Appendix C

Duke Energy’s Miami Fort Station
Section 1 

CWA 308 Monitoring Letter and Instructions 



Enclosure 1 

Instructions for Sample Collection, Packaging, and Shipment

EPA Sampling Program

The samples you will be collecting are very important. The samples will be used by the 

U.S. Environmental Protection Agency (EPA) for revising the effluent limitations 

guidelines and standards for the Steam Electric Power Generating Industry. 

These instructions are being provided to Duke Energy’s Miami Fort Station to aid in 

collecting, packaging, and shipping samples for this sampling program. 

The plant must collect grab samples for all analytes at the influent to the FGD wastewater 

treatment sampling point and 24-hour composite samples for all analytes except mercury 

and cyanide at the effluent from the FGD wastewater treatment sampling point. At the 

FGD wastewater treatment effluent, the plant must collect cyanide as a single grab 

sample and mercury must be collected as four individual grab samples over the 24-hour 

period (i.e., a grab sample collected every six hours).

Samples will be collected once a month for four months. The samples should be 

collected and shipped to the laboratories according to the schedule provided in the cover 

letter of this request. If the plant has any questions regarding the timeline or the steps 

provided, please contact Mr. Ronald Jordan at (202) 566-1003 or jordan.ronald@epa.gov. 

Equipment Needed

The plant will need to obtain the following equipment to collect, pack, and ship the 

samples to the laboratories: 

• Sample bottles, composite containers, and tubing sets (specially-cleaned 

according to EPA Method 1669); 

• Automatic compositor; 

• Powder-free gloves; 

• Tyvek® coveralls or suitable alternative; 

• Dust masks (for use while collecting mercury samples) 

• Labels (for sample bottles and shipping samples to laboratories); 

• Preservation supplies (see the “Sample Bottles and Preservation” Section); 

• Coolers; 

• Garbage bags; 

• Packing material; 

• Strapping tape; and 

• Traffic Report (will be provided by ERG). 
Sampling Points

The plant must collect samples once per month for four months, based on the schedule 

specified in the letter. Samples are to be collected from each of the two sampling points 

included in the EPA’s sampling episode. Figure 1 identifies each of the sampling points 

for this sampling program. The following is a description of the two sampling points: 

• FGD wastewater treatment influent (FGD scrubber purge) (SP-1): This 

sampling point shall represent the FGD purge stream (e.g., hydroclone overflow) 

transferred to the FGD wastewater treatment system prior to any commingling 

with other wastewaters or treatment system recycle streams. This sample should 

be collected from the sample tap on the pipe that flows from the secondary 

hydroclone overflow to the equalization tank, which is located on top of the 

equalization tank. NOTE: the plant must collect secondary hydroclone overflow 

from Unit 7 for two of the sample sets and secondary hydroclone overflow from 

Unit 8 for two of the sample sets. 

• FGD wastewater treatment effluent (SP-2): This sampling point shall represent 

the effluent from the FGD wastewater treatment system, prior to mixing with 

dilution water or other streams. This sampling point should be collected from 

sample tap that is located on the suction side of the pump that transfers the 

wastewater from the effluent tank to the ash pond. 

Analytes

The analytes included in this sampling program include all analytes from EPA’s sampling 

program, except for the dissolved metals analyses (which includes hexavalent 

chromium). Table 1 contains the listing of all the analytes included in the monitoring 

program, as well as the analytical methods that will be used to analyze the samples. 
Table 1. Analytes and Analytical Methods Included in the Monitoring Program 

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 Metals

Total mercury EPA 1631E 

Antimony, arsenic, cadmium, chromium, copper, lead, nickel, 

selenium, silver, thallium, vanadium, and zinc 

EPA 200.8 with collision 

cell 

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

magnesium, manganese, molybdenum, sodium, tin, and titanium 

EPA 200.7 

 
Due to a confidentiality claim, the Miami Fort FGD Wastewater Treatment diagram cannot be 

Figure 1. Miami Fort FGD Wastewater Treatment System Monitoring Program Sampling 
Sample Bottles and Preservation

Table 2 identifies the sample bottles that are needed for collecting samples. The table 

also identifies the on-site preservation that is required for the samples. Please note that 

the number of sample bottles listed in Table 2 refers to the number of bottles that will 

need to be collected from each sampling point for each of the four sets of samples. For 

the Group II samples, the plant can either preserve the samples with sulfuric acid after 

sample collection, or the plant can order pre-preserved sample bottles. 

For the total cyanide samples, the plant should test the wastewater from the sampling 

points with lead acetate paper (turns black in the presence of sulfide) and potassium 

iodide starch paper (turns blue/violet in the presence of chlorine). If sulfide is present, 

the plant will need to dilute the sample with blank water until the sulfide is not detected 

by the lead acetate paper. If chlorine is present, then the plant will need to add sodium 

arsenite until the chlorine is not detected by the potassium iodide starch paper. After any 

dilution and/or sodium arsenite is added to the sample, the plant will need to preserve the 

sample with sodium hydroxide until the sample reaches a pH of 10 S.U. Please see 

ASTM Method D 7365-09a for more details on the preservation requirements for total 

cyanide. 

Table 2. Summary of Sample Container and Planned Preservation 

Parameter 

Sample Container 

and Volume On-Site Preservation 

BOD5 One 1-L HDPE 

bottle 

≤6°C 

Group I a One 1-L HDPE 

bottle 

≤6°C 

Group II b Two 1-L HDPE 

bottles 

H2SO4 to pH <2, ≤6°C 

Total cyanide One 1-L HDPE 

bottle 

Dilution until sulfide is not detected, 

NaAsO2 until total chlorine is not 

present, NaOH to pH >10, ≤6°C 

Total metals (EPA Method 200.8 with 

collision cell) 

One 500-mL HDPE 

bottle 

None 

(acid preserve at laboratory) 

Total metals (EPA Method 200.7) One 500-mL HDPE 

bottle 

None 

(acid preserve at laboratory) 

Total mercury: 

Laboratory composite grab samples at FGD 

wastewater treatment effluent 

Four 125-mL glass 

bottles 

Influent samples and field blank samples Two 250-mL glass 

bottles 

None 

(acid preserve at laboratory) 

(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. 

NOTE: The number of sample bottles refers to the number of sample bottles needed for each sampling point for each of

the four sets of samples. 
Sample Labeling

Label each bottle prior to collecting the sample so it can be identified by the laboratory. 

Each self-adhesive label must be completed in indelible ink and must contain the 

following information: 

• Sample number (see Table 3); 

• Sampling episode number (see Table 3); 

• Sampling point/description (see Table 3); 

• Date of sample collection; 

• Analysis to be performed; 

• Sample bottle type; and 

• Required on-site preservation. 

If any of the information is incorrect, the plant must revise the label using indelible ink. 

Once applied to the sample container, the plant must cover the labels with clear tape to 

prevent tampering, abrasion, smearing, or loss during transit. For metal and mercury 

samples, do not place labels directly on the sample bottles because of the potential for 

contamination. Instead, place the label on the outer plastic bag of the sample bottle. To 

ensure that the sample label does not become separated from the bottle, the doublebagged sample bottle should be placed in an additional Ziploc bag after collection. 

Table 3 provides the sampling point descriptions, sample numbers, and sampling episode 

number for the plant for this monitoring program. The information in the table should be 

provided on the sample bottle labels for the appropriate bottles. The “analysis to be 

performed” should be shown on the label as the following, depending on the specific 

analysis: 

• BOD; 

• Group I; 

• Group II; 

• Total Cyanide; 

• Total Metals – 200.8 w/ CC; 

• Total Metals – 200.7; 

• Total Mercury (for influent and field blank samples); 

• Total Mercury – Grab 1 (for FGD wastewater treatment effluent 

laboratory composite samples. The bottles should be labeled as Grab 1, 

Grab 2, Grab 3, and Grab 4 for the four respective collection times). 

The “sample bottle type” should be shown on the label the same as the “Sample 

Container and Volume” column in Table 2, except that the quantity should not be 

included. For example, for total mercury, the “sample bottle type” should be “250-mL 

glass bottle.” The “required on-site preservation” should be shown on the label the same 

as the “On-Site Preservation” column in Table 2, except that “(acid preserve at 

laboratory)” does not need to be included for the total metals and total mercury sample 

bottles. 
Table 3. Sampling Point Descriptions and Sample Numbers for Monitoring 

Program 

 

Sampling Point Description Sample Number Sampling Episode Number

FGD Wastewater Treatment Influent – Set 1 72091 6567 

FGD Wastewater Treatment Influent – Set 2 72092 6567 

FGD Wastewater Treatment Influent – Set 3 72093 6567 

FGD Wastewater Treatment Influent – Set 4 72094 6567 

FGD Wastewater Treatment Effluent – Set 1 72095 6567 

FGD Wastewater Treatment Effluent – Set 2 72096 6567 

FGD Wastewater Treatment Effluent – Set 3 72097 6567 

FGD Wastewater Treatment Effluent – Set 4 72098 6567 

FGD Wastewater Treatment Influent Field Blank 72099 6567 

FGD Wastewater Treatment Effluent Field Blank – Set 1 72100 6567 

FGD Wastewater Treatment Effluent Field Blank – Set 2 72101 6567 

FGD Wastewater Treatment Effluent Field Blank – Set 3 72102 6567 

FGD Wastewater Treatment Effluent Field Blank – Set 4 72103 6567 

QC Samples

The plant is required to collect field blank samples as part of the sampling program. The 

field blank samples should be collected at the frequency specified in Table 4. 

Table 4. Field Blank Collection Frequency 

Sampling Point Total Mercury 

Total Metals (200.8 

and 200.7) Classicals1 

FGD Wastewater 

Treatment Influent 

Collected during one 

of the four sets 

Collected during one 

of the four sets 

No field blanks 

required 

FGD Wastewater 

Treatment Effluent 

Collected during all 

four sets 

Collected during all 

four sets 

No field blanks 

required 

1

 Classicals includes the analyses for BOD, Group I, Group II, and total cyanide. 

The laboratory will perform MS/MSD analyses on the total metals and total mercury 

analyses; however, no additional sample volume is required. 

Sample Collection

The plant must use clean sampling techniques when collecting the total metals and total 

mercury samples; therefore, the sampling team should follow the clean hands/dirty hands 

sampling techniques outlined in EPA Method 1669. Additionally, the plant must try to 

avoid significant contamination during sample collection, especially from sources such as 

airborne particles, dirt, and corrosion particulates from piping, railing, etc. 
The plant must collect grab samples for all analytes at the influent to the FGD wastewater 

treatment system. The plant must collect 24-hour composite samples for all analytes 

except cyanide and mercury at the FGD wastewater treatment effluent sampling point. 

The 24-hour composites must be set up to collect equal sample aliquots every hour over 

the 24-hour period. For mercury at the FGD wastewater treatment effluent sampling 

point, the plant must collect four individual grab samples over the 24-hour period (i.e., one 

mercury grab collected every six hours). For cyanide at the FGD wastewater treatment 

effluent sampling point, the plant must collect a single grab sample after the one of the 

mercury grab samples. 

If the plant collects the samples from the same taps used for the collection of samples 

during the EPA sampling episode, the plant can follow the instructions included in the 

sampling plan drafted for the EPA sampling episode to collect the field blank samples, set 

up the composite containers, and perform the composite pump-off procedures for the FGD 

wastewater treatment effluent sampling point. The following instructions can be used to 

collect the grab samples at the influent to the FGD wastewater treatment system sampling 

point and for the mercury and cyanide grab samples at the FGD wastewater treatment 

effluent sampling point: (NOTE: If a sample tap or valve is not available to collect these 

samples or if the FGD wastewater treatment effluent sampling point has intermittent flows 

which may interfere with the automatic composite collection, please contact TJ Finseth, 

(703) 633-1698 to discuss possible alternatives.) 

1. Arrive at the sampling point location and prepare supplies and bottles for 

the sample collection. 

2. Clean hands and dirty hands put on Tyvek® suits, masks, and powder-free 

gloves. 

3. Dirty hands gets a clear plastic bag and opens it slightly (touching only the 

outer part of the bag) so that clean hands can place hands in the bag and 

open the bag completely. 

4. Clean hands then uses the plastic bag to shroud the sample tap (note that 

there should be no flow through the sample tap at this time). Clean hands 

will need to puncture a small hole in the bag using the tap and dirty hands 

can cable tie the bag to the tap to prevent it from falling during sample 

collection. 

5. Dirty hands opens the outer bags of the field blank water and total mercury 

and total metals field blank sample bottles. Clean hands opens the inner 

bag of the field blank water and unscrews the lid. Clean hands then opens 

the inner bag of the total mercury and total metals field blank sample 

bottles. Clean hands pours the blank water into the field blank sample 

bottles under the shrouding, caps the bottles, and closes the inner bags. 

Clean hands then places the total mercury and total metals bottles in the 

outer bags and dirty hands closes the outer bag. 

6. Dirty hands then opens the valve to the sample tap and purges the tap for at 

least two minutes, then keeps the valve open until all samples have been 

collected. 
7. Dirty hands opens the outer bag for the total mercury sample bottle. Clean 

hands takes the sample bottle and inner bag and holds them under the 

shroud. Clean hands then opens the inner bag, opens the lid of the bottle 

and fills the total mercury sample bottle. Clean hands caps the sample 

bottle, closes the inner bag, and places the sample bottle in the outer bag. 

Dirty hands closes the outer bag. The samplers repeat this procedure for 

the collection of the total metals samples (both EPA 200.8 with collision 

cell and EPA 200.7), unless the plant is collecting the metals samples as 

composite samples. 

8. The samplers then collect the BOD, Group I, Group II, and total cyanide 

samples. NOTE: the samplers can collect these samples using the same 

technique as the mercury and metals samples, or they can remove the 

plastic bag shrouding and collect directly from the tap. 

9. The Group II and total cyanide samples must be preserved prior to 

shipment to the laboratories. Use the information provided in the “Sample 

Bottle and Preservation” section of these instruction for the preservation 

steps. Additionally, the BOD, Group I, Group II, and total cyanide samples 

should be placed on ice immediately after sample collection/preservation. 

Sample Packing and Shipment

The following steps should be used when packing and shipping the samples to the 

laboratories. 

1. Make sure that each sample bottle has a label, and that the label correctly 

specifies the sample point. 

2. Tighten the lid on each filled sample bottle, being careful not to 

overtighten the lid. If bottle threads are dirty to where the lid is impeded 

from closing, clean the threads on the bottle being careful to not introduce 

contamination into the sample. Clean the sample bottle with a cloth rag or 

paper towel. 

3. Prior to packaging, place each sample bottle requiring ≤6°C preservation 

into an ice chest with wet ice to cool. 

4. When each sample requiring ≤6°C preservation has reached the desired 

temperature, wrap each glass sample bottle with two layers of “bubble 

wrap” (or place bottle in two “bubble bags”). The bubble wrap must fit 

snugly and completely cover the sample bottle. Enclose each “bubblewrapped” container and plastic container in an individual sealable plastic 

freezer bag. 

5. Place two garbage bags inside each other in each of the coolers used to 

ship samples to the laboratories. 

6. Place the classicals samples in the garbage bags in the coolers with proper 

end up, close the interior garbage bag by tying, or with a twist-tie. 

7. Add ice to the cooler to keep samples cold during shipment. Arrange blue 

ice or sealed plastic freezer bags filled with wet ice on top of the sample 

bottles (if samples require ≤6°C preservation). If using wet ice, place the 
ice inside two one-gallon sealable freezer bags. Put at least 4 × 1⁄2 gallons 

of ice (4 × 2.5 pounds of ice) in each large cooler and 2 × 1⁄2 gallons of ice 

(2 × 2.5 pounds of ice) in each small cooler. Use more ice when ambient 

temperatures are very high. Place the ice inside the second garbage bag. 

8. Close the second garbage bag by tying, or with a twist-tie. 

9. Place the metals samples in the garbage bags in a different cooler with 

proper end up, close the interior garbage bag by tying or with a twist-tie. 

Close the second garbage bag by tying, or with a twist-tie. NOTE: the 

metals samples are not required to be cooled; however, because the metals 

and classicals are being analyzed by the same laboratory, the metals can 

be shipped with the classicals, but the metals samples would need to be 

chilled prior to packing them in the cooler with the classicals and ice 

would need to be added to the cooler between the interior and outer 

garbage bags to keep the samples cold. 

10. Fill in any free space around the bottles in the metals and classicals 

coolers with additional cushioning material. Sufficient packing material 

should be used so that the sample containers will not shift during 

shipment. 

11. Fill out and print a traffic report form for the classicals and metals samples 

(provided electronically by ERG). Seal the last two pages of the traffic 

report form(s) in a plastic envelope secured to the inside of the top of the 

cooler(s). NOTE: the top page of the traffic report must be sent to ERG at 

the following address: 

 Eastern Research Group 

 14555 Avion Parkway, Suite 200 

 Chantilly, VA 20151 

 Attn: TJ Finseth 

 (703) 633-1698 

12. Close the cooler(s). 

13. Place a completed laboratory address label on the lid of the cooler(s). The 

classicals and metals samples should be shipped to TestAmerica as 

follows: 

 TestAmerica 

 4955 Yarrow Street 

 Arvada, CO 80002 

 Attn: Elizabeth Eichelberger 

 (303) 736-0100 

14. Make several wraps with strapping tape around the cooler perpendicular to 

the seal to ensure that the lid will remain closed if the latch is accidentally 

released or damaged. 

15. Place the mercury samples in the garbage bags in a separate cooler with 

proper end up, close the interior garbage bag by tying, or with a twist-tie. 
16. Do not add ice to the mercury cooler, simply close the second garbage bag 

by tying, or with a twist-tie. 

17. Fill in any free space around the bottles with additional cushioning 

material. Sufficient packing material should be used so that the sample 

containers will not shift during shipment. 

18. Fill out and print a traffic report form for the mercury samples (provided 

electronically by ERG). Seal the last two pages of the traffic report form 

in a plastic envelope secured to the inside of the top of the cooler. NOTE: 

the top page of the traffic report must be sent to ERG at the same address 

provided in step 11: 

19. Close the cooler. 

20. Place a completed laboratory address label on the lid of the cooler. The 

mercury samples should be shipped to Frontier as follows:

 Frontier GeoSciences 

 414 Pontius Ave. North 

 Seattle, WA 98109 

 Attn: Patrick Garcia-Strickland 

 (206) 957-1428 

21. Make several wraps with strapping tape around the cooler perpendicular to 

the seal to ensure that the lid will remain closed if the latch is accidentally 

released or damaged. 

22. Fill out the necessary paperwork for FedEx or UPS to prepare the 

shipment for pick up or drop off. NOTE: the samples must be shipped 

priority overnight to arrive at the laboratories the following morning. Ship 

the coolers to the laboratories. 

23. After the coolers have been dropped off (or picked up), please contact TJ 

Finseth at (703) 633-1698, to notify him that the samples have been 

shipped to the laboratories. 

Traffic Reports

An example traffic report will be provided to the plant by ERG for the first sample 

collection event. The plant will need to make changes to the traffic report electronically 

for the other three sample collection events. Some information, such as the date and 

sample collection times must be entered by the plant after the sample collection and 

therefore, will not be included in the example provided by ERG. 

After the traffic report is completed by the plant, the plant must print the four pages in the 

file. The last two pages in the file must be placed in the cooler for shipment to the 

laboratories and the first page must be sent to ERG. The plant can keep the second page 

of the traffic report. 
Engineering Data

The plant must provide engineering data regarding the operation of the plant and FGD 

systems during the sample collection period. Additionally, the plant must make some 

field measurements when samples are collected, including pH, temperature, and visual 

observations, and provide the data to EPA after the sample collection period. The 

engineering data and field measurement data requirements are in an Excel® spreadsheet 

titled “Monitoring Program Engineering Data Tables,” which will be provided by ERG. 

The tables are also included at the end of this enclosure. The plant must complete the 

engineering data sheets and field measurement sheets in the Excel® file and e-mail the 

completed forms to TJ Finseth at thomas.finseth@erg.com. 

Certification Statement 

The individual responsible for directing and supervising the sample collection and the 

engineering data preparation must sign the certification statement (provided in Enclosure 

4) and submit it upon the completion of the sampling program. The signed certification 

statement should be scanned and e-mailed to TJ Finseth at thomas.finseth@erg.com, at 

the same time the engineering data is submitted. 
Complete the following tables for each sampling point

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Sample Collection 

Time Temperature (°C)

pH

(S.U.)

Set 1Set 2Set 3Set 4

Plant Name

Sample 

Collection 

Number

Unit Overflow 

Sampled at 

Influent 

(7 or 8)

Influent Samples 

Collected as Grabs

(Yes or No)

Mercury and Cyanide 

Samples Collected as 

Grabs

(Yes or No)

Effluent Samples 

Collected as 24-

Hour Composites

(Yes or No)

Tyvek Suits 

used

(Yes or No)

Dust Masks 

Used for 

Mercury 

(Yes or No)

Clean Hands/Dirty 

Hands Sampling 

Techniques Used

(Yes or No)

Description of Sample 

Collection Technique (if 

different than 

instructions)

Description of Abnormal 

Conditions in FGD System 

or FGD Wastewater 

Treatment System that May 

Impact Concentrations

Set 1Set 2Set 3Set 4
Complete the following tables based on the plant operating characteristics during each set of samples collected

Units Operating 

During Sampling 

Day

Units Off-line 

Entire 

Sampling Day

SCRs/SNCRs 

Operating on 

Units

Set 1Set 2Set 3Set 4

Flow Rate (gpm) Duration

Set 1Set 2Set 3Set 4

Lime Usage 

(tons)

Ferric Chloride 

Usage 

(Liters/day)

Organosulfide Usage 

(Liters/day)

Polymer Usage 

(Liters/day)

Acid Usage 

(Liters/day)

Chemical 

Precipitation 

System Effluent Flow Rate (gpd)

Set 1Set 2Set 3Set 4

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Plant Operation During Sample Collection

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Plant Operation During Sample Collection

Scrubber Slurry Blowdown Flow 

Rate Scrubber Slurry 

Percent Solids

Percent Hydroclone 

Overflow Recycled 

Back to Scrubber

FGD Wastewater Treatment Operation During Sample Collection

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Scrubber Purge 

Flow Rate During 

Influent Sample 

Collection

(gpm)
Unit 7 Unit 8

Daily Power Generation (MW-hrs)

Plant Name Date

Provide the daily power generation for each scrubbed unit starting two weeks 

prior to the first set of samples through the last set of samples
FGD Wastewater Treatment System Flow 

Rates

(gpd)

Plant Name Date Chemical Precipitation Effluent

Provide the average flow rate in the FGD wastewater treatment system for each stream included in the 

table starting two weeks prior to the first set of samples through the last set of samples
Enclosure 2 

Authority

This request for information is made under authority provided by Section 308 of the Federal 

Water Pollution Control Act, as amended, 33 USC 1318. Section 308 provides that, "Whenever 

required to carry out the objective of this Act, including but not limited to . . . developing or 

assisting in the development of any effluent limitation . . . pretreatment standard, or standard of 

performance under this Act," the Administrator shall require the owner or operator of any point 

source to "establish and maintain such records, . . make such reports, . . install, use, and maintain 

such monitoring equipment . . . sample such effluent . . . and provide such other information as 

he may reasonably require." 

Confidentiality

A business ("you") may not withhold information from EPA on the grounds that it is 

confidential. You may, however, if you desire, assert a business confidentiality claim covering 

part or all of the information that you furnish to EPA. 

EPA regulations concerning confidential business information are contained in 40 CFR Part 2, 

Subpart B. The manner of asserting such a claim is specified in 40 CFR 2.203(b). Information 

covered by such a claim will be disclosed by EPA only to the extent, and by means of the 

procedures, set forth in Subpart B. 

If you wish to claim as confidential any of the information covered by the enclosed request, you 

must do so at the time you submit the information to EPA. If no such claim accompanies the 

information when EPA receives it, EPA may make the information available to the public 

without further notice to you. 

EPA will notify you in the event that a request is made for release of information that you have 

claimed to be confidential or EPA otherwise decides to make a determination as to whether or 

not such information is entitled to confidential treatment. At that time, EPA will request that you 

substantiate any claim you have made that information is confidential. Therefore, we encourage 

you to consult 40 CFR Part 2, and to claim as confidential only those items that you truly believe 

satisfy the criteria for confidentiality. 

Note that effluent data are not eligible for confidential treatment (see 40 CFR 2.302). 
Enclosure 3

Notice of Intent to Transfer Confidential Information to Selected EPA Contractors

EPA intends to grant access to confidential information collected under the sampling program to 

selected EPA contractors. 

In accordance with 40 CFR Sections 2.301(h)(2-3), 2.302(h)(2-3), and 2.305(h)(2-3), EPA may 

allow those contractors identified below access to all data (including data claimed to be 

confidential) collected as part of the follow-on sampling program. Transfer of this information 

to these contractors is necessary in order for the contractors to assist EPA in performing 

technical, statistical, and environmental analyses to support the development of effluent 

limitations guidelines and standards for the Steam Electric Power Generating industry. 

