Appendix G

Allegheny Energy’s Hatfield’s Ferry Power 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 Allegheny Energy Supply Co, LLC’s Hatfield’s 

Ferry Power Station to aid in collecting, packaging, and shipping samples for this 

sampling program. 

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

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

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

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

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

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

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

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

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

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

Equipment Needed

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

samples to the laboratories: 

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

according to EPA Method 1669); 

• Automatic compositor; 

• Powder-free gloves; 

• Tyvek® coveralls or suitable alternative; 

• Dust masks (for use while collecting mercury samples) 

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

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

• Coolers; 

• Garbage bags; 

• Packing material; 

• Strapping tape; and 

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

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

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

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

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

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

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

transferred to the FGD wastewater treatment system prior to any commingling 

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

be collected from the sample tap located on the pipe that transfers the secondary 

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

secondary hydroclone overflow from Unit 1 for one of the sample sets, secondary 

hydroclone overflow from Unit 2 for one of the sample sets, and secondary 

hydroclone overflow from Unit 3 for two of the sample sets. 

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

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

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

sample tap that is located on the pipe downstream of the effluent storage tank at a 

point where a sample can be collected regardless of whether the effluent is being 

discharged or recirculated. 

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 
Figure 1. Hatfield’s Ferry FGD Wastewater Treatment System Monitoring Program Samplin

FGD Scrubber Purge 

Lime

Reaction Tank 1

SP-1.1

Indicates a Sampling Point

Gravity 

Filter

Clarifier 1

Sludge 

Storage 

Tank

Filter Press

Sump

Gravity 

Filter

Solids to Onsite Landfill

Wastewater Flow

Sludge Flow

Intermittent Wastewater Flow

Clarifier 

Sludge

Clarifier 2

Gravity Filter 

Backwash

Reaction 

Tank 2

Ferric Chloride

Treated 

Wastewater

Storage

Tank

Equalization 

Tank

Effluent 

Recycle

Wastewater 

from Sump

SP-2

Effluent 

Recycle

Polymer

Hydrochloric 

Acid

Organosulfide

Secondary

Hydroclone 

for Unit 1

Secondary

Hydroclone 

for Unit 2

Secondary

Hydroclone 

for Unit 3

Hydroclone 

overflow

Hydroclone 

overflow

Hydroclone 

overflow

SP-1.2

SP-1.3
Sample Bottles and Preservation

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

cyanide. 

Table 2. Summary of Sample Container and Planned Preservation 

Parameter 

Sample Container 

and Volume On-Site Preservation 

BOD5 One 1-L HDPE 

bottle 

≤6°C 

Group I a One 1-L HDPE 

bottle 

≤6°C 

Group II b Two 1-L HDPE 

bottles 

H2SO4 to pH <2, ≤6°C 

Total cyanide One 1-L HDPE 

bottle 

Dilution until sulfide is not detected, 

NaAsO2 until total chlorine is not 

present, NaOH to pH >10, ≤6°C 

Total metals (EPA Method 200.8 with 

collision cell) 

One 500-mL HDPE 

bottle 

None 

(acid preserve at laboratory) 

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

bottle 

None 

(acid preserve at laboratory) 

Total mercury: 

Laboratory composite grab samples at FGD 

wastewater treatment effluent 

Four 125-mL glass 

bottles 

Influent samples and field blank samples Two 250-mL glass 

bottles 

None 

(acid preserve at laboratory) 

(a) Group I includes TSS, TDS, sulfate, and chloride. 

(b) Group II includes ammonia as nitrogen, COD, nitrate/nitrite as nitrogen, TKN, and total phosphorus. 

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

the four sets of samples. 
Sample Labeling

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

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

following information: 

• Sample number (see Table 3); 

• Sampling episode number (see Table 3); 

• Sampling point/description (see Table 3); 

• Date of sample collection; 

• Analysis to be performed; 

• Sample bottle type; and 

• Required on-site preservation. 

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

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

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

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

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

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

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

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

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

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

analysis: 

• BOD; 

• Group I; 

• Group II; 

• Total Cyanide; 

• Total Metals – 200.8 w/ CC; 

• Total Metals – 200.7; 

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

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

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

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

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

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

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

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

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

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

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

Program 

 

Sampling Point Description Sample Number Sampling Episode Number 

FGD Wastewater Treatment Influent – Set 1 72291 6571 

FGD Wastewater Treatment Influent – Set 2 72292 6571 

FGD Wastewater Treatment Influent – Set 3 72293 6571 

FGD Wastewater Treatment Influent – Set 4 72294 6571 

FGD Wastewater Treatment Effluent – Set 1 72295 6571 

FGD Wastewater Treatment Effluent – Set 2 72296 6571 

FGD Wastewater Treatment Effluent – Set 3 72297 6571 

FGD Wastewater Treatment Effluent – Set 4 72298 6571 

FGD Wastewater Treatment Influent Field Blank 72299 6571 

FGD Wastewater Treatment Effluent Field Blank – Set 1 72300 6571 

FGD Wastewater Treatment Effluent Field Blank – Set 2 72301 6571 

FGD Wastewater Treatment Effluent Field Blank – Set 3 72302 6571 

FGD Wastewater Treatment Effluent Field Blank – Set 4 72303 6571 

QC Samples

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

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

Table 4. Field Blank Collection Frequency 

Sampling Point Total Mercury 

Total Metals (200.8 

and 200.7) Classicals1 

FGD Wastewater 

Treatment Influent 

Collected during one 

of the four sets 

Collected during one 

of the four sets 

No field blanks 

required 

FGD Wastewater 

Treatment Effluent 

Collected during all 

four sets 

Collected during all 

four sets 

No field blanks 

required 

1

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

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

analyses; however, no additional sample volume is required. 

Sample Collection

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

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

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

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

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

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

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

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

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

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

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

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

mercury grab samples. 

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

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

in the sampling plan drafted for the EPA sampling episode to collect the field blank 

samples, set up the composite containers, and perform the composite pump-off procedures 

for the FGD wastewater treatment effluent sampling point. The following instructions can 

be used to collect the grab samples at the influent to the FGD wastewater treatment system 

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

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

collect these samples or if the FGD wastewater treatment effluent sampling point has 

intermittent flows which may interfere with the automatic composite collection, please 

contact TJ Finseth, (703) 633-1698 to discuss possible alternatives.) 

