 

System 

Concentration (SP-4) 

Av

R

Classicals Ammonia 350.1 mg/L 2.90 3.30 Nitrate Nitrite as N 353.2 mg/L 38.0 38.0 Nitrogen, Total Kjeldahl 351.2 mg/L 10.0 B 11.0 B Biochemical Oxygen Demand 5210B mg/L NQ (2.50) NQ (2.50) NQ Chemical Oxygen Demand 410.4 mg/L 160 110 Chloride 300.0 mg/L 6,700 6,700 6Sulfate 300.0 mg/L 1,700 1,800 1Cyanide, Total 4500 CN E mg/L 0.0450 B 0.0590 B 0Total Dissolved Solids 2540C mg/L 12,000 13,000 1Total Suspended Solids 2540D mg/L 42.0 99.0 Phosphorus, Total 365.1 mg/L 0.0500 NQ (0.0500) < 0Total Metals Aluminum 200.7 ug/L 1,400 1,500 1Antimony 200.8 ug/L 4.50 4.70 Arsenic 200.8 ug/L 4.50 5.40 Barium 200.7 ug/L 240 260 Beryllium 200.7 ug/L ND (2.00) ND (2.00) ND Boron 200.7 ug/L 160,000 B 160,000 B 16Cadmium 200.8 ug/L NQ (4.00) NQ (4.00) NQ Calcium 200.7 ug/L 2,200,000 2,300,000 2,2Chromium 200.8 ug/L NQ (8.00) ^ NQ (8.00) ^ NQ Cobalt 200.7 ug/L NQ (20.0) NQ (20.0) NQ Copper 200.8 ug/L 54.0 57.0 Iron 200.7 ug/L 1,700 1,700 1
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

* - The dissolved mercury original sample result seems erroneous based on the Day 3 duplicate sample concentration and the other three sample days. 

was excluded from the presentation of the Day 3 average result in Table 4-2. Additionally, 5.56 ng/L (instead of 24.2 ng/L) was used in the calculatiopresented in Table 4-2 and 4-5. NC – Not calculated. ND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

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

value. ^ - 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. 

5-7 5-7 

Table 5-2. Field Duplicate Results – Influent to SBR System, Dickerson 

Analyte Method Units 

Original Influent 

to SBR 

System, Day 3 

Concentration (SP-2) 

Duplicate Influent 

to SBR 

System 

Concentration (SP-4) 

Av

R

Lead 200.8 ug/L 3.50 3.80 Magnesium 200.7 ug/L 1,200,000 1,200,000 1,2Manganese 200.7 ug/L 260 270 Mercury 1631E ng/L 454 437 Molybdenum 200.7 ug/L 240 250 Nickel 200.8 ug/L 52.0 49.0 Selenium 200.8 ug/L 110 100 Silver 200.8 ug/L ND (2.00) ND (2.00) ND Sodium 200.7 ug/L 180,000 190,000 18Thallium 200.8 ug/L NQ (2.00) NQ (2.00) NQ Tin 200.7 ug/L ND (200) ND (200) ND Titanium 200.7 ug/L 99.0 100 Vanadium 200.8 ug/L 10.0 11.0 Zinc 200.7 ug/L 53.0 53.0 Dissolved Metals Aluminum 200.7 ug/L NQ (200) NQ (200) NQ Antimony 200.8 ug/L 3.60 3.60 Arsenic 200.8 ug/L NQ (4.00) NQ (4.00) NQ Barium 200.7 ug/L 190 190 Beryllium 200.7 ug/L ND (2.00) ND (2.00) ND Boron 200.7 ug/L 160,000 B 160,000 B 16Cadmium 200.8 ug/L NQ (4.00) NQ (4.00) NQ Calcium 200.7 ug/L 2,300,000 2,300,000 2,3Chromium 200.8 ug/L ND (8.00) ^ ND (8.00) ^ ND Chromium (VI) 218.6 ug/L ND (10.0) ND (10.0) ND 
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

* - The dissolved mercury original sample result seems erroneous based on the Day 3 duplicate sample concentration and the other three sample days. 

was excluded from the presentation of the Day 3 average result in Table 4-2. Additionally, 5.56 ng/L (instead of 24.2 ng/L) was used in the calculatiopresented in Table 4-2 and 4-5. NC – Not calculated. ND – Not detected (number in parentheses is the quantitation limit). NQ – Analyte was measured above the method detection limit, but below the quantitation limit (number shown in parentheses is the quantitation limit

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

value. ^ - 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. 

5-8 5-8 

Table 5-2. Field Duplicate Results – Influent to SBR System, Dickerson 

Analyte Method Units 

Original Influent 

to SBR 

System, Day 3 

Concentration (SP-2) 

Duplicate Influent 

to SBR 

System 

Concentration (SP-4) 

Av

R

Cobalt 200.7 ug/L NQ (20.0) NQ (20.0) NQ Copper 200.8 ug/L 44.0 46.0 Iron 200.7 ug/L ND (200) ND (200) ND Lead 200.8 ug/L ND (2.00) ND (2.00) ND Magnesium 200.7 ug/L 1,200,000 1,200,000 1,2Manganese 200.7 ug/L 210 210 Mercury 1631E ng/L 42.8* 5.56 2Molybdenum 200.7 ug/L 240 240 Nickel 200.8 ug/L 49.0 50.0 Selenium 200.8 ug/L 94.0 100 Silver 200.8 ug/L ND (2.00) ND (2.00) ND Sodium 200.7 ug/L 180,000 180,000 18Thallium 200.8 ug/L NQ (2.00) NQ (2.00) NQ Tin 200.7 ug/L ND (200) ND (200) ND Titanium 200.7 ug/L NQ (20.0) NQ (20.0) NQ Vanadium 200.8 ug/L NQ (10.0) NQ (10.0) NQ Zinc 200.7 ug/L NQ (40.0) NQ (40.0) NQ 
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

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

value. ^ - 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. D – Laboratory duplicate RPD greater than method-specified criteria. 

5-9 

Table 5-3. Field Duplicate Results – Effluent from SBR System, Dickerson 

Analyte Method Units

Original Effluent 

from SBR

System, Day 2 

Concentration (SP-3)

Duplicate Effluent 

from SBR 

System 

Concentration (SP-5)

Ave

Re

ClassicalsAmmonia 350.1 mg/L NQ (1.00) NQ (1.00) NQ Nitrate Nitrite as N 353.2 mg/L 0.110 0.110 0.Nitrogen, Total Kjeldahl 351.2 mg/L 13.0 B 13.0 B 1Biochemical Oxygen Demand 5210B mg/L 4.70 4.70 4Chemical Oxygen Demand 410.4 mg/L 190 180 1Chloride 300.0 mg/L 8,200 7,800 8,Sulfate 300.0 mg/L 1,700 1,700 1,Cyanide, Total 4500 CN E mg/L NQ (0.0100) B NQ (0.0100) B NQ (0Total Dissolved Solids 2540C mg/L 14,000 13,000 13Total Suspended Solids 2540D mg/L 16.0 12.0 D 1Phosphorus, Total 365.1 mg/L NQ (0.0500) NQ (0.0500) NQ (0Total MetalsAluminum 200.7 ug/L 720 700 7Antimony 200.8 ug/L 5.70 5.30 5Arsenic 200.8 ug/L NQ (4.00) NQ (4.00) NQ Barium 200.7 ug/L 310 300 3Beryllium 200.7 ug/L ND (2.00) ND (2.00) ND Boron 200.7 ug/L 190,000 B 180,000 B 185Cadmium 200.8 ug/L NQ (4.00) NQ (4.00) NQ Calcium 200.7 ug/L 2,800,000 2,700,000 2,75Chromium 200.8 ug/L ND (8.00) ^ ND (8.00) ^ ND 
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

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

value. ^ - 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. D – Laboratory duplicate RPD greater than method-specified criteria. 