The contractors and subcontractors that will be providing support to EPA during the 

development of these regulations are listed below: 

EPA Office 

Receiving 

Support 

Contractor Name EPA Contract 

No. Type of Support 

Eastern Research Group, Inc. 68-C-02-095 Engineering analysis 

Office of Water/ 

Office of 

Science & 

Technology/ 

Engineering & 

Analysis 

Division 

Westat EP-C-10-023 Statistical analysis 

EPA has determined that it is necessary to transfer the information described above to the 

designated contractors and subcontractors in order that they may carry out the work required by 

their contracts. The contracts contain all provisions necessary to implement the confidentiality 

regulations (see 40 CFR 2.301(h)(2), 2.302(h)(2), and 2.305(h)(2)). 

In accordance with these confidentiality regulations, you are entitled to provide comments to 

EPA regarding this notice of contemplated disclosure. Any such comments must be received by 

EPA in writing within 10 days of your receipt of this notice. Please send such comments to: 

Ronald Jordan 

USEPA Headquarters 

Ariel Rios Building 

1200 Pennsylvania Ave., N.W. 

Mail Code: 4303T 

Washington, DC 20460 

jordan.ronald@epa.gov 
Enclosure 4 

Certification Statement 

The individual responsible for directing or supervising the sample collection and engineering 

data preparation for the sampling program must read and sign the Certification Statement listed 

below. The certifying official must be a responsible corporate official or his/her authorized 

representative. 

Certification Statement 

I certify under penalty of law that the samples collected for the sampling program were collected 

under my direction or supervision, that qualified personnel collected the samples following the 

procedures described in the instructions (including the use of clean hands/dirty hands sampling 

techniques described in EPA Method 1669), that qualified personnel gathered the engineering 

data required, and that the sampling and engineering data provided are complete and reflect 

normal operations for this plant. The engineering data submitted are, to the best of my 

knowledge and belief, accurate and complete. In those cases where we did not possess direct 

measurement, we provided best estimates. We have to the best of our ability indicated what we 

believe to be company confidential business information as defined under 40 CFR Part 2, 

Subpart B. We understand that we may be required at a later time to justify our claim in detail 

with respect to each item claimed confidential. I am aware that there are significant penalties 

for submitting false information, including the possibility of fines and imprisonment as explained 

in Section 308 of the Clean Water Act.

 

Signature of Certifying Official Date 

( ) 

Printed Name of Certifying Official Telephone Number of Certifying Official 

Title of Certifying Official 

Company Name 

 
Section 2

On-Site Audit Memorandum
DATE: 4 November 2010 

TO: Steam Electric Record 

FROM: Jezebele Alicea 

Engineering and Analysis Division 

 

SUBJECT: Notes from Audit of Industry Self-Monitoring Sampling at Duke Energy’s 

Miami Fort Station on November 1-2, 2010 

 EPA conducted an audit of the self-monitoring sampling conducted at Duke Energy’s 

Miami Fort Station located in North Bend, Ohio. This was Miami Fort’s second set (“Set 2”) of 

self-monitoring sampling that was being conducted to comply with the requirements established 

in a letter from Mary Smith, Director of EPA’s Engineering and Analysis Division, dated July 

30, 2010. EPA conducted the audit on November 1-2, 2010. These notes summarize the sample 

collection techniques used by Miami Fort staff at each of the sampling points and EPA’s 

observations/findings from the on-site review. A process water diagram for the flue gas 

desulfurization (FGD) wastewater treatment system at Miami Fort is provided as Attachment 1. 

The treatment system is described in EPA’s sampling plan for the Miami Fort plant.1 The 

checklists that EPA completed as part of the on-site review are provided as Attachment 2. 

 

The following sections describe the sample collection at each of the sampling points and 

the observations/findings from each sampling point. 

Influent to FGD Wastewater Treatment System - FGD Purge (SP-1) 

 Miami Fort personnel collected samples for the influent to the FGD wastewater treatment 

system from the sample tap on the pipe that flows from the secondary hydroclone overflow to the 

equalization tank, which is located on top of the equalization tank. EPA specified this location 

for the FGD purge sample (i.e., prior to the wastewater entering the equalization tank) because 

the FGD scrubber purge is commingled with other waste streams in the equalization tank and, 

therefore, the sampling point upstream of the tank provides the best representation of the FGD 

scrubber purge from the Miami Fort FGD system. This is the same sampling point that EPA used 

during its sample collection. This sample set collected secondary hydroclone overflow from Unit 

8. 

Sample Collection 

 Set 2 samples of the FGD purge were collected on November 2, 2010. To collect the 

samples of the FGD purge, Miami Fort personnel followed EPA Method 1669 protocols and the 

EPA-provided instructions. Miami Fort samplers shrouded the tap with a clean plastic bag and 

let the sample flow from the tap for two minutes prior to collecting any samples. The samplers 

then collected the samples underneath the shroud. All the mercury and metals samples were 

 

1

 Eastern Research Group, Inc. (ERG). Final Sampling Plan, Duke Energy’s Miami Fort Station, North Bend, Ohio, 

Sampling Episode 6560. July 1, 2010. 
Memorandum 

November 9, 2010 

Page 2 

filled while the samplers held the bottles under the shrouding. To collect the classicals samples, 

Miami Fort personnel did not remove the shrouding from the sample tap. 

 No field blanks were collected for the influent sample point during Set 2. Field blank 

samples were collected during Set 1. 

Preservation 

 Miami Fort personnel followed all method specifications when preserving the classical 

samples. The Group II samples were preserved using H2SO4 and the pH was confirmed to be 

below 2 S.U. The cyanide samples were checked for sulfides and chlorine using lead acetate 

paper and potassium iodide starch paper, respectively. The samplers did not detect sulfides or 

chlorine in the samples. The BOD, Group I, Group II, and cyanide samples were all placed on 

ice after collection or preservation. 

Field Measurements 

 Miami Fort personnel used a pH probe and a temperature probe to measure the pH and 

temperature of the influent field test bottle. Miami Fort personnel allowed the temperature and 

pH to stabilize and then recorded the values, which were 5.52 S.U. and 37.7°C. 

Observations/Findings 

 EPA observed the Miami Fort personnel setting up and collecting the Set 2 samples for 

the influent to wastewater treatment system. No field blanks were collected at this sample point 

because Miami Fort personnel previously collected field blanks during Set 1. The sampling crew 

followed the requirements of EPA Method 1669 (e.g., clean sampling protocols) while collecting 

samples. 

 Miami Fort personnel used the correct techniques to preserve the classical samples. The 

Group II and cyanide samples were placed in ice immediately after preservation. The BOD and 

Group I samples were placed on ice 20 minutes after sample collection. 

FGD Wastewater Treatment Effluent (SP-2) 

Miami Fort personnel collected samples of the FGD wastewater treatment system (SP-2) 

from a sample tap located on the suction side of the pump that transfers the wastewater from the 

effluent tank to the ash pond. This is the same sampling point that EPA used during its sample 

collection. The samples for this sampling point were collected as composite samples, except for 

the mercury and cyanide samples. For mercury samples, the plant collected four individual grab 

samples over the 24-hour period. For cyanide, the plant collected a single grab sample after the 

first mercury grab sample. 
Memorandum 

November 9, 2010 

Page 3 

Sample Collection 

 Miami Fort personnel collected the FGD wastewater treatment effluent as composite 

samples, except for the mercury and cyanide samples. One ISCO automatic compositor was 

programmed to collect individual sample volumes into a 20-liter container for the composite 

samples. The ISCO pump was calibrated and programmed to collect aliquots of equal volume in 

one-hour intervals during the 24-hour composite period. Following the composite period, Miami 

Fort personnel pumped off the specific sample volumes into the individual sample bottles for all 

analyses except mercury and cyanide. Mercury and cyanide samples were collected as grab 

samples. 

 To collect the composite samples, Miami Fort personnel connected a carboy to the 

sample tap using a length of silicone tubing. Prior to completing the setup for the composite 

samples, Miami Fort personnel collected field blanks for SP-2 by threading the tubing through 

the ISCO 3700 peristaltic pump and attaching the end of the tubing to a vented cap on a 10-liter 

carboy and pumping reagent grade water into the carboy. After collecting field blank volume, the 

10-L carboy was placed in ice. To collect the composite samples, Miami Fort personnel attached 

the one end of the silicone tubing to one of the barbed sample taps and the end of the tubing was 

attached to the vented cap, which was screwed onto a 20-liter carboy. The samplers 

programmed the compositor to collect 830 mL of sample every hour for a 24-hour period. 

 After the 24-hour period, the samplers took both carboys to the pump-off location and 

pumped the sample into the individual sample bottles. Miami Fort personnel used a short piece 

of Teflon® tubing connected to a length of silicone tubing and the peristaltic pump on the ISCO 

3700 to transfer the samples to individual sample bottles. The samplers first shook the 10-liter 

container to homogenize the field blank sample and then they attached a pump-off cap onto the 

carboy. The Teflon® end of the tubing was then inserted into the carboy and the tubing was 

purged with one liter of sample. Miami Fort personnel then collected the field blank samples 

(metals only) while placing the bottles in a cleanbox to reduce the potential for atmospheric 

contamination. 

 After the field blank samples were collected, the samplers then filled bottles for metals 

and classicals using the volume collected in the 20-liter carboy. The samplers first shook the 20-

liter container to homogenize the sample, and then they transferred the pump-off cap and tubing 

from the 10-liter field blank container to the 20-liter carboy. The tubing was then purged with 

two liters of sample. Miami Fort personnel then collected the metals samples with the bottles 

placed in the clean box. After all the metals samples were collected, the samplers filled the 

classical samples outside the cleanbox. 

 Miami Fort personnel also collected grab samples for mercury every six hours during the 

sampling. The samplers collected the mercury samples at this sampling point by shrouding the 

second tap on the two-way splitter with a clean plastic bag and letting sample flow through the 

sample tap for two minutes prior to collecting any samples. Samplers filled the mercury bottles 

directly from the tap, underneath the shroud. The cyanide samples were collected as a grab 

sample immediately after the first of the four mercury grab samples at the sampling point. 
Memorandum 

November 9, 2010 

Page 4 

Preservation 

 Miami Fort personnel followed all method specifications when preserving the classicals 

samples, which are the same as those described in the Preservation section for the FGD 

wastewater treatment influent stream. Additionally, the plant kept the composite container on 

ice during the sample collection time period. 

Field Measurements 

 Miami Fort personnel used a pH probe and a temperature probe to measure the pH and 

temperature of the influent field test bottle. Miami Fort personnel allowed the temperature and 

pH to stabilize and then recorded the values. 

Observations/Findings 

 EPA observed the following activities for SP-2 during the audit: collection of cyanide 

sample and mercury grab 1 (including field blank) and grab 2; field blank collection and set-up 

for the composite samples; breakdown of the composite sampler; pump-off of composite 

samples; and preservation. 

 The sampling crew followed the requirements of EPA Method 1669 (e.g., clean sampling 

protocols) while collecting samples. Miami Fort personnel followed applicable procedures for 

sample collection and preservation. Samples were preserved within 15 minutes. 

 No clean box was used during set-up for the composite sample; however, clean sampling 

protocols were followed. The sample tubing was provided double-bagged from the laboratory, 

with all tubing ends already covered by zip-tied plastic bags. 

 During field blank collection, samplers realized that volume collected in the 10-liter 

carboy may not be enough volume for purging the tubing and the required field blank samples. 

Therefore, samplers opened the reagent blank water bottle again, placed the tubing inside the 

bottle, and pumped additional volume into the 10-L carboy. EPA noted that the reagent blank 

water bottle was inside an inner bag and a second bag at all times. 

 During preparation for the pump-off of composite samples, the tubing was removed from 

double plastics bags while outside the clean box. All tubing ends were already covered in the 

laboratory by zip-tied plastic bags and clean sampling protocols were followed while handling 

the tubing. 

During the composite pump off, the transition of the pump-off cap from the field blank carboy to 

the sample carboy took less than 20 seconds, during which time the sample carboy was not 

covered. 
Memorandum 

November 9, 2010 

Page 5 

 All bottles were pre-labeled by the laboratory. The field blank container was a 10-liter 

carboy, instead of a 20-liter carboy (a 20-liter carboy was used to collect the 24-hour composite 

samples). 

All observations were informed to Miami Fort personnel. 

 

 

 
Attachment 1 

FGD Wastewater Treatment Process Flow Diagram 
Due to a confidentiality claim, the Miami Fort FGD Wastewater Treatment diagram cannot be 

Figure 1. Chemical Precipitation FGD Wastewater Treatment System, Miami Fort Stat
Attachment 2 

Checklists 















Section 3

Signed Certification Statement

Section 4

Engineering Data
Table C4-1. Field Measurements for Sample Collection at the Influent to FGD Wastewater Treatment System

Episode Number 

Sample Collection 

Number 

Date of Sample 

Collection 

Sample Collection 

Time 

Temperature 

(°C) 

6567 Set 1 - Grab 1 9/28/2010 0830 40.5 6567 Set 2 - Grab 1 11/2/2010 0826 37.7 6567 Set 3 - Grab 1 12/7/2010 0843 39.5 6567 Set 4 - Grab 1 1/14/2011 0818 43.7 
Table C4-2. Field Measurements for Sample Collection at the Effluent from FGD Wastewater Treatment Syste

Episode Number 

Sample Collection 

Number 

Date of Sample 

Collection 

Sample Collection 

Time 

Temperature 

(°C) 

6567 Set 1 - Grab 1 9/27/2010 1117 23.3 6567 Set 1 - Grab 2 9/27/2010 1713 27.8 6567 Set 1 - Grab 3 9/27/2010 2315 26.6 6567 Set 1 - Grab 4 9/28/2010 0516 26.5 6567 Set 2 - Grab 1 11/1/2010 0921 26.4 6567 Set 2 - Grab 2 11/1/2010 1523 25.2 6567 Set 2 - Grab 3 11/1/2010 2121 23.8 6567 Set 2 - Grab 4 11/2/2010 0320 23.0 6567 Set 3 - Grab 1 12/6/2010 0949 19.8 6567 Set 3 - Grab 2 12/6/2010 1554 17.7 6567 Set 3 - Grab 3 12/6/2010 2148 20.8 6567 Set 3 - Grab 4 12/7/2010 0350 20.8 6567 Set 4 - Grab 1 1/13/2011 0932 23.4 6567 Set 4 - Grab 2 1/13/2011 1533 21.8 6567 Set 4 - Grab 3 1/13/2011 2131 22.0 6567 Set 4 - Grab 4 1/14/2011 0327 21.3 
Table C4-3. Sample Collection Procedures Used during the Sampling Episode 

Episode 

Number 

Sample 

Collection 

Number 

Unit 

Overflow 

Sampled 

at Influent 

Influent 

Samples 

Collected as 

Grabs 

(Yes or No) 

Mercury 

and Cyanide 

Samples 

Collected as 

Grabs 

(Yes or No) 

Effluent Samples 

Collected as 24-

Hour Composites 

(Yes or No) 

Clean 

Hands/Dirty 

Hands Sampling 

Techniques Used

(Yes or No)* 

Description o

Sample 

Collection 

Technique (i

different tha

instructions

6567 Set 1 Unit 7 Yes Yes Yes Yes None 6567 Set 2 Unit 8 Yes Yes Yes Yes None 6567 Set 3 Unit 7 Yes Yes Yes Yes None 6567 Set 4 Unit 8 Yes Yes Yes Yes None 

* Includes the use of tyveks suits during all sampling events and dust masks during the collection of mercury samples. Note 1: Electric power was lost to part of the equipment in the wastewater treatment plant from 12:10 AM to 3:20 AM on December 7, Note 2: Unit 7 and 8 boilers and scrubbers were shut down just prior to the set 4 samples. Both units were operating normally during th

collection for set 4. 
Table C4-4. Generating Unit Operation at Time of Sampling, Miami Fort 

Episode Number 

Sample Collection 

Number 

Date of Sample 

Collection 

Plant Operation During Sample Colle

Units Operating 

During Sampling 

Day 

Units Off-line Entire 

Sampling Day 

6567 Set 1 9/27/10 - 9/28/10 Unit 7 none 6567 Set 1 9/27/10 - 9/28/10 Unit 8 none 6567 Set 2 11/1/10 - 11/2/10 Unit 7 none 6567 Set 2 11/1/10 - 11/2/10 Unit 8* none 6567 Set 3 12/6/10 - 12/7/10 Unit 7 none 6567 Set 3 12/6/10 - 12/7/10 Unit 8 none 6567 Set 4 1/13/11 - 1/14/11 Unit 7 none 6567 Set 4 1/13/11 - 1/14/11 Unit 8 none 

* Unit 8 ran full load until 9:42 AM on November 2, 2010 and stopped generating power at 10:01 AM on November 2, 201treatment system samples were complete at 8:00 AM, prior to the Unit 8 shut down. 
Table C4-5. FGD Scrubber Slurry Information at Time of Sampling, Miami Fort 

Episode 

Number 

Sample 

Collection 

Number 

Date of Sample 

Collection Units 

Plant Operation During Sample Colle

Scrubber Slurry Blowdown 

Flow Rate 

Scrubber 

Slurry 

Percent 

Solids 

(%) 

Flow Rate 

(gpm) 

Duration 

(hours) 

6567 Set 1 9/27/10 - 9/28/10 7 CBI CBI CBI 6567 Set 1 9/27/10 - 9/28/10 8 CBI CBI CBI 6567 Set 2 11/1/10 - 11/2/10 7 CBI CBI CBI 6567 Set 2 11/1/10 - 11/2/10 8 CBI CBI CBI 6567 Set 3 12/6/10 - 12/7/10 7 CBI CBI CBI 6567 Set 3 12/6/10 - 12/7/10 8 CBI CBI CBI 6567 Set 4 1/13/11 - 1/14/11 7 CBI CBI CBI 6567 Set 4 1/13/11 - 1/14/11 8 CBI CBI CBI 

. 
Table C4-6. FGD Scrubber Slurry Information at Time of Sampling, Miami Fort 

Episode 

Number 

Sample 

Collection 

Number 

Date of Sample 

Collection Units 

Plant Operation During Sample Coll

Secondary Hydroclone 

Overflow Flow Rate 

Secondary 

Hydroclone 

Overflow 

Percent Solids 

(%) 

Flow Rate 

(gpm) 

Duration 

(hours) 

6567 Set 1 9/27/10 - 9/28/10 7 CBI CBI CBI 6567 Set 1 9/27/10 - 9/28/10 8 CBI CBI CBI 6567 Set 2 11/1/10 - 11/2/10 7 CBI CBI CBI 6567 Set 2 11/1/10 - 11/2/10 8 CBI CBI CBI 6567 Set 3 12/6/10 - 12/7/10 7 CBI CBI CBI 6567 Set 3 12/6/10 - 12/7/10 8 CBI CBI CBI 6567 Set 4 1/13/11 - 1/14/11 7 CBI CBI CBI 6567 Set 4 1/13/11 - 1/14/11 8 CBI CBI CBI 
Table C4-7. FGD Wastewater Treatment System Operation Information, Miami Fort 

Episode 

Number 

Sample 

Collection 

Number 

Date of Sample 

Collection 

Scrubber Purge 

Flow Rate During 

Influent Sample 

Collection 

(gpm) 

FGD Wastewater Treatment Operation During Sam

Lime 

Usage 

(tons) 

Ferric 

Chloride 

Usage 

(Liters/day) 

Nalmet 1689 

Usage 

(Liters/day) 

Polymer Us

(Liters/da

6567 Set 1 9/28/2010 CBI CBI CBI CBI CBI 6567 Set 2 11/2/2010 CBI CBI CBI CBI CBI 6567 Set 3 12/7/2010 CBI CBI CBI CBI CBI 6567 Set 4 1/14/2011 CBI CBI CBI CBI CBI 
Table C4-8. Daily Power Generation During Sampling Period, Miami Fort 

Episode Number Date 

Daily Power Generation 

(MW-hrs) 

Unit 7 Unit 8 

6567 9/13/2010 11,819 12,181 

6567 9/14/2010 11,794 12,020 

6567 9/15/2010 11,586 12,167 

6567 9/16/2010 12,114 12,507 

6567 9/17/2010 12,756 12,048 

6567 9/18/2010 11,624 11,622 

6567 9/19/2010 11,363 11,403 

6567 9/20/2010 12,636 12,752 

6567 9/21/2010 12,219 11,831 

6567 9/22/2010 12,389 12,807 

6567 9/23/2010 11,618 11,889 

6567 9/24/2010 12,358 12,467 

6567 9/25/2010 11,939 12,486 

6567 9/26/2010 9,637 10,081 

6567 9/27/2010 11,973 12,199 

6567 9/28/2010 11,599 11,739 

6567 9/29/2010 12,682 12,992 

6567 9/30/2010 12,392 12,837 

6567 10/1/2010 11,456 12,857 

6567 10/2/2010 11,986 12,233 

6567 10/3/2010 11,306 11,529 

6567 10/4/2010 12,271 12,665 

6567 10/5/2010 12,403 12,867 

6567 10/6/2010 12,236 12,618 

6567 10/7/2010 11,753 12,393 

6567 10/8/2010 12,190 12,847 

6567 10/9/2010 11,602 12,038 

6567 10/10/2010 10,652 11,365 

6567 10/11/2010 11,516 11,961 

6567 10/12/2010 11,974 12,424 

6567 10/13/2010 12,386 12,847 

6567 10/14/2010 11,834 12,033 

6567 10/15/2010 12,038 12,645 

6567 10/16/2010 10,488 12,743 

6567 10/17/2010 11,981 12,505 

6567 10/18/2010 12,195 12,276 

6567 10/19/2010 12,233 12,820 

6567 10/20/2010 12,375 12,818 

6567 10/21/2010 12,041 12,232 

6567 10/22/2010 11,880 12,175 

6567 10/23/2010 10,364 10,538 
Table C4-8. Daily Power Generation During Sampling Period, Miami Fort 

Episode Number Date 

Daily Power Generation 

(MW-hrs) 

Unit 7 Unit 8 

6567 10/24/2010 10,966 11,256 

6567 10/25/2010 11,546 12,194 

6567 10/26/2010 11,677 11,960 

6567 10/27/2010 12,221 12,532 

6567 10/28/2010 12,240 12,446 

6567 10/29/2010 12,876 12,988 

6567 10/30/2010 12,847 12,982 

6567 10/31/2010 12,410 12,769 

6567 11/1/2010 12,015 13,017 

6567 11/2/2010 12,821 5,442 

6567 11/3/2010 11,426 0 

6567 11/4/2010 12,884 0 

6567 11/5/2010 13,062 0 

6567 11/6/2010 13,005 0 

6567 11/7/2010 12,774 2 

6567 11/8/2010 12,486 8,514 

6567 11/9/2010 12,557 10,533 

6567 11/10/2010 11,937 12,220 

6567 11/11/2010 12,176 12,235 

6567 11/12/2010 12,297 12,633 

6567 11/13/2010 9,427 12,843 

6567 11/14/2010 12,215 12,430 

6567 11/15/2010 12,841 12,867 

6567 11/16/2010 12,805 13,115 

6567 11/17/2010 12,941 13,109 

6567 11/18/2010 13,090 13,203 

6567 11/19/2010 12,799 12,904 

6567 11/20/2010 12,838 12,902 

6567 11/21/2010 12,131 12,377 

6567 11/22/2010 12,136 6,623 

6567 11/23/2010 12,100 0 

6567 11/24/2010 12,965 0 

6567 11/25/2010 12,586 0 

6567 11/26/2010 12,014 0 

6567 11/27/2010 12,998 0 

6567 11/28/2010 12,711 0 

6567 11/29/2010 12,623 0 

6567 11/30/2010 11,955 6,020 

6567 12/1/2010 12,595 12,503 

6567 12/2/2010 12,659 13,162 

6567 12/3/2010 13,007 13,186 

6567 12/4/2010 12,969 8,873 

6567 12/5/2010 12,913 11,666 
Table C4-8. Daily Power Generation During Sampling Period, Miami Fort 

Episode Number Date 

Daily Power Generation 

(MW-hrs) 

Unit 7 Unit 8 

6567 12/6/2010 12,886 13,178 

6567 12/7/2010 12,899 13,237 

6567 12/8/2010 11,704 13,184 

6567 12/9/2010 10,970 13,061 

6567 12/10/2010 11,879 12,663 

6567 12/11/2010 11,482 12,164 

6567 12/12/2010 11,777 12,535 

6567 12/13/2010 12,993 13,151 

6567 12/14/2010 13,028 13,029 

6567 12/15/2010 12,911 13,071 

6567 12/16/2010 12,944 13,120 

6567 12/17/2010 12,644 12,898 

6567 12/18/2010 12,885 10,634 

6567 12/19/2010 12,971 13,159 

6567 12/20/2010 12,567 12,824 

6567 12/21/2010 8,459 8,311 

6567 12/22/2010 10,920 11,524 

6567 12/23/2010 13,040 13,195 

6567 12/24/2010 12,730 13,018 

6567 12/25/2010 10,892 11,298 

6567 12/26/2010 12,591 12,868 

6567 12/27/2010 13,095 13,158 

6567 12/28/2010 12,950 13,117 

6567 12/29/2010 12,652 12,921 

6567 12/30/2010 12,530 12,872 

6567 12/31/2010 11,636 11,988 

6567 1/1/2011 10,750 10,948 

6567 1/2/2011 12,497 9,901 

6567 1/3/2011 13,045 13,210 

6567 1/4/2011 12,984 13,154 

6567 1/5/2011 13,102 7,388 

6567 1/6/2011 13,124 0 

6567 1/7/2011 11,410 0 

6567 1/8/2011 11,457 0 

6567 1/9/2011 11,620 0 

6567 1/10/2011 3,279 0 

6567 1/11/2011 0 144 

6567 1/14/2011 9,309 13,165 

6567 1/15/2011 0 13,053 

6567 1/16/2011 0 13,010 

6567 1/17/2011 0 13,101 

6567 1/18/2011 4,166 12,378 

6567 1/19/2011 12,654 12,840 
Table C4-8. Daily Power Generation During Sampling Period, Miami Fort 