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

the sample collection. 

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

gloves. 

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

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

open the bag completely. 

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

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

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

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

collection. 

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

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

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

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

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

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

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

outer bags and dirty hands closes the outer bag. 

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

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

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

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

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

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

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

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

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

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

composite samples. 

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

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

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

plastic bag shrouding and collect directly from the tap. 

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

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

Bottle and Preservation” section of these instruction for the preservation 

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

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

Sample Packing and Shipment

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

laboratories. 

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

specifies the sample point. 

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

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

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

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

paper towel. 

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

into an ice chest with wet ice to cool. 

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

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

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

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

freezer bag. 

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

ship samples to the laboratories. 

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

garbage bags to keep the samples cold. 

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

coolers with additional cushioning material. Sufficient packing material 

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

shipment. 

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

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

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

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

the following address: 

 Eastern Research Group 

 14555 Avion Parkway, Suite 200 

 Chantilly, VA 20151 

 Attn: TJ Finseth 

 (703) 633-1698 

12. Close the cooler(s). 

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

classicals and metals samples should be shipped to TestAmerica as 

follows: 

 TestAmerica 

 4955 Yarrow Street 

 Arvada, CO 80002 

 Attn: Elizabeth Eichelberger 

 (303) 736-0100 

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

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

released or damaged. 

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

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

by tying, or with a twist-tie. 

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

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

containers will not shift during shipment. 

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

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

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

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

provided in step 11: 

19. Close the cooler. 

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

mercury samples should be shipped to Frontier as follows:

 Frontier GeoSciences 

 414 Pontius Ave. North 

 Seattle, WA 98109 

 Attn: Patrick Garcia-Strickland 

 (206) 957-1428 

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

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

released or damaged. 

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

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

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

the coolers to the laboratories. 

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

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

shipped to the laboratories. 

Traffic Reports

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

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

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

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

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

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

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

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

of the traffic report. 
Engineering Data

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

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

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

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

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

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

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

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

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

Certification Statement 

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

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

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

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

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

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Sample Collection 

Time Temperature (°C)

pH

(S.U.)

Set 1Set 2Set 3Set 4

Plant Name

Sample 

Collection 

Number

Unit Overflow 

Sampled at 

Influent 

(7 or 8)

Influent Samples 

Collected as Grabs

(Yes or No)

Mercury and Cyanide 

Samples Collected as 

Grabs

(Yes or No)

Effluent Samples 

Collected as 24-

Hour Composites

(Yes or No)

Tyvek Suits 

used

(Yes or No)

Dust Masks 

Used for 

Mercury 

(Yes or No)

Clean Hands/Dirty 

Hands Sampling 

Techniques Used

(Yes or No)

Description of Sample 

Collection Technique (if 

different than 

instructions)

Description of Abnormal 

Conditions in FGD System 

or FGD Wastewater 

Treatment System that May 

Impact Concentrations

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

Units Operating 

During Sampling 

Day

Units Off-line 

Entire 

Sampling Day

SCRs/SNCRs 

Operating on 

Units

Set 1Set 2Set 3Set 4

Flow Rate (gpm) Duration

Set 1Set 2Set 3Set 4

Lime Usage 

(tons)

Ferric Chloride 

Usage 

(Liters/day)

Organosulfide Usage 

(Liters/day)

Polymer Usage 

(Liters/day)

Acid Usage 

(Liters/day)

Chemical 

Precipitation 

System Effluent Flow Rate (gpd)

Set 1Set 2Set 3Set 4

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Plant Operation During Sample Collection

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Plant Operation During Sample Collection

Scrubber Slurry Blowdown Flow 

Rate Scrubber Slurry 

Percent Solids

Percent Hydroclone 

Overflow Recycled 

Back to Scrubber

FGD Wastewater Treatment Operation During Sample Collection

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Scrubber Purge 

Flow Rate During 

Influent Sample 

Collection

(gpm)
Unit 1 Unit 2 Unit 3

Daily Power Generation (MW-hrs)

Plant Name Date

Provide the daily power generation for each scrubbed unit starting two weeks prior to the first set 

of samples through the last set of samples
FGD Wastewater Treatment System Flow 

Rates

(gpd)

Plant Name Date Chemical Precipitation Effluent

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

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

Authority

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

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

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

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

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

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

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

he may reasonably require." 

Confidentiality

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

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

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

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

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

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

procedures, set forth in Subpart B. 

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

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

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

without further notice to you. 

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

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

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

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

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

satisfy the criteria for confidentiality. 

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

Notice of Intent to Transfer Confidential Information to Selected EPA Contractors

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

selected EPA contractors. 

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

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

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

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

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

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

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

development of these regulations are listed below: 

EPA Office 

Receiving 

Support 

Contractor Name EPA Contract 

No. Type of Support 

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

Office of Water/ 

Office of 

Science & 

Technology/ 

Engineering & 

Analysis 

Division 

Westat EP-C-10-023 Statistical analysis 

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

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

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

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

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

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

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

Ronald Jordan 

USEPA Headquarters 

Ariel Rios Building 

1200 Pennsylvania Ave., N.W. 

Mail Code: 4303T 

Washington, DC 20460 

jordan.ronald@epa.gov 
Enclosure 4 

Certification Statement 

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

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

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

representative. 

Certification Statement 

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

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

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

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

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

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

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

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

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

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

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

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

in Section 308 of the Clean Water Act.

 

Signature of Certifying Official Date 

( ) 

Printed Name of Certifying Official Telephone Number of Certifying Official 

Title of Certifying Official 

Company Name 

 
Section 2

On-Site Audit Memorandum
MEMORANDUM 

TO: Ron Jordan, EPA 

Jezebele Alicea, EPA 

FROM: Jessica Gray, ERG 

 

DATE: 17 November 2010 

SUBJECT: Notes from On-Site Review of Industry Self-Monitoring Sampling at 

Allegheny Energy’s Hatfield’s Ferry Steam Electric Plant on November 9-10, 

2010 

 ERG conducted an on-site review of the self-monitoring sampling conducted at the 

Allegheny Energy’s Hatfield’s Ferry Steam Electric Plant (Hatfield’s Ferry) located in 

Masontown, PA. ERG was on site for all sample collection activities that Hatfield’s Ferry 

conducted for the second set of the industry self-monitoring sampling on November 9 and 10, 

2010. These notes summarize the sample collection techniques used by Hatfield’s Ferry at each 

of the sampling points and EPA’s observations/findings from the on-site review. A process flow 

diagram of the FGD wastewater treatment system at Hatfield’s Ferry is provided as Attachment 

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

Pictures from the on-site review are provided as Attachment 3. 