5-10 

Table 5-3. Field Duplicate Results – Effluent from SBR System, Dickerson 

Analyte Method Units

Original Effluent 

from SBR

System, Day 2 

Concentration (SP-3)

Duplicate Effluent 

from SBR 

System 

Concentration (SP-5)

Ave

Re

Cobalt 200.7 ug/L NQ (20.0) NQ (20.0) NQ Copper 200.8 ug/L 22.0 22.0 2Iron 200.7 ug/L NQ (200) NQ (200) NQ Lead 200.8 ug/L NQ (2.00) NQ (2.00) NQ Magnesium 200.7 ug/L 1,300,000 1,200,000 1,25Manganese 200.7 ug/L 86.0 83.0 8Mercury 1631E ng/L 13.0 6.30 9Molybdenum 200.7 ug/L 320 310 3Nickel 200.8 ug/L 64.0 64.0 6Selenium 200.8 ug/L 110 110 1Silver 200.8 ug/L ND (2.00) ND (2.00) ND Sodium 200.7 ug/L 230,000 220,000 225Thallium 200.8 ug/L NQ (2.00) NQ (2.00) NQ Tin 200.7 ug/L ND (200) ND (200) ND Titanium 200.7 ug/L NQ (20.0) NQ (20.0) NQ Vanadium 200.8 ug/L NQ (10.0) NQ (10.0) NQ Zinc 200.7 ug/L 42.0 43.0 4Dissolved MetalsAluminum 200.7 ug/L NQ (200) NQ (200) NQ Antimony 200.8 ug/L 5.40 4.80 5Arsenic 200.8 ug/L NQ (4.00) NQ (4.00) NQ Barium 200.7 ug/L 300 300 3
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

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

value. ^ - 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. D – Laboratory duplicate RPD greater than method-specified criteria. 

5-11 

Table 5-3. Field Duplicate Results – Effluent from SBR System, Dickerson 

Analyte Method Units

Original Effluent 

from SBR

System, Day 2 

Concentration (SP-3)

Duplicate Effluent 

from SBR 

System 

Concentration (SP-5)

Ave

Re

Beryllium 200.7 ug/L ND (2.00) ND (2.00) ND Boron 200.7 ug/L 180,000 B 180,000 B 180Cadmium 200.8 ug/L NQ (4.00) NQ (4.00) NQ Calcium 200.7 ug/L 2,800,000 2,700,000 2,75Chromium 200.8 ug/L ND (8.00) ^ ND (8.00) ^ ND Chromium (VI) 218.6 ug/L ND (10.0) ND (10.0) ND Cobalt 200.7 ug/L NQ (20.0) NQ (20.0) NQ Copper 200.8 ug/L 17.0 18.0 1Iron 200.7 ug/L NQ (200) NQ (200) NQ Lead 200.8 ug/L NQ (2.00) NQ (2.00) NQ Magnesium 200.7 ug/L 1,300,000 1,300,000 1,30Manganese 200.7 ug/L 86.0 84.0 8Mercury 1631E ng/L 6.52 2.03 4Molybdenum 200.7 ug/L 320 310 3Nickel 200.8 ug/L 67.0 66.0 6Selenium 200.8 ug/L 100 110 1Silver 200.8 ug/L ND (2.00) ND (2.00) ND Sodium 200.7 ug/L 220,000 220,000 220Thallium 200.8 ug/L NQ (2.00) NQ (2.00) NQ Tin 200.7 ug/L ND (200) ND (200) ND Titanium 200.7 ug/L NQ (20.0) NQ (20.0) NQ Vanadium 200.8 ug/L NQ (10.0) NQ (10.0) NQ 
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

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

value. ^ - 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. D – Laboratory duplicate RPD greater than method-specified criteria. 

5-12 

Table 5-3. Field Duplicate Results – Effluent from SBR System, Dickerson 

Analyte Method Units

Original Effluent 

from SBR

System, Day 2 

Concentration (SP-3)

Duplicate Effluent 

from SBR 

System 

Concentration (SP-5)

Ave

Re

Zinc 200.7 ug/L 42.0 NQ (40.0) < 
6-1

6. REFERENCES

1. Eastern Research Group, Inc., 2010. Final Sampling Plan, Mirant Mid-Atlantic, LLC’s 

Dickerson Generating Station. August 19. DCN SE00503. 

2. Eastern Research Group, Inc., 2010. Quality Assurance Project Plan for the Steam 

Electric Effluent Guidelines Rulemaking. (October). DCN SE00058. 
Appendix A 

ANALYTICAL RESULTS 
A-1 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. C – pH upon receipt was less than 10 S.U. L – LFB or LCS percent recovery not within method-specified criteria, but is within laboratory-specified criteria. 

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

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.11 1 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 Nitrogen, Total Kjeldahl 351.2 mg/L 1 1.5 20 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 500 130 1,500 Sulfate 300.0 mg/L 100 23 500 Cyanide, Total 4500 CN E mg/L 4 0.008 0.04 Total Dissolved Solids 2540C mg/L 1 470 1,000 Total Suspended Solids 2540D mg/L 1 11 40 Phosphorus, Total 365.1 mg/L 5 0.025 0.25 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 10 6.1 20 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 50 1,700 10,000 Chromium 200.8 ug/L 10 16 40 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 10 4.8 20 Iron 200.7 ug/L 50 800 5,000 Lead 200.8 ug/L 10 3.6 10 
A-2 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. C – pH upon receipt was less than 10 S.U. L – LFB or LCS percent recovery not within method-specified criteria, but is within laboratory-specified criteria. 

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

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 500 121 252 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 10 8.4 50 Zinc 200.7 ug/L 2 9.1 40 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 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 
A-3 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. C – pH upon receipt was less than 10 S.U. L – LFB or LCS percent recovery not within method-specified criteria, but is within laboratory-specified criteria. 

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

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 10 2.41 5.05 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 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 200.7 ug/L 2 9.1 40 
A-4 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. 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-2. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, Dick

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.11 1 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 500 130 1,500 Sulfate 300.0 mg/L 100 23 500 Cyanide, Total 4500 CN E mg/L 4 0.008 0.04 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 55 200 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 10 6.1 20 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 50 1,700 10,000 Chromium 200.8 ug/L 10 16 40 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 10 4.8 20 Iron 200.7 ug/L 50 800 5,000 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 
A-5 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 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-2. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, Dick

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 500 121 252 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 10 8.4 50 Zinc 200.7 ug/L 2 9.1 40 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 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 
A-6 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 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-2. Influent to FGD Wastewater Treatment System, Day 2 Analytical Results, Dick

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 10 2.41 5.05 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 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 200.7 ug/L 2 9.1 40 
A-7 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. 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-3. Influent to FGD Wastewater Treatment System, Day 3 Analytical Results, Dick

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 50 12 250 Cyanide, Total 4500 CN E mg/L 4 0.008 0.04 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 28 100 Phosphorus, Total 365.1 mg/L 5 0.025 0.25 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 Chromium 200.8 ug/L 10 16 40 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 10 4.8 20 Iron 200.7 ug/L 50 800 5,000 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 
A-8 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. 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-3. Influent to FGD Wastewater Treatment System, Day 3 Analytical Results, Dick