Episode Number Date 

Daily Power Generation 

(MW-hrs) 

Unit 7 Unit 8 

6567 1/20/2011 12,917 13,119 

6567 1/21/2011 13,140 13,174 

6567 1/22/2011 13,110 8,540 

6567 1/23/2011 12,943 12,552 

6567 1/24/2011 12,301 12,228 

6567 1/25/2011 13,120 13,095 
Table C4-9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Miami 

Fort 

Episode Number Date 

FGD Wastewater Treatment System Flow Rates 

(gpd) 

Chemical Precipitation Effluent 

6567 9/13/2010 CBI 

6567 9/14/2010 CBI 

6567 9/15/2010 CBI 

6567 9/16/2010 CBI 

6567 9/17/2010 CBI 

6567 9/18/2010 CBI 

6567 9/19/2010 CBI 

6567 9/20/2010 CBI 

6567 9/21/2010 CBI 

6567 9/22/2010 CBI 

6567 9/23/2010 CBI 

6567 9/24/2010 CBI 

6567 9/25/2010 CBI 

6567 9/26/2010 CBI 

6567 9/27/2010 CBI 

6567 9/28/2010 CBI 

6567 9/29/2010 CBI 

6567 9/30/2010 CBI 

6567 10/1/2010 CBI 

6567 10/2/2010 CBI 

6567 10/3/2010 CBI 

6567 10/4/2010 CBI 

6567 10/5/2010 CBI 

6567 10/6/2010 CBI 

6567 10/7/2010 CBI 

6567 10/8/2010 CBI 

6567 10/9/2010 CBI 

6567 10/10/2010 CBI 

6567 10/11/2010 CBI 

6567 10/12/2010 CBI 

6567 10/13/2010 CBI 

6567 10/14/2010 CBI 

6567 10/15/2010 CBI 

6567 10/16/2010 CBI 

6567 10/17/2010 CBI 

6567 10/18/2010 CBI 

6567 10/19/2010 CBI 

6567 10/20/2010 CBI 

6567 10/21/2010 CBI 
Table C4-9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Miami 

Fort 

Episode Number Date 

FGD Wastewater Treatment System Flow Rates 

(gpd) 

Chemical Precipitation Effluent 

6567 10/22/2010 CBI 

6567 10/23/2010 CBI 

6567 10/24/2010 CBI 

6567 10/25/2010 CBI 

6567 10/26/2010 CBI 

6567 10/27/2010 CBI 

6567 10/28/2010 CBI 

6567 10/29/2010 CBI 

6567 10/30/2010 CBI 

6567 10/31/2010 CBI 

6567 11/1/2010 CBI 

6567 11/2/2010 CBI 

6567 11/3/2010 CBI 

6567 11/4/2010 CBI 

6567 11/5/2010 CBI 

6567 11/6/2010 CBI 

6567 11/7/2010 CBI 

6567 11/8/2010 CBI 

6567 11/9/2010 CBI 

6567 11/10/2010 CBI 

6567 11/11/2010 CBI 

6567 11/12/2010 CBI 

6567 11/13/2010 CBI 

6567 11/14/2010 CBI 

6567 11/15/2010 CBI 

6567 11/16/2010 CBI 

6567 11/17/2010 CBI 

6567 11/18/2010 CBI 

6567 11/19/2010 CBI 

6567 11/20/2010 CBI 

6567 11/21/2010 CBI 

6567 11/22/2010 CBI 

6567 11/23/2010 CBI 

6567 11/24/2010 CBI 

6567 11/25/2010 CBI 

6567 11/26/2010 CBI 

6567 11/27/2010 CBI 

6567 11/28/2010 CBI 

6567 11/29/2010 CBI 

6567 11/30/2010 CBI 

6567 12/1/2010 CBI 
Table C4-9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Miami 

Fort 

Episode Number Date 

FGD Wastewater Treatment System Flow Rates 

(gpd) 

Chemical Precipitation Effluent 

6567 12/2/2010 CBI 

6567 12/3/2010 CBI 

6567 12/4/2010 CBI 

6567 12/5/2010 CBI 

6567 12/6/2010 CBI 

6567 12/7/2010 CBI 

6567 12/8/2010 CBI 

6567 12/9/2010 CBI 

6567 12/10/2010 CBI 

6567 12/11/2010 CBI 

6567 12/12/2010 CBI 

6567 12/13/2010 CBI 

6567 12/14/2010 CBI 

6567 12/15/2010 CBI 

6567 12/16/2010 CBI 

6567 12/17/2010 CBI 

6567 12/18/2010 CBI 

6567 12/19/2010 CBI 

6567 12/20/2010 CBI 

6567 12/21/2010 CBI 

6567 12/22/2010 CBI 

6567 12/23/2010 CBI 

6567 12/24/2010 CBI 

6567 12/25/2010 CBI 

6567 12/26/2010 CBI 

6567 12/27/2010 CBI 

6567 12/28/2010 CBI 

6567 12/29/2010 CBI 

6567 12/30/2010 CBI 

6567 12/31/2010 CBI 

6567 1/1/2011 CBI 

6567 1/2/2011 CBI 

6567 1/3/2011 CBI 

6567 1/4/2011 CBI 

6567 1/5/2011 CBI 

6567 1/6/2011 CBI 

6567 1/7/2011 CBI 

6567 1/8/2011 CBI 

6567 1/9/2011 CBI 

6567 1/10/2011 CBI 

6567 1/11/2011 CBI 
Table C4-9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Miami 

Fort 

Episode Number Date 

FGD Wastewater Treatment System Flow Rates 

(gpd) 

Chemical Precipitation Effluent 

6567 1/12/2011 CBI 

6567 1/13/2011 CBI 

6567 1/14/2011 CBI 

6567 1/15/2011 CBI 

6567 1/16/2011 CBI 

6567 1/17/2011 CBI 

6567 1/18/2011 CBI 

6567 1/19/2011 CBI 

6567 1/20/2011 CBI 

6567 1/21/2011 CBI 

6567 1/22/2011 CBI 

6567 1/23/2011 CBI 

6567 1/24/2011 CBI 

6567 1/25/2011 CBI 
Section 5

Analytical Data
< - 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 Tables C5-5 through C5-17 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantita

result is a J-value. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. E – MS and/or MSD exceeded the calibration range. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. 

Table C5-1. Influent to FGD Wastewater Treatment System, Miami Fort 

Analyte Units Method 

Influent to FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 

ClassicalsAmmonia mg/L 350.1 7.30 11.0 17.0 B 8.8Nitrate Nitrite as N mg/L 353.2 75.0 82.0 * 74.0 56Nitrogen, Total Kjeldahl mg/L 351.2 59.0 B, Min 67.0 97.0 48Biochemical Oxygen Demand mg/L 5210B ND (2.00) ND (2.00) NQ (5.00) 11Chemical Oxygen Demand mg/L 410.4 730 650 B 430 85Chloride mg/L 300.0 8,300 12,000 11,000 8,1Sulfate mg/L 300.0 35,000 36,000 27,000 21,0Cyanide, Total mg/L 4500 CN E 1.10 1.20 0.790 19Total Dissolved Solids mg/L 2540C 54,000 Est 53,000 55,000 41,0Total Suspended Solids mg/L 2540D 21,000 32,000 27,000 30,0Phosphorus, Total mg/L 365.1 17.0 0.0680 B NQ (0.0500) B 28Total MetalsAluminum ug/L 200.7 570,000 830,000 B 370,000 360,
< - 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 Tables C5-5 through C5-17 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantita

result is a J-value. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. E – MS and/or MSD exceeded the calibration range. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. 

Table C5-1. Influent to FGD Wastewater Treatment System, Miami Fort 

Analyte Units Method 

Influent to FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 

Antimony ug/L 200.8 34.0 50.0 45.0 43Arsenic ug/L 200.8 320 670 430 56Barium ug/L 200.7 590 1,000 B 400 50Beryllium ug/L 200.7 26.0 33.0 17.0 24Boron ug/L 200.7 1,200,000 B 1,000,000 B 1,000,000 B 870,Cadmium ug/L 200.8 610 840 580 57Calcium ug/L 200.7 1,200,000 1,300,000 B 1,500,000 1,900Chromium ug/L 200.8 2,700 2,900 ^ 1,600 2,0Cobalt ug/L 200.7 640 660 540 53Copper ug/L 200.8 890 1,100 540 88Iron ug/L 200.7 1,300,000 1,200,000 B 600,000 560,Lead ug/L 200.8 400 480 270 46Magnesium ug/L 200.7 13,000,000 B 14,000,000 B 9,700,000 B 7,800Manganese ug/L 200.7 200,000 B 200,000 B 200,000 170,Mercury ng/L 1631E 384,000 319,000 224,000 367,Molybdenum ug/L 200.7 340 610 670 60Nickel ug/L 200.8 3,600 3,700 4,200 3,9Selenium ug/L 200.8 930 1,700 1,600 2,1Silver ug/L 200.8 NQ (2.00) 3.00 2.60 2.4
< - 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 Tables C5-5 through C5-17 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantita

result is a J-value. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. E – MS and/or MSD exceeded the calibration range. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. 

Table C5-1. Influent to FGD Wastewater Treatment System, Miami Fort 

Analyte Units Method 

Influent to FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 

Sodium ug/L 200.7 830,000 B 950,000 B 750,000 430,Thallium ug/L 200.8 14.0 65.0 34.0 70Tin ug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (Titanium ug/L 200.7 2,800 4,500 B 2,000 3,6Vanadium ug/L 200.8 2,500 2,800 1,600 2,4Zinc ug/L 200.7 16,000 19,000 ^ 16,000 13,0
< - 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 Tables C5-5 through C5-17 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantita

result is a J-value. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. E – MS and/or MSD exceeded the calibration range. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. 

Table C5-2. Effluent from FGD Wastewater Treatment System, Miami Fort 

Analyte Units Method 

Effluent from FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 S

ClassicalsAmmonia mg/L 350.1 5.20 5.20 F 45.0 B 5.4Nitrate Nitrite as N mg/L 353.2 73.0 44.0 F,* 51.0 38Nitrogen, Total Kjeldahl mg/L 351.2 22.0 B, Min 22.0 4 74.0 24Biochemical Oxygen Demand mg/L 5210B 3.30 2.50 3.90 ND (Chemical Oxygen Demand mg/L 410.4 530 470 B,F 500 82Chloride mg/L 300.0 5,800 8,200 7,200 5,7Sulfate mg/L 300.0 14,000 11,000 14,000 9,6Cyanide, Total mg/L 4500 CN E NQ (0.100) 0.230 F 0.480 15Total Dissolved Solids mg/L 2540C 31,000 28,000 Est 32,000 26,0Total Suspended Solids mg/L 2540D 8.40 4.80 Est 8.80 8.8Phosphorus, Total mg/L 365.1 0.360 NQ (0.0500) B 0.0950 B 0.5
< - 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 Tables C5-5 through C5-17 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantita

result is a J-value. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. E – MS and/or MSD exceeded the calibration range. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. 

Table C5-2. Effluent from FGD Wastewater Treatment System, Miami Fort 

Analyte Units Method 

Effluent from FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 S

Total MetalsAluminum ug/L 200.7 ND (200) ND (200) ND (200) ND (Antimony ug/L 200.8 6.20 4.00 5.80 5.1Arsenic ug/L 200.8 4.40 NQ (4.00) 5.00 NQ (4Barium ug/L 200.7 130 F 130 B 100 97Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2Boron ug/L 200.7 300,000 B,4 210,000 B,4 520,000 B 590,Cadmium ug/L 200.8 ND (4.00) ND (4.00) ND (4.00) ND (4Calcium ug/L 200.7 750,000 4 1,000,000 B,4 950,000 1,100Chromium ug/L 200.8 16.0 14.0 ^ 8.60 NQ (Cobalt ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND (2Copper ug/L 200.8 ND (4.00) ND (4.00) NQ (4.00) NQ (4Iron ug/L 200.7 NQ (200) NQ (200) B NQ (200) NQ (Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2Magnesium ug/L 200.7 6,000,000 B,4 5,200,000 B,4 6,000,000 B 4,400Manganese ug/L 200.7 130 B 140 B 1,000 1,1Mercury ng/L 1631E 256 295 144 12Molybdenum ug/L 200.7 170 140 310 32Nickel ug/L 200.8 NQ (4.00) NQ (4.00) 4.20 4.0
< - 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 Tables C5-5 through C5-17 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantita

result is a J-value. * - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. E – MS and/or MSD exceeded the calibration range. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. Min – Minimum value. 

Table C5-2. Effluent from FGD Wastewater Treatment System, Miami Fort 

Analyte Units Method 

Effluent from FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 S

Selenium ug/L 200.8 360 4 290 4 660 83Silver ug/L 200.8 ND (2.00) F ND (2.00) F ND (2.00) ND (2Sodium ug/L 200.7 580,000 B,4 670,000 B,4 660,000 380,Thallium ug/L 200.8 6.30 4.50 6.40 10Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (Titanium ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND (2Vanadium ug/L 200.8 14.0 10.0 21.0 23Zinc ug/L 200.7 NQ (40.0) NQ (40.0) ^ ND (40.0) ND (4
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

Table C5-3. Classical Pollutants 4-Set Average Data Summary for FGD Wastewater Treat

System, Miami Fort 

Analyte Units Method 

Influent to FGD 

Wastewater Treatment 

System (SP-1) 4-Set Average 

Effluent from 

Wastewater Tr

System (SP4-Set Aver

ClassicalsAmmonia mg/L 350.1 11.0 15.2 Nitrate Nitrite as N mg/L 353.2 71.8 51.5 Nitrogen, Total Kjeldahl mg/L 351.2 67.8 35.5 Biochemical Oxygen Demand mg/L 5210B < 28.6 < 2.68 Chemical Oxygen Demand mg/L 410.4 665 580 Chloride mg/L 300.0 9,850 6,730 Sulfate mg/L 300.0 29,800 12,200 Cyanide, Total mg/L 4500 CN E 5.52 < 3.94 Total Dissolved Solids mg/L 2540C 50,800 29,300 Total Suspended Solids mg/L 2540D 27,500 7.70 Phosphorus, Total mg/L 365.1 < 11.3 < 0.245 
< - 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 Tables C5-5 through C5-17 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantita

result is a J-value. 

Table C5-4. Metals Pollutants 4-Set Average Data Summary for FGD Wastewater Treatm

System, Miami Fort 

Analyte Units Method

Influent to FGD 

Wastewater Treatment 

System (SP-1) 4-Set Average 

Effluent from FG

Wastewater Treatm

System (SP-2) 4-Set Average 

Total MetalsAluminum ug/L 200.7 533,000 ND (200) Antimony ug/L 200.8 43.0 5.28 Arsenic ug/L 200.8 495 < 3.35 Barium ug/L 200.7 623 114 Beryllium ug/L 200.7 25.0 ND (2.00) Boron ug/L 200.7 1,020,000 405,000 Cadmium ug/L 200.8 650 ND (4.00) Calcium ug/L 200.7 1,480,000 950,000 Chromium ug/L 200.8 2,300 < 10.7 Cobalt ug/L 200.7 593 ND (20.0) Copper ug/L 200.8 853 NQ (4.00) Iron ug/L 200.7 915,000 NQ (200) Lead ug/L 200.8 403 ND (2.00) Magnesium ug/L 200.7 11,100,000 5,400,000 Manganese ug/L 200.7 193,000 593 Mercury ng/L 1631E 324,000 206 Molybdenum ug/L 200.7 555 235 Nickel ug/L 200.8 3,850 < 3.05 Selenium ug/L 200.8 1,580 535 Silver ug/L 200.8 < 2.25 ND (2.00) 
< - 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 Tables C5-5 through C5-17 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantita

result is a J-value. 

Table C5-4. Metals Pollutants 4-Set Average Data Summary for FGD Wastewater Treatm

System, Miami Fort 

Analyte Units Method

Influent to FGD 

Wastewater Treatment 

System (SP-1) 4-Set Average 

Effluent from FG

Wastewater Treatm

System (SP-2) 4-Set Average 

Sodium ug/L 200.7 740,000 573,000 Thallium ug/L 200.8 45.8 6.80 Tin ug/L 200.7 NQ (200) ND (200) Titanium ug/L 200.7 3,230 ND (20.0) Vanadium ug/L 200.8 2,330 17.0 Zinc ug/L 200.7 16,000 NQ (40.0) 
ND – Not detected (number in parentheses is the quantitation limit). 

B – Analyte was found in the blank and sample. Est – Estimated value. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table C5-5. Influent to FGD Wastewater Treatment System, Set 1 Analytical Results, Miam

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

Classicals Ammonia 350.1 mg/L 1 0.055 1 7.3 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 75 Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.77 10 59 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) Chemical Oxygen Demand 410.4 mg/L 5 20 100 730 Chloride 300.0 mg/L 500 130 1,500 8,300 Sulfate 300.0 mg/L 1,000 230 5,000 35,000 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 1.1 Total Dissolved Solids 2540C mg/L 1 160 330 54,000 Total Suspended Solids 2540D mg/L 1 110 400 21,000 Phosphorus, Total 365.1 mg/L 20 0.1 1 17 Total MetalsAluminum 200.7 ug/L 2 9.4 200 570,000 Antimony 200.8 ug/L 2 0.72 2 34 Arsenic 200.8 ug/L 10 6.1 20 320 Barium 200.7 ug/L 2 2.5 20 590 Beryllium 200.7 ug/L 2 0.71 2 26 Boron 200.7 ug/L 250 830 25,000 1,200,00Cadmium 200.8 ug/L 2 1.2 4 610 Calcium 200.7 ug/L 50 1,700 10,000 1,200,00
ND – Not detected (number in parentheses is the quantitation limit). 

B – Analyte was found in the blank and sample. Est – Estimated value. J – Result measured above the MDL, but less than the quantitation limit. Min – Minimum value. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table C5-5. Influent to FGD Wastewater Treatment System, Set 1 Analytical Results, Miam

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

Chromium 200.8 ug/L 2 3.3 8 2,700 Cobalt 200.7 ug/L 2 1.1 20 640 Copper 200.8 ug/L 2 0.96 4 890 Iron 200.7 ug/L 50 800 5,000 1,300,00Lead 200.8 ug/L 2 0.73 2 400 Magnesium 200.7 ug/L 50 540 10,000 13,000,00Manganese 200.7 ug/L 50 13 500 200,000 Mercury 1631E ng/L 100,000 24,800 52,000 384,000 Molybdenum 200.7 ug/L 2 1.6 40 340 Nickel 200.8 ug/L 2 0.89 4 3,600 Selenium 200.8 ug/L 10 3.1 20 930 Silver 200.8 ug/L 2 0.59 2 0.76 Sodium 200.7 ug/L 2 180 10,000 830,000 Thallium 200.8 ug/L 2 0.47 2 14 Tin 200.7 ug/L 2 4.8 200 34 Titanium 200.7 ug/L 2 1.6 20 2,800 Vanadium 200.8 ug/L 2 1.7 10 2,500 Zinc 200.7 ug/L 2 9.1 40 16,000 
ND – Not detected (number in parentheses is the quantitation limit). 

* - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. 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 C5-6. Influent to FGD Wastewater Treatment System, Set 2 Analytical Results, Miam

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Con

Classicals Ammonia 350.1 mg/L 2 0.11 2 Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 Nitrogen, Total Kjeldahl 351.2 mg/L 20 1.5 20 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND Chemical Oxygen Demand 410.4 mg/L 5 20 100 6Chloride 300.0 mg/L 1,000 250 3,000 12Sulfate 300.0 mg/L 1,000 230 5,000 36Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 94 200 53Total Suspended Solids 2540D mg/L 1 55 200 32Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0Total MetalsAluminum 200.7 ug/L 2 9.4 200 830Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 5 3.1 10 6Barium 200.7 ug/L 2 2.5 20 1Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 1,00Cadmium 200.8 ug/L 2 1.2 4 8Calcium 200.7 ug/L 50 1,700 10,000 1,30Chromium 200.8 ug/L 2 3.3 8 2
ND – Not detected (number in parentheses is the quantitation limit). 

* - LCS or LCSD is outside the laboratory control limits. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. 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 C5-6. Influent to FGD Wastewater Treatment System, Set 2 Analytical Results, Miam

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Con

Cobalt 200.7 ug/L 2 1.1 20 6Copper 200.8 ug/L 2 0.96 4 1Iron 200.7 ug/L 50 800 5,000 1,20Lead 200.8 ug/L 2 0.73 2 4Magnesium 200.7 ug/L 50 540 10,000 14,0Manganese 200.7 ug/L 50 13 500 200Mercury 1631E ng/L 50,000 12,400 26,000 319Molybdenum 200.7 ug/L 2 1.6 40 6Nickel 200.8 ug/L 2 0.89 4 3Selenium 200.8 ug/L 50 16 100 1Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 950Thallium 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 4Vanadium 200.8 ug/L 2 1.7 10 2Zinc 200.7 ug/L 2 9.1 40 19
B – Analyte was found in the blank and sample. 

J – Result measured above the MDL, but less than the quantitation limit. 

Table C5-7. Influent to FGD Wastewater Treatment System, Set 3 Analytical Results, Miam

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Con

Classicals Ammonia 350.1 mg/L 4 0.22 4 1Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 7Nitrogen, Total Kjeldahl 351.2 mg/L 5 1.9 25 9Biochemical Oxygen Demand 5210B mg/L 1 0.59 5 4Chemical Oxygen Demand 410.4 mg/L 5 20 100 4Chloride 300.0 mg/L 500 130 1,500 11Sulfate 300.0 mg/L 1,000 230 5,000 27Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0Total Dissolved Solids 2540C mg/L 1 470 1,000 55Total Suspended Solids 2540D mg/L 1 140 500 27Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.0Total MetalsAluminum 200.7 ug/L 50 240 5,000 370Antimony 200.8 ug/L 2 0.72 2 4Arsenic 200.8 ug/L 2 1.2 4 4Barium 200.7 ug/L 2 2.5 20 4Beryllium 200.7 ug/L 2 0.71 2 1Boron 200.7 ug/L 500 1,700 50,000 1,00Cadmium 200.8 ug/L 2 1.2 4 5Calcium 200.7 ug/L 50 1,700 10,000 1,50Chromium 200.8 ug/L 2 3.3 8 1,6Cobalt 200.7 ug/L 2 1.1 20 5Copper 200.8 ug/L 2 0.96 4 5Iron 200.7 ug/L 2 32 200 600
B – Analyte was found in the blank and sample. 

J – Result measured above the MDL, but less than the quantitation limit. 

Table C5-7. Influent to FGD Wastewater Treatment System, Set 3 Analytical Results, Miam

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Con

Lead 200.8 ug/L 2 0.73 2 2Magnesium 200.7 ug/L 500 5,400 100,000 9,70Manganese 200.7 ug/L 50 13 500 200Mercury 1631E ng/L 40,000 9,650 20,200 224Molybdenum 200.7 ug/L 2 1.6 40 6Nickel 200.8 ug/L 5 2.2 10 4,2Selenium 200.8 ug/L 10 3.1 20 1,6Silver 200.8 ug/L 2 0.59 2 2Sodium 200.7 ug/L 2 180 10,000 750Thallium 200.8 ug/L 2 0.47 2 3Tin 200.7 ug/L 2 4.8 200 1Titanium 200.7 ug/L 2 1.6 20 2,0Vanadium 200.8 ug/L 2 1.7 10 1,6Zinc 200.7 ug/L 50 230 1,000 16
B – Analyte was found in the blank and sample. 

E – MS and/or MSD exceeded the calibration range. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. 

Table C5-8. Influent to FGD Wastewater Treatment System, Set 4 Analytical Results, Miam

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Con

Classicals Ammonia 350.1 mg/L 1 0.055 1 8Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 5Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 4Biochemical Oxygen Demand 5210B mg/L 1 7.1 60 11Chemical Oxygen Demand 410.4 mg/L 10 41 200 85Chloride 300.0 mg/L 200 51 600 8,1Sulfate 300.0 mg/L 500 120 2,500 21,Cyanide, Total 4500 CN E mg/L 10 0.2 1 1Total Dissolved Solids 2540C mg/L 1 240 500 41,Total Suspended Solids 2540D mg/L 1 140 500 30,Phosphorus, Total 365.1 mg/L 40 0.2 2 2Total MetalsAluminum 200.7 ug/L 2 9.4 200 360Antimony 200.8 ug/L 2 0.72 2 4Arsenic 200.8 ug/L 2 1.2 4 56Barium 200.7 ug/L 2 2.5 20 50Beryllium 200.7 ug/L 2 0.71 2 2Boron 200.7 ug/L 200 670 20,000 870Cadmium 200.8 ug/L 2 1.2 4 57Calcium 200.7 ug/L 50 1,700 10,000 1,900Chromium 200.8 ug/L 2 3.3 8 2,0Cobalt 200.7 ug/L 2 1.1 20 53Copper 200.8 ug/L 2 0.96 4 88
B – Analyte was found in the blank and sample. 