 During this set of the industry self-monitoring, Unit 2 started up on Monday, November 

8, 2010. All of the units operated throughout the self-monitoring sampling. 

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

the observations/findings from each sampling point. 

FGD Wastewater Treatment Influent (SP-1) 

 The FGD wastewater treatment influent consists of the secondary hydrocyclone overflow 

that is transferred to the equalization tank at the beginning of the FGD wastewater treatment 

system; therefore, the samples from this sampling point were collected as grab samples. For this 

sampling point, Hatfield’s Ferry personnel collected the secondary hydrocyclone overflow from 

Unit 1 because each unit’s secondary hydrocyclone overflow is transferred to the FGD 

wastewater treatment system separately. Hatfield’s Ferry samplers sampled Unit 3’s secondary 

hydrocyclone overflow for Set 1. Hatfield’s Ferry personnel collected the samples from a 

stainless steel sample tap located approximately one foot off the ground, which flows by gravity. 

Hatfield’s Ferry personnel connected a length of silicone tubing to the sample tap and dropped it 

through a hole in the secondary hydrocyclone to the floor below for sample collection. This is 

the same sampling point that EPA intends to use during its sample collection. 
Memorandum 

November 15, 2010 

Page 2 

Sample Collection 

 To collect the samples of the FGD wastewater treatment influent, Hatfield’s Ferry 

personnel followed EPA Method 1669 protocols and the EPA-provided instructions. Hatfield’s 

Ferry personnel attached one end of the specially-cleaned silicone tubing to the sample tap. A 

picture of the silicone tubing attached to the sample tap is included as Figure 1 in Attachment 3. 

The samplers then zip-tied a clean plastic bag to the other end of the silicone tubing before 

lowering it through the floor and weaving it through a ladder, as shown in Figure 2 in 

Attachment 3. After positioning the silicone tubing between the legs of the ladder, the samplers 

replaced the plastic bag with a clean shroud. The samplers let the sample flow from the tap for 

four minutes prior to collecting any samples. The samplers then collected the samples underneath 

the shroud. At this sampling point, Hatfield’s Ferry collected multi-fill split samples for the 

mercury and metals samples and duplicate samples for the BOD, Group I, and Group II. 

However, for the cyanide samples, the samplers only collected samples for EPA analyses. All 

samples were filled while the samplers held the bottles under the shrouding. 

Preservation 

 Hatfield’s Ferry personnel followed all method specifications when preserving the 

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

to be below 2 S.U. The cyanide sample was checked for sulfides and chlorine using lead acetate 

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

chlorine in the samples. The cyanide sample was 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 

 Hatfield’s Ferry personnel used a pH probe and a thermometer to measure the pH and 

temperature of the FGD wastewater influent samples. Hatfield’s Ferry personnel filled a small 

bottle with sample after collecting the classical samples and inserted the thermometer and pH 

probe into the sample bottle. Hatfield’s Ferry personnel stated that they calibrated the pH probe 

on Tuesday, November 9, 2010; however, ERG did not observe the calibration of the probe. 

Hatfield’s Ferry personnel allowed the temperature and pH to stabilize and then recorded the 

values. 

Observations/Findings 

 ERG observed the Hatfield’s Ferry personnel collecting the Set 2 samples of the FGD 

wastewater treatment influent stream. Hatfield’s Ferry did not collect the field blanks during the 

sample collection activities because they were collected during Set 1. Hatfield’s Ferry personnel 

followed all applicable procedures during the sample collection. The field pH measurement was 

made within 5 minutes of sample collection, but the temperature was measured 10 minutes after 

sample collection because the thermometer was left at the staging area. Hatfield’s Ferry 
Memorandum 

November 15, 2010 

Page 3 

personnel used the correct techniques to preserve the classical samples; however, the Group II 

and cyanide samples were not preserved within 15 minutes. The Group II samples were 

preserved in 1 hour and 21 minutes, while the cyanide sample was preserved in 43 minutes. 

FGD Wastewater Treatment Effluent (SP-2) 

 The FGD wastewater treatment effluent stream is the effluent from a chemical 

precipitation system used to treat the Hatfield’s Ferry FGD wastewater; therefore, the samples 

for this sampling point were collected as composite samples, except for the mercury and cyanide 

samples. For this sampling point, Hatfield’s Ferry collected the samples using the plant’s 

existing compliance monitoring point. Hatfield’s Ferry installed a 2-way splitter using stainless 

steel tubing; one of the taps was used to collect the composite samples, while the other was used 

to collect the mercury and cyanide samples. A picture of the sample taps is included as Figure 3 

in Attachment 3. 

Sample Collection 

 To collect the samples of the FGD wastewater treatment effluent stream, Hatfield’s Ferry 

personnel followed EPA Method 1669 protocols and the EPA-provided instructions. To collect 

the composite samples, Hatfield’s Ferry 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. Hatfield’s Ferry 

personnel attached one long end of the silicone tubing to one of the sample taps and the other 

long end was directed to a nearby drain. Hatfield’s Ferry personnel removed the ISCO pump 

cover and laid the short end of the sample tubing into the pump and attached the end of the 

tubing to a vented cap on a 20-liter carboy. A picture of the sampling configuration is included as 

Figure 4 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 pumped the sample into 

the individual sample bottles. Hatfield’s Ferry personnel used a short piece of Teflon® tubing 

connected to a length of silicone tubing and the pump to transfer the samples to individual 

sample bottles. The samplers first shook the 20-liter container to homogenize the 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 0.5 liters of sample. A picture of the 

pump-off set up is included as Figure 5 in Attachment 3. Hatfield’s Ferry personnel collected all 

of the samples using a cleanbox and the multi-fill approach for all of the samples. 

 Hatfield’s Ferry personnel also collected grab samples for mercury every six hours during 

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

one of their effluent sample taps with a clean plastic bag and letting sample flow through the 

sample tap for two minutes prior to collecting any samples. Hatfield’s Ferry personnel filled the 

mercury bottles directly from the tap, underneath the shroud. The samplers collected the mercury 

samples as multi-fill splits. Hatfield’s Ferry personnel also collected the cyanide samples as a 

multi-fill split immediately after the first of the four mercury grab samples at the sampling point. 

