Appendix A

Duke Energy Carolinas’ Belews Creek Steam 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 Carolinas’ Belews Creek Steam 

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 bioreactor influent and bioreactor effluent sampling points. At the 

bioreactor influent and bioreactor 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 three 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 three 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 purge tank to the 

equalization tank. 

• FGD bioreactor influent (SP-2): This sampling point shall represent the effluent 

from the chemical precipitation system and the influent to the biological treatment 

system (prior to nutrient addition). This sampling point should be collected from 

the sample tap on the pipe that is downstream of the sand filters and the hold tank, 

but upstream of the heat exchanger. 

• FGD wastewater treatment effluent (SP-3): This sampling point shall represent 

the effluent from the biological treatment system, prior to mixing with dilution 

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

tap that is located on the pipe downstream of the second-stage bioreactor cells. 

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 

 
FGD Scrubber Purge 

(from Purge Tank)

Lime

Polymer

Equalization 

Tank Reaction Tank 1 Reaction 

Tank 2

Reaction 

Tank 3

SP-1

SP-2

Indicates a Sampling Point

Ferric 

Chloride

Filter

2

Holding 

Tank

Clarifier 1

Sludge 

Storage 

Tank

Filter Press

Sump

Filter 

Backwash

Filter

1

Solids to Fly 

Ash Landfill Wastewater Flow

Intermittent Wastewater Flow

Sludge Flow

Clarifier 

Sludge

Mix 

Chamber

Clarifier 2

Filter

3

Cooling Water

Nutrient

First-Stage 

Bioreactors 

(8)

First-Stage 

Effluent 

Storage

Second-Stage 

Bioreactors 

(8)

Second-Stage 

Effluent 

Storage

To Ash Basin

Bio Reactor Backflush

Hydrochloric 

Acid

SP-3

Figure 1. Belews Creek FGD Wastewater Treatment System Monitoring Program Sampling Points
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 

bioreactor influent and bioreactor 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 bioreactor influent and bioreactor 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 71991 6565 

FGD Wastewater Treatment Influent – Set 2 71992 6565 

FGD Wastewater Treatment Influent – Set 3 71993 6565 

FGD Wastewater Treatment Influent – Set 4 71994 6565 

FGD Bioreactor Influent – Set 1 71995 6565 

FGD Bioreactor Influent – Set 2 71996 6565 

FGD Bioreactor Influent – Set 3 71997 6565 

FGD Bioreactor Influent – Set 4 71998 6565 

FGD Bioreactor Effluent – Set 1 71999 6565 

FGD Bioreactor Effluent – Set 2 72000 6565 

FGD Bioreactor Effluent – Set 3 72001 6565 

FGD Bioreactor Effluent – Set 4 72002 6565 

FGD Wastewater Treatment Influent Field Blank 72003 6565 

FGD Bioreactor Influent Field Blank – Set 1 72004 6565 

FGD Bioreactor Influent Field Blank – Set 2 72005 6565 

FGD Bioreactor Influent Field Blank – Set 3 72006 6565 

FGD Bioreactor Influent Field Blank – Set 4 72007 6565 

FGD Bioreactor Effluent Field Blank – Set 1 72008 6565 

FGD Bioreactor Effluent Field Blank – Set 2 72009 6565 

FGD Bioreactor Effluent Field Blank – Set 3 72010 6565 

FGD Bioreactor Effluent Field Blank – Set 4 72011 6565 

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 Bioreactor Influent Collected during all 

four sets 

Collected during all 

four sets 

No field blanks 

required 

FGD Bioreactor 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 bioreactor influent and bioreactor effluent sampling 

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

over the 24-hour period. For mercury at the bioreactor influent and bioreactor effluent 

sampling points, 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 bioreactor 

influent and bioreactor effluent sampling points, 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 

bioreactor influent and bioreactor effluent sampling points. 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 bioreactor 

influent and bioreactor effluent sampling points: (NOTE: If a sample tap or valve is not 

available to collect these samples or if the bioreactor influent and bioreactor effluent 

sampling points have 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 “bubble-
wrapped” 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

Influent Samples 

Collected as 

Grabs

(Yes or No)

Mercury and Cyanide 

Samples Collected as 

Grabs

(Yes or No)

Bioreactor Influent 

and Bioreactor 

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)

Dilution Water 

Addition Prior 

to Biological 

Treatment 

System

(gpd)

Biological 

Treatment 

System Effluent 

Flow Rate (gpd)

Set 1Set 2Set 3Set 4

Plant Name

Date of Sample 

Collection

Sample 

Collection 

Number

Plant Operation During Sample Collection

FGD Wastewater Treatment Operation During Sample Collection

Plant Name

Date of Sample 

Collection

Sample 

Collection 

Number

Scrubber Purge 

Flow Rate During 

Influent Sample 

Collection

(gpm)

Percent Hydroclone 

Overflow Recycled 

Back to Scrubber Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Scrubber Slurry Blowdown Flow 

Rate Scrubber Slurry 

Percent Solids

Plant Operation During Sample Collection
Unit 1 Unit 2

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
Chemical 

Precipitation 

Effluent

Dilution Water 

Addition Prior to 

Biological 

Treatment 

System

Biological Treatment 

Plant Name Date System Effluent

FGD Wastewater Treatment System Flow Rates

(gpd)

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: 10 November 2010 

TO: Steam Electric Record 

FROM: Ron Jordan 

Engineering and Analysis Division 

 

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

Carolinas’ Belews Creek Steam Station on November 3-4, 2010 

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

Carolinas’ Belews Creek Steam Station (Belews Creek) located in Belews Creek, North 

Carolina. This was Belews Creek’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 3-4, 2010. These notes summarize the sample collection techniques used by 

Belews Creek at each of the sampling points and EPA’s observations/findings from the audit. A 

process water diagram for the flue gas desulfurization (FGD) wastewater treatment system is 

provided as Attachment 1. The treatment system is described in EPA’s sampling plan for the 

Belews Creek plant.1 The checklists that EPA completed during the audit are provided as 

Attachment 2. Pictures from the audit are provided as Attachment 3. 

Both generating units and both FGD units were operating throughout the period of 

sampling for Set 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) 

 Belews Creek personnel collected samples for the influent to FGD wastewater treatment 

system from a sample tap located on the wastewater piping downstream of the FGD purge tank 

and upstream 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 

Belews Creek FGD system. This is the same sampling point that EPA used during its sample 

collection. The sample tap consisted of PVC piping with a three-way splitter with barbed ends. 

Each tap was separately valved, although only one tap was used to collect all influent samples. A 

picture of the sample tap is included as Figure 1 in Attachment 3. 

Sample Collection 

 Set 2 samples for the FGD purge were collected on November 4, 2010. To collect the 

samples of the FGD purge, Belews Creek personnel followed EPA Method 1669 protocols and 

the EPA-provided instructions. Belews Creek personnel shrouded the tap with a clean plastic 

 

1

 Eastern Research Group, Inc. (ERG). Final Sampling Plan, Duke Energy Carolinas’ Belews Creek Steam Station, 

Belews Creek, NC, Sampling Episode 6558. May 27, 2010. 
Page 2 

bag and let the sample flow from the tap for two minutes prior to collecting any samples. All of 

the mercury and metals samples were filled while the samplers held the bottles under the 

shrouding. EPA and industry sample bottles were filled as duplicates (i.e., split samples and 

multi-fill technique was not used for the influent samples), with one bottle filled after the other 

was full. After the mercury and metals samples were collected, the shrouding was pulled away 

from the sample tap and Belews Creek personnel filled the bottles for classicals without the 

shrouding. The flow through the sample tap continued without interruption until all influent 

samples were collected. 

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

samples were collected during Set 1. 

Preservation 

 Belews Creek personnel followed all method specifications when preserving the classical 

samples. The Group II samples were preserved by adding H2SO4 at the sample location 

immediately after filling the bottles. After completing sample collection at the influent, the 

Group II samples were then taken to the on-site laboratory and the pH was confirmed to be 

below 2 S.U. The cyanide samples were checked in the laboratory 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 cyanide samples were then preserved using 

NaOH and the pH was confirmed to be above 10 S.U. The BOD, Group I, Group II, and cyanide 

samples were all placed on ice after collection or preservation. 

Field Measurements 

 Belews Creek personnel used a pH probe and a temperature probe in the laboratory to 

measure the pH and temperature of the influent field test bottle. 

Observations/Findings 

 EPA observed the Belews Creek 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 Belews Creek 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. Belews Creek personnel collected samples for analysis by both EPAcontracted laboratories (metals and classicals) and industry laboratories (metals only). The 

sample bottles were filled as duplicates, with one bottle filled after the other was full – in 

contrast to the multi-fill sample collection technique used at the other two sample points, and the 

split samples collected during EPA’s four-day sampling episodes. The bottles used were prelabeled in the laboratory. 

 Belews Creek personnel followed applicable procedures for sample collection and 

preservation. Samples were preserved within 15 minutes. Temperature and pH of the field test 

sample were measured approximately twenty minutes after sample collection. 
Page 3 

Influent to Bioreactor System (SP-2) 

 Belews Creek personnel collected samples for the influent to the bioreactor system (SP-2) 

from a sample tap downstream of the sand filters after the wastewater from the three filters is 

commingled. The sample tap is located on the wastewater piping after the three sand filter 

effluent streams are commingled, downstream of the holding tank and upstream of the heat 

exchanger. This is the same sampling point that EPA used during its sample collection. The 

sample tap consisted of PVC piping with a three-way splitter with barbed ends. Each tap was 

separately valved, allowing the mercury and cyanide grab samples to be collected from a 

dedicated tap without interrupting the composite sampler. Pictures of the sample tap are included 

as Figures 2a and 2b in Attachment 3. 

Sample Collection 

 Belews Creek personnel collected the influent to the bioreactor system 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, Belews 

Creek 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, Belews Creek personnel used a T-splitter tubing set 

that consisted of a short length of silicone tubing attached to the perpendicular end of a T-splitter 

and two longer pieces of silicone tubing attached to the other two ends of the T-splitter. Prior to 

completing the setup for the composite samples, Belews Creek personnel collected field blanks 

for SP-2 by threading the short end of the tubing set through the peristaltic pump on the ISCO 

Avalanche® portable sampler and attaching the end of the tubing to a vented cap on a 10-liter 

carboy and pumping reagent grade water into the carboy. To collect the composite samples, 

Belews Creek personnel attached one long end of the silicone tubing to one of the barbed sample 

taps and the other long end was directed to a nearby drain, and attached the vented cap and 

shorter length of tubing to a 20-liter carboy. Pictures of the sampling configuration are included 

as Figures 3a and 3b in Attachment 3. 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. Belews Creek personnel used a short 

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

ISCO Avalanche® 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. Belews Creek personnel then collected the field 

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

atmospheric contamination. The field blank bottles were filled as multi-fill split samples (i.e., 
Page 4 

one bottle was filled one-third full, then a second and any additional bottles were filled one-third 

full, and then the process was repeated until all field blank bottles were full). 

 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. Belews Creek personnel then collected the metals samples with the bottles 

placed in the clean box. The bottles were filled as multi-fill split samples (i.e., one bottle was 

filled one-third full, then a second and any additional bottles were filled one-third full, and then 

the process was repeated until all metals bottles were full). After all the metals samples were 

collected, the samplers filled the classicals samples outside the cleanbox. No classical samples 

were collected for analysis by industry-contracted laboratories. 

Belews Creek personnel also collected grab samples for mercury every six hours during 

the sampling. The samplers took steps to minimize atmospheric contamination of the samples by 

shrouding a second tap on the three-way splitter with a clean plastic bag. A clean shroud was 

used for each grab sample (EPA observed only grabs 1 and 2). A mercury field blank sample was 

collected prior to the first of the four mercury grab samples. The field blank was collected by 

filling the bottle under the shroud with reagent grade water. For the field blank, one of the EPA 

bottles was completely filled, then the industry sample bottle was completely filled, and then the 

second EPA field blank bottle was completely filled. The valve was then opened to allow sample 

flow through the sample tap for at least two minutes prior to collecting any samples. Belews 

Creek personnel filled the mercury bottles directly from the tap, underneath the shroud. Two 

samplers collected the mercury samples under the shroud, filling the bottles as multi-fill split 

samples (i.e., one sampler filled the EPA sample bottle one-third full, then the second sampler 

filled the Belews Creek sample bottle one-third full, and then the process was repeated until the 

bottles were full). Belews Creek personnel also collected the cyanide sample as a grab sample 

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

Preservation 

 Belews Creek personnel followed all method specifications when preserving the classical 

samples. The Group II samples were preserved by adding H2SO4 at the pump-off location 

immediately after filling the bottles. After completing pump-off of the composite samples, the 

Group II samples were then taken to the on-site laboratory and the pH was confirmed to be 

below 2 S.U. The cyanide samples were checked in the laboratory 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 cyanide samples were then preserved using 

NaOH and the pH was confirmed to be above 10 S.U. The BOD, Group I, Group II, and cyanide 

samples were all placed on ice after collection or preservation. 