E – MS and/or MSD exceeded the calibration range. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. 

Table C5-8. Influent to FGD Wastewater Treatment System, Set 4 Analytical Results, Miam

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Con

Iron 200.7 ug/L 2 32 200 560Lead 200.8 ug/L 2 0.73 2 46Magnesium 200.7 ug/L 50 540 10,000 7,800Manganese 200.7 ug/L 50 13 500 170Mercury 1631E ng/L 10,000 2,480 5,200 367Molybdenum 200.7 ug/L 2 1.6 40 60Nickel 200.8 ug/L 2 0.89 4 3,9Selenium 200.8 ug/L 10 3.1 20 2,1Silver 200.8 ug/L 2 0.59 2 2Sodium 200.7 ug/L 2 180 10,000 430Thallium 200.8 ug/L 2 0.47 2 7Tin 200.7 ug/L 2 4.8 200 2Titanium 200.7 ug/L 2 1.6 20 3,6Vanadium 200.8 ug/L 2 1.7 10 2,4Zinc 200.7 ug/L 2 9.1 40 13,
ND – Not detected (number in parentheses is the quantitation limit). 

4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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

Table C5-9. Effluent from FGD Wastewater Treatment System, Set 1 Analytical Results, Mia

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conc

Classicals Ammonia 350.1 mg/L 1 0.055 1 5.2 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 73 Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 22 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 3.3 Chemical Oxygen Demand 410.4 mg/L 5 20 100 530 Chloride 300.0 mg/L 500 130 1,500 5,800 Sulfate 300.0 mg/L 500 120 2,500 14,000 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.068 Total Dissolved Solids 2540C mg/L 1 47 100 31,000 Total Suspended Solids 2540D mg/L 1 1.1 4 8.4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.36 Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND (20Antimony 200.8 ug/L 2 0.72 2 6.2 Arsenic 200.8 ug/L 2 1.2 4 4.4 Barium 200.7 ug/L 2 2.5 20 130 Beryllium 200.7 ug/L 2 0.71 2 ND (2Boron 200.7 ug/L 250 830 25,000 300,00Cadmium 200.8 ug/L 2 1.2 4 ND (4Calcium 200.7 ug/L 2 69 400 750,00Chromium 200.8 ug/L 2 3.3 8 16 
ND – Not detected (number in parentheses is the quantitation limit). 

4 – MS and/or MSD did not meet laboratory criteria, but sample concentration is four times greater than the matrix spike amount, so control limits are 

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

Table C5-9. Effluent from FGD Wastewater Treatment System, Set 1 Analytical Results, Mia

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conc

Cobalt 200.7 ug/L 2 1.1 20 ND (20Copper 200.8 ug/L 2 0.96 4 ND (4Iron 200.7 ug/L 2 32 200 160 Lead 200.8 ug/L 2 0.73 2 ND (2Magnesium 200.7 ug/L 50 540 10,000 6,000,00Manganese 200.7 ug/L 2 0.51 20 130 Mercury 1631E ng/L 20 4.87 10.2 256 Molybdenum 200.7 ug/L 2 1.6 40 170 Nickel 200.8 ug/L 2 0.89 4 2.8 Selenium 200.8 ug/L 5 1.6 10 360 Silver 200.8 ug/L 2 0.59 2 ND (2Sodium 200.7 ug/L 2 180 10,000 580,00Thallium 200.8 ug/L 2 0.47 2 6.3 Tin 200.7 ug/L 2 4.8 200 ND (20Titanium 200.7 ug/L 2 1.6 20 ND (20Vanadium 200.8 ug/L 2 1.7 10 14 Zinc 200.7 ug/L 2 9.1 40 9.6 
ND – Not detected (number in parentheses is the quantitation limit). 

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

B – Analyte was found in the blank and sample. Est – Estimated value. 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 C5-10. Effluent from FGD Wastewater Treatment System, Set 2 Analytical Results, Mi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Con

Classicals Ammonia 350.1 mg/L 1 0.055 1 5.Nitrate Nitrite as N 353.2 mg/L 5 0.095 0.5 4Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 2Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 2.Chemical Oxygen Demand 410.4 mg/L 5 20 100 47Chloride 300.0 mg/L 500 130 1,500 8,2Sulfate 300.0 mg/L 500 120 2,500 11,0Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.2Total Dissolved Solids 2540C mg/L 1 94 200 28,0Total Suspended Solids 2540D mg/L 1 1.1 4 4.Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.0Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND (Antimony 200.8 ug/L 2 0.72 2 4 Arsenic 200.8 ug/L 2 1.2 4 3.Barium 200.7 ug/L 2 2.5 20 13Beryllium 200.7 ug/L 2 0.71 2 ND Boron 200.7 ug/L 50 170 5,000 210,Cadmium 200.8 ug/L 2 1.2 4 ND 
ND – Not detected (number in parentheses is the quantitation limit). 

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

B – Analyte was found in the blank and sample. Est – Estimated value. 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 C5-10. Effluent from FGD Wastewater Treatment System, Set 2 Analytical Results, Mi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Con

Calcium 200.7 ug/L 50 1,700 10,000 1,000Chromium 200.8 ug/L 2 3.3 8 1Cobalt 200.7 ug/L 2 1.1 20 ND Copper 200.8 ug/L 2 0.96 4 ND Iron 200.7 ug/L 2 32 200 14Lead 200.8 ug/L 2 0.73 2 ND Magnesium 200.7 ug/L 50 540 10,000 5,200Manganese 200.7 ug/L 2 0.51 20 14Mercury 1631E ng/L 100 24.1 50.5 29Molybdenum 200.7 ug/L 2 1.6 40 14Nickel 200.8 ug/L 2 0.89 4 3.Selenium 200.8 ug/L 5 1.6 10 29Silver 200.8 ug/L 2 0.59 2 ND Sodium 200.7 ug/L 2 180 10,000 670,Thallium 200.8 ug/L 2 0.47 2 4.Tin 200.7 ug/L 2 4.8 200 ND (Titanium 200.7 ug/L 2 1.6 20 ND Vanadium 200.8 ug/L 2 1.7 10 1Zinc 200.7 ug/L 2 9.1 40 2
ND – Not detected (number in parentheses is the quantitation limit). 

B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table C5-11. Effluent from FGD Wastewater Treatment System, Set 3 Analytical Results, Mi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Con

Classicals Ammonia 350.1 mg/L 10 0.55 10 4Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 5Nitrogen, Total Kjeldahl 351.2 mg/L 10 0.77 10 7Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 3Chemical Oxygen Demand 410.4 mg/L 5 20 100 5Chloride 300.0 mg/L 500 130 1,500 7,2Sulfate 300.0 mg/L 500 120 2,500 14,Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.Total Dissolved Solids 2540C mg/L 1 94 200 32,Total Suspended Solids 2540D mg/L 1 1.1 4 8Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.0Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND Antimony 200.8 ug/L 2 0.72 2 5Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 1Beryllium 200.7 ug/L 2 0.71 2 ND Boron 200.7 ug/L 50 170 5,000 520Cadmium 200.8 ug/L 2 1.2 4 ND Calcium 200.7 ug/L 50 1,700 10,000 950Chromium 200.8 ug/L 2 3.3 8 8Cobalt 200.7 ug/L 2 1.1 20 ND Copper 200.8 ug/L 2 0.96 4 
ND – Not detected (number in parentheses is the quantitation limit). 

B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table C5-11. Effluent from FGD Wastewater Treatment System, Set 3 Analytical Results, Mi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Con

Iron 200.7 ug/L 2 32 200 1Lead 200.8 ug/L 2 0.73 2 ND Magnesium 200.7 ug/L 50 540 10,000 6,00Manganese 200.7 ug/L 2 0.51 20 1,0Mercury 1631E ng/L 20 4.97 10.4 1Molybdenum 200.7 ug/L 2 1.6 40 3Nickel 200.8 ug/L 2 0.89 4 4Selenium 200.8 ug/L 5 1.6 10 6Silver 200.8 ug/L 2 0.59 2 ND Sodium 200.7 ug/L 2 180 10,000 660Thallium 200.8 ug/L 2 0.47 2 6Tin 200.7 ug/L 2 4.8 200 ND Titanium 200.7 ug/L 2 1.6 20 ND Vanadium 200.8 ug/L 2 1.7 10 2Zinc 200.7 ug/L 2 9.1 40 ND 
ND – Not detected (number in parentheses is the quantitation limit). 

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 C5-12. Effluent from FGD Wastewater Treatment System, Set 4 Analytical Results, Mi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Co

Classicals Ammonia 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 5 0.38 5 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 NChemical Oxygen Demand 410.4 mg/L 10 41 200 Chloride 300.0 mg/L 200 51 600 5Sulfate 300.0 mg/L 200 46 1,000 9Cyanide, Total 4500 CN E mg/L 10 0.2 1 Total Dissolved Solids 2540C mg/L 1 94 200 2Total 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 ND 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 NBoron 200.7 ug/L 200 670 20,000 59Cadmium 200.8 ug/L 2 1.2 4 NCalcium 200.7 ug/L 50 1,700 10,000 1,1Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 ND 
ND – Not detected (number in parentheses is the quantitation limit). 

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 C5-12. Effluent from FGD Wastewater Treatment System, Set 4 Analytical Results, Mi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Co

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 NMagnesium 200.7 ug/L 50 540 10,000 4,4Manganese 200.7 ug/L 2 0.51 20 1Mercury 1631E ng/L 100 24.8 52 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 NSodium 200.7 ug/L 2 180 10,000 38Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 ND Titanium 200.7 ug/L 2 1.6 20 ND Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 ND 
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 C5-13. Influent to FGD Wastewater Treatment System Field Blank, Set 1 Analytical Results

Analyte Method Unit 

Dilution 

Factor 

Sample-Specific 

MDL 

Sample-Specific 

QL Concen

Total MetalsAluminum 200.7 ug/L 2 9.4 200 13 Antimony 200.8 ug/L 2 0.72 2 ND (2) Arsenic 200.8 ug/L 2 1.2 4 ND (4) Barium 200.7 ug/L 2 2.5 20 ND (20Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 2 6.7 200 30 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 ND (400Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 ND (20Copper 200.8 ug/L 2 0.96 4 ND (4) Iron 200.7 ug/L 2 32 200 89 Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 2 21 400 21 Manganese 200.7 ug/L 2 0.51 20 ND (20Mercury 1631E ng/L 1 0.24 0.5 ND (0.5Molybdenum 200.7 ug/L 2 1.6 40 ND (40Nickel 200.8 ug/L 2 0.89 4 ND (4) Selenium 200.8 ug/L 2 0.62 4 ND (4) Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 250 Thallium 200.8 ug/L 2 0.47 2 ND (2) Tin 200.7 ug/L 2 4.8 200 ND (200
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 C5-13. Influent to FGD Wastewater Treatment System Field Blank, Set 1 Analytical Results

Analyte Method Unit 

Dilution 

Factor 

Sample-Specific 

MDL 

Sample-Specific 

QL Concen

Titanium 200.7 ug/L 2 1.6 20 ND (20Vanadium 200.8 ug/L 2 1.7 10 ND (10Zinc 200.7 ug/L 2 9.1 40 ND (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. 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 C5-14. Effluent from FGD Wastewater Treatment System Field Blank, Set 1 Analytical Resu

Analyte Method Unit 

Dilution 

Factor 

Sample-Specific 

MDL 

Sample-Specific 

QL Co

Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND (Antimony 200.8 ug/L 2 0.72 2 ND Arsenic 200.8 ug/L 2 1.2 4 ND Barium 200.7 ug/L 2 2.5 20 ND (Beryllium 200.7 ug/L 2 0.71 2 ND Boron 200.7 ug/L 2 6.7 200 44 Cadmium 200.8 ug/L 2 1.2 4 ND Calcium 200.7 ug/L 2 69 400 ND (4Chromium 200.8 ug/L 2 3.3 8 ND Cobalt 200.7 ug/L 2 1.1 20 ND (Copper 200.8 ug/L 2 0.96 4 ND Iron 200.7 ug/L 2 32 200 ND (2Lead 200.8 ug/L 2 0.73 2 ND Magnesium 200.7 ug/L 2 21 400 84 Manganese 200.7 ug/L 2 0.51 20 0.Mercury 1631E ng/L 1 0.24 0.5 ND (Molybdenum 200.7 ug/L 2 1.6 40 ND (Nickel 200.8 ug/L 2 0.89 4 ND Selenium 200.8 ug/L 2 0.62 4 ND Silver 200.8 ug/L 2 0.59 2 ND Sodium 200.7 ug/L 2 180 10,000 48Thallium 200.8 ug/L 2 0.47 2 ND Tin 200.7 ug/L 2 4.8 200 ND (
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 C5-14. Effluent from FGD Wastewater Treatment System Field Blank, Set 1 Analytical Resu

Analyte Method Unit 

Dilution 

Factor 

Sample-Specific 

MDL 

Sample-Specific 

QL Co

Titanium 200.7 ug/L 2 1.6 20 ND (Vanadium 200.8 ug/L 2 1.7 10 ND (Zinc 200.7 ug/L 2 9.1 40 ND (
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 C5-15. Effluent from FGD Wastewater Treatment System Field Blank, Set 2 Analytical Resu

Analyte Method Unit 

Dilution 

Factor 

Sample-Specific 

MDL 

Sample-Specific 

QL Con

Total MetalsAluminum 200.7 ug/L 2 9.4 200 14 Antimony 200.8 ug/L 2 0.72 2 ND (2Arsenic 200.8 ug/L 2 1.2 4 ND (4Barium 200.7 ug/L 2 2.5 20 ND (2Beryllium 200.7 ug/L 2 0.71 2 ND (2Boron 200.7 ug/L 2 6.7 200 34 Cadmium 200.8 ug/L 2 1.2 4 ND (4Calcium 200.7 ug/L 2 69 400 ND (40Chromium 200.8 ug/L 2 3.3 8 ND (8Cobalt 200.7 ug/L 2 1.1 20 ND (2Copper 200.8 ug/L 2 0.96 4 ND (4Iron 200.7 ug/L 2 32 200 ND (20Lead 200.8 ug/L 2 0.73 2 ND (2Magnesium 200.7 ug/L 2 21 400 55 Manganese 200.7 ug/L 2 0.51 20 0.7 Mercury 1631E ng/L 1 0.24 0.5 ND (0Molybdenum 200.7 ug/L 2 1.6 40 ND (4Nickel 200.8 ug/L 2 0.89 4 ND (4Selenium 200.8 ug/L 2 0.62 4 ND (4Silver 200.8 ug/L 2 0.59 2 ND (2Sodium 200.7 ug/L 2 180 10,000 ND (10,Thallium 200.8 ug/L 2 0.47 2 ND (2Tin 200.7 ug/L 2 4.8 200 ND (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 C5-15. Effluent from FGD Wastewater Treatment System Field Blank, Set 2 Analytical Resu

Analyte Method Unit 

Dilution 

Factor 

Sample-Specific 

MDL 

Sample-Specific 

QL Con

Titanium 200.7 ug/L 2 1.6 20 ND (2Vanadium 200.8 ug/L 2 1.7 10 2.2 Zinc 200.7 ug/L 2 9.1 40 ND (4
ND – Not detected (number in parentheses is the quantitation limit). 

B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table C5-16. Effluent from FGD Wastewater Treatment System Field Blank, Set 3 Analytical 

Miami Fort 

Analyte Method Unit

Dilution 

Factor 

Sample-Specific 

MDL 

Sample-Specific 

QL Concen

Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200Antimony 200.8 ug/L 2 0.72 2 ND (2) Arsenic 200.8 ug/L 2 1.2 4 ND (4) Barium 200.7 ug/L 2 2.5 20 ND (20) Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 2 6.7 200 95 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 76 Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 ND (4) Iron 200.7 ug/L 2 32 200 ND (200Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 2 21 400 170 Manganese 200.7 ug/L 2 0.51 20 0.8 Mercury 1631E ng/L 1 0.24 0.5 ND (0.5Molybdenum 200.7 ug/L 2 1.6 40 ND (40) Nickel 200.8 ug/L 2 0.89 4 ND (4) Selenium 200.8 ug/L 2 0.62 4 1.1 Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 610 Thallium 200.8 ug/L 2 0.47 2 ND (2) Tin 200.7 ug/L 2 4.8 200 ND (200
ND – Not detected (number in parentheses is the quantitation limit). 

B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table C5-16. Effluent from FGD Wastewater Treatment System Field Blank, Set 3 Analytical 

Miami Fort 

Analyte Method Unit

Dilution 

Factor 

Sample-Specific 

MDL 

Sample-Specific 

QL Concen

Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 2.1 Zinc 200.7 ug/L 2 9.1 40 ND (40) 
ND – Not detected (number in parentheses is the quantitation limit). 

B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table C5-17. Effluent from FGD Wastewater Treatment System Field Blank, Set 4 Analytical Resu

Analyte Method Unit

Dilution 

Factor 

Sample-Specific 

MDL 

Sample-Specific 

QL Co

Total MetalsAluminum 200.7 ug/L 2 9.4 200 9.9 Antimony 200.8 ug/L 2 0.72 2 ND Arsenic 200.8 ug/L 2 1.2 4 ND Barium 200.7 ug/L 2 2.5 20 ND (Beryllium 200.7 ug/L 2 0.71 2 ND Boron 200.7 ug/L 2 6.7 200 62 Cadmium 200.8 ug/L 2 1.2 4 ND Calcium 200.7 ug/L 2 69 400 71 Chromium 200.8 ug/L 2 3.3 8 ND Cobalt 200.7 ug/L 2 1.1 20 ND (Copper 200.8 ug/L 2 0.96 4 ND Iron 200.7 ug/L 2 32 200 58 Lead 200.8 ug/L 2 0.73 2 ND Magnesium 200.7 ug/L 2 21 400 27 Manganese 200.7 ug/L 2 0.51 20 0.Mercury 1631E ng/L 1 0.24 0.5 ND (Molybdenum 200.7 ug/L 2 1.6 40 ND (Nickel 200.8 ug/L 2 0.89 4 ND Selenium 200.8 ug/L 2 0.62 4 2.9 Silver 200.8 ug/L 2 0.59 2 ND Sodium 200.7 ug/L 2 180 10,000 ND (10Thallium 200.8 ug/L 2 0.47 2 ND Tin 200.7 ug/L 2 4.8 200 ND (2Titanium 200.7 ug/L 2 1.6 20 ND (
ND – Not detected (number in parentheses is the quantitation limit). 

B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table C5-17. Effluent from FGD Wastewater Treatment System Field Blank, Set 4 Analytical Resu

Analyte Method Unit

Dilution 

Factor 

Sample-Specific 

MDL 

Sample-Specific 

QL Co

Vanadium 200.8 ug/L 2 1.7 10 2.Zinc 200.7 ug/L 2 9.1 40 16 
Section 6 

Data Review Narratives 

[A concentration noted as “XXX” indicates that the sample result applies to a different power plant and has been 

removed.] 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD 

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Donna Tedder, ERG 

Date: 2/9/2012

Subject: FGS Data Review Narrative for Total Mercury – Long-Term Monitoring: 

Month 1 (Part 1)

Frontier Global Sciences (FGS) generated analytical data for total mercury. FGS 

analyzed the samples according to EPA Method 1631E for mercury by Cold Vapor 

Atomic Fluorescence Spectrometry (CVAFS) analysis. 

Table 1 summarizes the 14 samples (excluding laboratory prep blanks) FGS extracted 

and analyzed for total mercury. 

Table 1. Long-Term Monitoring Month 1 (Part 1) Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72041 1010010-01 Aqueous FGD Influent, Set 1 9/30/2010 

72045 1010010-02 Aqueous FGD Effluent, Set 1 9/30/2010

72049 1010010-04 Aqueous FGD Influent Field Blank 9/30/2010

72050 1010010-03 Aqueous FGD Effluent Field Blank, Set 1 9/30/2010 

72091 1009237-07 Aqueous FGD Influent, Set 1 9/28/2010

72095 1009237-08 Aqueous FGD Effluent, Set 1 9/28/2010

72099 1009237-10 Aqueous FGD Influent Field Blank 9/28/2010

72100 1009237-09 Aqueous FGD Effluent Field Blank, Set 1 9/27/2010

72191 1009237-01 Aqueous FGD Influent Set 1 9/29/2010 

72195 1009237-02 Aqueous FGD SBR Influent, Set 1 9/29/2010

72199 1009237-03 Aqueous FGD SBR Effluent, Set 1 9/29/2010

72203 1009237-06 Aqueous FGD Influent Field Blank 9/29/2010

72204 1009237-04 Aqueous FGD SBR Influent Field Blank, Set 1 9/28/2010

72208 1009237-05 Aqueous FGD SBR Effluent Field Blank, Set 1 9/28/2010

SUMMARY 

The samples were prepared according to EPA Method 1631E to be analyzed by CVAFS. 
2

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. 

BLANKS 

All the preparation blanks or laboratory reagent blanks (LRBs) and the continuing 

calibration blanks (CCBs) met method-specified criteria. Some preparation blanks had 

mercury levels greater than the MDL (0.24 ng/L), but less than the RL associated with 

each individual blank (different RLs based on preparation). Because all of the blank 

results were less than the RL, no samples were qualified based on these preparation blank 

results. 

DUPLICATES 

No field duplicate samples were collected with these sampling episodes. Two samples 

were analyzed in duplicate at the laboratory, samples 72095 and 72195. The relative 

percent difference (RPD) for samples 72095 and 72195 were 2.45% and 3.32%, 

respectively. The laboratory’s RPD criteria between analytical duplicates is 24%. 

LABORATORY CONTROL SAMPLES 

All laboratory control samples were within FGS’s control limits of 80-120% recovery 

and 24% RPD. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES 

Matrix spikes (MS) and matrix spike duplicates (MSD) were performed on samples 

72095, 72199, and 72195 for the total mercury analyses. All aqueous MS/MSD 

recoveries were within method specifications of 71-125%. All RPDs met methodspecified criteria. 
3

DETECTION LIMITS 

The laboratory MDL in the synthetic matrix was 0.239 ng/L. Results below this MDL 

were reported as not detected (ND). 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD 

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Randy Mercurio, ERG 

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.8 – Long-Term 

Monitoring: Month 1 (Part 1)

TestAmerica generated analytical data for total metals (antimony, arsenic, cadmium, 

chromium, copper, lead, nickel, selenium, silver, thallium, and vanadium) for these longterm monitoring samples. The samples were analyzed according to EPA Method 200.8. 

Table 1 summarizes the samples TestAmerica extracted and analyzed for total metals by 

EPA Method 200.8. 

Table 1. Long-Term Monitoring Month 1 (Part 1) Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72041 FGD Influent, Set 1 280-7918-1 Aqueous 9/30/2010 10/1/2010

72045 FGD Effluent, Set 1 280-7918-2 Aqueous 9/30/2010 10/1/2010

72049 FGD Influent Field Blank 280-7918-4 Aqueous 9/30/2010 10/1/2010

72050 FGD Effluent Field Blank, Set 1 280-7918-3 Aqueous 9/30/2010 10/1/2010

72091 FGD Influent, Set 1 280-7817-1 Aqueous 9/28/2010 9/29/2010

72095 FGD Effluent, Set 1 280-7817-2 Aqueous 9/28/2010 9/29/2010

72099 FGD Influent Field Blank, Set 1 280-7817-4 Aqueous 9/28/2010 9/29/2010

72100 FGD Effluent Field Blank, Set 1 280-7817-3 Aqueous 9/28/2010 9/29/2010

72191 FGD Influent, Set 1 280-7870-1 Aqueous 9/29/2010 9/30/2010

72195 FGD SBR Influent, Set 1 280-7870-2 Aqueous 9/29/2010 9/30/2010

72199 FGD SBR Effluent, Set 1 280-7870-3 Aqueous 9/29/2010 9/30/2010

72203 FGD Influent Field Blank 280-7870-6 Aqueous 9/29/2010 9/30/2010

72204 FGD SBR Influent Field Blank, 

Set 1 

280-7870-4 Aqueous 9/29/2010 9/30/2010

72208 FGD SBR Effluent Field Blank, 

Set 2 

280-7870-5 Aqueous 9/29/2010 9/30/2010
2

SUMMARY 

The samples were prepared for total metals analysis according to TestAmerica’s “FGD 

ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Elements 

Analysis in Flue Gas Desulfurization Wastewaters,” dated October 6, 2010, based on 

EPA Method 200.8, by ICP/MS analysis. 

Any significant findings are summarized below. No additional data qualifiers were 

required. 

• The matrix spike (MS) and matrix spike duplicate (MSD) recoveries for total 

silver for samples 72045 and 72095 failed the EPA Method 200.8 control limits of 

70–130%. 

• The MS/MSD relative percent difference (RPD) for total silver for sample 72095 

failed the FGD ICP/MS SOP control limits of ±20%. 

• The post digestion spike (PDS) recoveries for the following analytes failed 

TestAmerica’s control limits of 85–115%: arsenic, chromium, selenium, silver, 

and vanadium. 

INTERNAL STANDARDIZATION 

All internal standards used by TestAmerica were within the method criteria. 