A picture of the mercury grab sample collection is included as Figure 6 in Attachment 3. 
Memorandum 

November 15, 2010 

Page 4 

Preservation 

 Hatfield’s Ferry personnel followed all method specifications when preserving the 

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

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

during the sample collection time period. 

Field Measurements 

 Hatfield’s Ferry personnel used a pH probe and a thermometer to measure the pH and 

temperature of the FGD wastewater effluent samples, which are the same as those described in 

the Field Measurements section for the FGD wastewater influent stream. Hatfield’s Ferry 

personnel filled a small bottle with sample after each mercury grab was collected, which was 

every six hours. Hatfield’s Ferry samplers also collected a small bottle at the end of transferring 

samples from the carboy to individual sample bottles.

Observations/Findings 

 ERG observed the Hatfield’s Ferry personnel collecting the composite set up, composite 

breakdown, and composite pump off for the Set 2 samples. Hatfield’s Ferry personnel collected 

field blank samples for the total metals samples during this set. ERG also observed the Grab 1 

and 2 mercury grab samples and the cyanide grab sample. Hatfield’s Ferry personnel collected 

the mercury field blank sample during the Grab 1 sample. 

 Hatfield’s Ferry personnel attached the T-splitter tubing to the sample tap and began the 

sample purge prior to pumping blank water through the sample tubing and into the field blank 

carboy. ERG communicated this issue to the samplers and determined that the samplers should 

collect the field blank by pouring the blank water into the 10-liter carboy. Therefore, the field 

blank does not include a blank on the T-splitter tubing or vented cap. Hatfield’s Ferry personnel 

followed the remainder of the applicable procedures during the sample collection and 

preservation. 

 ERG noted that at the end of the composite sample collection the 20-liter carboy only 

contained 11 L. ERG noted that the flow of the FGD wastewater treatment effluent stream, 

measured with an in-line flow meter, varied from approximately 80 gpd to 300 gpd, which might 

have contributed to the composite volume. Because of the limited volume, Hatfield’s Ferry 

samplers purged only 0.5 L prior to sample collection. The samplers also only filled the bottles to 

the shoulder rather than to the neck. 

 For Grab 2, the field temperature measurement was not made because the samplers 

thought the probe was reading temperature; however, other samplers indicated that the probe 

read 25°C because it adjusts the pH reading to standard temperature. Hatfield’s Ferry personnel 

used the correct techniques to preserve the classical samples; however, the Group II samples 

were not preserved within 15 minutes. The Group II samples were preserved in 28 minutes. 
Attachment 1 

Overall Process Water Diagram 

Attachment 2 

Checklists 














Attachment 3 

Pictures from the On-Site Review 
Figure 1. FGD Wastewater Influent (SP-1) Sample Tap with Extension 
Figure 2. FGD Wastewater Influent (SP-1) Sample Tap Extension Configuration 
Figure 3. FGD Wastewater Effluent (SP-2) Sample Taps 
Figure 4. FGD Wastewater Effluent (SP-2) Composite Sample Configuration 
Figure 5. FGD Wastewater Effluent (SP-2) Pump-Off Configuration 
Figure 6. FGD Wastewater Effluent (SP-2) Mercury Grab Configuration 
Section 3

Signed Certification Statement

Section 4

Engineering Data
Table G4-1. Field Measurements for Sample Collection at the Influent to FGD Wastewater Treatment System, H

Episode Number 

Sample Collection 

Number 

Date of Sample 

Collection 

Sample Collection 

Time 

Temperature 

(°C) 

6571 Set 1 - Grab 1 10/5/2010 1358 39.6 6571 Set 2 - Grab 1 11/10/2010 0925 42 6571 Set 3 - Grab 1 1/12/2011 0820 47 6571 Set 4 - Grab 1 2/9/2011 0753 48 
Table G4-2. Field Measurements for Sample Collection at the Effluent from FGD Wastewater Treatment System

Episode Number 

Sample Collection 

Number 

Date of Sample 

Collection 

Sample Collection 

Time 

Temperature 

(°C) 

6571 Set 1 - Grab 1 10/4/2010 1722 25 6571 Set 1 - Grab 2 10/4/2010 2320 26 6571 Set 1 - Grab 3 10/5/2010 0522 25 6571 Set 1 - Grab 4 10/5/2010 1116 24 6571 Set 2 - Grab 1 11/9/2010 1211 25 6571 Set 2 - Grab 2 11/9/2010 1815 25 6571 Set 2 - Grab 3 11/10/2010 0015 24 6571 Set 2 - Grab 4 11/10/2010 0615 27 6571 Set 3 - Grab 1 1/11/2011 1200 28 6571 Set 3 - Grab 2 1/11/2011 1800 30 6571 Set 3 - Grab 3 1/12/2011 0002 25 6571 Set 3 - Grab 4 1/12/2011 0600 29 6571 Set 4 - Grab 1 2/8/2011 1207 28.0 6571 Set 4 - Grab 2 2/8/2011 1800 28.5 6571 Set 4 - Grab 3 2/9/2011 0005 27.5 6571 Set 4 - Grab 4 2/9/2011 0602 27.0 
Table G4-3. Sample Collection Procedures Used during the Sampling Episode 

Episode 

Number 

Sample 

Collection 

Number 

Unit 

Overflow 

Sampled 

at 

Influent 

Influent 

Samples 

Collected as 

Grabs 

(Yes or No) 

Mercury 

and Cyanide 

Samples 

Collected as 

Grabs 

(Yes or No) 

Effluent Samples 

Collected as 24-

Hour Composites 

(Yes or No) 

Clean 

Hands/Dirty 

Hands Sampling 

Techniques Used

(Yes or No)* 

Description of 

Sample 

Collection 

Technique (if 

different than 

instructions) 

6571 Set 1 3 Yes Yes Yes Yes None 6571 Set 2 2 Yes Yes Yes Yes None 6571 Set 3 3 Yes Yes Yes Yes None 6571 Set 4 1 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 G4-4. Generating Unit Operation at Time of Sampling, Hatfield’s Ferry 