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 500 121 252 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 10 8.4 50 Zinc 200.7 ug/L 2 9.1 40 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 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 
A-9 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

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

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 20 4.83 10.1 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 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 200.7 ug/L 2 9.1 40 
A-10 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. D – Laboratory duplicate RPD greater than method-specified criteria. 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-4. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, Dick

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 0.59 5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 50 12 250 Cyanide, Total 4500 CN E mg/L 4 0.008 0.04 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 18 67 Phosphorus, Total 365.1 mg/L 5 0.025 0.25 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 10 6.1 20 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 50 1,700 10,000 Chromium 200.8 ug/L 10 16 40 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 10 4.8 20 Iron 200.7 ug/L 50 800 5,000 Lead 200.8 ug/L 2 0.73 2 
A-11 

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. D – Laboratory duplicate RPD greater than method-specified criteria. 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-4. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, Dick

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 500 121 252 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 10 8.4 50 Zinc 200.7 ug/L 2 9.1 40 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 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 
A-12 

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. D – Laboratory duplicate RPD greater than method-specified criteria. 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-4. Influent to FGD Wastewater Treatment System, Day 4 Analytical Results, Dick

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 20 4.83 10.1 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 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 200.7 ug/L 2 9.1 40 
A-13 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-5. Influent to SBR System, Day 1 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.11 1 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 500 130 1,500 Sulfate 300.0 mg/L 100 23 500 Cyanide, Total 4500 CN E mg/L 1 0.002 0.01 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 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 
A-14 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-5. Influent to SBR System, Day 1 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 10 2.41 5.05 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 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 200.7 ug/L 2 9.1 40 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 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 
A-15 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-5. Influent to SBR System, Day 1 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

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 200.7 ug/L 2 9.1 40 
A-16 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-6. Influent to SBR System, Day 2 Analytical Results, Dickerson 

Analyte Method Units Dilution Value

Sample-Specific 

MDL

Sample-Specifi

QL 

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 Nitrogen, Kjeldahl 351.2 mg/L 1 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 50 12 250 Cyanide, Total 4500 CN E mg/L 1 0.002 0.01 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 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 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 
A-17 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-6. Influent to SBR System, Day 2 Analytical Results, Dickerson 

Analyte Method Units Dilution Value

Sample-Specific 

MDL

Sample-Specifi

QL 

Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 100 24.1 50.5 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 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 200.7 ug/L 2 9.1 40 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 50 1,700 10,000 
A-18 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-6. Influent to SBR System, Day 2 Analytical Results, Dickerson 

Analyte Method Units Dilution Value

Sample-Specific 

MDL

Sample-Specifi

QL 

Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 4 0.97 2.02 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 200.7 ug/L 2 9.1 40 
A-19 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-7. Influent to SBR System, Day 3 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 50 12 250 Cyanide, Total 4500 CN E mg/L 1 0.002 0.01 Total Dissolved Solids 2540C mg/L 1 19 40 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 
A-20 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-7. Influent to SBR System, Day 3 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 20 4.83 10.1 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 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 200.7 ug/L 2 9.1 40 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 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 
A-21 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-7. Influent to SBR System, Day 3 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 10 2.41 5.05 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 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 200.7 ug/L 2 9.1 40 
A-22 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-8. Influent to SBR System, Day 4 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 50 12 250 Cyanide, Total 4500 CN E mg/L 1 0.002 0.01 Total Dissolved Solids 2540C mg/L 1 19 40 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 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 
A-23 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-8. Influent to SBR System, Day 4 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 500 121 252 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 200.7 ug/L 2 9.1 40 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 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 
A-24 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-8. Influent to SBR System, Day 4 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 2 0.48 1.01 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 200.7 ug/L 2 9.1 40 
A-25 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-9. Effluent from SBR System, Day 1 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.11 1 Nitrate Nitrite as N 353.2 mg/L 1 0.019 0.1 Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 500 130 1,500 Sulfate 300.0 mg/L 100 23 500 Cyanide, Total 4500 CN E mg/L 1 0.002 0.01 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 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 
A-26 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-9. Effluent from SBR System, Day 1 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Mercury 1631E ng/L 10 2.41 5.05 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 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 200.7 ug/L 2 9.1 40 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 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 
A-27 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-9. Effluent from SBR System, Day 1 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

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 200.7 ug/L 2 9.1 40 
A-28 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-10. Effluent from SBR System, Day 2 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 1 0.019 0.1 Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 50 12 250 Cyanide, Total 4500 CN E mg/L 1 0.002 0.01 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 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 
A-29 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-10. Effluent from SBR System, Day 2 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Mercury 1631E ng/L 2 0.48 1.01 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 200.7 ug/L 2 9.1 40 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 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 
A-30 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-10. Effluent from SBR System, Day 2 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Mercury 1631E ng/L 2 0.48 1.01 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 200.7 ug/L 2 9.1 40 
A-31 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-11. Effluent from SBR System, Day 3 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 1 0.019 0.1 Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 50 12 250 Cyanide, Total 4500 CN E mg/L 1 0.002 0.01 Total Dissolved Solids 2540C mg/L 1 19 40 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 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 
A-32 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-11. Effluent from SBR System, Day 3 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Magnesium 200.7 ug/L 50 540 10,000 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 200.7 ug/L 2 9.1 40 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 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 
A-33 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. 4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

B – Analyte was found in the blank and sample. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-11. Effluent from SBR System, Day 3 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 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 200.7 ug/L 2 9.1 40 
A-34 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-12. Effluent from SBR System, Day 4 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 1 0.019 0.1 Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 1 4.1 20 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 50 12 250 Cyanide, Total 4500 CN E mg/L 1 0.002 0.01 Total Dissolved Solids 2540C mg/L 1 19 40 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 
A-35 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-12. Effluent from SBR System, Day 4 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Mercury 1631E ng/L 10 2.41 5.05 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 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 200.7 ug/L 2 9.1 40 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 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 
A-36 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-12. Effluent from SBR System, Day 4 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

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 200.7 ug/L 2 9.1 40 
A-37 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-13. Duplicate of Influent to SBR System, Day 3 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 50 12 250 Cyanide, Total 4500 CN E mg/L 1 0.002 0.01 Total Dissolved Solids 2540C mg/L 1 19 40 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 
A-38 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-13. Duplicate of Influent to SBR System, Day 3 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 20 4.83 10.1 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 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 200.7 ug/L 2 9.1 40 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 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 
A-39 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-13. Duplicate of Influent to SBR System, Day 3 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 2 0.48 1.01 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 200.7 ug/L 2 9.1 40 
A-40 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. D – Laboratory duplicate RPD greater than method-specified criteria. 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-14. Duplicate of Effluent from SBR System, Day 2 Analytical Results, Dickers

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

ClassicalsAmmonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 1 0.019 0.1 Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 50 12 250 Cyanide, Total 4500 CN E mg/L 1 0.002 0.01 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 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 
A-41 

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. D – Laboratory duplicate RPD greater than method-specified criteria. 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-14. Duplicate of Effluent from SBR System, Day 2 Analytical Results, Dickers

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 4 0.97 2.02 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 200.7 ug/L 2 9.1 40 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 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 Chromium (VI) 218.6 ug/L 5 1.96 10 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 
A-42 

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. D – Laboratory duplicate RPD greater than method-specified criteria. 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-14. Duplicate of Effluent from SBR System, Day 2 Analytical Results, Dickers

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Magnesium 200.7 ug/L 50 540 10,000 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 200.7 ug/L 2 9.1 40 
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 quantitation limit). 