INITIAL CALIBRATION 

TestAmerica performed the initial calibrations on each analysis 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 (RL); however, some elements 

were above the MDL and flagged with a “J” qualifier. No additional qualifiers were 

required for method blanks. 

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank 

(CCB)) were less than the RL; however, some elements were above the MDL and 

flagged with a “J” qualifier. No additional qualifiers were required for instrument blanks. 
3

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

All CRI samples passed TestAmerica’s SOP control limits of 50–150% recovery. 

LABORATORY CONTROL SAMPLES (LCS) 

All LCS samples passed the method QC limits of 85–115% recovery. 

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION 

Based on TestAmerica’s SOP, all interference check sample A (ICSA) results had 

analytes of interest with concentrations less than the RL or less than five times the RL 

when known inherent contaminants are present in the stock solution used to make the 

ICS. 

All interference check sample B (ICSAB) synthetic spikes recovered within 

TestAmerica’s SOP criteria of 70–130% of the true value. 

SERIAL DILUTION 

The serial dilution performed on sample 72095 passed TestAmerica’s criteria of ±10% 

difference. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES 

MS and MSD were performed on samples 72045 and 72095. The total selenium results in 

the MS and MSD samples for sample 72045 and the MS sample for sample 72095 failed 

the 70-130% recovery method control limits and were flagged with a “4” qualifier 

indicating concentrations in the parent samples were greater than four times the spike 

amounts. These data were considered acceptable based on the LCS passing the method 

control limits. 

The total silver results in the MS and MSD samples for both samples 72045 and 72095 

failed the 70-130% method control limits with low recoveries and were flagged with an 

“F” qualifier. Additionally, the RPD for silver between the MS and MSD for sample 

72095 failed the ICP/MS SOP ±20% control limits. The poor recoveries and RPD of 

silver are probably due to high sulfates in this episode’s samples capable of forming 

insoluble silver sulfide and/or silver sulfate. 
4

Otherwise, all MS/MSD spike recoveries were within the method control limits of 70-

130% and the RPD for the MS/MSDs were within the FGD ICP/MS SOP control limits 

of ±20 percent. No additional data qualifiers were required. 

POST DIGESTION SPIKES 

The PDS performed on sample 72095 passed TestAmerica’s control limits of 85–115% 

recovery for all analytes, except for arsenic, chromium, selenium, silver, and vanadium, 

which were all flagged with a “W” qualifier. No additional data qualifiers were required 

for PDS samples. 

DETECTION LIMITS 

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water. 
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: 2/9/2012 

Subject: TestAmerica Data Review Narrative for Total Metals by 200.7 – Long-Term 

Monitoring: Month 1 (Part 1)

TestAmerica generated analytical data for total metals (aluminum, boron, barium, 

beryllium, calcium, cobalt, iron, magnesium, manganese, molybdenum, sodium, tin, 

titanium, and zinc) for these long-term monitoring samples. The samples were analyzed 

according to EPA Method 200.7. 

Table 1 summarizes the samples TestAmerica extracted and analyzed for total metals by 

EPA Method 200.7.

Table 1. Long-Term Monitoring Month 1 (Part 1) Total Metals – Sample 

Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72041 FGD Influent, Set 1 280-7918-1 Aqueous 9/30/2010 10/1/2010

72045 FGD Effluent, Set 1 280-7918-2 Aqueous 9/30/2010 10/1/2010

72049 FGD Influent Field Blank 280-7918-4 Aqueous 9/30/2010 10/1/2010

72050 FGD Effluent Field Blank, 

Set 1 

280-7918-3 Aqueous 9/30/2010 10/1/2010

72091 FGD Influent, Set 1 280-7817-1 Aqueous 9/28/2010 9/29/2010

72095 FGD Effluent, Set 1 280-7817-2 Aqueous 9/28/2010 9/29/2010

72099 FGD Influent Field Blank, 

Set 1 

280-7817-4 Aqueous 9/28/2010 9/29/2010

72100 FGD Effluent Field Blank, 

Set 1 

280-7817-3 Aqueous 9/28/2010 9/29/2010

72191 FGD Influent, Set 1 280-7870-1 Aqueous 9/29/2010 9/30/2010

72195 FGD SBR Influent, Set 1 280-7870-2 Aqueous 9/29/2010 9/30/2010

72199 FGD SBR Effluent, Set 1 280-7870-3 Aqueous 9/29/2010 9/30/2010

72203 FGD Influent Field Blank 280-7870-6 Aqueous 9/29/2010 9/30/2010

72204 FGD SBR Influent Field 

Blank, Set 1 

280-7870-4 Aqueous 9/29/2010 9/30/2010

72208 FGD SBR Effluent Field 

Blank, Set 2 

280-7870-5 Aqueous 9/29/2010 9/30/2010
2

SUMMARY 

The samples were prepared for total metals analysis according to TestAmerica’s SOP for 

ICP Analysis for Trace Metals by Method 200.7. Any significant findings are 

summarized below. No additional data qualifiers were required. 

• The matrix spike (MS) and matrix spike duplicate (MSD) recoveries for total 

barium for sample 72095 failed the EPA Method 200.7 control limits of 70–

130%. 

• The MS/MSD relative percent difference (RPD) for total magnesium for sample 

72095 failed TestAmerica’s SOP control limits of ±20%. 

• The post digestion spike (PDS) for titanium for sample 72095 failed 

TestAmerica’s control limits of 85–115% recovery. 

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 

TestAmerica performed the initial calibrations on each analysis day. The initial 

calibration for the ICP analysis consisted of a blank and one calibration standard. 

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS 

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 (RL); however, some elements 

were above the method detection limit (MDL) and were flagged with the “J” qualifier. 

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank 

(CCB)) were less than the RL; however, some elements were above the MDL and were 

flagged with the “J” qualifier. 
3

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

All CRI samples passed TestAmerica’s SOP control limits of 50–150% recovery. 

LABORATORY CONTROL SAMPLES (LCS) 

All LCSs passed the method control limits of 85–115% recovery. 

INTERFERENCE CHECK SOLUTIONS 

Interference checks were performed using the synthetic matrix as the check solution. All 

data quality objectives met TestAmerica’s SOP criteria.

SERIAL DILUTION (SRD) 

Serial dilutions were performed for each batch of total samples. All serial dilution percent 

differences were less than 10% as required by TestAmerica’s SOP. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

MS and MSDs were performed on the total samples of 72095 and 72045. Some elements 

with high concentrations 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. 

These data were considered acceptable based on the LCS passing the method control 

limits. Otherwise, all MS/MSD spike recoveries were within the method control criteria 

of 70-130%, except for barium for sample 72095, which had a recovery of 65% and was 

qualified with an “F”. The RPD for all MS/MSDs were within TestAmerica’s ± 20% 

requirement, except for magnesium for sample 72095. No additional data qualifiers were 

needed. 

POST DIGESTION SPIKE (PDS) 

The PDS performed on sample 72095 passed TestAmerica’s control limits of 85–115% 

recovery for all analytes except titanium, which was qualified with a “W”. No additional 

data qualifiers were required. 

DETECTION LIMITS 

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water. 
1 

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD 

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Donna Tedder, ERG 

Date: 2/9/2012 

Subject: TestAmerica Data Review Narrative for Classicals Analyses – Long-Term 

Monitoring: Month 1 (Part 1) 

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for these long-term monitoring samples. All samples were tested for the 

following analytes: 

• Ammonia by EPA method 350.1, 

• Biochemical Oxygen Demand – 5 day (BOD5) by SM 5210B, 

• Chloride and Sulfate by EPA method 300.0, 

• Chemical Oxygen Demand (COD) by EPA method 410.4, 

• Cyanide (total) by SM 4500 CN- E, 

• Nitrate/Nitrite by EPA method 353.2, 

• Phosphorus (total) by EPA method 365.1, 

• Total Dissolved Solids (TDS) by SM 2540C, 

• Total Kjeldahl Nitrogen (TKN) by EPA method 351.2, and 

• Total Suspended Solids (TSS) by SM 2540D. 

Table 1 summarizes the seven samples that TestAmerica analyzed for the above analytes. 

Table 1. Long-Term Monitoring Month 1 (Part 1) Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72041 Water FGD Influent, Set 1 9/30/10 

72045 Water FGD Effluent, Set 1 9/30/10 

72091 Water FGD Influent, Set 1 9/28/10 

72095 Water FGD Effluent, Set 1 9/28/10 

72191 Water FGD Influent, Set 1 9/29/10 

72195 Water FGD SBR Influent, Set 1 9/29/10 

72199 Water FGD SBR Effluent, Set 1 9/29/10 
2 

SUMMARY 

All samples were analyzed within the holding time specified in 40 CFR 136 Table II. All 

samples were preserved appropriately unless otherwise specified below. 

 

Field duplicate samples were not collected for these episodes. Depending on the method, 

a laboratory duplicate was analyzed, instead. The Relative Percent Difference (RPD) 

between the sample and its duplicate was less than 20% unless otherwise noted below. 

If applicable, the appropriate number of standards was used to create a calibration curve. 

If sample results were above the highest standard used to create the curve, the sample was 

diluted and reanalyzed. All sample results were between the lowest and highest standards 

unless noted below. Additionally, 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 sample 72045 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 

No issues were identified by the data reviewer. 

BOD5 

TestAmerica analyzed five dilutions, but no dilutions had a dissolved oxygen (DO) 

depletion greater than 2.0 mg/L for sample 72041 and 72091. Therefore, BOD5 was 

reported as not detected for these samples. The rest of the samples had at least one 

dilution with a DO depletion greater than 2.0 mg/L. As required in the method, the final 

result was calculated by taking the average of the results for all dilutions with a DO 

depletion greater than 2.0 mg/L and a final DO greater than 1.0 mg/L. 

BOD was not detected above the RL in any method blanks. However, for one batch, the 

results for the three water/unseeded blanks were 0.22 mg/L, 0.14 mg/L, and 0.16 mg/L. 
3 

One of these water blanks was above the method control criteria of 0.20 mg/L. However, 

all samples contained in this batch (samples 72041 and 72045) were either qualified with 

a “J” meaning that the sample result was an estimated value because it was below the RL 

or BOD was not detected in the sample, so no further qualification was necessary. 

One of the three batches had a seed correction factor lower than 0.6 mg/L. The seed 

correction factors were 0.6267 mg/L, 0.5776 mg/L, and 0.6384 mg/L for batches 33523, 

33769, and 33938, respectively. Unlike previous episodes, TestAmerica did not flag 

samples in batch 33769 with an “s” indicating the seed correction blank (SCB) recovery 

was low. This low seed correction factor suggests that samples 72191, 72195, and 72199 

may be biased low. Therefore, these samples were also flagged with an “s”. Sample 

72191 was already flagged by TestAmerica with a “J” meaning that the sample result was 

an estimated value because it was below the RL, so no further qualification was 

necessary. However, samples 72195 and 72199 were flagged as minimum values. Due to 

the short holding time for the analysis, the samples could not be reanalyzed. 

All glucose-glutamic acid standards and laboratory duplicates were analyzed 

appropriately and met the criteria specified in SM 5210B. 

Chloride and Sulfate 

The MS and matrix spike duplicate (MSD) results for sample 72045 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/MSD results will be qualified as estimated 

values. The LFB associated with this sample met the method criteria. The analyzed result 

for sample 72045 was within the calibration curve, so there was no need to qualify this 

sample. 

COD 

The percent recovery for the MSD analyses for sample 72045 was below the control 

limits of 90-110% required by EPA method 410.4. The percent recoveries for the MS and 

MSD analyses for this sample were 109% and 87%, respectively. Because the MS 

percent recovery met the method criteria and an MSD is not required by the method, 

sample 72045 was not qualified. The LFB percent recoveries associated with sample 

72045 met the method criteria. 

Cyanide 

Samples 72041 and 72045 were received by the laboratory at neutral pH. The lab added 

more NaOH to increase the pH to greater than 10 S.U. These samples are qualified as 

estimated values. 

Results for the following samples were less than the lowest calibration standard (0.01 

mg/L): 72095, 72195, and 72199. Because all of these samples were already flagged by 
4 

TestAmerica with a “J”, meaning the sample result was an estimated value because it was 

below the RL, no further qualification was necessary. 

The percent recoveries for the MS and MSD analyses of sample 72045 were both 85%, 

which is outside of the laboratory control criteria of 90-110%. However, because there 

are no criteria for MS/MSD analyses specified in SM 4500 CN- E, no further 

qualification was necessary. 

Nitrate/Nitrite 

No issues were identified by the data reviewer. 

Phosphorus 

The percent recoveries for the MS/MSD analysis of sample 72045 were not within the 

control limits of 90-110% specified in EPA Method 365.1 or within the laboratory 

control limits of 71-128%. The percent recoveries of the MS and MSD samples were 

19% and 21%, respectively. The result for sample 72045 was only slightly above the RL. 

This low sample result could have caused the low percent recovery. Nevertheless, sample 

72045 was qualified as a minimum value. The LFB percent recovery met the method 

criteria. 

TDS 

Constant weight was not achieved after 3 drying cycles for all samples. 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 72045 and 72191 were less than 10% 

as required by SM 2540C. However, the RPD for sample 72091 was 14%. Because the 

RPD was greater than the method control limits, sample 72091 was qualified as an 

estimated value. 

TDS was detected at 6.0 mg/L in the method blank associated with samples 72191, 

72195, and 72199. The method blank result was greater than the MDL (4.7 mg/L), but 

less than the RL (10 mg/L). No qualification was necessary because the blank result was 

less than the RL. 

TKN 

The percent recovery for the LFB associated with samples 72041, 72045, 72091, 72095, 

72191, 72195, and 72199 was not within the method control limits of 90-110%, but was 
5 

within the laboratory control limits of 77-115%. The percent recoveries for the LFB and 

LFBD were 84% and 86%, respectively. Because the percent recovery of the LFB was 

below the method criteria, samples 72041, 72045, 72091, 72095, 72191, 72195, and 

72199 were qualified as minimum values. 

TestAmerica performed MS/MSD analysis on sample 72045. The percent recoveries for 

the MS and MSD samples were 77% and 93%, respectively. The MS sample 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 also not within the laboratory control 

limits, so this may have caused the low MS percent recovery. Also, 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. 

Therefore, sample 72045 was not additionally qualified based on the MS failure because 

it is not possible to determine if the MS failure was a result of matrix interferences or the 

low spiking level. 

TKN was detected at 0.133 mg/L in the LRB associated with samples 72041, 72045, 

72091, 72095, 72191, 72195, and 72199. 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, no samples were qualified based on the LRB result. 

TSS 

The RPD for the laboratory duplicate of sample 72045 was 13%. This RPD was greater 

than the method control criteria of 10%. Sample 72045 and its duplicate were already 

qualified by TestAmerica with a “J” meaning that the result is an estimated value because 

the result is below the RL, so no further qualification was necessary. 

Table 2. Data Review Summary Table 

Sample Analyte Qualifier/Ac

tion 

Reason Level Detected

72191 BOD s SCB Recovery Low XXX mg/L 

72195 BOD s, Minimum 

Value 

SCB Recovery Low XXX mg/L 

72199 BOD s, Minimum 

Value 

SCB Recovery Low XXX mg/L 

72041 Cyanide Estimated 

Value 

Sample pH < 10 S.U. 

at receipt 

XXX mg/L 

72045 Cyanide Estimated 

Value 

Sample pH < 10 S.U. 

at receipt 

XXX mg/L 

72045 Phosphorus Minimum 

Value 

MS % recovery < 

method-specified 

criteria 

XXX mg/L 
6 

Table 2. Data Review Summary Table 

Sample Analyte Qualifier/Ac

tion 

Reason Level Detected

72091 TDS Estimated 

Value 

Lab duplicate RPD > 

method-specified 

criteria 

54,000 mg/L 

72041 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

XXX mg/L 

72045 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

XXX mg/L 

72091 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

59 mg/L 

72095 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

22 mg/L 

72191 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

XXX mg/L 

72195 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

XXX mg/L 

72199 TKN Minimum 

Value 

LFB% recovery < 

method-specified 

criteria 

XXX mg/L 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD 

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Donna Tedder, ERG 

Date: 2/9/2012

Subject: FGS Data Review Narrative for Total Mercury – Long-Term Monitoring: 

Month 2 (Part 1)

Frontier Global Sciences (FGS) generated analytical data for total mercury. FGS 

analyzed the samples according to EPA Method 1631E for mercury by Cold Vapor 

Atomic Fluorescence Spectrometry (CVAFS) analysis. 

Table 1 summarizes the 19 samples (excluding laboratory prep blanks) FGS extracted 

and analyzed for total mercury. 

Table 1. Long-Term Monitoring Month 2 (Part 1) Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71992 1011064-01 Aqueous FGD Influent, Set 2 11/3/2010

71996 1011064-06 Aqueous FGD Bioreactor Influent, Set 2 11/3/2010

72000 1011064-11 Aqueous FGD Bioreactor Effluent, Set 2 11/3/2010

72005 1011064-12 Aqueous FGD Bioreactor Influent Field Blank, Set 2 11/3/2010

72009 1011064-13 Aqueous FGD Bioreactor Effluent Field Blank, Set 2 11/3/2010

72042 1011043-01 Aqueous FGD Influent, Set 2 11/3/2010

72046 1011043-02 Aqueous FGD Effluent, Set 2 11/2/2010

72051 1011043-03 Aqueous FGD Effluent Field Blank, Set 2 11/2/2010

72092 1011031-01 Aqueous FGD Influent, Set 2 11/2/2010 

72096 1011031-02 Aqueous FGD Effluent, Set 2 11/2/2010

72101 1011031-03 Aqueous FGD Effluent, Field Blank, Set 2 11/1/2010

72142 1011032-01 Aqueous FGD Influent, Set 2 11/1/2010

72146 1011032-02 Aqueous FGD Bioreactor Influent, Set 2 11/1/2010

72150 1011032-03 Aqueous FGD Bioreactor Effluent, Set 2 11/1/2010

72155 1011032-04 Aqueous FGD Bioreactor Influent Field Blank, Set 2 11/1/2010

72159 1011032-05 Aqueous FGD Bioreactor Effluent Field Blank, Set 2 11/1/2010

72242 1011061-01 Aqueous FGD Influent, Set 2 11/4/2010

72246 1011061-06 Aqueous FGD Effluent, Set 2 11/4/2010

72251 1011061-07 Aqueous FGD Effluent Field Blank, Set 2 11/3/2010
2

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. The following summarizes the findings from the data review: 

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES 

There were no sample receipt issues in this data package. 

INITIAL CALIBRATION 

FGS performed the initial calibrations on each analysis day. The initial calibration for 

the CVAFS analysis consisted of a blank and five calibration standards with a correlation 

coefficient ≥ 0.995. All method-specified criteria were met. 

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS 

All initial and continuing calibration verifications (ICVs, CCVs) met method-specified 

criteria. 

BLANKS 

All the preparation blanks or laboratory reagent blanks (LRBs) and the continuing 

calibration blanks (CCBs) met the method-specified criteria. Because all of the blank 

results were less than the RL, no samples were qualified based on these preparation blank 

results. 

DUPLICATES 

No field duplicate samples were collected with these sampling episodes. Two samples 

were analyzed in duplicate at the laboratory, samples 72046 and 72246. The relative 

percent difference (RPD) for samples 72046 and 72246 were 4.25% and 0.84%, 

respectively. The laboratory’s RPD criteria between analytical duplicates is 24%. 

LABORATORY CONTROL SAMPLES 

All laboratory control samples were within FGS’s control limits of 80-120% recovery 

and 24% RPD. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES 

Matrix spikes (MS) and matrix spike duplicates (MSD) were performed on samples 

71996, 72046, 72150, and 72246. All aqueous MS/MSD recoveries were within the 
3

method specifications of 71-125%, except for the MS samples for 72046 and 72150, 

which had recoveries of 20.1% and 54.5%, respectively. All RPDs met method-specified 

criteria of less than or equal to 24%, except for samples 72046 and 72150, which had 

RPDs of 72.2% and 24.5%, respectively. Because the MSDs and the associated LCSs 

were within the method specifications, no data qualification is required for these samples. 

DETECTION LIMITS 

The laboratory MDL in the synthetic matrix was 0.239 ng/L. Results below this MDL 

were reported as not detected (ND). 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD 

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Randy Mercurio, ERG 

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.8 – Long-Term 

Monitoring: Month 2 (Part 1) 

TestAmerica generated analytical data for total metals (antimony, arsenic, cadmium, 

chromium, copper, lead, nickel, selenium, silver, thallium and vanadium) for these longterm monitoring samples. The samples were analyzed according to EPA Method 200.8. 

Table 1 summarizes the samples TestAmerica extracted and analyzed for total metals by 

EPA Method 200.8. 

Table 1. Long-Term Monitoring Month 2 (Part 1) Total Metals – Sample 

Identification 

EPA 

Sample # 

EPA Sample 

Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71992 FGD Influent, Set 2 280-9327-1 Aqueous 11/03/2010 11/04/2010

71996 FGD Bioreactor Influent, 

Set 2 

280-9389-1 Aqueous 11/04/2010 11/05/2010

72000 FGD Bioreactor Effluent, 

Set 2 

280-9389-2 Aqueous 11/04/2010 11/05/2010

72005 FGD Bioreactor Influent 

Field Blank, Set 2 

280-9389-3 Aqueous 11/04/2010 11/05/2010

72009 FGD Bioreactor Effluent 

Field Blank, Set 2 

280-9389-4 Aqueous 11/04/2010 11/05/2010

72042 FGD Influent, Set 2 280-9326-1 Aqueous 11/03/2010 11/04/2010

72046 FGD Effluent, Set 2 280-9326-2 Aqueous 11/03/2010 11/04/2010

72051 FGD Bioreactor Effluent 

Field Blank, Set 2 

280-9326-3 Aqueous 11/03/2010 11/04/2010

72092 FGD Influent, Set 2 280-9249-1 Aqueous 11/02/2010 11/03/2010

72096 FGD Effluent, Set 2 280-9249-2 Aqueous 11/02/2010 11/03/2010

72101 FGD Effluent Field 

Blank, Set 2 

280-9249-3 Aqueous 11/02/2010 11/03/2010

72142 FGD Influent, Set 2 280-9202-1 Aqueous 11/01/2010 11/02/2010

72146 FGD Bioreactor Influent, 

Set 2 

280-9250-1 Aqueous 11/02/2010 11/03/2010
2

Table 1. Long-Term Monitoring Month 2 (Part 1) Total Metals – Sample 

Identification 

EPA 

Sample # 

EPA Sample 

Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72150 FGD Bioreactor Effluent, 

Set 2 

280-9250-2 Aqueous 11/02/2010 11/03/2010

72155 FGD Bioreactor Influent 

Field Blank, Set 2 

280-9250-3 Aqueous 11/02/2010 11/03/2010

72159 FGD Bioreactor Effluent 

Field Blank, Set 2 

280-9250-4 Aqueous 11/02/2010 11/03/2010

72242 FGD Influent, Set 2 280-9388-1 Aqueous 11/04/2010 11/05/2010

72246 FGD Effluent, Set 2 280-9388-2 Aqueous 11/04/2010 11/05/2010

72251 FGD Bioreactor Effluent 

Field Blank, Set 2 

280-9388-3 Aqueous 11/04/2010 11/05/2010

SUMMARY 

The samples were prepared for total metals analysis according to TestAmerica’s “FGD 

ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Elements 

Analysis in Flue Gas Desulfurization Wastewaters,” dated October 6, 2010, based on 

EPA Method 200.8, by ICP/MS analysis. 

Any significant findings are summarized below. No additional data qualifiers were 

required. 

• The serial dilution for selenium for sample 72096 failed TestAmerica’s criteria of 

±10% difference. 

• The matrix spike (MS) and matrix spike duplicate (MSD) recoveries for silver for 

sample 72096 failed the EPA Method 200.8 control limits of 70–130%. 

• The MS and MSD recoveries for selenium and silver for sample 72246 failed the 

EPA Method 200.8 control limits of 70–130%. 

• The MS/MSD relative percent difference (RPD) for silver for sample 72246 failed 

the FGD ICP/MS SOP control limits of ±20%. 

• The post digestion spike (PDS) recoveries for silver failed TestAmerica’s control 

limits of 85–115%. 

INTERNAL STANDARDIZATION 

All internal standards used by TestAmerica were within the method criteria. 

INITIAL CALIBRATION 
3

TestAmerica performed the initial calibrations on each analysis 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 (RL); however, some elements 

were above the MDL and flagged with a “J” qualifier. No additional qualifiers were 

required for method blanks. 

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank 

(CCB)) were less than the RL; however, some elements were above the MDL and 

flagged with a “J” qualifier. No additional qualifiers were required for instrument blanks. 

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

All CRI samples passed TestAmerica’s SOP control limits of 50–150% recovery. 

LABORATORY CONTROL SAMPLES (LCS) 

All LCS samples passed the method QC limits of 85–115% recovery. 

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION 

Based on TestAmerica’s SOP, all interference check sample A (ICSA) results had 

analytes of interest with concentrations less than the RL or less than five times the RL 

when known inherent contaminants are present in the stock solution used to make the 

ICS. 

All interference check sample B (ICSAB) synthetic spikes recovered within 

TestAmerica’s SOP criteria of 70–130% of the true value. 