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 

6571 Set 1 10/5/2010 Unit 3 Units 1,2 6571 Set 2 11/10/2010 Units 1,2,3 None 6571 Set 3 1/12/2010 Units 1,2,3 None 6571 Set 4 2/9/2010 Units 1,2,3 None 
Table G4-5. FGD Scrubber Slurry Information at Time of Sampling, Hatfield’s Ferry 

Episode 

Number 

Sample 

Collection 

Number 

Date of Sample 

Collection 

Plant Operation During Sample Collection 

Scrubber Slurry Blowdown 

Flow Rate 

Scrubber 

Slurry 

Percent 

Solids 

Percen

Hydrocl

Overflow Re

Back to Scr

Flow Rate 

(gpm) Duration 

6571 Set 1 10/5/2010 1,400 18 hr. 40min 21% 70% 6571 Set 2 11/10/2010 1,400 15 hr. 5min 21% 70% 6571 Set 3 1/12/2011 1,550 13 hr. 40min 21% 70% 6571 Set 4 2/9/2011 1,550 12 hr. 40min 21% 70% 
Table G4-6. FGD Wastewater Treatment System Operation Information, Hatfield’s Ferry 

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

6571 Set 1 10/5/2010 100 2.4 43 11 15 6571 Set 2 11/10/2010 100 4 73 18 25 6571 Set 3 1/12/2010 110 3.2 58 14 20 6571 Set 4 2/9/2010 110 2.4 43 11 15 
Table G4-7. Daily Power Generation During Sampling Period, Hatfield’s Ferry 

Episode Number Date 

Daily Power Generation 

(MW-hrs) 

Unit 1 Unit 2 Unit 3 

6571 9/20/2010 7,972 Planned Outage 11,384 

6571 9/21/2010 11,672 0 10,934 

6571 9/22/2010 10,338 0 10,917 

6571 9/23/2010 11,152 0 10,942 

6571 9/24/2010 11,247 0 11,096 

6571 9/25/2010 8,294 0 587 

6571 9/26/2010 7,323 0 Planned Outage 

6571 9/27/2010 7,284 0 0 

6571 9/28/2010 1,035 0 0 

6571 9/29/2010 Boiler leak 0 0 

6571 9/30/2010 0 0 0 

6571 10/1/2010 0 0 0 

6571 10/2/2010 0 0 Reserve SD 

6571 10/3/2010 0 0 3,670 

6571 10/4/2010 Reserve SD 0 10,712 

6571 10/5/2010 0 0 8,277 

6571 10/6/2010 0 0 328 

6571 10/7/2010 0 0 Reserve SD 

6571 10/8/2010 0 0 0 

6571 10/9/2010 0 0 

Cooling tower 

work 

6571 10/10/2010 0 0 0 

6571 10/11/2010 0 0 0 

6571 10/12/2010 109 0 0 

6571 10/13/2010 9,182 0 0 

6571 10/14/2010 12,004 0 0 

6571 10/15/2010 11,152 0 0 

6571 10/16/2010 10,795 0 0 

6571 10/17/2010 9,222 0 0 

6571 10/18/2010 11,389 0 0 

6571 10/19/2010 11,448 Reserve SD 0 

6571 10/20/2010 11,819 0 0 

6571 10/21/2010 10,891 0 Reserve SD 

6571 10/22/2010 11,383 0 0 

6571 10/23/2010 7,485 0 0 

6571 10/24/2010 7,058 0 0 

6571 10/25/2010 13,033 4,014 0 

6571 10/26/2010 12,046 6,116 0 

6571 10/27/2010 7,010 Boiler leak 0 

6571 10/28/2010 10,325 11 0 

6571 10/29/2010 12,248 9,742 0 
Table G4-7. Daily Power Generation During Sampling Period, Hatfield’s Ferry 

Episode Number Date 

Daily Power Generation 

(MW-hrs) 

Unit 1 Unit 2 Unit 3 

6571 10/30/2010 6,642 10,550 0 

6571 10/31/2010 6,416 9,471 0 

6571 11/1/2010 8,640 8,731 0 

6571 11/2/2010 7,053 7,134 0 

6571 11/3/2010 9,370 239 0 

6571 11/4/2010 256 Tube leak 0 

6571 11/5/2010 9,202 Reserve SD 0 

6571 11/6/2010 8,152 0 0 

6571 11/7/2010 9,328 0 0 

6571 11/8/2010 12,611 1,704 9,018 

6571 11/9/2010 11,663 9,760 12,330 

6571 11/10/2010 13,473 13,202 13,018 

6571 11/11/2010 13,712 719 12,626 

6571 11/12/2010 11,524 Reserve SD 11,605 

6571 11/13/2010 8,856 0 12,218 

6571 11/14/2010 8,393 0 9,969 

6571 11/15/2010 12,646 0 12,818 

6571 11/16/2010 12,155 0 12,385 

6571 11/17/2010 12,418 0 12,511 

6571 11/18/2010 11,333 0 9,239 

6571 11/19/2010 12,469 9,533 11,325 

6571 11/20/2010 8,952 12,302 13,004 

6571 11/21/2010 8,472 11,596 12,009 

6571 11/22/2010 12,149 12,050 12,782 

6571 11/23/2010 12,626 11,113 12,674 

6571 11/24/2010 12,749 11,190 12,794 

6571 11/25/2010 9,015 11,509 10,840 

6571 11/26/2010 8,877 11,580 10,711 

6571 11/27/2010 12,905 13,251 8,719 

6571 11/28/2010 12,472 12,175 8,269 

6571 11/29/2010 13,283 13,316 10,500 

6571 11/30/2010 12,565 12,504 12,275 

6571 12/1/2010 10,228 9,767 10,189 

6571 12/2/2010 6,453 6,601 6,246 

6571 12/3/2010 7,255 7,971 6,034 

6571 12/4/2010 9,798 11,392 8,811 

6571 12/5/2010 12,572 12,637 11,547 

6571 12/6/2010 13,049 13,004 11,920 

6571 12/7/2010 12,655 12,624 12,970 

6571 12/8/2010 11,110 11,083 12,795 

6571 12/9/2010 12,963 10,962 11,064 

6571 12/10/2010 11,873 9,011 9,140 

6571 12/11/2010 12,606 8,530 6,104 
Table G4-7. Daily Power Generation During Sampling Period, Hatfield’s Ferry 

Episode Number Date 

Daily Power Generation 

(MW-hrs) 