Field Measurements 

 Belews Creek personnel used a pH probe and a temperature probe in the laboratory to 

measure the pH and temperature of the bioreactor influent field test bottle. 
Page 5 

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. Belews Creek personnel collected samples for analysis by 

both EPA-contracted laboratories (metals and classicals) and industry laboratories (metals only). 

The sample bottles (except mercury field blanks) were filled as multi-fill split samples. Belews 

Creek 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 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. 

 The ISCO pump cover was not easily removed, so during set-up of the composite sample 

the tubing end was threaded through the pump. The tubing end remained covered while 

threading. The bag on the end of the tubing was then replaced with a clean bag prior to the clean 

hands person handling the tubing end and the caps for the carboy. During pump-off, the 

sampling crew unscrewed and removed the pump cover so they could “lay” the tubing into the 

pump without having to thread the end of the tubing through the ISCO. 

 At the end of the 24-hour composite period, the carboy contained 20 liters. The 

temperature of the field blank carboy after filling all bottles (measured at 9:20 a.m.) was 5° C. 

The 20-liter carboy temperature after filling all sample bottles was 9.4° C (measured at 9:16 

a.m.). The carboy was kept on ice throughout the compositing period and until the carboy was 

placed on the sampling table for pump-off. The elevated temperature was unexpected and the 

sampling crew speculated that the reason may be that the drain hole on the trash can allowed 

water from melting ice to continuously exit the can, resulting in an ice-only environment instead 

of an ice-water bath that would have provided greater thermal conductivity. The EPA auditor 

recommended that future sampling sets either: (1) cover the existing drain hole and create a new 

drain hole at a higher level that allows the trash can to hold an ice-water mixture; or (2) cover the 

drain hole and use a pump and tubing to periodically remove excess water from the trash can. 

 Mercury grabs began approximately 2 hours after compositor for SP-2 was started. 
Page 6 

 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). 

 

Effluent from the Bioreactor System (SP-3) 

 Belews Creek personnel collected samples for the effluent from the bioreactor system 

(SP-3) from a sample tap on a section of piping downstream of the second-stage effluent storage 

tank from the second-stage bioreactor cells. This is the same sampling point that EPA used 

during its sample collection. The sample tap consisted of PVC piping with a three-way splitter 

with barbed ends. Each tap was separately valved, allowing the mercury and cyanide grab 

samples to be collected from a dedicated tap without interrupting the composite sampler. Pictures 

of the sample tap are included as Figures 3a, 3b and 3c in Attachment 3. 

Sample Collection 

 Belews Creek personnel collected samples for SP-3 using the same approach described 

above for SP-2. 

Preservation 

 Belews Creek personnel followed all method specifications when preserving the 

classical samples. The Group II samples were preserved by adding H2SO4 at the pump-off 

location immediately after filling the bottles. After completing pump-off of the composite 

samples, the Group II samples were then taken to the on-site laboratory and the pH was 

confirmed to be below 2 S.U. The cyanide samples were checked in the laboratory 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 cyanide samples were then 

preserved using NaOH and the pH was confirmed to be above 10 S.U. The BOD, Group I, 

Group II, and cyanide samples were all placed on ice after collection or preservation. 

Field Measurements 

 Belews Creek personnel used a pH probe and a temperature probe in the laboratory to 

measure the pH and temperature of the bioreactor effluent field test bottle. 

Observations/Findings 

 EPA observed the following activities for SP-3 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. Belews Creek personnel collected samples for analysis by 

both EPA-contracted laboratories (metals and classicals) and industry laboratories (metals only). 
Page 7 

The sample bottles (except mercury field blanks) were filled as multi-fill split samples. Belews 

Creek 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 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. 

 The ISCO pump cover was not easily removed, so during set-up of the composite sample 

and pump-off the sampling crew unscrewed and removed the pump cover so they could “lay” the 

tubing into the pump without having to thread the end of the tubing through the ISCO. 

 At the end of the 24-hour composite period, the carboy contained 20 liters (equal to the 

programmed volume). The temperature of the field blank carboy after filling all bottles was 4.7° 

C (measured at 10:35 a.m.). The 20-liter carboy temperature after filling all sample bottles was 

7.6° C (measured at 10:34 a.m.). The carboy was kept on ice throughout the compositing period 

and until the carboy was placed on the sampling table for pump-off. The elevated temperature 

was unexpected and the sampling crew speculated that the reason may be that the drain hole on 

the trash can allowed water from melting ice to continuously exit the can, resulting in an ice-only 

environment instead of an ice-water bath that would have provided greater thermal conductivity. 

The EPA auditor recommended that future sampling sets either: (1) cover the existing drain hole 

and create a new drain hole at a higher level that allows the trash can to hold an ice-water 

mixture; or (2) cover the drain hole and use a pump and tubing to periodically remove excess 

water from the trash can. 

 Mercury grabs began approximately 2 hours after compositor for SP-2 was started. 

 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). 
Attachment 1

Treatment System Process Water Diagram

   

Attachment 2

Audit Checklists

   



























Attachment 3

Photographs of Sample Points

   
Figure 1 – Influent to the FGD Wastewater Treatment System (FGD Purge; SP‐1)

   
Figure 2a – Influent to the Bioreactor System (SP‐2)
Figure 2b – Influent to the Bioreactor System (SP‐2)

   
Figure 3a – Effluent from the Bioreactor System (SP‐3)

   
Figure 3b – Effluent from the Bioreactor System (SP‐3)

   
Figure 3c – Collecting Mercury Samples at the Effluent from the Bioreactor System (SP‐3)
Section 3

Signed Certification Statement

Section 4

Engineering Data
Table A4-1. 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) 

6565 Set 1 - Grab 1 10/6/2010 1129 39.3 6565 Set 2 - Grab 1 11/3/2010 1145 32.7 

6565 Set 3 - Grab 1 12/8/2010 1038 34.3 6565 Set 4 - Grab 1 1/17/2011 1121 38.2 
Table A4-2. Field Measurements for Sample Collection at the Influent to the Bioreactor System, Belews 

Episode Number 

Sample Collection 

Number 

Date of Sample 

Collection 

Sample Collection 

Time 

Temperature

(°C) 

6565 Set 1 - Grab 1 10/6/2010 0845 31.7 

6565 Set 1 - Grab 2 10/6/2010 1442 33.9 6565 Set 1 - Grab 3 10/6/2010 2044 32.7 

6565 Set 1 - Grab 4 10/7/2010 0240 33.4 6565 Set 2 - Grab 1 11/3/2010 1055 31.1 

6565 Set 2 - Grab 2 11/3/2010 1716 31.3 6565 Set 2 - Grab 3 11/3/2010 2256 32.2 

6565 Set 2 - Grab 4 11/4/2010 0455 33.4 6565 Set 3 - Grab 1 12/8/2010 1003 26.9 

6565 Set 3 - Grab 2 12/8/2010 1606 27.3 6565 Set 3 - Grab 3 12/8/2010 2200 27.9 

6565 Set 3 - Grab 4 12/9/2010 0401 27.8 6565 Set 4 - Grab 1 1/17/2011 1048 27.8 

6565 Set 4 - Grab 2 1/17/2011 1655 28.0 6565 Set 4 - Grab 3 1/18/2011 2248 27.6 

6565 Set 4 - Grab 4 1/18/2011 0449 27.6 
Table A4-3. Field Measurements for Sample Collection at the Effluent from the Bioreactor System, Belew

Episode Number 

Sample Collection 

Number 

Date of Sample 

Collection 

Sample Collection 

Time 

Temperature

(°C) 

6565 Set 1 - Grab 1 10/6/2010 1035 30.2 

6565 Set 1 - Grab 2 10/6/2010 1650 30.2 6565 Set 1 - Grab 3 10/6/2010 2242 31.1 

6565 Set 1 - Grab 4 10/7/2010 0440 31.5 6565 Set 2 - Grab 1 11/3/2010 1007 29.5 

6565 Set 2 - Grab 2 11/3/2010 1608 28.5 6565 Set 2 - Grab 3 11/3/2010 2209 28.9 

6565 Set 2 - Grab 4 11/4/2010 0407 30.5 6565 Set 3 - Grab 1 12/8/2010 0923 25.4 

6565 Set 3 - Grab 2 12/8/2010 1526 25.5 6565 Set 3 - Grab 3 12/8/2010 2124 24.9 

6565 Set 3 - Grab 4 12/9/2010 0324 25.1 6565 Set 4 - Grab 1 1/17/2011 0956 26.6 

6565 Set 4 - Grab 2 1/17/2011 1608 26.6 6565 Set 4 - Grab 3 1/18/2011 2156 26.0 

6565 Set 4 - Grab 4 1/18/2011 0357 25.9 
Table A4-4. Sample Collection Procedures Used during the Sampling Episode 

Episode 

Number 

Sample 

Collection 

Number 

Influent 

Samples 

Collected as 

Grabs 

(Yes or No) 

Mercury 

and Cyanide 

Samples 

Collected as 

Grabs 

(Yes or No) 

Bioreactor Influent 

and Bioreactor 

Effluent Samples 

Collected as 24-

Hour Composites 

(Yes or No) 

Clean 

Hands/Dirty 

Hands Sampling 

Techniques Used

(Yes or No)* 

Description of 

Sample 

Collection 

Technique (if 

different than 

instructions) 

6565 Set 1 Yes Yes Yes Yes None 6565 Set 2 Yes Yes Yes Yes None 6565 Set 3 Yes Yes Yes Yes None 6565 Set 4 Yes Yes Yes Yes None 

* Includes the use of tyveks suits during all sampling events and dust masks during the collection of mercury samples.
Table A4-5. Generating Unit Operation at Time of Sampling, Belews Creek

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 

6565 Set 1 10/6/10 - 10/7/10 Unit 1/2 None 6565 Set 2 11/3/10 - 11/4/10 Unit 1/2 None 

6565 Set 3 12/8/10 - 12/9/10 Unit 1/2 None 6565 Set 4 1/17/11 - 1/18/11 Unit 1/2 None 
Table A4-6. FGD Scrubber Slurry Information at Time of Sampling, Belews Creek

Episode 

Number 

Sample 

Collection 

Number 

Date of Sample 

Collection Units 

Plant Operation During Sample Collec

Scrubber Slurry Blowdown 

Flow Rate 

Scrubber 

Slurry 

Percent 

Solids 

O

Flow Rate 

(gpm) Duration 

6565 Set 1 10/6/10 - 10/7/10 1 URE 17 hrs 15 - 17% 

6565 Set 1 10/6/10 - 10/7/10 2 URE 17 hrs 15 - 17% 6565 Set 2 11/3/10 - 11/4/10 1 URE 16 hrs 15 - 17% 

6565 Set 2 11/3/10 - 11/4/10 2 URE 10 hrs 15 - 17% 6565 Set 3 12/8/10 - 12/9/10 1 URE 12 hrs 15 - 17% 

6565 Set 3 12/8/10 - 12/9/10 2 URE 17 hrs 15 - 17% 6565 Set 4 1/17/11 - 1/18/11 1 URE 21 hrs 15 - 17% 

6565 Set 4 1/17/11 - 1/18/11 2 URE 0 hrs NA 

NA – not applicable. URE – Unable to reasonable estimate. 
Table A4-7. FGD Wastewater Treatment System Operation Information, Belews Creek

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) 

Organosulfide 

Usage 

(Liters/day) 

Polymer Us

(Liters/da

6565 Set 1 10/6/10 - 10/7/10 562 1 48.9 NA 43.8 6565 Set 2 11/3/10 - 11/4/10 446 1 40.0 NA 35.8 6565 Set 3 12/8/10 - 12/9/10 574 1 45.0 NA 10.3 6565 Set 4 1/17/11 - 1/18/11 476 1 35.5 NA 31.8 
Table A4-8. Daily Power Generation During Sampling Period, Belews Creek 

Episode Number Date 

Daily Power Generation 

(MW-hrs) 