The ICSA solution for the method 200.8 analysis exceeded the acceptance limits for 

Chromium in analytical batch 280-40682. 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 “^”. 
4

SERIAL DILUTION 

The serial dilution performed on sample 72096 passed TestAmerica’s criteria of ±10% 

difference for all analytes except selenium, which was flagged “V.” No further data 

qualifiers were needed for the serial dilution. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

MS and MSD were performed on samples 72096 and 72246. The MS/MSD for sample 

72096 failed the method control limits of 70–130% recovery for selenium and silver. 

Selenium was flagged for the MS/MSD 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. This result was considered acceptable based on the LCS passing the 

method control limits. Silver was flagged for the MS/MSD with an “F” qualifier and it is 

likely that silver failed due to matrix interference from the high concentration of sulfates, 

which can form insoluble silver sulfide and/or silver sulfate. The silver recoveries in the 

associated LCS/LCSD were acceptable. 

The MS/MSD for sample 72246 failed the method control limits of 70–130% recovery 

for selenium and silver, which were flagged with an “F” qualifier. The RPD failed the 

FGD ICP/MS SOP control limits of ±20% for silver for sample 72246. No additional data 

qualifiers were required for MS/MSD samples. 

Otherwise, all MS/MSD spike recoveries were within the method control limits of 70-

130% and the RPD for the MS/MSDs were within the FGD ICP/MS SOP control limits 

of ±20 percent. No additional data qualifiers were required. 

POST DIGESTION SPIKES (PDS) 

The PDS performed on sample 72096 passed TestAmerica’s control limits of 85–115% 

recovery for all analytes, except for silver, which was flagged with a “W” qualifier. It is 

likely that silver failed due to matrix interference from the high concentration of sulfates, 

which can form insoluble silver sulfide and/or silver sulfate. The silver recoveries in the 

associated LCS/LCSD were acceptable. No additional data qualifiers were required. 

DETECTION LIMITS 

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water. 
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: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.7 – Long-Term 

Monitoring: Month 2 (Part 1)

TestAmerica generated analytical data for total 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 TestAmerica extracted and analyzed for total metals by 

EPA Method 200.7. 

Table 1. Long-Term Monitoring Month 2 (Part 1) Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71992 FGD Influent, Set 2 280-9327-1 Aqueous 11/03/2010 11/04/2010

71996 FGD Bioreactor Influent, Set 2 280-9389-1 Aqueous 11/04/2010 11/05/2010

72000 FGD Bioreactor Effluent, Set 2 280-9389-2 Aqueous 11/04/2010 11/05/2010

72005 FGD Bioreactor Influent Field 

Blank, Set 2 

280-9389-3 Aqueous 11/04/2010 11/05/2010

72009 FGD Bioreactor Effluent Field 

Blank, Set 2 

280-9389-4 Aqueous 11/04/2010 11/05/2010

72042 FGD Influent, Set 2 280-9326-1 Aqueous 11/03/2010 11/04/2010

72046 FGD Effluent, Set 2 280-9326-2 Aqueous 11/03/2010 11/04/2010

72051 FGD Bioreactor Effluent Field 

Blank, Set 2 

280-9326-3 Aqueous 11/03/2010 11/04/2010

72092 FGD Influent, Set 2 280-9249-1 Aqueous 11/02/2010 11/03/2010

72101 FGD Effluent Field Blank, Set 2 280-9249-3 Aqueous 11/02/2010 11/03/2010

72142 FGD Influent, Set 2 280-9202-1 Aqueous 11/01/2010 11/02/2010

72146 FGD Bioreactor Influent, Set 2 280-9250-1 Aqueous 11/02/2010 11/03/2010

72150 FGD Bioreactor Effluent, Set 2 280-9250-2 Aqueous 11/02/2010 11/03/2010

72155 FGD Bioreactor Influent Field 

Blank, Set 2 

280-9250-3 Aqueous 11/02/2010 11/03/2010

72159 FGD Bioreactor Effluent Field 

Blank, Set 2 

280-9250-4 Aqueous 11/02/2010 11/03/2010

72242 FGD Influent, Set 2 280-9388-1 Aqueous 11/04/2010 11/05/2010
2

Table 1. Long-Term Monitoring Month 2 (Part 1) Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72251 FGD Bioreactor Effluent Field 

Blank, Set 2 

280-9388-3 Aqueous 11/04/2010 11/05/2010

SUMMARY 

The samples were prepared for total metals analysis according to TestAmerica’s SOP for 

ICP Analysis for Trace Metals by Method 200.7. Any significant findings are 

summarized below. No additional data qualifiers were required for this data set. 

• Aluminum, calcium, iron, magnesium, and manganese were measured above the 

reporting limit (RL) in a method blank; however, the concentration of these 

elements in the samples associated with this method blank were at least 10 times 

the blank result or below the RL. 

• The matrix spike (MS)/matrix spike duplicate (MSD) relative percent difference 

(RPD) for boron, calcium, and magnesium for sample 72096 failed TestAmerica’s 

± 20% requirement. 

• The post digestion spike (PDS) for calcium, manganese, titanium, and zinc for 

sample 72096 failed TestAmerica’s control limits of 85-115% recovery. 

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 TestAmerica’s SOP control limits. 

INITIAL CALIBRATION 

TestAmerica performed the initial calibrations on each analysis day. The initial 

calibration for the ICP analysis consisted of a blank and one calibration standard. 

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS 

The initial calibration verifications (ICV) and continuing calibration verifications (CCV) 

performed by TestAmerica all had recoveries within the method criteria. 
3

METHOD/INSTRUMENT BLANKS 

All the method blanks were less than the RL, except for MB 280-40683/1-A. Aluminum, 

calcium, iron, magnesium, and manganese were measured above the RL in this method 

blank; however, the concentration of these elements in the samples associated with this 

method blank were at least 10 times the blank result or below the RL. Therefore, no data 

needed qualification regarding the method blank result. In the other method blanks, some 

elements were above the method detection limit (MDL), but less than the RL; therefore, 

these blanks and were flagged with the “J” qualifier. 

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank 

(CCB)) were less than the RL; however, some elements were above the MDL and were 

flagged with the “J” qualifier. 

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

All CRI samples passed TestAmerica’s SOP control limits of 50–150% recovery. 

LABORATORY CONTROL SAMPLES (LCS) 

All LCSs passed the method control limits of 85–115% recovery. 

INTERFERENCE CHECK SOLUTIONS 

Interference checks were performed using the synthetic matrix as the check solution. All 

data quality objectives met TestAmerica’s SOP criteria.

SERIAL DILUTION (SRD) 

All serial dilution percent differences were less than 10% as required by TestAmerica’s 

SOP. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

Matrix spikes (MS) and matrix spike duplicates (MSD) were performed on the total 

samples of 72096 and 72246. Some elements with high concentrations 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. These data were considered acceptable 

based on the LCS passing the method criteria. Otherwise, all MS/MSD spike recoveries 

were within the method control criteria of 70-130%. The RPD for all MS/MSDs were 
4

within TestAmerica’s ± 20% requirement, except for boron, calcium, and magnesium for 

sample 72096. These elements were flagged with an “F” qualifier. 

POST DIGESTION SPIKE (PDS) 

The PDS performed on sample 72096 passed TestAmerica’s control limits of 85-115% 

recovery for all analytes except boron, calcium, manganese, sodium, titanium, and zinc. 

Calcium, manganese, titanium, and zinc were qualified with a “W;” however, Because 

the spike level in the MS/MSD analyses for these elements was less than 4 times the 

sample concentration, there is no evidence of matrix interferences. Additionally, these 

elements passed TestAmerica’s requirement of percent differences less than 10% for the 

serial dilution for sample 72096. Boron and sodium failed the PDS; however, the percent 

recoveries were not calculated by the laboratory because their concentrations were 

greater than 4 times the PDS spike level. Boron and sodium also passed the serial dilution 

for sample 72096 demonstrating no significant matrix interferences. 

DETECTION LIMITS 

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water. 
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: Ariel Atkinson, ERG 

Date: 2/9/2012 

Subject: TestAmerica Data Review Narrative for Classicals Analyses – Long Term 

Monitoring: Month 2 (Part 1) 

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for these long-term monitoring samples. All samples were tested for the 

following analytes: 

• Ammonia by EPA method 350.1, 

• Biochemical Oxygen Demand – 5 day (BOD5) by SM 5210B, 

• Chloride and Sulfate by EPA method 300.0, 

• Chemical Oxygen Demand (COD) by EPA method 410.4, 

• Cyanide (total) by SM 4500 CN- E, 

• Nitrate/Nitrite by EPA method 353.2, 

• Phosphorus (total) by EPA method 365.1, 

• Total Dissolved Solids (TDS) by SM 2540C, 

• Total Kjeldahl Nitrogen (TKN) by EPA method 351.2, and 

• Total Suspended Solids (TSS) by SM 2540D. 

Table 1 summarizes the 12 samples that TestAmerica analyzed for the above analytes. 

Table 1. Long-Term Monitoring Month 2 (Part 1) Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71992 Water FGD Influent, Set 2 11/3/10 

71996 Water FGD Bioreactor Influent, Set 2 11/3/10(CN) 

11/4/10(All other 

analytes) 

72000 Water FGD Bioreactor Effluent, Set 2 11/3/10(CN) 

11/4/10(All other 

analytes) 

72042 Water FGD Influent, Set 2 11/3/2010 

72046 Water FGD Effluent, Set 2 11/3/2010 
2 

Table 1. Long-Term Monitoring Month 2 (Part 1) Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72092 Water FGD Influent, Set 2 11/2/2010 

72096 Water FGD Effluent, Set 2 11/2/2010 

72142 Water FGD Influent, Set 2 11/1/2010 

72146 Water FGD Bioreactor Influent, Set 2 11/2/2010 

72150 Water FGD Bioreactor Effluent, Set 2 11/1/10(CN) 

11/2/10(All other 

analytes) 

72242 Water FGD Influent, Set 2 11/4/10 

72246 Water FGD Effluent, Set 2 11/4/10 

SUMMARY 

All samples were analyzed within the holding time specified in 40 CFR 136 Table II. All 

samples were preserved appropriately unless otherwise specified below. 

 

Field duplicate samples were not collected for these episodes. Depending on the method, 

a laboratory duplicate was analyzed, instead. 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 unless otherwise specified below. All sample results were between 

the lowest and highest standards unless 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 

unless otherwise noted below. 

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 72042, 

72096, and/or 72246 for each analyte to check for matrix interferences. For some 

analytes, TestAmerica spiked more samples than required. MS samples analyzed met the 

criteria specified in the method unless described below. 
3 

DATA NOTES/ISSUES 

Ammonia 

The MS result failed criteria at 111% recovery and was qualified with an “F” flag. The 

MSD and LCS recoveries demonstrate that the analysis was under control. No additional 

qualifiers were required.

BOD5 

TestAmerica analyzed five dilutions, but no dilutions had a dissolved oxygen (DO) 

depletion greater than 2.0 mg/L for samples 72092, 72146, 72150 72042, 72046, 71992, 

71996, and 72246. Therefore, BOD5 was reported as not detected for these samples. The 

rest of the samples had at least one dilution with a DO depletion greater than 2.0 mg/L. 

As required in the method, the final result was calculated by taking the average of the 

results for all dilutions with a DO depletion greater than 2.0 mg/L and a final DO greater 

than 1.0 mg/L. 

One of the three batches had a seed correction factor lower than 0.6 mg/L. The seed 

correction factors were 0.632 mg/L, 0.5533 mg/L, and 0.6267 mg/L for batches 38776, 

39101, and 39326 respectively. The samples in batch 39101 should be flagged with an 

“s” indicating the seed correction blank (SCB) recovery was low. This low seed 

correction factor suggests that samples 72042, 72046, and 71992 may be biased low; 

however all these samples had a result of ND and therefore do not require qualification. 

All glucose-glutamic acid standards and laboratory duplicates were analyzed 

appropriately and met the criteria specified in SM 5210B. 

Chloride and Sulfate 

The MS/MSD results of samples 72246 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/MSD results will be qualified as estimated values. The LFB associated with 

this sample met the method criteria. The analyzed result for sample 72246 was within the 

calibration curve, so there was no need to qualify this sample. 

COD 

Several LRB and Calibration Blanks (CB) had results greater than the MDL; however, all 

the LRB and CB results less than the RL and were flagged with a “J” qualifier. No further 

qualifications are necessary. 

One LFB, LCSD from batch 41304, had a percent recovery greater that the 90-110% 

criteria. The LFB was flagged with a “*” qualifier indicating the LCS or LCSD exceeds 
4 

the control limits. The sample 72046, which is associated with this LFB, was also flagged 

with “*” qualifier. 

 

The percent recovery for the MS/MSD analyses for samples 72096 and 72246 were 

above the control limits of 90-110% required by EPA method 410.4. The percent 

recoveries for the MS and MSD analyses for sample 72096 were 115% and 118%, 

respectively and the recoveries for sample 72246 were 131% and 132%, respectively. 

These results were flagged with an “F” qualifier because they exceed control limits. The 

LFB percent recoveries associated with samples 72096 and 72246 met the method 

criteria. 

MS/MSDs were not performed in batches 41739 and 41304. The samples associated with 

these batches include 72042 and 72046. These sample results were qualified with an “F” 

qualifier because there were no MS/MSD results. 

Cyanide 

The calibration was performed using standards ranging from 0.00 ppb to 400.0 ppb. The 

method states that the appropriate calibration range of standard concentrations for this 

method are between 5 ppb and 20 ppb. Samples 72142, 72092, 72096, 72046, 72242, all 

had results ≥ 20 ug/L; but were not diluted because they were within the calibration range 

performed by the laboratory. 

The MS/MSD results for sample 72246 passed the recovery criteria; however, the 

MS/MSD results for sample 72096 failed recovery criteria. The MS/MSD results for 

72096 were qualified with an “F” flag. The associated LCS/LCSD recoveries were 

within control limits. 

Nitrate/Nitrite 

The RPD between the LFB and a duplicate LFB from batch 280-40320 is 10.7%. This 

does not meet the control limits, and therefore the LFB, LFB duplicate, and associated 

samples are flagged with a “*” qualifier meaning RPD of the LCS and LCSD exceeds the 

control limit. The RPD for the MS/MSD in this batch was 1 percent; therefore the system 

appears to be in control. No further qualifiers were needed. 

The MS/MSD results for samples 72042, 72096, and 72246 were above the calibration 

curve. TestAmerica did not reanalyze these MS/MSDs with a higher dilution factor, but 

the MS/MSD results for samples 72246 and 72042 were flagged with an “E” qualifier 

because the results exceeded calibration range. The MS/MSD results for sample 72096 

were not flagged with “E” qualifier because the percent recoveries for the MS/MSD 

analysis of sample 72096 were not within the method control limits of 90-110 percent; 

therefore, these MS/MSD results were flagged with an “F” qualifier. The percent 

recoveries for the MS/MSD of 72096 were 118% and 121%, respectively. Additionally, 

the MS of sample 72042, and the MSD of sample 72246 were not within the method 

control limits of 90-110%. The percent recovery of the MSD for sample 72246 was 89% 
5 

and the percent recovery of the MS of sample 72042 was 88 percent; however neither 

MS/MSDs were flagged with an “F’ qualifier because they did meet the laboratory 

control limits. If reported, the 72042 MS should be flagged with an “F” qualifier, the 

72096 MS/MSD should be qualified as estimated, and the 72246 MS should be flagged 

with an “F” qualifier. 

Phosphorus 

The LRB was greater than the MDL at 0.0141 mg/L, however the result was less than the 

RL. The LRB results were flagged with a “J” qualifier because the result was less than 

the RL but greater than the MDL. No further qualifiers are needed. All samples that 

contained the analyte were also flagged with a “B” qualifier because the compound was 

found in the blank and the sample. All calibration blank results were also above the MDL 

but less than the RL, and therefore are also flagged with a “J” qualifier. 

The percent recoveries for the MS/MSD analysis of samples 72096 and 72246 were not 

within the control limits of 90-110% specified in EPA Method 365.1. However the 

MS/MSD of sample 72096 were within the laboratory control limits of 71-128%. The 

percent recoveries of the MS and MSD for sample 72096 were 87% and 84%, 

respectively, and the MS and MSD recoveries for sample 72246 were 26% and 31%, 

respectively. Because the MS/MSD of sample 72096 met laboratory control limits it was 

not flagged by the laboratory, but if the MS/MSD results for sample 72096 are reported, 

they should be flagged with an “F” qualifier. 

Samples 72146, 72150, 72046, 72242, 71996, 72000, and the LRB had results that were 

lower than the lowest calibration standard. Each of these results was flagged with a “J” 

qualifier because each result was less than the RL but greater than or equal to the MDL, 

and therefore the concentrations are approximate values. No further qualifiers are needed. 

TDS 

Constant weight was not achieved after 3 drying cycles for all samples. It should be noted 

that the weight increased from the first weighing to the second weighing for all samples 

except 72042, 72046, 71992, 72242, 72246, 71996, and 72000. 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. Samples 72142, 72092, 72096, 72146, and 72150 were not qualified, 

but results may be biased high. 

The RPD for the laboratory duplicate from sample 72096 was 12%, which is not less than 

10% as required by SM 2540C. The laboratory control limits are 20%; therefore, the 

laboratory did not qualify the sample. The sample result will be qualified as an estimated 

value as shown in Table 2. Laboratory duplicates were not performed in the other 

batches. 
6 

TKN 

TestAmerica performed MS/MSD analysis on samples 72096 and 72246. The percent 

recoveries for the MS and MSD for sample 72096 were 161% and 147%, respectively, 

and 145% and 149% for the MS and MSD for sample 72246. These samples did not meet 

the method control limits of 90-110%, nor the laboratory control limits of 54-131%. The 

sample concentration was greater than 4 times the spike amount in the MS and MSD 

samples, so TestAmerica stated that the percent recoveries and RPDs could not be 

reliably calculated. The associated LCS/LCSD were also acceptable, therefore, no 

additional data qualifiers are required. 

TKN was detected in the calibration blanks. The results were greater than the MDL 

(0.077 mg/L), but less than the RL (1.0 mg/L). Because the results were less than the RL, 

no samples were qualified, but the CBs were flagged with a “J” qualifier. 

TSS 

The RPDs for the laboratory duplicates performed on samples 72142, 72096, 72046, and 

72246 were greater than the method control criteria of 10%, at 11%, 18%, 22%, and 18%, 

respectively. The laboratory control criterion is 20 percent; therefore, samples 72142, 

72096, and 72246 were not qualified by the laboratory. Sample 72046 and its duplicate 

were already qualified by TestAmerica with a “J” meaning that the result is an estimated 

value because the result is below the RL, so no further qualification was necessary for 

this sample. Because the RPD was greater than the method control limits, sample 72142, 

72096, and 72246 were qualified as estimated values. 

Table 2. Data Review Summary Table 

Sample Analyte Qualifier/Ac

tion 

Reason Level Detected

72042 COD F MS/MSD not 

performed in batch 

XXX mg/L

72046 COD F MS/MSD not 

performed in batch 

XXX mg/L

72096 TDS Estimated 

Value 

Lab duplicate RPD > 

method-specified 

criteria 

Sample: 28000 

mg/L 

Dup: 24900 

mg/L,12%RPD 

72142 TSS Estimated 

Value 

Lab duplicate RPD > 

method-specified 

criteria 

Sample: XXX

mg/L Dup: XXX 

mg/L; 11%RPD 

72096 TSS Estimated 

Value 

Lab duplicate RPD > 

method-specified 

criteria 

Sample: 4.8 

mg/L 

Dup: 4 mg/L; 

18% RPD 
7 

Table 2. Data Review Summary Table 

Sample Analyte Qualifier/Ac

tion 

Reason Level Detected

72246 TSS Estimated 

Value 

Lab duplicate RPD > 

method-specified 

criteria 

Sample: XXX

mg/L 

Dup: XXX 

mg/L; 18% RPD 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD 

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Donna Tedder, ERG 

Date: 2/9/2012

Subject: FGS Data Review Narrative for Total Mercury – Long-Term Monitoring: 

Month 3

Frontier Global Sciences (FGS) generated analytical data for total mercury. FGS 

analyzed the samples according to EPA Method 1631E for mercury by Cold Vapor 

Atomic Fluorescence Spectrometry (CVAFS) analysis. 

Table 1 summarizes the 24 samples (excluding laboratory prep blanks) FGS extracted 

and analyzed for total mercury. 

Table 1. Long-Term Monitoring Month 3 Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71993 1012119-01 Aqueous FGD Influent, Set 3 12/8/2010

71997 1012119-06 Aqueous FGD Bioreactor Influent, Set 3 12/8/2010

72001 1012119-11 Aqueous FGD Bioreactor Effluent, Set 3 12/8/2010

72006 1012119-12 Aqueous FGD Bioreactor Influent Field Blank, Set 3 12/8/2010

72010 1012119-13 Aqueous FGD Bioreactor Effluent Field Blank, Set 3 12/8/2010

72043 1012094-01 Aqueous FGD Influent, Set 3 12/8/2010

72047 1012094-02 Aqueous FGD Effluent, Set 3 12/7/2010

72052 1012094-03 Aqueous FGD Effluent Field Blank, Set 3 12/7/2010

72093 1012077-01 Aqueous FGD Influent Set 3 12/7/2010 

72097 1012077-02 Aqueous FGD Effluent, Set 3 12/7/2010

72102 1012077-03 Aqueous FGD Effluent Field Blank, Set 3 12/7/2010

72143 1012080-01 Aqueous FGD Influent, Set 3 12/6/2010

72147 1012080-06 Aqueous FGD Bioreactor Influent, Set 3 12/6/2010

72151 1012080-11 Aqueous FGD Bioreactor Effluent, Set 3 12/6/2010

72156 1012080-12 Aqueous FGD Bioreactor Influent Field Blank, Set 3 12/6/2010

72160 1012080-13 Aqueous FGD Bioreactor Effluent Field Blank, Set 3 12/6/2010

72192 1012105-01 Aqueous FGD Influent, Set 1 12/8/2010

72196 1012105-02 Aqueous FGD SBR Influent, Set 1 12/8/2010

72200 1012105-03 Aqueous FGD SBR Effluent, Set 1 12/8/2010
2

Table 1. Long-Term Monitoring Month 3 Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72205 1012105-04 Aqueous FGD SBR Influent Field Blank, Set 1 12/8/2010

72209 1012105-05 Aqueous FGD SBR Effluent Field Blank, Set 1 12/8/2010

72243 1012117-01 Aqueous FGD Influent, Set 3 12/9/2010

72247 1012117-06 Aqueous FGD Effluent, Set 3 12/9/2010

72252 1012117-07 Aqueous FGD Effluent Field Blank, Set 3 12/8/2010

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. 

BLANKS 

All the preparation blanks or laboratory reagent blanks (LRBs) and the continuing 

calibration blanks (CCBs) met method-specified criteria. Some preparation blanks had 

mercury levels greater than the MDL (0.24 ng/L), but less than the RL associated with 

each individual blank (different RLs based on preparation). Because all of the blank 

results were less than the RL, no samples were qualified based on these preparation blank 

results. 

DUPLICATES 

No field duplicate samples were collected with these sampling episodes. Three samples 

were analyzed in duplicate at the laboratory, Bioreactor Influent sample 72147, SBR 

Influent sample 72196, and Effluent sample 72247. The relative percent difference (RPD) 
3

for samples 72147, 72196, and 72247 were 9.74%, 4.36%, and 9.10%, respectively. A 

sample from another work order was analyzed in duplicate with these batches that 

resulted in an RPD of 79.7%, which is outside of the laboratory’s criteria. The 

laboratory’s RPD criteria between analytical duplicates is 24%. No sample qualifications 

were needed based on these analytical duplicate results.

LABORATORY CONTROL SAMPLES 

All laboratory control samples were within FGS’s control limits of 80-120% recovery 

and 24% RPD. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

Matrix spikes (MS) and matrix spike duplicates (MSD) were performed on samples 

72097, 72147, and 72196. Additionally, an MS/MSD was performed on sample 72296, 

which was a rerun from the long-term monitoring, month 2 set of samples. All aqueous 

MS/MSD recoveries were within method specifications of 71-125%. All RPDs met 

method-specified criteria. 

DETECTION LIMITS 

The laboratory MDL in the synthetic matrix was 0.239 ng/L. Results below this MDL 

were reported as not detected (ND). 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD 

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Randy Mercurio, ERG 

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.8 – Long-Term 

Monitoring: Month 3 

TestAmerica generated analytical data for total metals (antimony, arsenic, cadmium, 

chromium, copper, lead, nickel, selenium, silver, thallium and vanadium) for these longterm monitoring samples. The samples were analyzed according to EPA Method 200.8. 

Table 1 summarizes the samples TestAmerica extracted and analyzed for total metals by 

EPA method 200.8.