Unit 1 Unit 2 Unit 3 

6571 12/12/2010 11,006 8,812 12,247 

6571 12/13/2010 13,260 9,080 13,152 

6571 12/14/2010 13,913 9,475 13,318 

6571 12/15/2010 13,906 10,392 9,650 

6571 12/16/2010 14,225 12,135 Boiler Leak 

6571 12/17/2010 12,457 12,969 0 

6571 12/18/2010 11,023 12,431 4,910 

6571 12/19/2010 11,060 752 13,622 

6571 12/20/2010 9,862 Boiler leak 11,803 

6571 12/21/2010 12,021 3 12,868 

6571 12/22/2010 11,984 12,219 13,023 

6571 12/23/2010 12,636 13,202 12,744 

6571 12/24/2010 12,582 12,637 12,511 

6571 12/25/2010 12,842 13,091 12,130 

6571 12/26/2010 12,327 12,551 11,605 

6571 12/27/2010 11,775 13,373 13,062 

6571 12/28/2010 9,250 13,278 13,223 

6571 12/29/2010 9,007 13,070 13,061 

6571 12/30/2010 7,064 13,411 12,933 

6571 12/31/2010 3,078 12,427 12,537 

6571 1/1/2011 2,602 12,135 12,785 

6571 1/2/2011 10,879 11,014 11,231 

6571 1/3/2011 11,796 12,056 11,805 

6571 1/4/2011 13,057 13,137 12,369 

6571 1/5/2011 12,695 12,802 12,247 

6571 1/6/2011 12,519 12,579 12,141 

6571 1/7/2011 12,059 12,034 12,159 

6571 1/8/2011 11,785 11,259 12,364 

6571 1/9/2011 10,982 10,891 11,993 

6571 1/10/2011 12,857 13,054 12,841 

6571 1/11/2011 11,997 12,014 12,618 

6571 1/12/2011 11,772 11,846 12,541 

6571 1/13/2011 12,324 12,587 12,613 

6571 1/14/2011 12,281 12,542 12,662 

6571 1/15/2011 12,100 12,172 12,519 
Table G4-8. FGD Wastewater Treatment System Flow Rate during Sampling Period, 

Hatfield’s Ferry 

Episode Number Date 

FGD Wastewater Treatment System Flow Rates 

(gpd) 

Chemical Precipitation Effluent 

6571 9/20/2010 126,602 

6571 9/21/2010 140,602 

6571 9/22/2010 171,676 

6571 9/23/2010 164,426 

6571 9/24/2010 65,727 

6571 9/25/2010 45,844 

6571 9/26/2010 83,836 

6571 9/27/2010 99,320 

6571 9/28/2010 205,520 

6571 9/29/2010 217,367 

6571 9/30/2010 201,461 

6571 10/1/2010 173,957 

6571 10/2/2010 103,438 

6571 10/3/2010 96,594 

6571 10/4/2010 127,875 

6571 10/5/2010 133,992 

6571 10/6/2010 167,746 

6571 10/7/2010 197,328 

6571 10/8/2010 54,031 

6571 10/9/2010 196,215 

6571 10/10/2010 6,848 

6571 10/11/2010 0 

6571 10/12/2010 96,488 

6571 10/13/2010 50,531 

6571 10/14/2010 240,637 

6571 10/15/2010 216,750 

6571 10/16/2010 133,316 

6571 10/17/2010 95,676 

6571 10/18/2010 148,621 

6571 10/19/2010 179,035 

6571 10/20/2010 126,520 

6571 10/21/2010 135,145 

6571 10/22/2010 131,047 

6571 10/23/2010 193,563 

6571 10/24/2010 195,957 

6571 10/25/2010 181,652 

6571 10/26/2010 177,973 

6571 10/27/2010 242,359 

6571 10/28/2010 134,156 
Table G4-8. FGD Wastewater Treatment System Flow Rate during Sampling Period, 

Hatfield’s Ferry 

Episode Number Date 

FGD Wastewater Treatment System Flow Rates 

(gpd) 

Chemical Precipitation Effluent 

6571 10/29/2010 0 

6571 10/30/2010 0 

6571 10/31/2010 117,586 

6571 11/1/2010 181,367 

6571 11/2/2010 93,313 

6571 11/3/2010 0 

6571 11/4/2010 145,984 

6571 11/5/2010 238,906 

6571 11/6/2010 206,215 

6571 11/7/2010 226,906 

6571 11/8/2010 232,527 

6571 11/9/2010 225,211 

6571 11/10/2010 203,586 

6571 11/11/2010 173,809 

6571 11/12/2010 146,289 

6571 11/13/2010 251,695 

6571 11/14/2010 163,293 

6571 11/15/2010 188,172 

6571 11/16/2010 215,582 

6571 11/17/2010 116,953 

6571 11/18/2010 78,590 

6571 11/19/2010 61,324 

6571 11/20/2010 57,004 

6571 11/21/2010 58,449 

6571 11/22/2010 108,637 

6571 11/23/2010 70,801 

6571 11/24/2010 113,621 

6571 11/25/2010 77,125 

6571 11/26/2010 142,316 

6571 11/27/2010 84,094 

6571 11/28/2010 67,000 

6571 11/29/2010 66,395 

6571 11/30/2010 117,898 

6571 12/1/2010 73,832 

6571 12/2/2010 35,219 

6571 12/3/2010 0 

6571 12/4/2010 0 

6571 12/5/2010 0 

6571 12/6/2010 67,500 

6571 12/7/2010 172,805 

6571 12/8/2010 170,133 
Table G4-8. FGD Wastewater Treatment System Flow Rate during Sampling Period, 

Hatfield’s Ferry 

Episode Number Date 

FGD Wastewater Treatment System Flow Rates 

(gpd) 