Unit 1 Unit 2 

6565 9/20/2010 27,698 26,899 

6565 9/21/2010 27,624 26,075

6565 9/22/2010 28,111 26,848

6565 9/23/2010 27,713 25,944 

6565 9/24/2010 27,180 26,463 

6565 9/25/2010 26,143 23,956

6565 9/26/2010 27,915 902

6565 9/27/2010 27,286 0 

6565 9/28/2010 28,095 2 

6565 9/29/2010 25,967 22,135

6565 9/30/2010 23,581 22,695

6565 10/1/2010 22,823 22,552 

6565 10/2/2010 23,433 21,770 

6565 10/3/2010 22,504 19,434

6565 10/4/2010 23,484 22,153

6565 10/5/2010 25,332 22,566 

6565 10/6/2010 26,918 23,872 

6565 10/7/2010 25,717 24,425

6565 10/8/2010 25,676 23,331

6565 10/9/2010 25,740 23,570 

6565 10/10/2010 24,907 22,858 

6565 10/11/2010 27,102 25,534

6565 10/12/2010 24,980 23,013

6565 10/13/2010 26,020 24,782 

6565 10/14/2010 25,499 24,297 

6565 10/15/2010 25,865 24,575

6565 10/16/2010 26,652 23,538

6565 10/17/2010 27,283 23,495 

6565 10/18/2010 26,824 25,420 

6565 10/19/2010 27,577 24,689

6565 10/20/2010 27,198 24,889

6565 10/21/2010 26,653 24,249 

6565 10/22/2010 26,305 23,873 

6565 10/23/2010 27,329 26,267

6565 10/24/2010 27,910 25,270

6565 10/25/2010 27,930 27,085 

6565 10/26/2010 27,523 26,100 

6565 10/27/2010 28,240 26,987

6565 10/28/2010 27,229 25,175

6565 10/29/2010 26,248 24,991 

6565 10/30/2010 25,096 24,643 
Table A4-8. Daily Power Generation During Sampling Period, Belews Creek 

Episode Number Date 

Daily Power Generation

(MW-hrs) 

Unit 1 Unit 2

6565 10/31/2010 23,212 23,076 

6565 11/1/2010 27,690 23,600 

6565 11/2/2010 27,697 24,820

6565 11/3/2010 28,186 25,557

6565 11/4/2010 27,862 25,656 

6565 11/5/2010 26,534 25,724 

6565 11/6/2010 27,628 26,178

6565 11/7/2010 27,469 28,314

6565 11/8/2010 28,322 28,010 

6565 11/9/2010 27,435 26,873 

6565 11/10/2010 25,621 27,272

6565 11/11/2010 24,804 25,564

6565 11/12/2010 25,566 27,098 

6565 11/13/2010 26,156 27,811 

6565 11/14/2010 26,800 28,056

6565 11/15/2010 25,280 26,099

6565 11/16/2010 24,560 27,342 

6565 11/17/2010 9,884 24,747 

6565 11/18/2010 0 26,792

6565 11/19/2010 0 28,122

6565 11/20/2010 0 27,715 

6565 11/21/2010 0 25,458 

6565 11/22/2010 0 26,659

6565 11/23/2010 0 23,948

6565 11/24/2010 0 25,174 

6565 11/25/2010 0 25,045 

6565 11/26/2010 0 24,221

6565 11/27/2010 118 26,284

6565 11/28/2010 21,198 26,493 

6565 11/29/2010 27,689 27,921 

6565 11/30/2010 25,812 27,749

6565 12/1/2010 25,670 25,194

6565 12/2/2010 28,297 28,097 

6565 12/3/2010 25,920 28,077 

6565 12/4/2010 25,842 28,074

6565 12/5/2010 26,531 26,616

6565 12/6/2010 28,321 28,321 

6565 12/7/2010 28,314 28,260 

6565 12/8/2010 28,310 28,279

6565 12/9/2010 28,280 28,260

6565 12/10/2010 28,119 26,690 

6565 12/11/2010 28,320 27,098 

6565 12/12/2010 25,957 27,395
Table A4-8. Daily Power Generation During Sampling Period, Belews Creek 

Episode Number Date 

Daily Power Generation

(MW-hrs) 

Unit 1 Unit 2

6565 12/13/2010 26,537 28,320 

6565 12/14/2010 28,330 28,319 

6565 12/15/2010 28,329 28,323

6565 12/16/2010 21,628 28,319

6565 12/17/2010 0 28,320 

6565 12/18/2010 2,334 28,296 

6565 12/19/2010 28,048 26,794

6565 12/20/2010 28,328 28,319

6565 12/21/2010 28,321 28,320 

6565 12/22/2010 25,823 26,193 

6565 12/23/2010 25,973 27,530

6565 12/24/2010 27,370 27,855

6565 12/25/2010 25,457 27,419 

6565 12/26/2010 27,998 28,328 

6565 12/27/2010 28,002 28,240

6565 12/28/2010 27,341 28,228

6565 12/29/2010 28,320 28,320 

6565 12/30/2010 28,103 28,316 

6565 12/31/2010 26,311 28,001

6565 1/1/2011 26,100 24,947

6565 1/2/2011 21,107 24,846 

6565 1/3/2011 27,647 28,320 

6565 1/4/2011 28,320 28,320

6565 1/5/2011 28,320 28,321

6565 1/6/2011 28,009 27,244 

6565 1/7/2011 27,829 28,034 

6565 1/8/2011 27,891 25,518

6565 1/9/2011 28,311 28,320

6565 1/10/2011 28,320 28,320 

6565 1/11/2011 28,320 28,319 

6565 1/12/2011 28,320 28,284

6565 1/13/2011 28,320 28,316

6565 1/14/2011 28,320 28,321 

6565 1/15/2011 26,425 26,692 

6565 1/16/2011 28,320 414

6565 1/17/2011 28,318 0

6565 1/18/2011 28,325 11,564 
Table A4-9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Belews 

Creek 

Episode 

Number Date 

FGD Wastewater Treatment System Flow Rates

(gpd) 

Chemical 

Precipitation 

Effluent 

Dilution Water 

Addition Prior to 

Biological Treatment 

System 

Biological 

Treatment System 

Effluent 

6565 9/20/2010 706,256 0 653,466

6565 9/21/2010 639,850 0 609,509

6565 9/22/2010 677,894 0 624,325 

6565 9/23/2010 840,951 0 760,600

6565 9/24/2010 735,328 0 370,634

6565 9/25/2010 660,858 0 598,833

6565 9/26/2010 656,579 0 615,693 

6565 9/27/2010 525,199 0 531,526

6565 9/28/2010 444,631 0 387,091

6565 9/29/2010 406,171 0 374,603

6565 9/30/2010 566,207 0 501,427 

6565 10/1/2010 660,667 0 599,597

6565 10/2/2010 684,161 0 619,025

6565 10/3/2010 664,081 0 608,294

6565 10/4/2010 643,462 0 571,850 

6565 10/5/2010 753,394 0 707,550

6565 10/6/2010 673,977 0 631,725

6565 10/7/2010 715,224 0 684,285

6565 10/8/2010 701,492 0 638,531 

6565 10/9/2010 680,179 0 550,773

6565 10/10/2010 646,665 0 537,001

6565 10/11/2010 807,618 0 726,870

6565 10/12/2010 654,350 0 576,079 

6565 10/13/2010 601,489 0 598,878

6565 10/14/2010 597,007 0 550,905

6565 10/15/2010 541,134 0 518,106

6565 10/16/2010 617,902 0 518,885 

6565 10/17/2010 646,346 0 603,260

6565 10/18/2010 601,388 0 571,273

6565 10/19/2010 626,625 0 620,523

6565 10/20/2010 735,410 0 684,780 

6565 10/21/2010 600,972 0 594,851

6565 10/22/2010 560,127 0 495,207

6565 10/23/2010 686,334 0 642,367

6565 10/24/2010 676,409 0 616,462 

6565 10/25/2010 598,526 0 589,056

6565 10/26/2010 643,249 0 580,206
Table A4-9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Belews 

Creek 

Episode 

Number Date 

FGD Wastewater Treatment System Flow Rates 

(gpd) 

Chemical 

Precipitation 

Effluent 

Dilution Water 

Addition Prior to 

Biological Treatment 

System 

Biological 

Treatment System 

Effluent 

6565 10/27/2010 523,936 0 510,195

6565 10/28/2010 636,351 0 580,012

6565 10/29/2010 702,597 0 693,348

6565 10/30/2010 695,368 0 675,872 

6565 10/31/2010 619,118 0 613,784

6565 11/1/2010 667,227 0 628,371

6565 11/2/2010 631,422 0 610,251

6565 11/3/2010 550,457 0 497,156 

6565 11/4/2010 604,340 0 584,849

6565 11/5/2010 712,054 0 649,779

6565 11/6/2010 650,251 0 630,298

6565 11/7/2010 574,075 0 524,802 

6565 11/8/2010 643,192 0 617,130

6565 11/9/2010 701,917 0 598,526

6565 11/10/2010 676,120 0 634,792

6565 11/11/2010 604,798 0 543,168 

6565 11/12/2010 634,320 0 616,971

6565 11/13/2010 629,354 0 558,009

6565 11/14/2010 657,941 0 645,981

6565 11/15/2010 672,355 0 611,759 

6565 11/16/2010 645,042 0 617,885

6565 11/17/2010 624,574 0 573,176

6565 11/18/2010 431,117 0 421,809

6565 11/19/2010 327,193 0 304,260 

6565 11/20/2010 459,224 0 395,597

6565 11/21/2010 398,390 0 338,640

6565 11/22/2010 475,493 0 453,811

6565 11/23/2010 321,053 0 287,083 

6565 11/24/2010 360,562 0 317,463

6565 11/25/2010 212,701 0 161,533

6565 11/26/2010 512,945 0 480,913

6565 11/27/2010 354,404 0 298,010 

6565 11/28/2010 325,808 0 314,439

6565 11/29/2010 635,072 0 550,096

6565 11/30/2010 613,015 0 587,347

6565 12/1/2010 682,640 0 634,207 

6565 12/2/2010 608,521 0 591,683

6565 12/3/2010 713,763 0 638,061

6565 12/4/2010 612,491 0 577,772
Table A4-9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Belews 

Creek 

Episode 

Number Date 

FGD Wastewater Treatment System Flow Rates 

(gpd) 

Chemical 

Precipitation 

Effluent 

Dilution Water 

Addition Prior to 

Biological Treatment 

System 

Biological 

Treatment System 

Effluent 

6565 12/5/2010 749,637 0 691,468

6565 12/6/2010 707,767 0 685,714

6565 12/7/2010 670,589 0 570,605

6565 12/8/2010 634,133 0 610,976 

6565 12/9/2010 736,413 0 677,426

6565 12/10/2010 712,877 0 662,154

6565 12/11/2010 741,248 0 650,067

6565 12/12/2010 803,273 0 755,955 

6565 12/13/2010 807,277 0 735,913

6565 12/14/2010 831,267 0 767,424

6565 12/15/2010 704,652 0 640,099

6565 12/16/2010 806,653 0 778,567 

6565 12/17/2010 555,142 0 494,520

6565 12/18/2010 567,803 0 507,245

6565 12/19/2010 853,543 0 724,140

6565 12/20/2010 867,948 0 766,597 

6565 12/21/2010 818,960 0 728,866

6565 12/22/2010 720,616 0 689,370

6565 12/23/2010 729,921 0 700,263

6565 12/24/2010 819,617 0 801,906 

6565 12/25/2010 709,825 0 634,704

6565 12/26/2010 610,361 0 603,902

6565 12/27/2010 668,365 0 606,210

6565 12/28/2010 639,919 0 627,548 

6565 12/29/2010 700,584 0 677,755

6565 12/30/2010 687,805 0 691,305

6565 12/31/2010 629,254 0 573,049

6565 1/1/2011 614,054 0 602,259 

6565 1/2/2011 735,811 0 659,125

6565 1/3/2011 740,958 0 661,823

6565 1/4/2011 762,541 0 726,261

6565 1/5/2011 670,794 0 697,206 

6565 1/6/2011 692,636 0 659,152

6565 1/7/2011 677,100 0 688,275

6565 1/8/2011 620,483 0 591,875

6565 1/9/2011 664,391 0 687,862 

6565 1/10/2011 671,873 0 637,413

6565 1/11/2011 608,396 0 591,990

6565 1/12/2011 716,111 0 699,082
Table A4-9. FGD Wastewater Treatment System Flow Rate during Sampling Period, Belews 

Creek 

Episode 

Number Date 

FGD Wastewater Treatment System Flow Rates 

(gpd) 

Chemical 

Precipitation 

Effluent 

Dilution Water 

Addition Prior to 

Biological Treatment 

System 

Biological 

Treatment System 

Effluent 

6565 1/13/2011 643,593 0 664,841

6565 1/14/2011 647,890 0 620,460

6565 1/15/2011 687,496 0 673,236

6565 1/16/2011 575,722 0 532,612 

6565 1/17/2011 472,513 0 469,003

6565 1/18/2011 444,255 0 392,650
Section 5

Analytical Data
1 – Based on data review, data point needs to be excluded from the data set. 