Table 1. Long-Term Monitoring Month 3 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71993 FGD Influent, Set 3 280-10586-1 Aqueous 12/08/2010 12/09/2010

71997 FGD Bioreactor Influent, Set 3 280-10586-2 Aqueous 12/08/2010 12/09/2010

71997 FGD Bioreactor Influent, Set 3 280-10654-1 Aqueous 12/09/2010 12/10/2010

72001 FGD Bioreactor Effluent, Set 3 280-10654-2 Aqueous 12/09/2010 12/10/2010

72006 FGD Bioreactor Influent Field 

Blank, Set 3 

280-10654-3 Aqueous 12/09/2010 12/10/2010

72010 FGD Bioreactor Effluent Field 

Blank, Set 3 

280-10654-4 Aqueous 12/09/2010 12/10/2010

72043 FGD Influent, Set 3 280-10584-1 Aqueous 12/08/2010 12/09/2010

72047 FGD Effluent, Set 3 280-10584-2 Aqueous 12/08/2010 12/09/2010

72052 FGD Bioreactor Effluent Field 

Blank, Set 3 

280-10584-3 Aqueous 12/08/2010 12/09/2010

72093 FGD Influent, Set 3 280-10515-1 Aqueous 12/07/2010 12/08/2010

72097 FGD Effluent, Set 3 280-10515-2 Aqueous 12/07/2010 12/08/2010

72102 FGD Effluent Field Blank, Set 3 280-10515-3 Aqueous 12/07/2010 12/08/2010

72143 FGD Influent, Set 3 280-10455-1 Aqueous 12/06/2010 12/07/2010

72147 FGD Bioreactor Influent, Set 3 280-10517-1 Aqueous 12/07/2010 12/08/2010

72151 FGD Bioreactor Effluent, Set 3 280-10517-2 Aqueous 12/07/2010 12/08/2010

72156 FGD Bioreactor Influent Field 

Blank, Set 3 

280-10517-3 Aqueous 12/07/2010 12/08/2010

72160 FGD Bioreactor Effluent Field 280-10517-4 Aqueous 12/07/2010 12/08/2010
2

Table 1. Long-Term Monitoring Month 3 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

Blank, Set 3

72192 FGD Influent, Set 1 280-10585-1 Aqueous 12/08/2010 12/09/2010

72196 FGD SBR Influent, Set 1 280-10585-2 Aqueous 12/08/2010 12/09/2010

72200 FGD SBR Effluent, Set 1 280-10585-3 Aqueous 12/08/2010 12/09/2010

72205 FGD SBR Influent Field Blank, 

Set 1 

280-10585-4 Aqueous 12/08/2010 12/09/2010

72209 FGD SBR Effluent Field Blank, 

Set 1 

280-10585-5 Aqueous 12/08/2010 12/09/2010

72243 FGD Influent, Set 3 280-10655-1 Aqueous 12/09/2010 12/10/2010

72247 FGD Effluent, Set 3 280-10655-2 Aqueous 12/09/2010 12/10/2010

72252 FGD Effluent Field Blank, Set 3 280-10655-3 Aqueous 12/09/2010 12/10/2010

SUMMARY 

The samples were prepared for total metals analysis according to TestAmerica’s “FGD 

ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Elements 

Analysis in Flue Gas Desulfurization Wastewaters,” dated October 6, 2010, based on 

EPA Method 200.8, by ICP/MS analysis. 

Any significant findings are summarized below. No additional data qualifiers were 

required. 

• One of the continuing calibration verifications (CCV) performed on 12/21/2010 

failed the method criteria for selenium. 

• The matrix spike (MS) and matrix spike duplicate (MSD) recoveries for total 

silver for sample 72196 failed the EPA Method 200.8 control limits of 70-130%. 

The MSD recovery for total silver for sample 72147 also failed the method 

control limits. 

• The MS/MSD relative percent difference (RPD) for total silver for samples 72147 

and 72196 failed the FGD ICP/MS SOP control limits of ±20%. 

• The post digestion spike (PDS) recoveries for copper, nickel, and silver for 

sample 72147 failed TestAmerica’s control limits of 85–115%. The PDS 

recovery for silver for sample 71997 also failed TestAmerica’s control limits. 

INTERNAL STANDARDIZATION 

All internal standards used by TestAmerica were within the method criteria. 
3

INITIAL CALIBRATION 

TestAmerica performed the initial calibrations on each analysis 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 CCV performed by TestAmerica all had 

recoveries within the method criteria, except for selenium for one CCV on 12/21/2010. 

Samples associated with this CCV that had selenium values less than the reporting limit 

were reported. Any samples with selenium values above the reporting limit were 

reanalyzed. 

METHOD/INSTRUMENT BLANKS 

All the method blanks were less than the reporting limit (RL); however, some elements 

were above the MDL and flagged with a “J” qualifier. No additional qualifiers were 

required for method blanks. 

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank 

(CCB)) were less than the RL; however, some elements were above the MDL and 

flagged with a “J” qualifier. No additional qualifiers were required for instrument blanks. 

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

All CRI samples passed TestAmerica’s SOP control limits of 50–150% recovery. 

LABORATORY CONTROL SAMPLES (LCS) 

All LCS samples passed the method QC limits of 85–115% recovery. 

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION 

Based on TestAmerica’s SOP, all interference check sample A (ICSA) results had 

analytes of interest with concentrations less than the RL or less than five times the RL 

when known inherent contaminants are present in the stock solution used to make the 

ICS. 

All interference check sample B (ICSAB) synthetic spikes recovered within 

TestAmerica’s SOP criteria of 70–130% of the true value. 

SERIAL DILUTION 

The serial dilution performed on samples 72147 and 72196 passed TestAmerica’s criteria 

of ±10% difference. 
4

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

MS and MSD were performed on samples of 72147, 72196, and 71997. The MSD of 

sample 72147 failed the method control limits of 70–130% recovery for silver at 69%, 

which was flagged with an “F” qualifier. The MS/MSD of sample 72196 failed the 

method control limits of 70–130% recovery for silver, which was flagged with an “F” 

qualifier. These silver failures are likely due to matrix interference from the high 

concentration of sulfates, which can form insoluble silver sulfide and/or silver sulfate. 

The silver recoveries in the associated LCS/LCSDs were acceptable. The RPD for the 

MS/MSDs for samples 72147 and 72196 failed the FGD ICP/MS SOP ±20% control 

limits for silver. 

Otherwise, all MS/MSD spike recoveries were within the method control limits of 70-

130% and the RPD for the MS/MSDs were within the FGD ICP/MS SOP control limits 

of ±20 percent. No additional data qualifiers were required. 

POST DIGESTION SPIKES (PDS) 

The PDS performed on samples 72147 and 71997 passed TestAmerica’s control limits of 

85–115% recovery for all analytes, except for copper, nickel, and silver for PDS sample 

72147 and silver for PDS sample 71997, which were flagged with a “W” qualifier. No 

additional data qualifiers were required. 

DETECTION LIMITS 

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water. 
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: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.7 – Long-Term 

Monitoring: Month 3

TestAmerica generated analytical data for total 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 TestAmerica extracted and analyzed for total metals by 

EPA Method 200.7 

Table 1. Long-Term Monitoring Month 3 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71993 FGD Influent, Set 3 280-10586-1 Aqueous 12/08/2010 12/09/2010

71997 FGD Bioreactor Influent, Set 3 280-10654-1 Aqueous 12/09/2010 12/10/2010

72001 FGD Bioreactor Effluent, Set 3 280-10654-2 Aqueous 12/09/2010 12/10/2010

72006 FGD Bioreactor Influent Field 

Blank, Set 3 

280-10654-3 Aqueous 12/09/2010 12/10/2010

72010 FGD Bioreactor Effluent Field 

Blank, Set 3 

280-10654-4 Aqueous 12/09/2010 12/10/2010

72043 FGD Influent, Set 3 280-10584-1 Aqueous 12/08/2010 12/09/2010

72047 FGD Effluent, Set 3 280-10584-2 Aqueous 12/08/2010 12/09/2010

72052 FGD Bioreactor Effluent Field 

Blank, Set 3 

280-10584-3 Aqueous 12/08/2010 12/09/2010

72093 FGD Influent, Set 3 280-10515-1 Aqueous 12/07/2010 12/08/2010

72097 FGD Effluent, Set 3 280-10515-2 Aqueous 12/07/2010 12/08/2010

72102 FGD Effluent Field Blank, Set 3 280-10515-3 Aqueous 12/07/2010 12/08/2010

72143 FGD Influent, Set 3 280-10455-1 Aqueous 12/06/2010 12/07/2010

72147 FGD Bioreactor Influent, Set 3 280-10517-1 Aqueous 12/07/2010 12/08/2010

72151 FGD Bioreactor Effluent, Set 3 280-10517-2 Aqueous 12/07/2010 12/08/2010

72156 FGD Bioreactor Influent Field 

Blank, Set 3 

280-10517-3 Aqueous 12/07/2010 12/08/2010

72160 FGD Bioreactor Effluent Field 

Blank, Set 3 

280-10517-4 Aqueous 12/07/2010 12/08/2010

72192 FGD Influent, Set 1 280-10585-1 Aqueous 12/08/2010 12/09/2010
2

Table 1. Long-Term Monitoring Month 3 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72196 FGD SBR Influent, Set 1 280-10585-2 Aqueous 12/08/2010 12/09/2010

72200 FGD SBR Effluent, Set 1 280-10585-3 Aqueous 12/08/2010 12/09/2010

72205 FGD SBR Influent Field Blank, 

Set 1 

280-10585-4 Aqueous 12/08/2010 12/09/2010

72209 FGD SBR Effluent Field Blank, 

Set 1 

280-10585-5 Aqueous 12/08/2010 12/09/2010

72243 FGD Influent, Set 3 280-10655-1 Aqueous 12/09/2010 12/10/2010

72247 FGD Effluent, Set 3 280-10655-2 Aqueous 12/09/2010 12/10/2010

72252 FGD Effluent Field Blank, Set 3 280-10655-3 Aqueous 12/09/2010 12/10/2010

SUMMARY 

The samples were prepared for total metals analysis according to TestAmerica’s SOP for 

ICP Analysis for Trace Metals by Method 200.7. Any significant findings are 

summarized below. Additional data qualifiers were required (see Table 2). 

• The serial dilution for cobalt, iron, and zinc for sample 72143 failed 

TestAmerica’s SOP control limit of percent differences less than 10%. 

• The post digestion spike (PDS) for calcium, iron, magnesium, and zinc for sample 

72143 failed TestAmerica’s control limits of 85–115% recovery. 

• The PDS for manganese for sample 72147 failed TestAmerica’s control limits of 

85–115% recovery. 

SAMPLE RECEIPT, HANDLING AND STORAGE ISSUES 

The samples associated with Episode 6569 (72192, 72196, 72200, 72205, and 72209) did

not have a sample date or time on the traffic report. 

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 

TestAmerica performed the initial calibrations on each analysis day. The initial 

calibration for the ICP analysis consisted of a blank and one calibration standard. 
3

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 (RL); however, some elements 

were above the method detection limit (MDL) and were flagged with the “J” qualifier. 

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank 

(CCB)) were less than the RL; however, some elements were above the MDL and were 

flagged with the “J” qualifier. 

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

All CRI samples passed TestAmerica’s SOP control limits of 50–150% recovery. 

LABORATORY CONTROL SAMPLES (LCS) 

All LCSs passed the method control limits of 85–115% recovery. 

INTERFERENCE CHECK SOLUTIONS 

Interference checks were performed using the synthetic matrix as the check solution. All 

data quality objectives met TestAmerica’s SOP criteria.

SERIAL DILUTION (SRD) 

Serial dilutions were performed for each batch of total samples. All serial dilution percent 

differences were less than 10% as required by TestAmerica’s SOP, except for cobalt, 

iron, and zinc for sample 72143, which were flagged with a “V” qualifier. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

Matrix spikes (MS) and matrix spike duplicates (MSD) were performed on the total 

samples of 72143, 72147, and 72196. Some elements with high concentrations 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. These data were considered acceptable 

based on the LCS passing the method control limits. Otherwise, all MS/MSD spike 

recoveries were within the method control criteria of 70-130%. The RPD for all 
4

MS/MSDs were within TestAmerica’s ± 20% requirement. No additional data qualifiers 

were needed. 

POST DIGESTION SPIKE (PDS) 

The PDS performed on sample 72143 passed TestAmerica’s control limits of 85–115% 

recovery for all analytes except aluminum, boron, calcium, iron, magnesium, titanium, 

and zinc. Calcium, magnesium, and zinc were qualified with a “W”. Calcium and 

magnesium did pass in the matrix spike for this sample. Aluminum, boron, iron and 

titanium failed the PDS; however, the percent recoveries were not calculated by the 

laboratory because their concentrations were greater than 4 times the PDS spike level. 

Aluminum, boron, and titanium passed TestAmerica’s requirement of percent differences 

less than 10% for the serial dilution for this sample demonstrating that there were no 

significant matrix interference with these elements. Iron and zinc failed TestAmerica’s 

requirements for the serial dilution; therefore, based on these cumulative results, iron and 

zinc are being qualified as suspect due to matrix interference. These additional qualifiers 

appear in Table 2. 

The PDS performed on sample 72147 passed TestAmerica’s control limits of 85–115% 

recovery for all analytes except boron and manganese. Manganese was qualified with a 

“W”. Boron failed the PDS; however, the percent recovery was not calculated by the 

laboratory because its concentration was greater the 4 times the PDS spike level. Both 

boron and manganese passed TestAmerica’s requirement of percent differences less than 

10% for the serial dilution for sample 72147 demonstrating that there were no significant 

matrix interferences. No additional qualifier is required due to this PDS. 

The PDS performed on sample 72196 passed TestAmerica’s control limits of 85–115% 

recovery for all analytes except boron and manganese; however, the percent recoveries 

were not calculated by the laboratory because their concentrations were greater than 4 

times the PDS spike level. Both boron and manganese passed TestAmerica’s requirement 

of percent differences less than 10% for the serial dilution for sample 72196 

demonstrating that there were no significant matrix interferences. No additional qualifier 

is required due to this PDS. 

DETECTION LIMITS 

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water. 

Table 2. Data Review Summary 

Sample Analyte Qualifier/Action Reason Level Detected 

72143 Iron (total) Matrix 

Interference 

PDS and SD Failed XXX μg/L 

72143 Zinc (total) Matrix 

Interference 

PDS and SD Failed XXX ug/L 
1 

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

CC: Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Jennifer Colby, ERG 

Date: 2/9/2012 

Subject: TestAmerica Data Review Narrative for Classicals Analyses – Long-Term 

Monitoring: Month 3 

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for these long-term monitoring samples. All samples were tested for the 

following analytes: 

• Ammonia by EPA method 350.1, 

• Biochemical Oxygen Demand – 5 day (BOD5) by SM 5210B, 

• Chloride and Sulfate by EPA method 300.0, 

• Chemical Oxygen Demand (COD) by EPA method 410.4, 

• Cyanide (total) by SM 4500 CN- E, 

• Nitrate/Nitrite by EPA method 353.2 

• Phosphorus (total) by EPA method 365.1, 

• Total Dissolved Solids (TDS) by SM 2540C, 

• Total Kjeldakl Nitrogen (TKN) by EPA method 351.2, and 

• Total Suspended Solids (TSS) by SM 2540D. 

Table 1 summarizes the 15 samples that TestAmerica analyzed for the above analytes. 

Table 1. Long-Term Monitoring Month 3 Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71993 Water FGD Influent, Set 3 12/08/2010 

71997 Water FGD Bioreactor Influent, Set 3 12/09/2010 

72001 Water FGD Bioreactor Effluent, Set 3 12/09/2010 

72043 Water FGD Influent, Set 3 12/08/2010 

72047 Water FGD Effluent, Set 3 12/08/2010 

72093 Water FGD Influent, Set 3 12/07/2010 

72097 Water FGD Effluent, Set 3 12/07/2010 

72143 Water FGD Influent, Set 3 12/06/2010 

72147 Water FGD Bioreactor Influent, Set 3 12/07/2010 
2 

Table 1. Long-Term Monitoring Month 3 Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72151 Water FGD Bioreactor Effluent, Set 3 12/07/2010 

72192 Water FGD Influent, Set 1 12/08/2010 

72196 Water FGD SBR Influent, Set 1 12/08/2010 

72200 Water FGD SBR Effluent, Set 1 12/08/2010 

72243 Water FGD Influent, Set 3 12/09/2010 

72247 Water FGD Effluent, Set 3 12/09/2010 

SUMMARY 

All samples were analyzed within the holding time specified in 40 CFR 136 Table II 

unless otherwise noted below. All samples were preserved appropriately unless 

otherwise specified below. Samples 72192, 72196, and 72200 had no collection dates or 

times listed on the traffic report, and were given the date of relinquishment. Many of the 

traffic reports did not have receipt temperatures.

 

Field duplicate samples were not collected for this episode. Depending on the method, a 

laboratory duplicate was analyzed instead. The Relative Percent Difference (RPD) 

between the sample and its duplicate was less than 20% unless otherwise noted below. 

If applicable, the appropriate number of standards was used to create a calibration curve. 

If sample results were above the highest standard used to create the curve, the sample was 

diluted and reanalyzed. All sample results were between the lowest and highest standards 

unless noted below. Additionally, 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) analysis was run on sample 72147 and 

sample 72196 for each analyte to check for matrix interferences. All MS samples 

analyzed met the criteria specified in the method unless described below. 
3 

DATA NOTES/ISSUES 

Ammonia 

The result for the method blank associated with one of the batches was greater than the 

MDL. All associated samples were flagged with a “B” qualifier. This affects samples 

72147, 72143, 72093, 72097, and 72151. No further action is required. 

The percent recoveries for the MS and matrix spike duplicate (MSD) for sample 72147 

were 93% and 102%, respectively, which is within the method control criteria; however, 

the results exceeded the calibration range. These MS and MSD and results were flagged 

with an “E” qualifier. 

BOD5 

TestAmerica analyzed five dilutions, but no dilutions had a dissolved oxygen (DO) 

depletion greater than 2.0 mg/L for samples 72143, 72151, 72043, 71993, and 72247. 

Therefore, BOD5 was reported as not detected for these samples. Additionally, for sample 

72200, the dilutions did not have a residual DO criteria of greater than 1.0 mg/L; 

therefore, BOD5 was reported as not detected for this sample. The rest of the samples had 

at least one dilution with a DO depletion greater than 2.0 mg/L. As required in the 

method, the final result was calculated by taking the average of the results for all 

dilutions with a DO depletion greater than 2.0 mg/L and a final DO greater than 1.0 

mg/L. 

Chloride and Sulfate 

MS and MSD were performed on samples 72147 and 72196. The MS/MSD recoveries 

for both samples were within the method control for both chloride and sulfate; however, 

the MS and MSD results for chloride exceeded the calibration range. Both sets of 

MS/MSD results were flagged with “E” qualifiers. 

COD 

MS and MSD were performed on samples 72147 and 72196. The MS and MSD 

recoveries for sample 72147 were 66% and 71%, respectively, which is outside the 

method control criteria. These MS/MSD results were flagged with an “F” qualifier. The 

MS and MSD recoveries for sample 72196 were 72% and 70%, respectively, which is 

outside the method control criteria. These MS/MSD results were flagged with an “F” 

qualifier. 

Cyanide 

Because of the nature of the sample matrix, all of the samples in this sampling episode 

used a lower volume, which resulted in elevated RLs being calculated and reported by 

TestAmerica with the sample results. 
4 

MS and MSD were performed on samples 72147 and 72196. The MS and MSD 

recoveries for sample 72147 were 76% and 75%, respectively. The MS and MSD 

recoveries for sample 72196 were 59% and 57%, respectively. The LCS/LCSD 

recoveries associated with these batches were acceptable, which indicates the analytical 

system was operating within control. Additionally, there is no method requirement for the 

analysis of a MS/MSD and therefore, no corrective action is necessary. 

Nitrate/Nitrite 

No MS/MSD data was reported for batch 45200 in the sample and QC sample report 

summary. The method requires that a known amount of analyte be added to 10% of 

samples per batch. The general chemistry worksheet indicates that MS samples were 

performed on a sample outside of these episodes, but no spiking concentrations or percent 

recoveries are indicated. The MS/MSD recoveries for the other batches were within 

control limits. 

Phosphorus 

The results for the method blanks associated with two of the batches was greater than the 

MDL, but less than the RL. The blank results were flagged with a “J” qualifier. All 

associated samples were qualified with a “B” flag. No additional corrective action is 

necessary. 

MS and MSD were performed on sample 72001, 72147 and 72196. The percent 

recoveries for the MS and MSD for sample 72147 were 69% and 70%, respectively, 

which is outside the method control criteria. These MS/MSD results were flagged with 

an “F” qualifier. The LCS/LCSD recoveries for this batch were acceptable and indicate 

that the analytical system was operating within control. The percent recoveries for the 

MS and MSD for sample 72196 were 91% and 85%, respectively. The MSD recovery is 

outside the method control criteria, but within the laboratory criteria and therefore, was 

not flagged. If reported, the MSD result should be flagged with an “F” qualifier. The 

LCS/LCSD recoveries for this batch were acceptable and indicate that the analytical 

system was operating within control. Additionally, the MS/MSD performed on sample 

72001 was in the same batch as the MS/MSD for 72196 and the percent recoveries for the 

MS and MSD were 96% and 97%, respectively, with are within the method control 

criteria. 

TDS 

TA reports that constant weight was not achieved after 3 drying cycles for the following 

samples: 72097, 72143, 72147, 72151, 71993, 72196, 72200, 71997, 72004, and 72243. 

Review of the general chemistry worksheets indicates that constant weight was achieved 

for all samples. No further action was necessary. 
5 

Because of the nature of the sample matrix, some of the samples in this sampling episode 

used a lower volume, which resulted in elevated RLs being calculated and reported by 

TestAmerica with the sample results. 

The analytical duplicate associated with sample 72143 exceeded the recovery criteria. 

The duplicate result was qualified with an “F” flag. Because an analytical duplicate was 

not required by the method, no further corrective action is necessary. 

TKN 

MS and MSD were performed on samples 72147 and 72196. The MS and MSD 

recoveries for sample 72147 were 76% and 57%, respectively. The concentration in the 

original sample was greater than four times the spike amount; therefore, the recoveries 

cannot be reliably calculated and the results were flagged with a “4” qualifier. The MS 

and MSD recoveries for sample 72196 were 81% and 78%, respectively, which do not 

meet the method control criteria, but do meet the laboratory control criteria and therefore, 

these results were not flagged by the laboratory. If reported, the MS and MSD results 

should be flagged with “F” qualifiers. The LCS/LCSD recoveries associated with these 

batches were acceptable, which indicates the analytical system was operating within 

control. 

TSS 

Because of the nature of the sample matrix, some of the samples in this sampling episode 

used a lower volume, which resulted in elevated RLs being calculated and reported by 

TestAmerica with the sample results. 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD 

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Donna Tedder, ERG 

Date: 2/9/2012

Subject: FGS Data Review Narrative for Total Mercury – Long-Term Monitoring: 

Month 4 and 5

Frontier Global Sciences (FGS) generated analytical data for total mercury. FGS 

analyzed the samples according to EPA Method 1631E for mercury by Cold Vapor 

Atomic Fluorescence Spectrometry (CVAFS) analysis. 

Table 1 summarizes the 30 samples (excluding laboratory prep blanks) FGS extracted 

and analyzed for total mercury. 

Table 1. Long-Term Monitoring Month 4 and 5 Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71994 1101223-48 Aqueous FGD Influent, Set 4 1/17/2011

71998 1101223-53 Aqueous FGD Bioreactor Influent, Set 4 1/17/2011

72002 1101223-58 Aqueous FGD Bioreactor Effluent, Set 4 1/17/2011

72007 1101223-59 Aqueous FGD Bioreactor Influent Field Blank, Set 4 1/17/2011

72011 1101223-60 Aqueous FGD Bioreactor Effluent Field Blank, Set 4 1/17/2011

72044 1101308-01 Aqueous FGD Influent, Set 4 1/26/2011

72048 1101308-06 Aqueous FGD Effluent, Set 4 1/25/2011

72053 1101308-07 Aqueous FGD Effluent Field Blank, Set 4 1/25/2011

72094 1101223-41 Aqueous FGD Influent, Set 4 1/14/2011

72098 1101223-46 Aqueous FGD Effluent, Set 4 1/14/2011

72103 1101223-47 Aqueous FGD Effluent Field Blank, Set 4 1/13/2011

72144 1101223-21 Aqueous FGD Influent, Set 4 1/12/2011

72148 1101223-26 Aqueous FGD Bioreactor Influent, Set 4 1/12/2011

72152 1101223-31 Aqueous FGD Bioreactor Effluent, Set 4 1/12/2011

72157 1101223-32 Aqueous FGD Bioreactor Influent Field Blank, Set 4 1/12/2011

72161 1101223-33 Aqueous FGD Bioreactor Effluent Field Blank, Set 4 1/12/2011

72193 1101223-08 Aqueous FGD Influent, Set 3 1/12/2011

72197 1101223-13 Aqueous FGD SBR Influent, Set 3 1/12/2011

72201 1101223-18 Aqueous FGD SBR Effluent, Set 3 1/12/2011
2

Table 1. Long-Term Monitoring Month 4 and 5 Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72206 1101223-19 Aqueous FGD SBR Influent Field Blank, Set 3 1/12/2011

72210 1101223-20 Aqueous FGD SBR Effluent Field Blank, Set 3 1/12/2011

72244 1101223-34 Aqueous FGD Influent, Set 4 1/12/2011

72248 1101223-39 Aqueous FGD Effluent, Set 4 1/13/2011

72253 1101223-40 Aqueous FGD Effluent Field Blank, Set 4 1/12/2011

72293 1101223-01 Aqueous FGD Influent, Set 3 1/12/2011 

72297 1101223-06 Aqueous FGD Effluent, Set 3 1/12/2011

72302 1101223-07 Aqueous FGD Effluent, Field Blank, Set 3 1/12/2011

72294 1102108-01 Aqueous FGD Influent, Set 4 2/9/2011

72298 1102108-06 Aqueous FGD Effluent, Set 4 2/9/2011

72303 1102108-07 Aqueous FGD Effluent Field Blank, Set 4 2/9/2011

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. The following summarizes the findings from the data review: 

• The sample number for Sample 72157 was labeled incorrectly on the traffic 

report. 