Chemical Precipitation Effluent 

6571 12/9/2010 172,137 

6571 12/10/2010 153,051 

6571 12/11/2010 151,719 

6571 12/12/2010 143,434 

6571 12/13/2010 135,898 

6571 12/14/2010 111,852 

6571 12/15/2010 147,684 

6571 12/16/2010 232,668 

6571 12/17/2010 267,129 

6571 12/18/2010 233,770 

6571 12/19/2010 205,418 

6571 12/20/2010 184,977 

6571 12/21/2010 155,539 

6571 12/22/2010 160,887 

6571 12/23/2010 145,066 

6571 12/24/2010 135,531 

6571 12/25/2010 191,164 

6571 12/26/2010 181,969 

6571 12/27/2010 168,523 

6571 12/28/2010 172,375 

6571 12/29/2010 153,531 

6571 12/30/2010 170,773 

6571 12/31/2010 171,008 

6571 1/1/2011 192,441 

6571 1/2/2011 177,988 

6571 1/3/2011 128,516 

6571 1/4/2011 120,516 

6571 1/5/2011 163,141 

6571 1/6/2011 171,945 

6571 1/7/2011 161,641 

6571 1/8/2011 176,395 

6571 1/9/2011 176,324 

6571 1/10/2011 158,527 

6571 1/11/2011 176,523 

6571 1/12/2011 165,828 

6571 1/13/2011 151,469 

6571 1/14/2011 128,469 
Section 5

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

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

presented in Tables G5-6 through G5-18 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. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. s – Seed correction blank recovery low. 

Table G5-1. Influent to FGD Wastewater Treatment System, Hatfield’s Ferry 

Analyte Units Method 

Influent to FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 

ClassicalsAmmonia mg/L 350.1 1.20 1.50 1.00 Est 1.90 Nitrate Nitrite as N mg/L 353.2 120 120 150 Est 100 Nitrogen, Total Kjeldahl mg/L 351.2 28.0 B 47.0 47.0 Est 130 Biochemical Oxygen Demand mg/L 5210B NQ (2.50) s NQ (2.50) 45.0 70.0 Chemical Oxygen Demand mg/L 410.4 230 140 490 Est 500 Chloride mg/L 300.0 5,000 4,700 8,400 7,50Sulfate mg/L 300.0 8,700 6,500 7,700 11,00Cyanide, Total mg/L 4500 CN E ND (0.100) 0.360 2.70 0.48Total Dissolved Solids mg/L 2540C 34,000 B 23,000 28,000 31,00Total Suspended Solids mg/L 2540D 38,000 50,000 54,000 33,00Phosphorus, Total mg/L 365.1 NQ (0.0500) 0.700 B 2.60 B, Est NQ (0.0Total MetalsAluminum ug/L 200.7 580,000 B,^ 470,000 1,100,000 B 630,0Antimony ug/L 200.8 18.0 20.0 8.60 29.0 Arsenic ug/L 200.8 550 300 630 1,00Barium ug/L 200.7 460 3,000 830 1,30Beryllium ug/L 200.7 34.0 16.0 56.0 34.0 Boron ug/L 200.7 280,000 160,000 B 320,000 B 290,0
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

presented in Tables G5-6 through G5-18 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. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. s – Seed correction blank recovery low. 

Table G5-1. Influent to FGD Wastewater Treatment System, Hatfield’s Ferry 

Analyte Units Method 

Influent to FGD Wastewater Treatment System 

Set 1 Set 2 Set 3 

Cadmium ug/L 200.8 340 290 540 490 Calcium ug/L 200.7 4,000,000 4,200,000 5,300,000 B 3,400,0Chromium ug/L 200.8 1,500 1,300 ^ 3,100 3,20Cobalt ug/L 200.7 330 250 800 550 Copper ug/L 200.8 680 540 1,400 1,10Iron ug/L 200.7 710,000 540,000 1,400,000 1,300,0Lead ug/L 200.8 250 240 130 650 Magnesium ug/L 200.7 4,400,000 3,600,000 5,400,000 B 5,400,0Manganese ug/L 200.7 66,000 39,000 100,000 B 140,0Mercury ng/L 1631E 247,000 184,000 413,000 289,0Molybdenum ug/L 200.7 530 230 760 620 Nickel ug/L 200.8 2,100 1,400 2,200 2,20Selenium ug/L 200.8 1,400 1,100 510 1,20Silver ug/L 200.8 NQ (2.00) NQ (2.00) 5.50 4.70 Sodium ug/L 200.7 490,000 350,000 430,000 B 360,0Thallium ug/L 200.8 43.0 24.0 100 70.0 Tin ug/L 200.7 NQ (200) NQ (200) NQ (500) NQ (5Titanium ug/L 200.7 9,900 6,700 22,000 9,90Vanadium ug/L 200.8 1,300 1,100 2,500 3,30Zinc ug/L 200.7 9,300 6,100 21,000 16,00
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

presented in Tables G5-6 through G5-18 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. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. s – Seed correction blank recovery low. 

Table G5-2. Effluent from FGD Wastewater Treatment System, Hatfield’s Ferry 

Analyte Units Method 

Effluent from FGD Wastewater Treatment Syst

Set 1 Set 2 Set 3 

ClassicalsAmmonia mg/L 350.1 NQ (1.00) NQ (1.00) NQ (1.00) 1Nitrate Nitrite as N mg/L 353.2 130 86.0 150 Est 8Nitrogen, Total Kjeldahl mg/L 351.2 25.0 B 5.40 16.0 Est 2Biochemical Oxygen Demand mg/L 5210B ND (2.00) NQ (2.50) 4.00 3Chemical Oxygen Demand mg/L 410.4 250 130 460 Est 3Chloride mg/L 300.0 6,300 2,900 8,100 8,Sulfate mg/L 300.0 5,200 3,800 4,700 4,Cyanide, Total mg/L 4500 CN E ND (0.100) NQ (0.100) F 0.270 0.Total Dissolved Solids mg/L 2540C 20,000 B 10,000 19,000 18Total Suspended Solids mg/L 2540D 4.40 NQ (4.00) NQ (4.00) NQ Phosphorus, Total mg/L 365.1 NQ (0.0500) NQ (0.0500) B 0.0700 B,F, Est 0.0Total MetalsAluminum ug/L 200.7 480 B ND (200) ^ ND (200) ND Antimony ug/L 200.8 5.70 3.90 12.0 1Arsenic ug/L 200.8 NQ (4.00) NQ (4.00) 11.0 1Barium ug/L 200.7 110 88.0 170 2Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND Boron ug/L 200.7 160,000 80,000 B,4 240,000 B 220Cadmium ug/L 200.8 ND (4.00) NQ (4.00) NQ (4.00) 1
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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 G5-6 through G5-18 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. ^ - ICV, CCV, ICB, CCB, ISA, ISB, CRI, or MRL standard: Instrument related QC exceeds the control limits. B – Analyte was found in the blank and sample. Est – Estimated value. s – Seed correction blank recovery low. 