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

presented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantit

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. Exc – Excluded from data set. 

Table A5-1. Influent to Wastewater Treatment System, Belews Creek 

Analyte Units Method 

Influent to FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 S

ClassicalsAmmonia mg/L 350.1 1.90 NQ (1.00) 2.00 1.1Nitrate Nitrite as N mg/L 353.2 18.0 21.0 * 14.0 15.Nitrogen, Total Kjeldahl mg/L 351.2 NQ (5.00) B 7.10 5.00 1.8Biochemical Oxygen Demand mg/L 5210B ND (2.00) ND (2.00) ND (2.00) ND (2Chemical Oxygen Demand mg/L 410.4 40.0 130 B 140 12Chloride mg/L 300.0 7,500 9,200 8,900 8,90Sulfate mg/L 300.0 1,100 1,100 1,200 1,10Cyanide, Total mg/L 4500 CN E NQ (0.100) NQ (0.100) ND (0.100) NQ (0Total Dissolved Solids mg/L 2540C --- Exc1 15,000 18,000 17,0Total Suspended Solids mg/L 2540D 2,200 2,600 3,300 2,90Phosphorus, Total mg/L 365.1 0.0780 2.70 B 5.20 B NQ (0.0Total MetalsAluminum ug/L 200.7 49,000 B,^ 100,000 B 150,000 140,0Antimony ug/L 200.8 6.50 20.0 33.0 26.Arsenic ug/L 200.8 92.0 230 280 34Barium ug/L 200.7 1,100 1,200 B 1,900 1,70
1 – Based on data review, data point needs to be excluded from the data set. 

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

presented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantit

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. Exc – Excluded from data set. 

Table A5-1. Influent to Wastewater Treatment System, Belews Creek 

Analyte Units Method 

Influent to FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 S

Beryllium ug/L 200.7 7.70 13.0 22.0 22.Boron ug/L 200.7 160,000 200,000 B 200,000 B 200,0Cadmium ug/L 200.8 4.00 5.10 5.70 7.8Calcium ug/L 200.7 3,300,000 4,300,000 B 4,600,000 B 4,600Chromium ug/L 200.8 100 270 ^ 340 32Cobalt ug/L 200.7 60.0 84.0 140 16Copper ug/L 200.8 80.0 190 270 33Iron ug/L 200.7 72,000 80,000 B 100,000 89,0Lead ug/L 200.8 67.0 200 320 33Magnesium ug/L 200.7 690,000 760,000 B 740,000 B 630,0Manganese ug/L 200.7 7,200 7,800 B 8,200 B 6,50Mercury ng/L 1631E 228,000 299,000 129,000 131,0Molybdenum ug/L 200.7 NQ (40.0) 57.0 76.0 89.Nickel ug/L 200.8 170 270 340 37Selenium ug/L 200.8 3,400 5,700 7,400 6,00Silver ug/L 200.8 ND (2.00) NQ (2.00) NQ (2.00) NQ (2Sodium ug/L 200.7 52,000 48,000 B 50,000 46,0Thallium ug/L 200.8 5.10 8.30 8.50 11.Tin ug/L 200.7 NQ (200) NQ (200) NQ (200) NQ (2
1 – Based on data review, data point needs to be excluded from the data set. 

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

presented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantit

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. Exc – Excluded from data set. 

Table A5-1. Influent to Wastewater Treatment System, Belews Creek 

Analyte Units Method 

Influent to FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 S

Titanium ug/L 200.7 940 2,500 B 3,800 4,70Vanadium ug/L 200.8 120 350 560 59Zinc ug/L 200.7 240 340 ^ 1,000 68
1 – Based on data review, data point needs to be excluded from the data set. 

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

presented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantit

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. Exc – Excluded from data set. 

Table A5-2. Influent to Bioreactor System, Belews Creek 

Analyte Units Method 

Influent to the Bioreactor System (SP-2) 

Set 1 Set 2 Set 3 Set 

ClassicalsAmmonia mg/L 350.1 2.20 NQ (1.00) 3.20 1.00 Nitrate Nitrite as N mg/L 353.2 16.0 16.0 * 12.0 14.0 Nitrogen, Total Kjeldahl mg/L 351.2 NQ (5.00) B 7.10 5.50 2.30 Biochemical Oxygen Demand mg/L 5210B ND (2.00) ND (2.00) NQ (2.50) ND (2.0Chemical Oxygen Demand mg/L 410.4 150 190 B 280 200 Chloride mg/L 300.0 7,500 8,800 8,800 8,700 Sulfate mg/L 300.0 1,200 1,300 1,200 1,200 Cyanide, Total mg/L 4500 CN E NQ (0.100) NQ (0.100) ND (0.100) NQ (0.1Total Dissolved Solids mg/L 2540C 13,000 14,000 14,000 12,000 Total Suspended Solids mg/L 2540D NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.0Phosphorus, Total mg/L 365.1 ND (0.0500) NQ (0.0500) B NQ (0.0500) B NQ (0.05
1 – Based on data review, data point needs to be excluded from the data set. 

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

presented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantit

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. Exc – Excluded from data set. 

Table A5-2. Influent to Bioreactor System, Belews Creek 

Analyte Units Method 

Influent to the Bioreactor System (SP-2) 

Set 1 Set 2 Set 3 Set 

Total MetalsAluminum ug/L 200.7 ND (200) ^ ND (200) ND (200) ND (20Antimony ug/L 200.8 2.30 3.00 6.60 8.40 Arsenic ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.0Barium ug/L 200.7 430 380 B 440 440 Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.0Boron ug/L 200.7 150,000 B 190,000 B 180,000 B,4 180,00Cadmium ug/L 200.8 ND (4.00) NQ (4.00) NQ (4.00) NQ (4.0Calcium ug/L 200.7 3,700,000 3,800,000 B 3,700,000 4 4,000,0Chromium ug/L 200.8 ND (8.00) ND (8.00) ^ ND (8.00) ND (8.0Cobalt ug/L 200.7 NQ (20.0) NQ (20.0) NQ (20.0) NQ (20Copper ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.0Iron ug/L 200.7 ND (200) NQ (200) B ND (200) NQ (20Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.0Magnesium ug/L 200.7 710,000 B 780,000 B 640,000 B,4 630,00Manganese ug/L 200.7 2,700 B 5,600 B 2,400 4 2,800 Mercury ng/L 1631E 508 119 752 117 Molybdenum ug/L 200.7 NQ (40.0) NQ (40.0) NQ (40.0) 45.0 Nickel ug/L 200.8 36.0 67.0 70.0 59.0 
1 – Based on data review, data point needs to be excluded from the data set. 

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

presented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantit

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. Exc – Excluded from data set. 

Table A5-2. Influent to Bioreactor System, Belews Creek 

Analyte Units Method 

Influent to the Bioreactor System (SP-2) 

Set 1 Set 2 Set 3 Set 

Selenium ug/L 200.8 120 89.0 900 4 110 Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.0Sodium ug/L 200.7 48,000 B 49,000 B 49,000 46,000 Thallium ug/L 200.8 3.50 3.70 6.00 6.60 Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (20Titanium ug/L 200.7 NQ (20.0) NQ (20.0) B NQ (20.0) NQ (20Vanadium ug/L 200.8 NQ (10.0) NQ (10.0) NQ (10.0) NQ (10Zinc ug/L 200.7 NQ (40.0) ND (40.0) ^ ND (40.0) ND (40
1 – Based on data review, data point needs to be excluded from the data set. 

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

presented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantit

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. Exc – Excluded from data set. 

Table A5-3. Effluent from Bioreactor System, Belews Creek 

Analyte Units Method 

Effluent from the Bioreactor System (SP

Set 1 Set 2 Set 3 Se

ClassicalsAmmonia mg/L 350.1 6.30 4.70 5.00 3.30 Nitrate Nitrite as N mg/L 353.2 NQ (0.100) 0.150 * 0.130 0.140 Nitrogen, Total Kjeldahl mg/L 351.2 7.40 B 10.0 7.10 3.60 Biochemical Oxygen Demand mg/L 5210B NQ (2.50) NQ (2.50) 3.50 ND (2.0Chemical Oxygen Demand mg/L 410.4 160 F 200 B 220 190 Chloride mg/L 300.0 7,300 8,400 9,100 8,300 Sulfate mg/L 300.0 1,300 1,300 1,300 1,200 Cyanide, Total mg/L 4500 CN E NQ (0.100) F NQ (0.100) ND (0.100) NQ (0.1Total Dissolved Solids mg/L 2540C 15,000 13,000 11,000 14,000 Total Suspended Solids mg/L 2540D 4.00 NQ (4.00) NQ (4.00) ND (4.0Phosphorus, Total mg/L 365.1 0.0840 0.120 B 0.0740 B 0.120 Total MetalsAluminum ug/L 200.7 NQ (200) ^ NQ (200) B ND (200) ND (20Antimony ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.0Arsenic ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.0Barium ug/L 200.7 450 420 B 450 480 
1 – Based on data review, data point needs to be excluded from the data set. 

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

presented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantit

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. Exc – Excluded from data set. 

Table A5-3. Effluent from Bioreactor System, Belews Creek 

Analyte Units Method 

Effluent from the Bioreactor System (SP

Set 1 Set 2 Set 3 Se

Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.0Boron ug/L 200.7 160,000 B 170,000 B 170,000 B 170,00Cadmium ug/L 200.8 ND (4.00) ND (4.00) ND (4.00) ND (4.0Calcium ug/L 200.7 3,200,000 3,800,000 B 4,000,000 4,100,0Chromium ug/L 200.8 ND (8.00) ND (8.00) ^ ND (8.00) ND (8.0Cobalt ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND (20Copper ug/L 200.8 ND (4.00) ND (4.00) ND (4.00) ND (4.0Iron ug/L 200.7 NQ (200) NQ (200) B NQ (200) NQ (20Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.0Magnesium ug/L 200.7 740,000 B 790,000 B 710,000 B 670,00Manganese ug/L 200.7 2,400 B 5,200 B 3,500 2,800 Mercury ng/L 1631E 403 162 24.2 2.99 Molybdenum ug/L 200.7 NQ (40.0) NQ (40.0) NQ (40.0) NQ (40Nickel ug/L 200.8 ND (4.00) NQ (4.00) ND (4.00) ND (4.0Selenium ug/L 200.8 NQ (4.00) NQ (10.0) 32.0 NQ (4.0Silver ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.0Sodium ug/L 200.7 53,000 B 49,000 B 51,000 47,000 Thallium ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.0Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (20
1 – Based on data review, data point needs to be excluded from the data set. 

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

presented in Tables A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantit

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. Exc – Excluded from data set. 

Table A5-3. Effluent from Bioreactor System, Belews Creek 

Analyte Units Method 

Effluent from the Bioreactor System (SP

Set 1 Set 2 Set 3 Se

Titanium ug/L 200.7 NQ (20.0) NQ (20.0) B NQ (20.0) NQ (20Vanadium ug/L 200.8 ND (10.0) NQ (10.0) NQ (10.0) ND (10Zinc ug/L 200.7 ND (40.0) NQ (40.0) ^ ND (40.0) ND (40
< - 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 A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantit

result is a J-value. 

Table A5-4. Classical Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment Sy

Creek 

Analyte Unit Method

Influent to FGD 

Wastewater Treatment 

System (SP-1) 4-Set Average 

Influent to 

Bioreactor System 

(SP-2) 

4-Set Average 

E

Bio

4

ClassicalsAmmonia mg/L 350.1 < 1.38 < 1.73 Nitrate Nitrite as N mg/L 353.2 17.0 14.5 Nitrogen, Total Kjeldahl mg/L 351.2 < 4.10 < 4.35 Biochemical Oxygen Demand mg/L 5210B ND (2.00) NQ (2.13) Chemical Oxygen Demand mg/L 410.4 108 205 Chloride mg/L 300.0 8,630 8,450 Sulfate mg/L 300.0 1,130 1,230 Cyanide, Total mg/L 4500 CN E NQ (0.100) NQ (0.100) Total Dissolved Solids mg/L 2540C 16,700 13,300 Total Suspended Solids mg/L 2540D 2,750 NQ (4.00) Phosphorus, Total mg/L 365.1 < 2.00 NQ (0.0500) 
< - 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 A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantit

result is a J-value. 