A-43 

Table A-15. Bottle Blank and Equipment Blank Analytical Data, Dickerson 

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 quantitation limit). 

A-44 

Table A-15. Bottle Blank and Equipment Blank Analytical Data, Dickerson 

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)
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 quantitation limit). 

A-45 

Table A-15. Bottle Blank and Equipment Blank Analytical Data, Dickerson 

Analyte Method Process Units Concentration 

Aluminum EPA 1638 Dissolved ug/L ND (2.0) 

Antimony EPA 1638 Dissolved ug/L ND (0.50) 

Arsenic EPA 1638 Dissolved ug/L ND (0.50) 

Barium EPA 1638 Dissolved ug/L ND (0.10) 

Beryllium EPA 1638 Dissolved ug/L ND (0.10) 

Cadmium EPA 1638 Dissolved ug/L ND (0.10) 

Chromium EPA 1638 Dissolved ug/L ND (1.0) 

Cobalt EPA 1638 Dissolved ug/L ND (0.10) 

Copper EPA 1638 Dissolved ug/L ND (0.30) 

Lead EPA 1638 Dissolved ug/L ND (0.050) 

Manganese EPA 1638 Dissolved ug/L ND (0.50) 

Molybdenum EPA 1638 Dissolved ug/L ND (0.50) 

Nickel EPA 1638 Dissolved ug/L ND (0.50) 

Selenium EPA 1638 Dissolved ug/L ND (2.0) 

Silver EPA 1638 Dissolved ug/L ND (0.10) 

Thallium EPA 1638 Dissolved ug/L ND (0.050) 

Vanadium EPA 1638 Dissolved ug/L ND (1.0) 

Zinc EPA 1638 Dissolved ug/L ND (0.50) 

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) 
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 quantitation limit). 

A-46 

Table A-15. Bottle Blank and Equipment Blank Analytical Data, Dickerson 

Analyte Method Process Units Concentration 

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) 

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) 
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 quantitation limit). 

A-47 

Table A-15. Bottle Blank and Equipment Blank Analytical Data, Dickerson 

Analyte Method Process Units Concentration 

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) 
A-48 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-16. Influent to FGD Wastewater Treatment System Field Blank, Day 1 Analytical Result

Analyte Method Units 

Dilution 

Value 

SampleSpecific MDL Sample- Specific QL 

Total Metals Aluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 NThallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 Dissolved Metals Aluminum 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 
A-49 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-16. Influent to FGD Wastewater Treatment System Field Blank, Day 1 Analytical Result

Analyte Method Units 

Dilution 

Value 

SampleSpecific MDL Sample- Specific QL 

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 NThallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 
A-50 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-17. Influent to SBR System Field Blank, Day 1 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Total 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 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 NChromium 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 NLead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 NManganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 NThallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 NTitanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 
A-51 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-17. Influent to SBR System Field Blank, Day 1 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 NChromium 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 NLead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 NManganese 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 NThallium 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 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 
A-52 

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. Influent to SBR System Field Blank, Day 2 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL Concentr

Total MetalsMercury 1631E ng/L 1 0.24 0.5 ND (0.5) 
A-53 

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. Influent to SBR System Field Blank, Day 3 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL Con

Total MetalsMercury 1631E ng/L 1 0.24 0.5 ND (0.5) 
A-54 

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-20. Influent to SBR System Field Blank, Day 4 Analytical Results, Dickerson 

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL Concentr

Total MetalsMercury 1631E ng/L 1 0.24 0.5 ND (0.5) 
A-55 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-21. Effluent from SBR System Field Blank, Day 1 Analytical Results, Dickerso

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Total 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 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 NChromium 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 NLead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 NManganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 NThallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 NTitanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 Dissolved MetalsAluminum 200.7 ug/L 2 9.4 200 N
A-56 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-21. Effluent from SBR System Field Blank, Day 1 Analytical Results, Dickerso

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL 

Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 NChromium 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 NManganese 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 NThallium 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 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 
A-57 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-22. Effluent from SBR System Field Blank, Day 2 Analytical Results, Dickerso

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL Concentr

Total MetalsMercury 1631E ng/L 1 0.24 0.5 ND (0.5) 
A-58 

ND – Not detected (number in parentheses is the quantitation limit). ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A-23. Effluent from SBR System Field Blank, Day 3 Analytical Results, Dickerso

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL Concentr

Total MetalsMercury 1631E ng/L 1 0.24 0.5 ND (0.5) 
A-59 

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-24. Effluent from SBR System Field Blank, Day 4 Analytical Results, Dickerso

Analyte Method Units

Dilution

Value

SampleSpecific MDL Sample- Specific QL Conce

Total MetalsMercury 1631E ng/L 1 0.24 0.5 ND (0
Appendix B 

DATA REVIEW NARRATIVES 
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: FGS Data Review Narrative for Total and Dissolved Mercury – Episode 6562 

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 (CVA-FS) analysis. 

Table 1 summarizes the 37 samples (excluding laboratory filter blanks) FGS extracted 

and analyzed for total and dissolved mercury. 

Table 1. EPA Episode 6562 Total & Dissolved Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71841 1008203-01 Aqueous FGD Influent Day 1 8/23/2010 