• The sample description for Sample 72148 was entered incorrectly by FGS at the 

time of sample receipt. 

• Two laboratory duplicates were out of the method-suggested relative percent 

difference (RPD) criteria. 

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES 

Sample 72157 was labeled incorrectly as Sample 721557 in the traffic report submitted to 

the laboratory. The error was identified and corrected during the data review based on 

the sample description. FGS incorrectly labeled Sample 72148 as the FGD Bioreactor 

Effluent, Set 4, when the correct sample description is FGD Bioreactor Influent, Set 4. 

This error was identified and corrected during the data review and confirmed based on 

the traffic report. 
3

INITIAL CALIBRATION 

FGS performed the initial calibrations on each analysis day. The initial calibration for 

the CVAFS analysis consisted of a blank and five calibration standards with a correlation 

coefficient ≥ 0.995. All method-specified criteria were met. 

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS 

All initial and continuing calibration verifications (ICVs, CCVs) met method-specified 

criteria. 

BLANKS 

All the preparation blanks or laboratory reagent blanks (LRBs) and the continuing 

calibration blanks (CCBs) met the method-specified criteria. Because all of the blank 

results were less than the RL, no samples were qualified based on these preparation blank 

results. 

DUPLICATES 

No field duplicate samples were collected with these sampling episodes. Four samples 

were analyzed in duplicate at the laboratory, Influent samples 72144 and 71994 and 

Effluent samples 72048 and 72298. The relative percent difference (RPD) for samples 

72144, 71994, 72048, and 72298 were 30.6%, 7.66%, 19.4% and 43.9%, respectively. 

Two of these RPDs were outside of laboratory criteria. The samples from another 

sampling episode were also analyzed in duplicate with RPDs of 13.3%, 22.4%, and 

3.03%. The laboratory’s RPD criteria between analytical duplicates is 24%. Analytical 

duplicates are not a method requirement; therefore, no samples were qualified based on 

analytical duplicates. 

LABORATORY CONTROL SAMPLES 

All laboratory control samples were within Frontier’s control limits of 80-120% recovery 

and 24% RPD. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

Matrix spikes (MS) and matrix spike duplicates (MSD) were performed on Influent 

sample 72144 and Effluent samples 72048 and 72298. MS/MSDs were also performed 

on samples from another sampling episode. All aqueous MS/MSD recoveries were 

within method specifications of 71-125%. All RPDs met method-specifiec criteria. 

DETECTION LIMITS 

The laboratory MDL in the synthetic matrix was 0.239 ng/L. Results below this MDL 

were reported as not detected (ND). 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD 

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Randy Mercurio, ERG 

Date: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.8 – Long-Term 

Monitoring: Month 4 

TestAmerica generated analytical data for total metals (antimony, arsenic, cadmium, 

chromium, copper, lead, nickel, selenium, silver, thallium and vanadium) for these longterm monitoring samples. The samples were analyzed according to EPA Method 200.8. 

Table 1 summarizes the samples TestAmerica extracted and analyzed for total metals by 

EPA Method 200.8.

Table 1. Long-Term Monitoring Month 4 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71994 FGD Influent, Set 4 280-11658-1 Aqueous 1/17/2011 1/18/2011

71998 FGD Bioreactor Influent, Set 4 280-11690-1 Aqueous 1/18/2011 1/19/2011

72002 FGD Bioreactor Effluent, Set 4 280-11690-2 Aqueous 1/18/2011 1/19/2011

72007 FGD Bioreactor Influent Field 

Blank, Set 4 

280-11690-3 Aqueous 1/18/2011 1/19/2011

72011 FGD Bioreactor Effluent Field 

Blank, Set 4 

280-11690-4 Aqueous 1/18/2011 1/19/2011

72094 FGD Influent, Set 4 280-11635-1 Aqueous 1/14/2011 1/15/2011

72098 FGD Effluent, Set 4 280-11635-2 Aqueous 1/14/2011 1/15/2011

72103 FGD Effluent Field Blank, Set 4 280-11635-3 Aqueous 1/14/2011 1/15/2011

72144 FGD Influent, Set 4 280-11555-1 Aqueous 1/12/2011 1/13/2011

72148 FGD Bioreactor Influent, Set 4 280-11597-1 Aqueous 1/13/2011 1/14/2011

72152 FGD Bioreactor Effluent, Set 4 280-11597-2 Aqueous 1/13/2011 1/14/2011

72157 FGD Bioreactor Influent Field 

Blank, Set 4 

280-11597-3 Aqueous 1/13/2011 1/14/2011

72161 FGD Bioreactor Effluent Field 

Blank, Set 4 

280-11597-4 Aqueous 1/13/2011 1/14/2011

72193 FGD Influent, Set 3 280-11552-1 Aqueous 1/12/2011 1/13/2011

72197 FGD SBR Influent, Set 3 280-11552-2 Aqueous 1/12/2011 1/13/2011

72201 FGD SBR Effluent, Set 3 280-11552-3 Aqueous 1/12/2011 1/13/2011
2

Table 1. Long-Term Monitoring Month 4 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72206 FGD SBR Influent Field Blank, 

Set 3 

280-11552-4 Aqueous 1/12/2011 1/13/2011

72210 FGD SBR Effluent Field Blank, 

Set 3 

280-11552-5 Aqueous 1/12/2011 1/13/2011

72244 FGD Influent, Set 4 280-11598-1 Aqueous 1/13/2011 1/14/2011

72248 FGD Effluent, Set 4 280-11598-2 Aqueous 1/13/2011 1/14/2011

72253 FGD Effluent Field Blank, Set 4 280-11598-3 Aqueous 1/13/2011 1/14/2011

72293 FGD Influent, Set 3 280-11553-1 Aqueous 1/12/2011 1/13/2011

72297 FGD Effluent, Set 3 280-11553-3 Aqueous 1/12/2011 1/13/2011

72302 FGD Effluent Field Blank, Set 3 280-11553-4 Aqueous 1/12/2011 1/13/2011

SUMMARY 

The samples were prepared for total metals analysis according to TestAmerica’s “FGD 

ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Elements 

Analysis in Flue Gas Desulfurization Wastewaters,” dated October 6, 2010, based on 

EPA Method 200.8, by ICP/MS analysis. 

Any significant findings are summarized below. No additional data qualifiers were 

required. 

• The sample for FGD Effluent, Set 3 associated with Episode 6571 was incorrectly 

labeled as sample 72295 on the traffic report. The correct sample number (72297) 

was found on the sample bottle label and confirmed with ERG prior to analysis. 

• The matrix spike (MS) and matrix spike duplicate (MSD) recoveries for total 

silver for sample 72248 failed the EPA Method 200.8 control limits of 70-130%. 

The MSD recovery for total silver for sample 72201 also failed the method 

control limits. 

• The MS/MSD relative percent difference (RPD) for total silver for samples 72201 

and 72248 failed the FGD ICP/MS SOP control limits of ±20%. 

• The post digestion spike (PDS) recoveries for silver for samples 72201 and 72002 

failed TestAmerica’s control limits of 85–115%. 

INTERNAL STANDARDIZATION 

All internal standards used by TestAmerica were within the method criteria. 
3

INITIAL CALIBRATION 

TestAmerica performed the initial calibrations on each analysis 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 (RL); however, some elements 

were above the MDL and flagged with a “J” qualifier. No additional qualifiers were 

required for method blanks. 

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank 

(CCB)) were less than the RL; however, some elements were above the MDL and 

flagged with a “J” qualifier. No additional qualifiers were required for instrument blanks. 

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

All CRI samples passed TestAmerica’s SOP control limits of 50–150% recovery. 

LABORATORY CONTROL SAMPLES (LCS) 

All LCS samples passed the method QC limits of 85–115% recovery. 

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION 

Based on TestAmerica’s SOP, all interference check sample A (ICSA) results had 

analytes of interest with concentrations less than the RL or less than five times the RL 

when known inherent contaminants are present in the stock solution used to make the 

ICS. 

All interference check sample B (ICSAB) synthetic spikes recovered within 

TestAmerica’s SOP criteria of 70–130% of the true value. 

SERIAL DILUTION 

The serial dilution performed on samples 72201 and 72002 passed TestAmerica’s criteria 

of ±10% difference. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 
4

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

MS and MSD were performed on samples of 72201, 72248, and 72002. The MSD of 

sample 72201 failed the method control limits of 70–130% recovery for silver at 61%, 

which was flagged with an “F” qualifier. The MS/MSD of sample 72248 failed the 

method control limits of 70–130% recovery for silver at 66% and 45% respectively, 

which were flagged with an “F” qualifier. These silver failures are likely due to matrix 

interference from the high concentration of sulfates, which can form insoluble silver 

sulfide and/or silver sulfate. The silver recoveries in the associated LCS/LCSDs were 

acceptable. The RPD for the MS/MSDs for samples 72201 and 72248 failed the FGD 

ICP/MS SOP ±20% control limits for silver. 

Otherwise, all MS/MSD spike recoveries were within the method control limits of 70-

130% and the RPD for the MS/MSDs were within the FGD ICP/MS SOP control limits 

of ±20 percent. No additional data qualifiers were required. 

POST DIGESTION SPIKES (PDS) 

The PDS performed on samples 72201 and 72002 passed TestAmerica’s control limits of 

85–115% recovery for all analytes, except for silver for both PDS samples, which were 

flagged with a “W” qualifier. Additional data qualifiers would be required; however 

silver was not detected in these samples. 

DETECTION LIMITS 

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water. 
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: 2/9/2012

Subject: TestAmerica Data Review Narrative for Total Metals by 200.7 – Long-Term 

Monitoring: Month 4

TestAmerica generated analytical data for total metals (aluminum, boron, barium, 

beryllium, calcium, cobalt, iron, magnesium, manganese, molybdenum, sodium, tin, 

titanium and zinc) for these long-term monitoring samples. The samples were analyzed 

according to EPA Method 200.7. 

Table 1 summarizes the samples TestAmerica extracted and analyzed for total metals by 

EPA Method 200.7. 

Table 1. Long-Term Monitoring Month 4 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71994 FGD Influent, Set 4 280-11658-1 Aqueous 1/17/2011 1/18/2011

71998 FGD Bioreactor Influent, Set 4 280-11690-1 Aqueous 1/18/2011 1/19/2011

72002 FGD Bioreactor Effluent, Set 4 280-11690-2 Aqueous 1/18/2011 1/19/2011

72007 FGD Bioreactor Influent Field 

Blank, Set 4 

280-11690-3 Aqueous 1/18/2011 1/19/2011

72011 FGD Bioreactor Effluent Field 

Blank, Set 4 

280-11690-4 Aqueous 1/18/2011 1/19/2011

72094 FGD Influent, Set 4 280-11635-1 Aqueous 1/14/2011 1/15/2011

72098 FGD Effluent, Set 4 280-11635-2 Aqueous 1/14/2011 1/15/2011

72103 FGD Effluent Field Blank, Set 4 280-11635-3 Aqueous 1/14/2011 1/15/2011

72144 FGD Influent, Set 4 280-11555-1 Aqueous 1/12/2011 1/13/2011

72148 FGD Bioreactor Influent, Set 4 280-11597-1 Aqueous 1/13/2011 1/14/2011

72152 FGD Bioreactor Effluent, Set 4 280-11597-2 Aqueous 1/13/2011 1/14/2011

72157 FGD Bioreactor Influent Field 

Blank, Set 4 

280-11597-3 Aqueous 1/13/2011 1/14/2011

72161 FGD Bioreactor Effluent Field 

Blank, Set 4 

280-11597-4 Aqueous 1/13/2011 1/14/2011

72193 FGD Influent, Set 3 280-11552-1 Aqueous 1/12/2011 1/13/2011

72197 FGD SBR Influent, Set 3 280-11552-2 Aqueous 1/12/2011 1/13/2011

72201 FGD SBR Effluent, Set 3 280-11552-3 Aqueous 1/12/2011 1/13/2011
2

Table 1. Long-Term Monitoring Month 4 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72206 FGD SBR Influent Field Blank, 

Set 3 

280-11552-4 Aqueous 1/12/2011 1/13/2011

72210 FGD SBR Effluent Field Blank, 

Set 3 

280-11552-5 Aqueous 1/12/2011 1/13/2011

72244 FGD Influent, Set 4 280-11598-1 Aqueous 1/13/2011 1/14/2011

72248 FGD Effluent, Set 4 280-11598-2 Aqueous 1/13/2011 1/14/2011

72253 FGD Effluent Field Blank, Set 4 280-11598-3 Aqueous 1/13/2011 1/14/2011

72293 FGD Influent, Set 3 280-11553-1 Aqueous 1/12/2011 1/13/2011

72297 FGD Effluent, Set 3 280-11553-3 Aqueous 1/12/2011 1/13/2011

72302 FGD Effluent Field Blank, Set 3 280-11553-4 Aqueous 1/12/2011 1/13/2011

SUMMARY 

The samples were prepared for total metals analysis according to TestAmerica’s SOP for 

ICP Analysis for Trace Metals by Method 200.7. Any significant findings are 

summarized below. No additional data qualifiers were required for this set of data. 

• Several samples did not have the date and time of sample collection listed on the 

traffic reports. 

• One sample was listed with the wrong sample number on the traffic report. 

• The post digestion spike (PDS) for sodium for sample 72002 failed 

TestAmerica’s control limits of 85–115% recovery. 

SAMPLE RECEIPT, HANDLING AND STORAGE ISSUES 

Samples associated with Episode 6569 (72193, 72197, 72201, 72206, and 72210) did not 

have a sample date or time on the traffic report or sample labels. 

Samples associated with Episode 6571 (72293, 72297, and 72302) did not have a sample 

date or time on the traffic report or sample labels. Additionally, a field sampler name was 

not present on the traffic report. The sample FGD Effluent, Set3 was listed on the traffic 

report as sample 72295, which is incorrect; however, the sample bottle was labeled 

correctly as sample 72297. TestAmerica used 72297 for processing the sample. 

Samples of 72144 FGD Influent, Set 4 did not have a sample date or time listed on the 

sample bottles. 
3

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 

TestAmerica performed the initial calibrations on each analysis day. The initial 

calibration for the ICP analysis consisted of a blank and one calibration standard. 

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS 

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 (RL); however, some elements 

were above the method detection limit (MDL) and were flagged with the “J” qualifier. 

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank 

(CCB)) were less than the RL; however, some elements were above the MDL and were 

flagged with the “J” qualifier. 

REPORTING LIMIT VERIFICATION STANDARD (CRI) 

All CRI samples passed TestAmerica’s SOP control limits of 50–150% recovery. 

LABORATORY CONTROL SAMPLES (LCS) 

All LCSs passed the method control limits of 85–115% recovery. 

INTERFERENCE CHECK SOLUTIONS 

Interference checks were performed using the synthetic matrix as the check solution. All 

data quality objectives met TestAmerica’s SOP criteria.

SERIAL DILUTION (SRD) 

Serial dilutions were performed for each batch of total samples. All serial dilution percent 

differences were less than 10% as required by TestAmerica’s SOP. 

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 
4

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

Matrix spikes (MS) and matrix spike duplicates (MSD) were performed on the total 

samples of 72201, 72248, and 72002. Some elements with high concentrations 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. These data were considered acceptable 

based on the LCS passing the method control limits. Otherwise, all MS/MSD spike 

recoveries were within the method control criteria of 70-130%. The relative percent 

difference (RPD) for all MS/MSDs were within TestAmerica’s ± 20% requirement, 

except for magnesium for sample 72095. No additional data qualifiers were needed. 

POST DIGESTION SPIKE (PDS) 

The PDS performed on sample 72201 failed the method criteria of 85–115% recovery for 

boron; however, the result was not qualified with a “W” because the sample 

concentration was greater than 4 times the spike amount. 

The PDS performed on sample 72002 failed the method criteria of 85–115% recovery for 

boron, magnesium and manganese; however, these results were not qualified with a “W” 

because their sample concentrations were greater than 4 times the spike amount. Sodium 

also failed the method criteria and was flagged with a “W” qualifier. All elements passed 

the serial dilution for this sample demonstrating that there were no significant matrix 

interferences. No additional data qualifiers are required.

DETECTION LIMITS 

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water. 
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: Jennifer Colby, ERG 

 Donna Tedder, ERG 

Date: 2/9/2012 

Subject: TestAmerica Data Review Narrative for Classicals Analyses – Long-Term 

Monitoring: Month 4 

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for these long-term monitoring samples. All samples were tested for the 

following analytes: 

• Ammonia by EPA method 350.1, 

• Biochemical Oxygen Demand – 5 day (BOD5) by SM 5210B, 

• Chloride and Sulfate by EPA method 300.0, 

• Chemical Oxygen Demand (COD) by EPA method 410.4, 

• Cyanide (total) by SM 4500 CN- E, 

• Nitrate/Nitrite by EPA method 353.2 

• Phosphorus (total) by EPA method 365.1, 

• Total Dissolved Solids (TDS) by SM 2540C, 

• Total Kjeldakl Nitrogen (TKN) by EPA method 351.2, and 

• Total Suspended Solids (TSS) by SM 2540D. 

Table 1 summarizes the 15 samples that TestAmerica analyzed for the above analytes. 

Table 1. Long-Term Monitoring Month 4 Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71994 Water FGD Influent, Set 4 1/21/2011 

71998 Water FGD Bioreactor Influent, Set 4 1/21/2011 

72002 Water FGD Bioreactor Effluent, Set 4 1/21/2011 

72094 Water FGD Influent, Set 4 1/18/2011 

72098 Water FGD Effluent, Set 4 1/18/2011 

72144 Water FGD Influent, Set 4 1/14/2011 

72148 Water FGD Bioreactor Influent, Set 4 1/17/2011 
2 

Table 1. Long-Term Monitoring Month 4 Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72152 Water FGD Bioreactor Effluent, Set 4 1/17/2011 

72193 Water FGD Influent, Set 3 1/14/2011 

72197 Water FGD SBR Influent, Set 3 1/14/2011 

72201 Water FGD SBR Effluent, Set 3 1/14/2011 

72244 Water FGD Influent, Set 4 1/17/2011 

72248 Water FGD Effluent, Set 4 1/17/2011 

72293 Water FGD Influent, Set 3 1/14/2011 

72297 Water FGD Effluent, Set 3 1/14/2011 

SUMMARY 

All samples were analyzed within the holding time specified in 40 CFR 136 Table II 

unless otherwise noted below. All samples were preserved appropriately unless 

otherwise specified. Group II samples 72293 and 72297 were received at the laboratory 

at a neutral pH. The laboratory preserved the volume and proceeded with the requested 

analyses. 

 

Field duplicate samples were not collected for this episode. Depending on the method, a 

laboratory duplicate was analyzed instead. The Relative Percent Difference (RPD) 

between the sample and its duplicate was less than 20% unless otherwise noted below. 

If applicable, the appropriate number of standards was used to create a calibration curve. 

If sample results were above the highest standard used to create the curve, the sample was 

diluted and reanalyzed. All sample results were between the lowest and highest standards 

unless noted below. Additionally, 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) analysis was run on samples 72002, 

72094, 72193, 72201, 72244, and 72297 for each analyte to check for matrix 

interferences. All MS samples analyzed met the criteria specified in the method unless 

described below. 
3 

DATA NOTES/ISSUES 

Ammonia 

Samples 72293 and 72297 were received by the laboratory at a neutral pH. Sample 

72293 was qualified as an estimated, as shown in Table 2. Sample 72297 had a result 

greater than the MDL, but less than the RL, so the result was already flagged with a ”J” 

qualifier, so further qualification was not necessary. 

The percent recoveries for the MS and MSD performed on sample 72094 were 77% and 

76%, respectively, which is outside of method control criteria. Additionally, the MS and 

MSD results exceeded the calibration range. The MS/MSD results for sample 72094 were 

flagged with “E” and “F” qualifiers. No further qualification is needed.

BOD5 

No issues were identified by the data reviewer. 

Chloride and Sulfate 

MS and MSD were performed on samples 72002, 72094, and 72201. The percent 

recoveries for the MS and MSD for all chloride and sulfate results were within the 

method control criteria; however, all the MS and MSD results exceeded the exceeded the 

calibration range, except for the MSD sulfate result for sample 72002. All these chloride 

and sulfate MS and MSD results were qualified with “E” qualifiers, except for the MSD 

sulfate result for sample 72002. 

COD 

Samples 72293 and 72297 were received by the laboratory at neutral pH. These results 

were qualified as estimated values, as shown in Table 2. 

MS and MSD were performed on samples 72002 and 72098. The percent recoveries for 

the MS and MSD for sample 72002 were 91% and 87%, respectively. The percent 

recoveries for the MS and MSD for sample 72098 were 90% and 88%, respectively. 

Both the MSD results are outside the method control criteria. These MSD results were 

flagged with “F” qualifiers. 

Cyanide 

MS and MSD were performed on samples 72193 and 72002. The percent recoveries for 

the MS and MSD for sample 72193 were 74% and 78%, respectively. The percent 

recoveries for the MS and MSD for sample 72002 were both 88%. The LCS/LCSD 

recoveries were acceptable, indicating that the analytical system was operating within 

control. Additionally, there is no method requirement for the analysis of a MS/MSD and 

no corrective action is necessary. 
4 

Nitrate/Nitrite 

Samples 72293 and 72297 were received by the laboratory at neutral pH. These results 

were qualified as estimated values, as shown in Table 2. 

Phosphorus 

Samples 72293 and 72297 were received by the laboratory at neutral pH. These results 

were qualified as estimated values, as shown in Table 2. 

The method blank associated with two of the batches detected phosphorus at levels 

greater than the MDL, but less than the RL. All affected samples were flagged with a “B” 

qualifier. No additional corrective action is necessary.

MS and MSD were performed on samples 72002 and 72297. The percent recoveries for 

the MS and MSD for sample 72002 were 72% and 56%, respectively, which are outside 

the method control criteria. The MS result was within the laboratory control criteria and 

therefore, was not flagged by the laboratory; however, the MSD result was outside the 

laboratory control criteria and was flagged with an “F” qualifier. The LCS/LCSD 

recoveries for this batch were acceptable, indicating the analytical system was operating 

within control. If reported, the MS result should be flagged with an “F” qualifier. 

The percent recoveries for the MS and MSD for sample 72297 were 66% and 58%, 

respectively, which are outside the method control criteria. There results were flagged 

with “F” qualifiers. The LCS/LCSD recoveries for this batch were acceptable, indicating 

the analytical system was operating within control. 

TDS 

TA reports that constant weight was not achieved after 3 drying cycles for the following 

samples: 72293, 72244, 71994, 72152, and 72248. Review of the general chemistry 

worksheets indicates that constant weight was achieved for all. No further action was 

necessary. 

The analytical duplicate performed on sample 72002 exceeded the recovery criteria. The 

duplicate result was flagged with an “F” qualifier. Because an analytical duplicate was 

not required by the method, no further corrective action is necessary. 

TKN 

Samples 72293 and 72297 were received by the laboratory at neutral pH. These results 

were qualified as estimated values, as shown in Table 2. 

MS and MSD were performed on samples 72001 and 72002. The percent recoveries for 

the MS and MSD for sample 72002 were both 93%, which is within the method control 
5 

criteria. The percent recoveries for the MS and MSD for sample 72001 were 48% and 

46%, respectively, which are outside the method control criteria. There results were 

flagged with “F” qualifiers. The LCS/LCSD recoveries for this batch were acceptable, 

indicating that the analytical system was operating within control. 

TSS 

Because of the nature of the sample matrix, some of the samples in this sampling episode 

used a lower volume, which resulted in elevated RLs being calculated and reported by 

TestAmerica with the sample results. 

The analytical duplicate performed on sample 72248 exceeded the recovery criteria. 

Because the sample result is below the RL, further qualification was not necessary. 

Table 2. Data Review Summary Table 

Sample Analyte Qualifier/Ac

tion 

Reason Level Detected

72293 Ammonia Estimated 

Value 

Received at neutral pH XXX mg/L 

72293 COD Estimated 

Value 

Received at neutral pH XXX mg/L 

72297 COD Estimated 

Value 

Received at neutral pH XXX mg/L 

72293 Nitrate/Nitrite Estimated 

Value 

Received at neutral pH XXX mg/L 

72297 Nitrate/Nitrite Estimated 

Value 

Received at neutral pH XXX mg/L 

72293 Phosphorus Estimated 

Value 

Received at neutral pH XXX mg/L 

72297 Phosphorus Estimated 

Value 

Received at neutral pH XXX mg/L 

72293 TKN Estimated 

Value 

Received at neutral pH XXX mg/L 

72297 TKN Estimated 

Value 

Received at neutral pH XXX mg/L