Table A5-5. Metal Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment System

Analyte Unit Method

Influent to FGD 

Wastewater Treatment 

System (SP-1) 4-Set Average 

Influent to Bioreactor 

System (SP-2) 4-Set Average 

Effluent f

Sys4-Se

Total MetalsAluminum ug/L 200.7 110,000 ND (200) NAntimony ug/L 200.8 21.4 5.08 NArsenic ug/L 200.8 236 NQ (4.00) NBarium ug/L 200.7 1,480 423 Beryllium ug/L 200.7 16.2 ND (2.00) NBoron ug/L 200.7 190,000 175,000 Cadmium ug/L 200.8 5.65 NQ (4.00) NCalcium ug/L 200.7 4,200,000 3,800,000 3Chromium ug/L 200.8 258 ND (8.00) NCobalt ug/L 200.7 111 NQ (20.0) NCopper ug/L 200.8 218 NQ (4.00) NIron ug/L 200.7 85,300 NQ (200) NLead ug/L 200.8 229 ND (2.00) NMagnesium ug/L 200.7 705,000 690,000 7Manganese ug/L 200.7 7,430 3,380 Mercury ng/L 1631E 197,000 374 Molybdenum ug/L 200.7 < 60.5 < 26.3 NNickel ug/L 200.8 288 58.0 NSelenium ug/L 200.8 5,630 305 Silver ug/L 200.8 NQ (2.00) ND (2.00) N
< - 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 A5-7 through A5-27 with a J flag designation. A “NQ” for the 4-set average result indicates that all results were below the quantit

result is a J-value. 

Table A5-5. Metal Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment System

Analyte Unit Method

Influent to FGD 

Wastewater Treatment 

System (SP-1) 4-Set Average 

Influent to Bioreactor 

System (SP-2) 4-Set Average 

Effluent f

Sys4-Se

Sodium ug/L 200.7 49,000 48,000 Thallium ug/L 200.8 8.23 4.95 NTin ug/L 200.7 NQ (200) ND (200) NTitanium ug/L 200.7 2,990 NQ (20.0) NVanadium ug/L 200.8 405 NQ (10.0) NZinc ug/L 200.7 565 NQ (40.0) N
Table A5-6. Field Blank Analytical Results, Belews Creek 

Analyte Sample Point Method Unit Concentration

Total Metals

Boron 

Influent to FGD Wastewater Treatment System 

Field Blank - Set 1 200.7 ug/L 200 
1 – Based on data review, data point needs to be excluded from the data set. 

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. Exc – Excluded from data set. 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 A5-7. Influent to FGD Wastewater Treatment System, Set 1 Analytical Results, Belew

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

Classicals Ammonia 350.1 mg/L 1 0.055 1 1.9 Nitrate Nitrite as N 353.2 mg/L 2 0.038 0.2 18 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.38 5 3.6 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 40 Chloride 300.0 mg/L 500 130 1,500 7,500 Sulfate 300.0 mg/L 50 12 250 1,100 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.039 Total Dissolved Solids 2540C mg/L 1 4.7 10 --- Total Suspended Solids 2540D mg/L 1 18 67 2,200 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.078 Total MetalsAluminum 200.7 ug/L 2 9.4 200 49,000 Antimony 200.8 ug/L 2 0.72 2 6.5 Arsenic 200.8 ug/L 2 1.2 4 92 Barium 200.7 ug/L 2 2.5 20 1,100 Beryllium 200.7 ug/L 2 0.71 2 7.7 Boron 200.7 ug/L 250 830 25,000 160,00Cadmium 200.8 ug/L 2 1.2 4 4 Calcium 200.7 ug/L 50 1,700 10,000 3,300,0
1 – Based on data review, data point needs to be excluded from the data set. 

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. Exc – Excluded from data set. 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 A5-7. Influent to FGD Wastewater Treatment System, Set 1 Analytical Results, Belew

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

Chromium 200.8 ug/L 2 3.3 8 100 Cobalt 200.7 ug/L 2 1.1 20 60 Copper 200.8 ug/L 2 0.96 4 80 Iron 200.7 ug/L 2 32 200 72,000 Lead 200.8 ug/L 2 0.73 2 67 Magnesium 200.7 ug/L 2 21 400 690,00Manganese 200.7 ug/L 2 0.51 20 7,200 Mercury 1631E ng/L 40,000 9,940 20,800 228,00Molybdenum 200.7 ug/L 2 1.6 40 36 Nickel 200.8 ug/L 2 0.89 4 170 Selenium 200.8 ug/L 5 1.6 10 3,400 Silver 200.8 ug/L 2 0.59 2 ND (2Sodium 200.7 ug/L 2 180 10,000 52,000 Thallium 200.8 ug/L 2 0.47 2 5.1 Tin 200.7 ug/L 2 4.8 200 6.6 Titanium 200.7 ug/L 2 1.6 20 940 Vanadium 200.8 ug/L 2 1.7 10 120 Zinc 200.7 ug/L 2 9.1 40 240 
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 A5-8. Influent to FGD Wastewater Treatment System, Set 2 Analytical Results, Belew

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

Classicals Ammonia 350.1 mg/L 1 0.055 1 0.97 Nitrate Nitrite as N 353.2 mg/L 5 0.095 0.5 21 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 7.1 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 130 Chloride 300.0 mg/L 500 130 1,500 9,20Sulfate 300.0 mg/L 100 23 500 1,10Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.07Total Dissolved Solids 2540C mg/L 1 94 200 15,00Total Suspended Solids 2540D mg/L 1 11 40 2,60Phosphorus, Total 365.1 mg/L 5 0.025 0.25 2.7 Total MetalsAluminum 200.7 ug/L 2 9.4 200 100,0Antimony 200.8 ug/L 2 0.72 2 20 Arsenic 200.8 ug/L 5 3.1 10 230 Barium 200.7 ug/L 2 2.5 20 1,20Beryllium 200.7 ug/L 2 0.71 2 13 Boron 200.7 ug/L 50 170 5,000 200,0Cadmium 200.8 ug/L 2 1.2 4 5.1 Calcium 200.7 ug/L 50 1,700 10,000 4,300,Chromium 200.8 ug/L 2 3.3 8 270 
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 A5-8. Influent to FGD Wastewater Treatment System, Set 2 Analytical Results, Belew

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

Cobalt 200.7 ug/L 2 1.1 20 84 Copper 200.8 ug/L 2 0.96 4 190 Iron 200.7 ug/L 2 32 200 80,00Lead 200.8 ug/L 2 0.73 2 200 Magnesium 200.7 ug/L 2 21 400 760,0Manganese 200.7 ug/L 2 0.51 20 7,80Mercury 1631E ng/L 10,000 2,480 5,200 299,0Molybdenum 200.7 ug/L 2 1.6 40 57 Nickel 200.8 ug/L 2 0.89 4 270 Selenium 200.8 ug/L 5 1.6 10 5,70Silver 200.8 ug/L 2 0.59 2 0.62 Sodium 200.7 ug/L 2 180 10,000 48,00Thallium 200.8 ug/L 2 0.47 2 8.3 Tin 200.7 ug/L 2 4.8 200 13 Titanium 200.7 ug/L 2 1.6 20 2,50Vanadium 200.8 ug/L 2 1.7 10 350 Zinc 200.7 ug/L 2 9.1 40 340 
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 A5-9. Influent to FGD Wastewater Treatment System, Set 3 Analytical Results, Belew

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conc

Classicals Ammonia 350.1 mg/L 1 0.055 1 2 Nitrate Nitrite as N 353.2 mg/L 2 0.038 0.2 14 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 5 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 14Chloride 300.0 mg/L 200 51 600 8,9Sulfate 300.0 mg/L 100 23 500 1,20Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 ND (Total Dissolved Solids 2540C mg/L 1 240 500 18,0Total Suspended Solids 2540D mg/L 1 11 40 3,30Phosphorus, Total 365.1 mg/L 10 0.05 0.5 5.2 Total MetalsAluminum 200.7 ug/L 50 240 5,000 150,Antimony 200.8 ug/L 2 0.72 2 33 Arsenic 200.8 ug/L 2 1.2 4 28Barium 200.7 ug/L 2 2.5 20 1,90Beryllium 200.7 ug/L 2 0.71 2 22 Boron 200.7 ug/L 50 170 5,000 200,0Cadmium 200.8 ug/L 2 1.2 4 5.7 Calcium 200.7 ug/L 50 1,700 10,000 4,600Chromium 200.8 ug/L 2 3.3 8 34Cobalt 200.7 ug/L 2 1.1 20 14
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 A5-9. Influent to FGD Wastewater Treatment System, Set 3 Analytical Results, Belew

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conc

Copper 200.8 ug/L 2 0.96 4 27Iron 200.7 ug/L 2 32 200 100,0Lead 200.8 ug/L 2 0.73 2 32Magnesium 200.7 ug/L 50 540 10,000 740,0Manganese 200.7 ug/L 50 13 500 8,20Mercury 1631E ng/L 50,000 12,100 25,200 129,0Molybdenum 200.7 ug/L 2 1.6 40 76 Nickel 200.8 ug/L 2 0.89 4 34Selenium 200.8 ug/L 50 16 100 7,40Silver 200.8 ug/L 2 0.59 2 0.7Sodium 200.7 ug/L 2 180 10,000 50,0Thallium 200.8 ug/L 2 0.47 2 8.Tin 200.7 ug/L 2 4.8 200 21 Titanium 200.7 ug/L 2 1.6 20 3,80Vanadium 200.8 ug/L 2 1.7 10 56Zinc 200.7 ug/L 2 9.1 40 1,00
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 A5-10. Influent to FGD Wastewater Treatment System, Set 4 Analytical Results, Belew

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conc

Classicals Ammonia 350.1 mg/L 1 0.055 1 1.Nitrate Nitrite as N 353.2 mg/L 2 0.038 0.2 15 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 1.Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 12Chloride 300.0 mg/L 200 51 600 8,9Sulfate 300.0 mg/L 50 12 250 1,1Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.0Total Dissolved Solids 2540C mg/L 1 240 500 17,0Total Suspended Solids 2540D mg/L 1 11 40 2,9Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.0Total MetalsAluminum 200.7 ug/L 2 9.4 200 140,Antimony 200.8 ug/L 2 0.72 2 26 Arsenic 200.8 ug/L 2 1.2 4 34Barium 200.7 ug/L 2 2.5 20 1,7Beryllium 200.7 ug/L 2 0.71 2 22 Boron 200.7 ug/L 50 170 5,000 200,Cadmium 200.8 ug/L 2 1.2 4 7.Calcium 200.7 ug/L 50 1,700 10,000 4,600Chromium 200.8 ug/L 2 3.3 8 32Cobalt 200.7 ug/L 2 1.1 20 16
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 A5-10. Influent to FGD Wastewater Treatment System, Set 4 Analytical Results, Belew

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conc

Copper 200.8 ug/L 2 0.96 4 33Iron 200.7 ug/L 2 32 200 89,0Lead 200.8 ug/L 2 0.73 2 33Magnesium 200.7 ug/L 2 21 400 630,Manganese 200.7 ug/L 2 0.51 20 6,5Mercury 1631E ng/L 10,000 2,410 5,050 131,Molybdenum 200.7 ug/L 2 1.6 40 89 Nickel 200.8 ug/L 2 0.89 4 37Selenium 200.8 ug/L 10 3.1 20 6,0Silver 200.8 ug/L 2 0.59 2 1.Sodium 200.7 ug/L 2 180 10,000 46,0Thallium 200.8 ug/L 2 0.47 2 1Tin 200.7 ug/L 2 4.8 200 20 Titanium 200.7 ug/L 2 1.6 20 4,7Vanadium 200.8 ug/L 2 1.7 10 59Zinc 200.7 ug/L 2 9.1 40 68
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 A5-11. Influent to Bioreactor System, Set 1 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Concen

Classicals Ammonia 350.1 mg/L 1 0.055 1 2.2 Nitrate Nitrite as N 353.2 mg/L 2 0.038 0.2 16 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.38 5 3.6 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 150 Chloride 300.0 mg/L 500 130 1,500 7,500 Sulfate 300.0 mg/L 50 12 250 1,200 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.042 Total Dissolved Solids 2540C mg/L 1 47 100 13,000 Total Suspended Solids 2540D mg/L 1 1.1 4 2.8 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 ND (0.0Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200Antimony 200.8 ug/L 2 0.72 2 2.3 Arsenic 200.8 ug/L 2 1.2 4 2 Barium 200.7 ug/L 2 2.5 20 430 Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 250 830 25,000 150,000 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 50 1,700 10,000 3,700,00Chromium 200.8 ug/L 2 3.3 8 ND (8) 
ND – Not detected (number in parentheses is the quantitation limit). 