71841 1008203-02 Aqueous Dissolved FGD Influent, Day 1 8/23/2010 

71842 1008207-06 Aqueous FGD Influent, Day 2 8/24/2010 

71842 1008207-07 Aqueous Dissolved FGD Influent, Day 2 8/24/2010 

71843 1008223-13 Aqueous FGD Influent, Day 3 8/25/2010 

71843 1008223-14 Aqueous Dissolved FGD Influent, Day 3 8/25/2010 

71844 1008240-09 Aqueous FGD Influent, Day 4 8/26/2010 

71844 1008240-10 Aqueous Dissolved FGD Influent, Day 4 8/26/2010 

71845 1008207-08 Aqueous FGD SBR Influent, Day 1 8/24/2010 

71845 1008207-09 Aqueous Dissolved FGD SBR Influent, Day 1 8/24/2010 

71846 1008223-15 Aqueous FGD SBR Influent, Day 2 8/25/2010 

71846 1008223-16 Aqueous Dissolved FGD SBR Influent, Day 2 8/25/2010 

71847 1008240-11 Aqueous FGD SBR Influent, Day 3 8/26/2010 

71847 1008240-12 Aqueous Dissolved FGD SBR Influent, Day 3 8/26/2010 

71848 1008250-03 Aqueous FGD SBR Influent , Day 4 8/27/2010 

71848 1008250-04 Aqueous Dissolved FGD SBR Influent , Day 4 8/27/2010 

71849 1008207-10 Aqueous FGD SBR Effluent, Day 1 8/24/2010 

71849 1008207-11 Aqueous Dissolved FGD SBR Effluent, Day 1 8/24/2010 

71850 1008223-17 Aqueous FGD SBR Effluent, Day 2 8/25/2010 

71850 1008223-18 Aqueous Dissolved FGD SBR Effluent, Day 2 8/25/2010 

1
Table 1. EPA Episode 6562 Total & Dissolved Mercury – Sample Identification 

EPA Lab Sample Sample Sampling 

Sample # ID # Matrix Sample Description Date 

71851 1008240-13 Aqueous FGD SBR Effluent, Day 3 8/26/2010 

71851 1008240-14 Aqueous Dissolved FGD SBR Effluent, Day 3 8/26/2010 

71852 1008250-05 Aqueous FGD SBR Effluent , Day 4 8/27/2010 

71852 1008250-06 Aqueous Dissolved FGD SBR Effluent , Day 4 8/27/2010 

71853 1008240-15 Aqueous FGD SBR Influent - Duplicate 8/26/2010 

71853 1008240-16 Aqueous Dissolved FGD SBR Influent - Duplicate 8/26/2010 

71854 1008223-19 Aqueous FGD SBR Effluent Duplicate, Day 2 8/25/2010 

71854 1008223-20 Aqueous Dissolved FGD SBR Effluent Duplicate, Day 2 8/25/2010 

71855 1008203-03 Aqueous FGD Influent Field Blank, Day 1 8/23/2010 

71856 1008203-06 Aqueous FGD SBR Influent Field Blank, Day 1 8/23/2010 

71857 1008207-12 Aqueous FGD SBR Influent Field Blank, Day 2 8/24/2010 

71858 1008223-11 Aqueous FGD SBR Influent Field Blank, Day 3 8/25/2010 

71859 1008240-07 Aqueous FGD SBR Influent Field Blank, Day 4 8/26/2010 

71860 1008203-09 Aqueous FGD SBR Effluent Field Blank, Day 1 8/23/2010 

71861 1008207-19 Aqueous FGD SBR Effluent Field Blank, Day 2 8/24/2010 

71862 1008223-12 Aqueous FGD SBR Effluent Field Blank, Day 3 8/25/2010 

71863 1008240-08 Aqueous FGD SBR Effluent Field Blank, Day 4 8/26/2010 

SUMMARY 

The samples were prepared according to EPA Method 1631E to be analyzed by CVAFS. 

There were no findings from the data review that required additional qualifiers in this 

dataset. 

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. 

2
3

BLANKS 

All instrument and preparation blanks met method-specified criteria. Preparation Blanks 

F009230-BLK1, F009230-BLK2, F009252-BLK5, F009277-BLK1, F009277-BLK3, 

F009277-BLK4 and F009277-BLK5 had mercury levels greater than or equal to the 

MDL but less than the reporting limit and these were appropriately flagged with the “J” 

qualifier. No additional qualifiers were required. 

DUPLICATES 

Field duplicates, samples 71854 and 71853, were collected on samples 71850 and 71847, 

respectively. The 71850/71854 relative percent difference (RPD) was 17.4% for total 

mercury and 26.3% for dissolved mercury. The 71847/71853 RPD was 3.8% for total 

mercury and 154% for dissolved mercury. The method-suggested RPD criteria between 

field duplicates is 20%. 

Laboratory duplicates were performed in this episode on samples 71848, 71846, and 

71847. All RPDs were less than 20% (the method-suggested RPD criterion between field 

duplicates; the method does not require the analysis of laboratory duplicates). 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES 

Matrix spikes (MS) and matrix spike duplicates (MSD) were performed on samples 

71846, 71844, 71847, 71851 and 71848 for the total mercury analyses. MS and MSDs 

were performed on samples 71851 and 71848 for the dissolved mercury analyses. All 

aqueous MS/MSD recoveries were within the method specifications of 71-125%, except 

for the dissolved mercury MSD for sample 71851, which had a recovery of 60.1%. 

Therefore, the dissolved mercury result for sample 71851 was flagged with the 

laboratory’s QM-07 qualifier. All RPDs met method-specified criteria. 
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 6562

Test America generated analytical data for total and dissolved metals (antimony, arsenic, 

cadmium, chromium, copper, lead, nickel, selenium, silver, thallium, and vanadium).The 

samples were analyzed according to EPA Method 200.8. 

Table 1 summarizes the samples Test America extracted and analyzed for total and 

dissolved metals by EPA Method 200.8.

Table 1. EPA Episode 6562 Total & Dissolved Metals – Sample Identification 

EPA 

Sample 

# 

EPA Sample 

Description 

Lab 

Sample ID 

# 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71841 FGD Influent, Day 1 280-6658-1 Aqueous 8/23/2010 8/24/2010 

71842 FGD Influent, Day 2 280-6685-1 Aqueous 8/24/2010 8/25/2010 

71843 FGD Influent, Day 3 280-6742-1 Aqueous 8/25/2010 8/26/2010 

71844 FGD Influent, Day 4 280-6791-1 Aqueous 8/26/2010 8/27/2010 

71845 FGD SBR Influent, Day 1 280-6685-2 Aqueous 8/24/2010 8/25/2010 

71846 FGD SBR Influent, Day 2 280-6742-2 Aqueous 8/25/2010 8/26/2010 

71847 FGD SBR Influent, Day 3 280-6791-2 Aqueous 8/26/2010 8/27/2010 

71848 FGD SBR Influent, Day 4 280-6827-1 Aqueous 8/27/2010 8/28/2010 

71849 FGD SBR Effluent, Day 1 280-6685-3 Aqueous 8/24/2010 8/25/2010 

71850 FGD SBR Effluent, Day 2 280-6742-3 Aqueous 8/25/2010 8/26/2010 

71851 FGD SBR Effluent, Day 3 280-6791-3 Aqueous 8/26/2010 8/27/2010 

71852 FGD SBR Effluent, Day 4 280-6827-2 Aqueous 8/27/2010 8/28/2010 

71853 

FGD SBR Influent -

Duplicate, Day 3 280-6791-4 Aqueous 8/26/2010 8/27/2010 

71854 

FGD SBR Effluent -

Duplicate, Day 2 280-6742-4 Aqueous 8/25/2010 8/26/2010 

71855 

FGD Influent Field Blank, 

Day 1 280-6658-2 Aqueous 8/23/2010 8/24/2010 

71856 

FGD SBR Influent Field 

Blank, Day 1 280-6685-4 Aqueous 8/24/2010 8/25/2010 
2

Table 1. EPA Episode 6562 Total & Dissolved Metals – Sample Identification 

EPA 

Sample 

# 

EPA Sample 

Description 

Lab 

Sample ID 

# 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71860 

FGD SBR Effluent Field 

Blank, Day 1 280-6685-5 Aqueous 8/24/2010 8/25/2010 

SUMMARY 

The samples were prepared for total and dissolved metals analysis according to Test 

America’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. No additional data qualifiers were required. 

• All matrix spike (MS) and matrix spike duplicates (MSD) for total and dissolved 

silver failed the 70-130% control limits with poor recoveries. The poor recoveries 

are probably due to high sulfates in this episode’s samples that could form 

insoluble silver sulfide and/or silver sulfate. 

INTERNAL STANDARDIZATION 

All internal standards used by TestAmerica were within the method criteria. 

INITIAL CALIBRATION 

Test America 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 (ICV/CCV) 

The initial calibration verifications (ICV) and continuing calibration verifications (CCV) 

performed by TestAmerica all had recoveries within the method criteria. 

METHOD/INSTRUMENT BLANKS 

All the method blanks were less than the reporting limit. No additional qualifiers were 

required for method blanks. 

All instrument blanks (ICB and CCB) were less than the reporting limit. 
3

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

All CRI samples passed Test America’s 50–150% recovery limits. 

LABORATORY CONTROL SAMPLES (LCS) 

All LCS samples passed the method limits of 85–115%. 