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A5-11. Influent to Bioreactor System, Set 1 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Concen

Cobalt 200.7 ug/L 2 1.1 20 3 Copper 200.8 ug/L 2 0.96 4 1.2 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 21 400 710,000 Manganese 200.7 ug/L 2 0.51 20 2,700 Mercury 1631E ng/L 100 24.4 51 508 Molybdenum 200.7 ug/L 2 1.6 40 23 Nickel 200.8 ug/L 2 0.89 4 36 Selenium 200.8 ug/L 5 1.6 10 120 Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 48,000 Thallium 200.8 ug/L 2 0.47 2 3.5 Tin 200.7 ug/L 2 4.8 200 ND (200Titanium 200.7 ug/L 2 1.6 20 9.2 Vanadium 200.8 ug/L 2 1.7 10 1.7 Zinc 200.7 ug/L 2 9.1 40 9.5 
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 A5-12. Influent to Bioreactor System, Set 2 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

Classicals Ammonia 350.1 mg/L 1 0.055 1 0.92 Nitrate Nitrite as N 353.2 mg/L 2 0.038 0.2 16 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 7.1 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2Chemical Oxygen Demand 410.4 mg/L 5 20 100 190 Chloride 300.0 mg/L 500 130 1,500 8,800 Sulfate 300.0 mg/L 100 23 500 1,300 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.065 Total Dissolved Solids 2540C mg/L 1 47 100 14,00Total Suspended Solids 2540D mg/L 1 1.1 4 3.2 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.018 Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND (20Antimony 200.8 ug/L 2 0.72 2 3 Arsenic 200.8 ug/L 2 1.2 4 3.2 Barium 200.7 ug/L 2 2.5 20 380 Beryllium 200.7 ug/L 2 0.71 2 ND (2Boron 200.7 ug/L 50 170 5,000 190,00Cadmium 200.8 ug/L 2 1.2 4 2 Calcium 200.7 ug/L 50 1,700 10,000 3,800,0Chromium 200.8 ug/L 2 3.3 8 ND (8
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 A5-12. Influent to Bioreactor System, Set 2 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

Cobalt 200.7 ug/L 2 1.1 20 12 Copper 200.8 ug/L 2 0.96 4 1.2 Iron 200.7 ug/L 2 32 200 47 Lead 200.8 ug/L 2 0.73 2 ND (2Magnesium 200.7 ug/L 2 21 400 780,00Manganese 200.7 ug/L 2 0.51 20 5,600 Mercury 1631E ng/L 100 24.1 50.5 119 Molybdenum 200.7 ug/L 2 1.6 40 23 Nickel 200.8 ug/L 5 2.2 10 67 Selenium 200.8 ug/L 5 1.6 10 89 Silver 200.8 ug/L 2 0.59 2 ND (2Sodium 200.7 ug/L 2 180 10,000 49,00Thallium 200.8 ug/L 2 0.47 2 3.7 Tin 200.7 ug/L 2 4.8 200 ND (20Titanium 200.7 ug/L 2 1.6 20 12 Vanadium 200.8 ug/L 2 1.7 10 4.1 Zinc 200.7 ug/L 2 9.1 40 ND (4
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. 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 A5-13. Influent to Bioreactor System, Set 3 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

Classicals Ammonia 350.1 mg/L 1 0.055 1 3.2 Nitrate Nitrite as N 353.2 mg/L 2 0.038 0.2 12 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 5.5 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 1.8 Chemical Oxygen Demand 410.4 mg/L 5 20 100 280 Chloride 300.0 mg/L 200 51 600 8,800 Sulfate 300.0 mg/L 100 23 500 1,200 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 ND (0.Total Dissolved Solids 2540C mg/L 1 94 200 14,00Total Suspended Solids 2540D mg/L 1 1.1 4 3.2 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.045 Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND (20Antimony 200.8 ug/L 2 0.72 2 6.6 Arsenic 200.8 ug/L 2 1.2 4 2.1 Barium 200.7 ug/L 2 2.5 20 440 Beryllium 200.7 ug/L 2 0.71 2 ND (2Boron 200.7 ug/L 50 170 5,000 180,00Cadmium 200.8 ug/L 2 1.2 4 2.4 Calcium 200.7 ug/L 50 1,700 10,000 3,700,0Chromium 200.8 ug/L 2 3.3 8 ND (8
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. 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 A5-13. Influent to Bioreactor System, Set 3 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

Cobalt 200.7 ug/L 2 1.1 20 10 Copper 200.8 ug/L 2 0.96 4 1.3 Iron 200.7 ug/L 2 32 200 ND (20Lead 200.8 ug/L 2 0.73 2 ND (2Magnesium 200.7 ug/L 50 540 10,000 640,00Manganese 200.7 ug/L 2 0.51 20 2,400 Mercury 1631E ng/L 500 122 255 752 Molybdenum 200.7 ug/L 2 1.6 40 28 Nickel 200.8 ug/L 2 0.89 4 70 Selenium 200.8 ug/L 5 1.6 10 900 Silver 200.8 ug/L 2 0.59 2 ND (2Sodium 200.7 ug/L 2 180 10,000 49,00Thallium 200.8 ug/L 2 0.47 2 6 Tin 200.7 ug/L 2 4.8 200 ND (20Titanium 200.7 ug/L 2 1.6 20 15 Vanadium 200.8 ug/L 2 1.7 10 3.7 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 A5-14. Influent to Bioreactor System, Set 4 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

Classicals Ammonia 350.1 mg/L 1 0.055 1 1 Nitrate Nitrite as N 353.2 mg/L 5 0.095 0.5 14 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 2.3 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 200 Chloride 300.0 mg/L 200 51 600 8,700 Sulfate 300.0 mg/L 50 12 250 1,200 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.04 Total Dissolved Solids 2540C mg/L 1 94 200 12,000 Total Suspended Solids 2540D mg/L 1 1.1 4 1.2 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.031 Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200Antimony 200.8 ug/L 2 0.72 2 8.4 Arsenic 200.8 ug/L 2 1.2 4 2.6 Barium 200.7 ug/L 2 2.5 20 440 Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 50 170 5,000 180,000 Cadmium 200.8 ug/L 2 1.2 4 1.8 Calcium 200.7 ug/L 50 1,700 10,000 4,000,00Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 7.6 
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 A5-14. Influent to Bioreactor System, Set 4 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

Copper 200.8 ug/L 2 0.96 4 1.7 Iron 200.7 ug/L 2 32 200 36 Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 2 21 400 630,000 Manganese 200.7 ug/L 2 0.51 20 2,800 Mercury 1631E ng/L 100 24.1 50.5 117 Molybdenum 200.7 ug/L 2 1.6 40 45 Nickel 200.8 ug/L 2 0.89 4 59 Selenium 200.8 ug/L 2 0.62 4 110 Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 46,000 Thallium 200.8 ug/L 2 0.47 2 6.6 Tin 200.7 ug/L 2 4.8 200 ND (200Titanium 200.7 ug/L 2 1.6 20 17 Vanadium 200.8 ug/L 2 1.7 10 3.6 Zinc 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. 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 A5-15. Effluent from Bioreactor System, Set 1 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Concen

Classicals Ammonia 350.1 mg/L 1 0.055 1 6.3 Nitrate Nitrite as N 353.2 mg/L 1 0.019 0.1 0.061 Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.15 2 7.4 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 2.2 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 160 Chloride 300.0 mg/L 500 130 1,500 7,300 Sulfate 300.0 mg/L 50 12 250 1,300 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.036 Total Dissolved Solids 2540C mg/L 1 47 100 15,000 Total Suspended Solids 2540D mg/L 1 1.1 4 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.084 Total MetalsAluminum 200.7 ug/L 2 9.4 200 79 Antimony 200.8 ug/L 2 0.72 2 ND (2) Arsenic 200.8 ug/L 2 1.2 4 2 Barium 200.7 ug/L 2 2.5 20 450 Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 250 830 25,000 160,000 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 3,200,00Chromium 200.8 ug/L 2 3.3 8 ND (8) 
ND – Not detected (number in parentheses is the quantitation limit). 

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. 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 A5-15. Effluent from Bioreactor System, Set 1 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Concen

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 32 200 110 Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 2 21 400 740,000 Manganese 200.7 ug/L 2 0.51 20 2,400 Mercury 1631E ng/L 100 24.4 51 403 Molybdenum 200.7 ug/L 2 1.6 40 1.8 Nickel 200.8 ug/L 2 0.89 4 ND (4) Selenium 200.8 ug/L 2 0.62 4 3.9 Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 53,000 Thallium 200.8 ug/L 2 0.47 2 ND (2) Tin 200.7 ug/L 2 4.8 200 ND (200Titanium 200.7 ug/L 2 1.6 20 7.9 Vanadium 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). 

* - 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 A5-16. Effluent from Bioreactor System, Set 2 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

Classicals Ammonia 350.1 mg/L 1 0.055 1 4.7 Nitrate Nitrite as N 353.2 mg/L 1 0.019 0.1 0.15 Nitrogen, Total Kjeldahl 351.2 mg/L 2 0.15 2 10 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 2 Chemical Oxygen Demand 410.4 mg/L 5 20 100 200 Chloride 300.0 mg/L 500 130 1,500 8,400 Sulfate 300.0 mg/L 100 23 500 1,300 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.052 Total Dissolved Solids 2540C mg/L 1 47 100 13,00Total Suspended Solids 2540D mg/L 1 1.1 4 2 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.12 Total MetalsAluminum 200.7 ug/L 2 9.4 200 39 Antimony 200.8 ug/L 2 0.72 2 ND (2Arsenic 200.8 ug/L 2 1.2 4 2 Barium 200.7 ug/L 2 2.5 20 420 Beryllium 200.7 ug/L 2 0.71 2 ND (2Boron 200.7 ug/L 50 170 5,000 170,00Cadmium 200.8 ug/L 2 1.2 4 ND (4Calcium 200.7 ug/L 50 1,700 10,000 3,800,0Chromium 200.8 ug/L 2 3.3 8 ND (8
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 A5-16. Effluent from Bioreactor System, Set 2 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Conce

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 32 200 170 Lead 200.8 ug/L 2 0.73 2 ND (2Magnesium 200.7 ug/L 2 21 400 790,00Manganese 200.7 ug/L 2 0.51 20 5,200 Mercury 1631E ng/L 20 4.83 10.1 162 Molybdenum 200.7 ug/L 2 1.6 40 1.9 Nickel 200.8 ug/L 2 0.89 4 1.2 Selenium 200.8 ug/L 5 1.6 10 1.8 Silver 200.8 ug/L 2 0.59 2 ND (2Sodium 200.7 ug/L 2 180 10,000 49,00Thallium 200.8 ug/L 2 0.47 2 ND (2Tin 200.7 ug/L 2 4.8 200 ND (20Titanium 200.7 ug/L 2 1.6 20 12 Vanadium 200.8 ug/L 2 1.7 10 2.3 Zinc 200.7 ug/L 2 9.1 40 9.4 
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 A5-17. Effluent from Bioreactor System, Set 3 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Concen

Classicals Ammonia 350.1 mg/L 1 0.055 1 5 Nitrate Nitrite as N 353.2 mg/L 1 0.019 0.1 0.13 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 7.1 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 3.5 Chemical Oxygen Demand 410.4 mg/L 5 20 100 220 Chloride 300.0 mg/L 200 51 600 9,100 Sulfate 300.0 mg/L 100 23 500 1,300 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 ND (0.Total Dissolved Solids 2540C mg/L 1 94 200 11,000 Total Suspended Solids 2540D mg/L 1 1.1 4 1.6 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.074 Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND (20Antimony 200.8 ug/L 2 0.72 2 ND (2Arsenic 200.8 ug/L 2 1.2 4 2.7 Barium 200.7 ug/L 2 2.5 20 450 Beryllium 200.7 ug/L 2 0.71 2 ND (2Boron 200.7 ug/L 50 170 5,000 170,00Cadmium 200.8 ug/L 2 1.2 4 ND (4Calcium 200.7 ug/L 50 1,700 10,000 4,000,0Chromium 200.8 ug/L 2 3.3 8 ND (8Cobalt 200.7 ug/L 2 1.1 20 ND (20
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 A5-17. Effluent from Bioreactor System, Set 3 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Concen

Copper 200.8 ug/L 2 0.96 4 ND (4Iron 200.7 ug/L 2 32 200 65 Lead 200.8 ug/L 2 0.73 2 ND (2Magnesium 200.7 ug/L 50 540 10,000 710,00Manganese 200.7 ug/L 2 0.51 20 3,500 Mercury 1631E ng/L 20 4.87 10.2 24.2 Molybdenum 200.7 ug/L 2 1.6 40 2.3 Nickel 200.8 ug/L 2 0.89 4 ND (4Selenium 200.8 ug/L 5 1.6 10 32 Silver 200.8 ug/L 2 0.59 2 ND (2Sodium 200.7 ug/L 2 180 10,000 51,000 Thallium 200.8 ug/L 2 0.47 2 ND (2Tin 200.7 ug/L 2 4.8 200 ND (20Titanium 200.7 ug/L 2 1.6 20 13 Vanadium 200.8 ug/L 2 1.7 10 1.9 Zinc 200.7 ug/L 2 9.1 40 ND (40
ND – Not detected (number in parentheses is the quantitation limit). 

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

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

Table A5-18. Effluent from Bioreactor System, Set 4 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Concen

Classicals Ammonia 350.1 mg/L 1 0.055 1 3.3 Nitrate Nitrite as N 353.2 mg/L 1 0.019 0.1 0.14 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 3.6 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 190 Chloride 300.0 mg/L 200 51 600 8,300 Sulfate 300.0 mg/L 50 12 250 1,200 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.032 Total Dissolved Solids 2540C mg/L 1 94 200 14,000 Total Suspended Solids 2540D mg/L 1 1.1 4 ND (4) Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.12 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 1.6 Barium 200.7 ug/L 2 2.5 20 480 Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 50 170 5,000 170,000 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 50 1,700 10,000 4,100,00Chromium 200.8 ug/L 2 3.3 8 ND (8) 
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. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A5-18. Effluent from Bioreactor System, Set 4 Analytical Results, Belews Creek 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific 

MDL 

SampleSpecific 

QL Concen

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 32 200 150 Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 2 21 400 670,000 Manganese 200.7 ug/L 2 0.51 20 2,800 Mercury 1631E ng/L 1 0.24 0.5 2.99 Molybdenum 200.7 ug/L 2 1.6 40 2.5 Nickel 200.8 ug/L 2 0.89 4 ND (4) Selenium 200.8 ug/L 2 0.62 4 0.9 Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 47,000 Thallium 200.8 ug/L 2 0.47 2 ND (2) Tin 200.7 ug/L 2 4.8 200 ND (200Titanium 200.7 ug/L 2 1.6 20 16 Vanadium 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). 

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 A5-19. Influent to FGD Wastewater Treatment System Field Blank Analytical Results, Be

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL Conc

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 20Cadmium 200.8 ug/L 2 1.2 4 ND Calcium 200.7 ug/L 2 69 400 36Chromium 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 (Lead 200.8 ug/L 2 0.73 2 ND Magnesium 200.7 ug/L 2 21 400 4Manganese 200.7 ug/L 2 0.51 20 ND 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 ND (10Thallium 200.8 ug/L 2 0.47 2 ND Tin 200.7 ug/L 2 4.8 200 ND (Titanium 200.7 ug/L 2 1.6 20 ND 
ND – Not detected (number in parentheses is the quantitation limit). 

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 A5-19. Influent to FGD Wastewater Treatment System Field Blank Analytical Results, Be

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL Conc

Vanadium 200.8 ug/L 2 1.7 10 ND Zinc 200.7 ug/L 2 9.1 40 9.
ND – Not detected (number in parentheses is the quantitation limit). 

^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table A5-20. Influent to Bioreactor System Field Blank, Set 1 Analytical Results, Belews C

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Total MetalsAluminum 200.7 ug/L 2 9.4 200 NAntimony 200.8 ug/L 2 0.72 2 NArsenic 200.8 ug/L 2 1.2 4 NBarium 200.7 ug/L 2 2.5 20 NBeryllium 200.7 ug/L 2 0.71 2 NBoron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 NCalcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 NCobalt 200.7 ug/L 2 1.1 20 NCopper 200.8 ug/L 2 0.96 4 NIron 200.7 ug/L 2 32 200 NLead 200.8 ug/L 2 0.73 2 NMagnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 NMolybdenum 200.7 ug/L 2 1.6 40 NNickel 200.8 ug/L 2 0.89 4 NSelenium 200.8 ug/L 2 0.62 4 NSilver 200.8 ug/L 2 0.59 2 NSodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 N
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 A5-20. Influent to Bioreactor System Field Blank, Set 1 Analytical Results, Belews C

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Tin 200.7 ug/L 2 4.8 200 NTitanium 200.7 ug/L 2 1.6 20 NVanadium 200.8 ug/L 2 1.7 10 NZinc 200.7 ug/L 2 9.1 40 N
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 A5-21. Influent to Bioreactor System Field Blank, Set 2 Analytical Results, Belews C

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 NArsenic 200.8 ug/L 2 1.2 4 NBarium 200.7 ug/L 2 2.5 20 NBeryllium 200.7 ug/L 2 0.71 2 NBoron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 NCalcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 NCobalt 200.7 ug/L 2 1.1 20 NCopper 200.8 ug/L 2 0.96 4 NIron 200.7 ug/L 2 32 200 NLead 200.8 ug/L 2 0.73 2 NMagnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 NMolybdenum 200.7 ug/L 2 1.6 40 NNickel 200.8 ug/L 2 0.89 4 NSelenium 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 ND Thallium 200.8 ug/L 2 0.47 2 N
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 A5-21. Influent to Bioreactor System Field Blank, Set 2 Analytical Results, Belews C

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Tin 200.7 ug/L 2 4.8 200 NTitanium 200.7 ug/L 2 1.6 20 NVanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 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 A5-22. Influent to Bioreactor System Field Blank, Set 3 Analytical Results, Belews C

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Total MetalsAluminum 200.7 ug/L 2 9.4 200 NAntimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 NBeryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 NCopper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 NLead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 NMercury 1631E ng/L 1 0.25 0.52 NMolybdenum 200.7 ug/L 2 1.6 40 NNickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 N
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 A5-22. Influent to Bioreactor System Field Blank, Set 3 Analytical Results, Belews C

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Titanium 200.7 ug/L 2 1.6 20 NVanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 N
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 A5-23. Influent to Bioreactor System Field Blank, Set 4 Analytical Results, Belews C

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Total MetalsAluminum 200.7 ug/L 2 9.4 200 NAntimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 NBeryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 NChromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 NCopper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 NLead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 NManganese 200.7 ug/L 2 0.51 20 NMercury 1631E ng/L 1 0.24 0.5 NMolybdenum 200.7 ug/L 2 1.6 40 NNickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 N
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 A5-23. Influent to Bioreactor System Field Blank, Set 4 Analytical Results, Belews C

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Titanium 200.7 ug/L 2 1.6 20 NVanadium 200.8 ug/L 2 1.7 10 NZinc 200.7 ug/L 2 9.1 40 N
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 A5-24. Effluent from Bioreactor System Field Blank, Set 1 Analytical Results, Belews 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Total MetalsAluminum 200.7 ug/L 2 9.4 200 NAntimony 200.8 ug/L 2 0.72 2 NArsenic 200.8 ug/L 2 1.2 4 NBarium 200.7 ug/L 2 2.5 20 NBeryllium 200.7 ug/L 2 0.71 2 NBoron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 NCalcium 200.7 ug/L 2 69 400 NChromium 200.8 ug/L 2 3.3 8 NCobalt 200.7 ug/L 2 1.1 20 NCopper 200.8 ug/L 2 0.96 4 NIron 200.7 ug/L 2 32 200 NLead 200.8 ug/L 2 0.73 2 NMagnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 NMolybdenum 200.7 ug/L 2 1.6 40 NNickel 200.8 ug/L 2 0.89 4 NSelenium 200.8 ug/L 2 0.62 4 NSilver 200.8 ug/L 2 0.59 2 NSodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 N
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 A5-24. Effluent from Bioreactor System Field Blank, Set 1 Analytical Results, Belews 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Tin 200.7 ug/L 2 4.8 200 NTitanium 200.7 ug/L 2 1.6 20 NVanadium 200.8 ug/L 2 1.7 10 NZinc 200.7 ug/L 2 9.1 40 N
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 A5-25. Effluent from Bioreactor System Field Blank, Set 2 Analytical Results, Belews 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Total MetalsAluminum 200.7 ug/L 2 9.4 200 NAntimony 200.8 ug/L 2 0.72 2 NArsenic 200.8 ug/L 2 1.2 4 NBarium 200.7 ug/L 2 2.5 20 NBeryllium 200.7 ug/L 2 0.71 2 NBoron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 NCalcium 200.7 ug/L 2 69 400 NChromium 200.8 ug/L 2 3.3 8 NCobalt 200.7 ug/L 2 1.1 20 NCopper 200.8 ug/L 2 0.96 4 NIron 200.7 ug/L 2 32 200 NLead 200.8 ug/L 2 0.73 2 NMagnesium 200.7 ug/L 2 21 400 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 1 0.24 0.5 NMolybdenum 200.7 ug/L 2 1.6 40 NNickel 200.8 ug/L 2 0.89 4 NSelenium 200.8 ug/L 2 0.62 4 NSilver 200.8 ug/L 2 0.59 2 NSodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 N
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 A5-25. Effluent from Bioreactor System Field Blank, Set 2 Analytical Results, Belews 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Tin 200.7 ug/L 2 4.8 200 NTitanium 200.7 ug/L 2 1.6 20 NVanadium 200.8 ug/L 2 1.7 10 NZinc 200.7 ug/L 2 9.1 40 N
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 A5-26. Effluent from Bioreactor System Field Blank, Set 3 Analytical Results, Belews 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Total MetalsAluminum 200.7 ug/L 2 9.4 200 NAntimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 NBeryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 NChromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 NCopper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 NLead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 NManganese 200.7 ug/L 2 0.51 20 NMercury 1631E ng/L 1 0.24 0.5 Molybdenum 200.7 ug/L 2 1.6 40 NNickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 N
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 A5-26. Effluent from Bioreactor System Field Blank, Set 3 Analytical Results, Belews 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Titanium 200.7 ug/L 2 1.6 20 NVanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 N
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 A5-27. Effluent from Bioreactor System Field Blank, Set 4 Analytical Results, Belews 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Total MetalsAluminum 200.7 ug/L 2 9.4 200 NAntimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 NBeryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 2 6.7 200 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 2 69 400 NChromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 NCopper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 NLead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 2 21 400 NManganese 200.7 ug/L 2 0.51 20 NMercury 1631E ng/L 1 0.24 0.5 NMolybdenum 200.7 ug/L 2 1.6 40 NNickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 N
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 A5-27. Effluent from Bioreactor System Field Blank, Set 4 Analytical Results, Belews 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample-Specific QL C

Titanium 200.7 ug/L 2 1.6 20 NVanadium 200.8 ug/L 2 1.7 10 NZinc 200.7 ug/L 2 9.1 40 N
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 2)

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 20 samples (excluding laboratory prep blanks) FGS extracted 

and analyzed for total mercury. 

Table 1. Long-Term Monitoring Month 1 (Part 2) Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

71991 1010066-05 Aqueous FGD Influent, Set 1 10/6/2010

71995 1010066-06 Aqueous FGD Bioreactor Influent, Set 1 10/6/2010

71999 1010066-07 Aqueous FGD Bioreactor Effluent, Set 1 10/6/2010

72003 1010066-10 Aqueous FGD Influent Field Blank 10/6/2010

72004 1010066-08 Aqueous FGD Bioreactor Influent Field Blank, Set 1 10/6/2010

72008 1010066-09 Aqueous FGD Bioreactor Effluent Field Blank, Set 1 10/6/2010

72141 1010048-01 Aqueous FGD Influent, Set 1 10/5/2010

72145 1010048-02 Aqueous FGD Bioreactor Influent, Set 1 10/4/2010

72149 1010048-03 Aqueous FGD Bioreactor Effluent, Set 1 10/4/2010

72153 1010048-06 Aqueous FGD Influent Field Blank 10/5/2010

72154 1010048-04 Aqueous FGD Bioreactor Influent Field Blank, Set 1 10/4/2010

72158 1010048-05 Aqueous FGD Bioreactor Effluent Field Blank, Set 1 10/4/2010

72241 1010066-01 Aqueous FGD Influent, Set 1 10/7/2010

72245 1010066-02 Aqueous FGD Effluent, Set 1 10/7/2010

72249 1010066-04 Aqueous FGD Influent Field Blank 10/7/2010

72250 1010066-03 Aqueous FGD Effluent Field Blank, Set 1 10/6/2010

72291 1010046-01 Aqueous FGD Influent Set 1 10/5/2010 

72295 1010046-05 Aqueous FGD Effluent, Set 1 10/5/2010

72299 1010046-07 Aqueous FGD Influent Field Blank 10/5/2010
2

Table 1. Long-Term Monitoring Month 1 (Part 2) Mercury – Sample Identification 

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72300 1010046-06 Aqueous FGD Effluent, Field Blank, Set 1 10/4/2010

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. 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. One sample was 

analyzed in duplicate at the laboratory, sample 71999. The relative percent difference 

(RPD) for sample 71999 was 1.31%. 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. 
3

MATRIX SPIKE AND MATIX SPIKE DUPLICATES 

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

71995 and 71999. MS/MSD were also performed on samples 72199 and 72195 in the

same preparatory batch but discussed in a previous narrative. All aqueous MS/MSD 

recoveries were within method specifications of 71-125%. All RPDs met methodspecified 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 1 (Part 2)