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION (ICSA) 

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 280-29239 and 280-29244. 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 (SRD) 

The serial dilution performed for the total and dissolved sample 71851 FGD SBR 

Effluent, Day 3 (280-6791-3) met Test America’s requirement of ±10% difference. 

FIELD DUPLICATES 

The relative percent difference (RPD) of the field duplicates (71850/71854 & 

71847/71853) were less than ±20% for all values equal to or greater than the reporting 

limit. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES 

MS and MSDs were performed on the total and dissolved samples of 71848 and 71851. 

Many spikes that failed outside of the 70–130% method control limits were flagged with 

a “4” qualifier indicating concentrations in the parent samples were greater than 4 times 

the spike amounts. All MS/MSDs for total and dissolved silver failed the 70–130% 

control limits. The poor recoveries of Silver are probably due to high sulfates (1600–1800 

mg/L) in this episode’s samples that could form insoluble silver sulfide and/or silver 

sulfate. Otherwise, all MS/MSDs were within the 70–130% method control limits. The 

RPD for all MS/MSD passed the method-specified criteria of 20 percent, except for total 

silver for sample 71748 MS/MSD analyses, which had an RPD of 96%. 
4

POST DIGESITON SPIKES 

The post digestion spike performed on sample 71851 FGD SBR Effluent, Day 3 (280-

6791-3) for total and dissolved analytes passed TestAmerica’s 85–115% control limits 

with the exception of silver. The poor recoveries of silver are probably due to high 

sulfates (1600–1800 mg/L) in this episode’s samples that could form insoluble silver 

sulfide and/or silver sulfate. 

DETECTION LIMITS 

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water. 
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 6562

Test America generated analytical data for total and dissolved metals (aluminum, boron, 

barium, beryllium, calcium, cobalt, iron, magnesium, manganese, molybdenum, sodium, 

tin, titanium, and zinc). The samples were analyzed according to EPA Method 200.7. 

Table 1 summarizes the samples Test America extracted and analyzed for total and 

dissolved metals by EPA Method 200.7. 

Table 1. EPA Episode 6562 Total & Dissolved Metals – Sample Identification 

EPA 

Sample 

# 

EPA Sample 

Description 

Lab 

Sample ID 

# 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71841 FGD Influent, Day 1 280-6658-1 Aqueous 8/23/2010 8/24/2010 

71842 FGD Influent, Day 2 280-6685-1 Aqueous 8/24/2010 8/25/2010 

71843 FGD Influent, Day 3 280-6742-1 Aqueous 8/25/2010 8/26/2010 

71844 FGD Influent, Day 4 280-6791-1 Aqueous 8/26/2010 8/27/2010 

71845 FGD SBR Influent, Day 1 280-6685-2 Aqueous 8/24/2010 8/25/2010 

71846 FGD SBR Influent, Day 2 280-6742-2 Aqueous 8/25/2010 8/26/2010 

71847 FGD SBR Influent, Day 3 280-6791-2 Aqueous 8/26/2010 8/27/2010 

71848 FGD SBR Influent, Day 4 280-6827-1 Aqueous 8/27/2010 8/28/2010 

71849 FGD SBR Effluent, Day 1 280-6685-3 Aqueous 8/24/2010 8/25/2010 

71850 FGD SBR Effluent, Day 2 280-6742-3 Aqueous 8/25/2010 8/26/2010 

71851 FGD SBR Effluent, Day 3 280-6791-3 Aqueous 8/26/2010 8/27/2010 

71852 FGD SBR Effluent, Day 4 280-6827-2 Aqueous 8/27/2010 8/28/2010 

71853 FGD SBR Influent - 

Duplicate, Day 3 

280-6791-4 Aqueous 8/26/2010 8/27/2010 

71854 FGD SBR Effluent -

Duplicate, Day 2 

280-6742-4 Aqueous 8/25/2010 8/26/2010 

71855 FGD Influent Field Blank, 

Day 1 

280-6658-2 Aqueous 8/23/2010 8/24/2010 

1
Table 1. EPA Episode 6562 Total & Dissolved Metals – Sample Identification 

EPA 

Sample 

# 

EPA Sample 

Description 

Lab 

Sample ID 

# 

Sample 

Matrix 

Sampling Receipt 

Date Date 

71856 FGD SBR Influent Field 

Blank, Day 1 

280-6685-4 Aqueous 8/24/2010 8/25/2010 

71860 FGD SBR Effluent Field 

Blank, Day 1 

280-6685-5 Aqueous 8/24/2010 8/25/2010 

SUMMARY 

The samples were prepared for total and dissolved metals analysis according to Test 

America’s SOP for ICP Analysis for Trace Metals by Method 200.7. 

There were no findings from the data review that required additional qualifiers (excluding 

those identified by the laboratory) in this dataset. 

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 for 

the ISTD recoveries within 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 

Test America 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 

The initial calibration verifications (ICV) and continuing calibration verifications (CCV) 

performed by TestAmerica all had recoveries within the method criteria. 

METHOD/INSTRUMENT BLANKS 

All the method blanks were less than the reporting limit; however, some had levels above 

the MDL and were flagged with the “J” qualifier. 

All instrument blanks (ICB and CCB) were less than the reporting limit; however, some 

elements were above the MDL and were flagged with the “J” qualifier. 

2
3

LABORATORY CONTROL SAMPLES (LCS) 

All LCSs passed the method control limits of 85–115%. 

INTERFERENCE CHECK SOLUTIONS 

Interference checks were performed using the synthetic matrix as the check solution. All 

data quality objectives met TestAmerica’s SOP criteria. 

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

All CRI samples passed Test America’s SOP control limits of 50–150%. 

FIELD DUPLICATES 

The total and dissolved relative percent differences (RPDs) of the field duplicates (71854 

and 71853) to parent samples (71850 and 71847, respectively) were less than 20% for 

values greater than the reporting limit. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

Matrix spikes (MS) and matrix spike duplicates (MSD) were performed on the total and 

dissolved samples of 71848 and 71851. Some elements with high concentrations 

frequently failed the EPA 200.7 Method spike recovery control limits of 70–130% but 

were flagged with a “4” qualifier indicating that the concentration in the parent sample 

was greater than 4 times the spike and could not be reliably calculated. No MS/MSD 

spike recoveries failed the EPA 200.7 Method control limits of 70–130%, except those 

already qualified with a “4” as mentioned above, and therefore no additional data 

qualifiers were needed. In addition, all RPDs of the MS/MSDs were within 

TestAmerica’s ± 20% requirements. 

SERIAL DILUTION (SRD) 

Serial dilutions were performed for each batch of total and dissolved samples. All serial 

dilution percent differences were less than 10% as required by Test America’s SOP. 

POST DIGESTION SPIKE 

Both total and dissolved post digestion spike samples performed passed the method 

criteria of 85–115%. 