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 2) Total Metals – Sample 

Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71991 FGD Influent, Set 1 280-8121-1 Aqueous 10/6/2010 10/7/2010

71995 FGD Bioreactor Influent, Set 1 280-8194-1 Aqueous 10/7/2010 10/8/2010

71999 FGD Bioreactor Effluent, Set 1 280-8194-2 Aqueous 10/7/2010 10/8/2010

72003 FGD Influent Field Blank 280-8121-2 Aqueous 10/6/2010 10/7/2010

72004 FGD Bioreactor Influent Field 

Blank, Set 1 

280-8194-3 Aqueous 10/7/2010 10/8/2010

72008 FGD Bioreactor Effluent Field 

Blank, Set 1 

280-8194-4 Aqueous 10/7/2010 10/8/2010

72141 FGD Influent, Set 1 280-8061-1 Aqueous 10/5/2010 10/6/2010

72145 FGD Bioreactor Influent, Set 1 280-8061-2 Aqueous 10/5/2010 10/6/2010

72149 FGD Bioreactor Effluent, Set 1 280-8061-3 Aqueous 10/5/2010 10/6/2010

72154 FGD Bioreactor Influent Field 

Blank, Set 1 

280-8061-4 Aqueous 10/5/2010 10/6/2010

72153 FGD Influent Field Blank 280-8061-6 Aqueous 10/5/2010 10/6/2010

72158 FGD Bioreactor Effluent Field 

Blank, Set 1 

280-8061-5 Aqueous 10/5/2010 10/6/2010

72241 FGD Influent, Set 1 280-8195-1 Aqueous 10/7/2010 10/8/2010

72245 FGD Effluent, Set 1 280-8195-2 Aqueous 10/7/2010 10/8/2010

72249 FGD Bioreactor Influent Field 

Blank, Set 1 

280-8195-4 Aqueous 10/7/2010 10/8/2010
2

Table 1. Long-Term Monitoring Month 1 (Part 2) Total Metals – Sample 

Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72250 FGD Effluent Field Blank, Set 1 280-8195-3 Aqueous 10/7/2010 10/8/2010

72291 FGD Influent, Set 1 280-8058-1 Aqueous 10/5/2010 10/6/2010

72295 FGD Effluent, Set 1 280-8058-2 Aqueous 10/5/2010 10/6/2010

72300 FGD Effluent Field Blank, Set 1 280-8058-3 Aqueous 10/5/2010 10/6/2010

72299 FGD Influent Field Blank, Set 1 280-8058-4 Aqueous 10/5/2010 10/6/2010

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

TestAmerica’s control limits of 85–115%: arsenic, antimony, 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. 
3

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 sample 72149 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/MSD) 

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

72149 and 72241. All MS/MSD spike recoveries were within the method control criteria 

of 70-130% for all analytes. The relative percent difference (RPD) for all MS/MSDs were 

within the FGD ICP/MS SOP ±20% control limits for both samples. No additional data 

qualifiers were required. 

POST DIGESTION SPIKES (PDS) 

The PDS performed on sample 72149 passed TestAmerica’s control limits of 85–115% 

recovery for all analytes, except for arsenic, antimony, and vanadium, which were 

flagged with a “W”. No additional data qualifiers were required for PDS samples. 
4

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 2)

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 2) Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

71991 FGD Influent, Set 1 280-8121-1 Aqueous 10/6/2010 10/7/2010

71995 FGD Bioreactor Influent, Set 1 280-8194-1 Aqueous 10/7/2010 10/8/2010

71999 FGD Bioreactor Effluent, Set 1 280-8194-2 Aqueous 10/7/2010 10/8/2010

72003 FGD Influent Field Blank 280-8121-2 Aqueous 10/6/2010 10/7/2010

72004 FGD Bioreactor Influent Field 

Blank, Set 1 

280-8194-3 Aqueous 10/7/2010 10/8/2010

72008 FGD Bioreactor Effluent Field 

Blank, Set 1 

280-8194-4 Aqueous 10/7/2010 10/8/2010

72141 FGD Influent, Set 1 280-8061-1 Aqueous 10/5/2010 10/6/2010

72145 FGD Bioreactor Influent, Set 1 280-8061-2 Aqueous 10/5/2010 10/6/2010

72149 FGD Bioreactor Effluent, Set 1 280-8061-3 Aqueous 10/5/2010 10/6/2010

72153 FGD Influent Field Blank 280-8061-6 Aqueous 10/5/2010 10/6/2010

72154 FGD Bioreactor Influent Field 

Blank, Set 1 

280-8061-4 Aqueous 10/5/2010 10/6/2010

72158 FGD Bioreactor Effluent Field 

Blank, Set 1 

280-8061-5 Aqueous 10/5/2010 10/6/2010

72241 FGD Influent, Set 1 280-8195-1 Aqueous 10/7/2010 10/8/2010

72245 FGD Effluent, Set 1 280-8195-2 Aqueous 10/7/2010 10/8/2010

72249 FGD Bioreactor Influent Field 

Blank, Set 1 

280-8195-4 Aqueous 10/7/2010 10/8/2010
2

Table 1. Long-Term Monitoring Month 1 (Part 2) Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72250 FGD Effluent Field Blank, Set 1 280-8195-3 Aqueous 10/7/2010 10/8/2010

72291 FGD Influent, Set 1 280-8058-1 Aqueous 10/5/2010 10/6/2010

72295 FGD Effluent, Set 1 280-8058-2 Aqueous 10/5/2010 10/6/2010

72299 FGD Influent Field Blank, Set 1 280-8058-4 Aqueous 10/5/2010 10/6/2010

72300 FGD Effluent Field Blank, Set 1 280-8058-3 Aqueous 10/5/2010 10/6/2010

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. 

• The serial dilution for cobalt, iron, molybdenum, sodium, and titanium for sample 

72241 failed TestAmerica’s SOP control limit of percent differences less than 

10%. 

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

beryllium, cobalt, iron, manganese, molybdenum, sodium, tin, titanium, and zinc 

for sample 72149 failed the method spike recovery limits of 70-130%. 

• The MS/MSD recoveries for barium and tin for sample 72241 failed the method 

spike recovery limits of 70-130%. The MS recovery for cobalt for sample 72241 

also failed the method spike recovery limits. 

• The post digestion spike (PDS) for barium and sodium for sample 72149 failed 

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

• The PDS for cobalt and tin for sample 72241 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. 
3

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, except for cobalt, 

iron, molybdenum, sodium, and titanium for Sample 72241. 

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 72149 and 72241. 
4

The MS/MSD of sample 72149 failed the method spike recovery limits of 70-130% for 

all elements except aluminum. Boron, calcium and magnesium had high concentrations 

and 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. 

The MS/MSD recoveries of sample 72241 failed the method spike recovery limits of 70-

130% for all elements except beryllium, molybdenum, and titanium, as well as the MSD 

recovery for cobalt. Aluminum, boron, calcium, iron, magnesium, manganese, sodium 

and zinc had high concentrations and 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. 

All RPDs of the MS/MSDs were within ± 20%. No additional data qualifiers were 

needed. 

POST DIGESTION SPIKE (PDS) 

The PDS performed on sample 72149 failed the method criteria of 85–115% for barium 

and sodium, which were qualified with a “W”. The PDS performed on sample 72241 

failed the method criteria of 85–115% recovery for cobalt and tin, which were 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: 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 1 (Part 2) 

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 ten samples analyzed by TestAmerica for the above analytes. 

Table 1. Long-Term Monitoring Month 1 (Part 2) Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72291 Water FGD Influent, Set 1 10/05/10 

72295 Water FGD Effluent, Set 1 10/05/10 

72141 Water FGD Influent, Set 1 10/05/10 

72145 Water FGD Bioreactor Influent, Set 1 10/05/10 

72149 Water FGD Bioreactor Effluent, Set 1 10/05/10 

71991 Water FGD Influent, Set 1 10/06/10 

71995 Water FGD Bioreactor Influent, Set 1 10/07/10 

71999 Water FGD Bioreactor Effluent, Set 1 10/07/10 

72241 Water FGD Influent, Set 1 10/07/10 
2 

Table 1. Long-Term Monitoring Month 1 (Part 2) Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72245 Water FGD Effluent, Set 1 10/07/10 

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. 

 

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) analysis was run on sample 72149 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 

MS and matrix spike duplicates (MSD) were performed on samples 71999 and 72149. 

The percent recoveries for the MS and MSD for both of these samples were within the 

method criteria; however the MS and MSD results for sample 71999 were above the 

calibration range. Only one set of MS/MSD are required per the method; therefore, the 

results from sample 72149 meet the requirements. No further action is required. 
3 

BOD5 

The traffic reports for the following samples did not indicate the receipt temperature for 

the following samples: 72291, 72295, 72141, 71995, 71999, 72241, and 72245. The 

sample receipt checklist provided by TestAmerica did note that the receipt temperatures 

were appropriate; however, this cannot be verified. 40 CFR 136 Table II requires that all 

samples must be stored and shipped at temperatures no greater than 6°C. 

TestAmerica analyzed five dilutions; the dilutions had dissolved oxygen (DO) depletion 

greater than 2.0 mg/L for samples 72291, 71999, and 72241. As required in the method, 

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

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

The seed correction factor was lower than 0.6 mg/L, at 0.531 mg/L for one of the batches. 

The samples were flagged with an “s” indicating the seed correction blank (SCB) 

recovery was low. This low seed correction factor suggests that the sample results may be 

biased low. 

Chloride and Sulfate 

MS and MSD were performed on samples 71999 and 72149. All chloride and sulfate MS 

and MSD recoveries for these samples met the method criteria; however, for sample 

71999, the MS/MSD results for sulfate exceeded the calibration range and for sample 

72149, the MS/MSD results for chloride exceeded the calibration range. These MS/MSD 

results were qualified as estimated values. No further action is required. 

COD 

MS and MSD were performed on samples 71999 and 72149. The percent recoveries for 

the MS and MSD for samples 72149 were within the method control criteria. The percent 

recoveries for the MS and MSD for sample 71999 were 25% and 44%, respectively, 

which are outside the method control criteria of 90-110% and therefore, the MS/MSD 

results were flagged with “F” qualifiers. The LCS/LCSD results were acceptable for this 

sample indicating the analytical system was operating within control. 

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. 

MS and MSD were performed on samples 71999 and 72149. The percent recoveries for 

the MS and MSD for samples 71999 were both 88%, which is outside the method control 

criteria of 90-110% and therefore, the MS and MSD results were flagged with an “F” 

qualifier. The percent recoveries for the MS and MSD for sample 72149 were 89% and 
4 

88%, respectively, which are outside the method control criteria and therefore, the MS 

and MSD results were flagged with “F” qualifiers. The LCS/LCSD results were 

acceptable for these samples indicating 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. 

Nitrate/Nitrite 

No issues were identified by the data reviewer.

Phosphorus 

MS and MSD were performed on samples 71999 and 72149. The percent recoveries for 

the MS and MSD for sample 71999 were within the method control criteria. The percent 

recoveries for the MS and MSD for sample 72149 were 77% and 79%, respectively, 

which are outside the method control criteria, but did meet the laboratory control criteria 

and therefore, were not flagged by the laboratory. The LCS/LCSD recoveries for this 

batch were acceptable and indicate that the analytical system was operating within 

control. 

TDS 

The method blank associated with one of the batches detected TDS at a level greater than 

the MDL, but less than the RL. All affected samples were flagged with a “B” qualifier, 

which includes samples 72141, 72145, 72149, 72291, and 72295. 

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. 

TA reports that constant weight was not achieved after 3 drying cycles for the following 

samples: 71991, 72241, and 72245. Review of the general chemistry worksheets 

indicates that constant weight was achieved for all three samples. No further action was 

necessary. 

The result for sample 71991 was two orders of magnitude lower than the concentrations 

for similar samples in this episode; therefore, TestAmerica reviewed the analyses and 

determined that the sample should have been run with a dilution factor of 10 or 20, but 

was run with a dilution of one. The laboratory has no way of confirming how the 

analysis was run and the issue was identified after the hold time had expired; therefore, 

this result is unreliable and should be excluded from the data set. 
5 

TKN 

Method blank results associated with one of the batches were greater than the MDL, but 

less than the RL. The blank results were flagged with a “J” qualifier. All associated 

samples were flagged with a “B” qualifier. No additional corrective action is necessary. 

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. 

Table 2. Data Review Summary Table 

Sample Analyte Qualifier/Action Reason 

Level 

Detected 

72291 BOD s SCB recovery low XXX mg/L 

71991 TDS EXCLUDE Dilution factor cannot be 

confirmed 

510 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: XXX

mg/L 

Dup: XXX 

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: XXX

mg/L 

Dup: XXX 

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