DETECTION LIMITS 

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water. 
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 

6562

Frontier Global Sciences (FGS) generated analytical data for dissolved hexavalent 

chromium for Sample Episode 6562. 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 6562 Dissolved Hexavalent Chromium – Sample Identification 

EPA 

Sample 

# 

Sample 

Matrix Sample Description 

Sampling 

Date Analysis Date 

71841 Aqueous FGD Influent Day 1 8/2/10 8/9/10 

71842 Aqueous FGD Influent Day 2 8/3/10 8/9/10

71843 Aqueous FGD Influent Day 3 8/4/10 8/9/10

71844 Aqueous FGD Influent Day 4 8/5/10 8/30/10

71845 Aqueous FGD Bioreactor Influent Day 1 8/3/10 8/9/10

71846 Aqueous FGD Bioreactor Influent Day 2 8/4/10 8/9/10

71847 Aqueous FGD Bioreactor Influent Day 3 8/5/10 8/30/10

71848 Aqueous FGD Bioreactor Influent Day 4 8/6/10 8/30/10

71849 Aqueous FGD Bioreactor Effluent Day 1 8/3/10 8/9/10

71850 Aqueous FGD Bioreactor Effluent Day 2 8/4/10 8/30/10

71851 Aqueous FGD Bioreactor Effluent Day 3 8/5/10 8/30/10

71852 Aqueous FGD Bioreactor Effluent Day 4 8/6/10 8/30/10

71853 Aqueous FGD Bioreactor Influent Dup Day 3 8/5/10 8/30/10

71854 Aqueous FGD Bioreactor Effluent Dup Day 2 8/4/10 8/30/10

71855 Aqueous FGD Influent Field Blank Day 1 8/2/10 8/9/10

71856 Aqueous FGD Bioreactor Influent Field Blank Day 1 8/3/10 8/9/10

71860 Aqueous FGD Bioreactor Effluent Field Blank Day 1 8/3/10 8/9/10

1
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. 

Several samples (71841, 71842, 71843, 71844, 71845, 71846, 71847, 71848, 71849, 

71850, 71851, 71852, 71853, and 71854) were diluted prior to analysis due to the 

presence of high levels of nontarget chloride interferences. 

There were no issues requiring additional data qualifiers for the hexavalent chromium 

data in this episode. 

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES 

There were no sample receipt issues in this data package. 

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 95 to 107%. 

BLANK 

All of the preparation blanks/laboratory reagent blanks (LRBs) and the continuing 

calibration blanks (CCBs) met method-specified requirements. 

2
3

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 97.9% and 102%. A second set of LFB/LFBD, for the later analysis date, 

had recoveries of 100% and 95.5%. The method suggested that a second source quality 

control sample (QCS) must be analyzed by the laboratory at least once a quarter. The 

second source ICV meets this recommendation. 

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). 

Two field duplicates were collected and analyzed. Sample 71854 was a duplicate of 

effluent sample 71850. These samples were nondetects (NDs), indicating the analyte was 

not detected at or above the method detection limit. Sample 71853 was a duplicate of 

influent sample 71847. These samples were also NDs. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES 

The MS and matrix spike duplicate (MSD) were performed using a secondary source 

spike on samples 71844, 71848, and 71851. All MS/MSD recoveries were within 75%-

125%, with RPDs of 0.461%, 0.274%, and 4.03%, respectively.
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 6562 

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for Sample Episode 6562. 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 by SM 4500 CN- E, 

 Nitrate/Nitrite by EPA method 353.2, 

 Phosphorus by EPA method 365.1, 

 Total Dissolved Solids (TDS) by SM 2540C, 

 Total Kjeldahl Nitrogen (TKN) by EPA method 351.2, and 

 Total Suspended Solids (TSS) by SM 2540D. 

Table 1 summarizes the 14 samples that TestAmerica analyzed for the above analytes. 

Table 1. EPA Episode 6562 Classical Analytes – Sample Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71841 Water FGD Influent, Day 1 8/23/10 

71842 Water FGD Influent, Day 2 8/24/10 

71843 Water FGD Influent, Day 3 8/25/10 

71844 Water FGD Influent, Day 4 8/26/10 

71845 Water FGD SBR Influent, Day 1 8/24/10 

71846 Water FGD SBR Influent, Day 2 8/25/10 

71847 Water FGD SBR Influent, Day 3 8/26/10 

71848 Water FGD SBR Influent, Day 4 8/27/10 

71849 Water FGD SBR Effluent, Day 1 8/24/10 

71850 Water FGD SBR Effluent, Day 2 8/25/10 

71851 Water FGD SBR Effluent, Day 3 8/26/10 

1 
Table 1. EPA Episode 6562 Classical Analytes – Sample Identification 

EPA 

Sample # 

Sample 

Matrix 

Sampling 

Sample Description Date 

71852 Water FGD SBR Effluent, Day 4 8/27/10 

71853 Water FGD SBR Influent - Duplicate 8/26/10 

71854 Water FGD SBR Effluent - Duplicate 8/25/10 

SUMMARY 

All samples were analyzed within the holding time specified in 40 CFR 136 Table II. All 

samples were preserved appropriately. 

 

Two field duplicate samples were 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 otherwise noted below. Additionally, unless otherwise noted, 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 unless specified 

below. 

If required by the method, a matrix spike (MS) sample was analyzed on samples 71848 

(FGD bioreactor influent) and 71851 (FGD bioreactor 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. 

DATA NOTES/ISSUES 

Ammonia 

The MS and MSD results for sample 71841 were above the calibration range. Because 

the percent recoveries were within the control limits specified by EPA method 350.1, the 

laboratory did not reanalyze the samples using a higher dilution factor. If reported, the 

MS and MSD results will be qualified as estimated values. The result for sample 71841 

2 
was within the calibration range, so this sample was not qualified. The LFB associated 

with this sample met the method criteria. 

BOD5 

The data reviewer identified no issues. All glucose-glutamic acid standards, water blanks, 

and laboratory duplicates were analyzed appropriately and met the criteria specified in 

SM 5210B. 

Chloride and Sulfate 

The MS and MSD results for samples 71848 and 71851 for sulfate and chloride were 

above the calibration curve. TestAmerica did not reanalyze the samples with a higher 

dilution factor because the percent recoveries were within EPA method 300.0 control 

limits. If reported, these MS and MSD results will be qualified as estimated values. The 

LFB associated with this sample met the method criteria. 

COD 

The RPD between sample 71847 and its field duplicate 71853 was 37.0%. 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 EPA method 410.4. 

The percent recoveries for the MS and MSD analyses for sample 71848 (FGD SBR 

influent) and 71851 (FGD SBR effluent) were below the control limits of 90-110% 

required by EPA method 410.4. The percent recoveries for the MS and MSD analyses for 

sample 71848 were 71% and 72%, respectively, and the percent recoveries for the MS 

and MSD analyses for sample 71851 were 75% and 76%, respectively. These low percent 

recoveries suggest that results for samples with a similar matrix (FGD SBR influent and 

FGD SBR effluent) could be biased low. Samples 71848 and 71851 were qualified as 

minimum values. The LFB percent recoveries associated with all samples met the method 

criteria. 

Cyanide 

Sample 71841 was preserved to a pH greater than 10 S.U. after sample collection, but 

when the laboratory received the sample, the pH was neutral. The laboratory added more 

NaOH to increase the pH to greater than 10 S.U. upon receipt. This sample was qualified 

as an estimated value. 

Cyanide was detected at 0.00273 mg/L in the laboratory reagent blank (LRB) associated 

with samples 71841, 71842, 71845, and 71849 and also detected at 0.00274 mg/L in the 

LRB associated with samples 71843, 71846, 71850, and 71854. Additionally, cyanide 

was detected at 0.00586 mg/L in the LRB associated with samples 71844, 71847, 71848, 

71851, 71852, and 71853. These blank results were greater than the MDL (0.0020 mg/L), 

3 
but less than the RL (0.010 mg/L). Because all of the blank results were less than the RL, 

no samples were qualified based on these LRB results. 

Results for the following samples were less than the lowest calibration standard (0.01 

mg/L): 71850, 71851, 71852, and 71854. Because all of these samples were already 

flagged by TestAmerica with a “J”, meaning the sample result was an estimated value 

because it was less than the RL, no further qualification was necessary. 

The percent recoveries for the MS and MSD analyses of sample 71851 were both 22%. 

The laboratory spiked the sample with 0.100 mg/L. The percent recoveries of both the 

MS and MSD samples were outside of the laboratory control criteria of 90-110%. 

However, because there are no criteria for MS/MSD analyses specified in SM 4500 CNE and sample 71851 was already qualified with a “J” meaning the result was less than the 

RL, further qualification was unnecessary. 

The RPD between sample 71847 and its field duplicate 71853 was 26.9%. Even though 

this RPD was greater than 20%, the samples were not qualified because there are no 

specific control limits for field duplicates specified in SM 4500 CN- E. 

Nitrate/Nitrite 

The MS and MSD results for 71841 were above the calibration curve. Because the 

percent recoveries were within the control limits specified by EPA method 353.2, the 

laboratory did not reanalyze the samples using a higher dilution factor. If reported, the 

MS and MSD results will be qualified as estimated values. The result for sample 71841 

was within the calibration range, so this sample was not qualified. The LFB associated 

with this sample met the method criteria. 

Phosphorus 

The percent recoveries for the MS/MSD analysis of sample 71851 were not within the 

control limits of 90-110% specified in EPA Method 365.1, but were within the laboratory 

control limits of 71-128%. The percent recoveries of the MS and MSD samples were 

83% and 86%, respectively. Sample 71851 was qualified by the laboratory with a “J” 

meaning the result was less than the RL, so no further qualification was necessary. The 

LRB percent recovery met the method criteria. 

Samples 71842, 71845, 71846, 71849, 71850, 71851, and 71854 were less than the 

lowest calibration standard (0.025 mg/L). TestAmerica flagged these samples with a “J”, 

so further qualification was not necessary. 

The RPD between sample 71847 and its field duplicate 71853 for phosphorus was 22.2%. 

The result for sample 71853 was greater than the MDL, but less than the RL and the 

result for sample 71847 was the RL itself. The low concentrations of these samples might 

be the reason for the high RPD. Even though the RPD was greater than 20%, the sample 

4 
was not qualified because there are no specific control limits for field duplicates specified 

in EPA Method 365.1. 

TDS 

Constant weight was not achieved after 3 drying cycles for samples 71843, 71844, 71845, 

71846, 71847, 71848, 71849, 71850, 71851, 71852, 71853, and 71854 in analytical batch 

29115. It should be noted that the weight increased from the first weighing to the second 

weighing for all samples. Method 2540C warns that samples which 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. This was likely the cause for the inconsistent weight calculations. The samples 

were not qualified, but results may be biased high. 

The RPDs for laboratory duplicates from samples 71842 and 71848 were less than 10% 

as required by SM 2540C; however, the RPD for sample 71844 was 14%. Because the 

RPD was greater than the method control limits, sample 71844 was qualified as an 

estimated value. 

TDS was detected above the MDL (4.7 mg/L), but below the RL (10 mg/L) at 7.0 mg/L 

in the method blank (MB) associated with sample 71841. Because the blank result was 

less than the RL, no samples were qualified. 

TKN 

The percent recovery for the LFB associated with sample 71841 was not within the 

method control limits of 90-110%, but was within the laboratory control limits of 77-

115%. The percent recoveries for the LFB and LFBD were 89% and 90%, respectively. 

Because the percent recovery of the LFB was below the method criteria, sample 71841 

was qualified as a minimum value. 

TestAmerica performed MS and MSD analyses on sample 71851. The percent recoveries 

for the MS and MSD samples were 114% and 113%, respectively. The samples did not 

meet the method control limits of 90-110%, but did meet the laboratory control limits of 

54-131%. The LFB associated with this batch was within the laboratory control limits. 

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. Sample 71851 was not qualified because it is not possible to 

determine if the MS/MSD failure was a result of matrix interferences or caused by low 

spiking level. 

TKN was detected at 0.237 mg/L in the laboratory reagent blank associated with samples 

71842 - 71854. The blank result was greater than the MDL (0.077 mg/L), but less than 

the RL (1.0 mg/L). Because the blank result was less than the RL, it was not necessary to 

qualify any samples. 

5 
6 

TSS 

One laboratory duplicate was analyzed per batch. The RPDs for the laboratory duplicates 

of samples 71841, 71842, 71848, 71851, and 71852 were less than 10% as required by 

the method. However, the RPD for the laboratory duplicate of sample 71854 was 18%. 

Because the laboratory duplicate RPD was greater than the method control criteria, 

sample 71854 was qualified as an estimated value. 

The RPD between sample 71847 and its field duplicate 71853 was 80.9%. The RPD 

between sample 71850 and its field duplicate 71854 was 28.6%. Even though these RPDs 

were greater than 20%, the samples were not qualified because there are no specific 

control limits for field duplicates specified in SM 2540D. 

Table 2. Data Review Summary Table 

Sample Analyte Qualifier/Action Reason Level Detected

71848 COD Minimum Value MS % recovery 

below methodspecified criteria 

130 mg/L 

71851 COD Minimum Value MS % recovery 

below methodspecified criteria 

140 mg/L 

71841 Cyanide Estimated Value pH upon receipt < 

10 S.U. 

1.2 mg/L 

71844 TDS Estimated Value Lab duplicate 

RPD > methodspecified criteria 

11,000 mg/L 

71841 TKN Minimum Value LFB % recovery 

below methodspecified criteria 

130 mg/L 

71854 TSS Estimated Value Lab duplicate 

RPD > methodspecified criteria 

12 mg/L 
Appendix C

PICTURES FROM THE SAMPLING EPISODE
C-1

Figure C-1. Sampler Working Inside a “Cleanbox”
C-2

Figure C-2. Sample Set Up at the Influent to the FGD Wastewater Treatment System
C-3

Figure C-3. Composite Sample Collection Set Up at the Influent to the SBR System
C-4

Figure C-4. Composite Sample Collection Set Up at the Effluent from the SBR 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. 
D-3 

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 

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 
D-4 

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 

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. 
D-6 

6.2 Supplies 

 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 
D-7 

standards are diluted to working levels using 2% nitric acid and 0.5% 

HCl acid matrix. Suggested concentrations are given in Attachment 8, 

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 
D-8 

prepared in 2% HNO3 and 0.5 % HCl acid to the concentrations shown 

in Attachment 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 
D-9 

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 

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 
D-10 

single element standard at the desired linear range. The result of the analysis 

must be within 10% of the true value. 

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. 
D-11 

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 

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. 
D-12 

10.2.4 Spike the LCS and MS/MSD samples per spiking protocols. 

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). 
D-13 

Acceptance Criteria: The ICV recovery must be within 90-110%. 

Additionally, the internal standard recoveries for 

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. 
D-14 

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. 

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) 
D-15 

CCV 

CCB 

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: 

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 

DU1 = Sample result 

DU2 = Sample duplicate result 

11.6 The final concentration for an aqueous sample is calculated as follows:

2

1 Result ( g/L) VC 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. 
D-17 

 Analyze the IDL blanks on three non-consecutive days. 

 The IDL is equal to three times the standard deviation of the blank results.

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. 
D-18 

15.2 EPA Method 1638, “Determination of Trace Elements in Ambient Waters by 

Inductively Coupled Plasma – Mass Spectrometry, January 1996 

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. 

####