Table G5-2. Effluent from FGD Wastewater Treatment System, Hatfield’s Ferry 

Analyte Units Method 

Effluent from FGD Wastewater Treatment Syst

Set 1 Set 2 Set 3 

Calcium ug/L 200.7 1,400,000 1,000,000 4 1,500,000 B 1,60Chromium ug/L 200.8 14.0 18.0 ^ ND (8.00) ND Cobalt ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND Copper ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ Iron ug/L 200.7 NQ (200) NQ (200) NQ (200) 2Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND Magnesium ug/L 200.7 3,100,000 1,600,000 4 3,100,000 B 3,20Manganese ug/L 200.7 800 NQ (20.0) 9,600 B 11Mercury ng/L 1631E 978 228 77.5 8Molybdenum ug/L 200.7 350 100 450 5Nickel ug/L 200.8 7.80 NQ (4.00) 6.50 5Selenium ug/L 200.8 750 610 4 880 5Silver ug/L 200.8 ND (2.00) ND (2.00) F ND (2.00) ND Sodium ug/L 200.7 690,000 300,000 4 410,000 B 520Thallium ug/L 200.8 7.00 2.90 11.0 1Tin ug/L 200.7 ND (200) ND (200) ND (200) ND Titanium ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND Vanadium ug/L 200.8 21.0 10.0 31.0 2Zinc ug/L 200.7 ND (40.0) NQ (40.0) ND (40.0) ND 
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

Table G5-3. Classical Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment Sy

Ferry 

Analyte Unit Method

Influent to FGD 

Wastewater Treatment 

System (SP-1) 4-Set Average 

Effluen

Wastewa

Syst4-Se

ClassicalsAmmonia mg/L 350.1 1.40 < Nitrate Nitrite as N mg/L 353.2 123 Nitrogen, Total Kjeldahl mg/L 351.2 63.0 Biochemical Oxygen Demand mg/L 5210B < 29.4 < Chemical Oxygen Demand mg/L 410.4 340 Chloride mg/L 300.0 6,400 Sulfate mg/L 300.0 8,480 Cyanide, Total mg/L 4500 CN E < 0.898 < Total Dissolved Solids mg/L 2540C 29,000 1Total Suspended Solids mg/L 2540D 43,800 < Phosphorus, Total mg/L 365.1 < 0.838 < 
< - 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 G5-6 through G5-18 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 G5-4. Metals Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment 

Hatfield’s Ferry 

Analyte Unit Method

Influent to FGD Wastewater 

Treatment System (SP-1) 

4-Set Average 

Effluent from FGD W

Treatment System 

4-Set Avera

Total MetalsAluminum ug/L 200.7 695,000 < 195 Antimony ug/L 200.8 18.9 8.65 Arsenic ug/L 200.8 620 < 6.25 Barium ug/L 200.7 1,400 147 Beryllium ug/L 200.7 35.0 ND (2.00) Boron ug/L 200.7 263,000 175,000 Cadmium ug/L 200.8 415 < 4.75 Calcium ug/L 200.7 4,230,000 1,380,000 Chromium ug/L 200.8 2,280 < 10.0 Cobalt ug/L 200.7 483 ND (20.0) Copper ug/L 200.8 930 NQ (4.00) Iron ug/L 200.7 988,000 < 140 Lead ug/L 200.8 318 ND (2.00) Magnesium ug/L 200.7 4,700,000 2,750,000 Manganese ug/L 200.7 86,300 < 5,350 Mercury ng/L 1631E 283,000 342 Molybdenum ug/L 200.7 535 373 Nickel ug/L 200.8 1,980 < 5.45 Selenium ug/L 200.8 1,050 705 Silver ug/L 200.8 < 3.05 ND (2.00) 
< - Average result includes at least one value measured below the quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the qu

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

presented in Tables G5-6 through G5-18 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 G5-4. Metals Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment 

Hatfield’s Ferry 

Analyte Unit Method

Influent to FGD Wastewater 

Treatment System (SP-1) 

4-Set Average 

Effluent from FGD W

Treatment System 

4-Set Avera

Sodium ug/L 200.7 408,000 480,000 Thallium ug/L 200.8 59.3 9.48 Tin ug/L 200.7 NQ (350) ND (200) Titanium ug/L 200.7 12,100 ND (20.0) Vanadium ug/L 200.8 2,050 21.5 Zinc ug/L 200.7 13,100 NQ (40.0) 
Table G5-5. Field Blank Analytical Results, Hatfield’s Ferry 

Analyte Sample Point Method Unit Concentration 

Total Metals 

Mercury 

Influent to FGD Wastewater 

Treatment System Field Blank - 

Set 1 1631E ng/L 0.650 
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. s – Seed correction blank recovery low. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table G5-6. Influent to FGD Wastewater Treatment System, Set 1 Analytical Results, Hatfiel

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Classicals Ammonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.38 5 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 500 120 2,500 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 160 330 Total Suspended Solids 2540D mg/L 1 140 500 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 10 6.1 20 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 250 830 25,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 Chromium 200.8 ug/L 2 3.3 8 
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. s – Seed correction blank recovery low. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table G5-6. Influent to FGD Wastewater Treatment System, Set 1 Analytical Results, Hatfiel

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 50 13 500 Mercury 1631E ng/L 10,000 2,410 5,050 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 10 3.1 20 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 
^ - 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. 

Table G5-7. Influent to FGD Wastewater Treatment System, Set 2 Analytical Results, Hatfiel

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL C

Classicals Ammonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 200 46 1,000 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 470 1,000 Total Suspended Solids 2540D mg/L 1 140 500 Phosphorus, Total 365.1 mg/L 5 0.025 0.25 Total MetalsAluminum 200.7 ug/L 50 240 5,000 4Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 5 3.1 10 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 4Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 
^ - 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. 

Table G5-7. Influent to FGD Wastewater Treatment System, Set 2 Analytical Results, Hatfiel

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL C

Iron 200.7 ug/L 50 800 5,000 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 3Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 40,000 9,940 20,800 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 5 1.6 10 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 
B – Analyte was found in the blank and sample. 

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

Table G5-8. Influent to FGD Wastewater Treatment System, Set 3 Analytical Results, Hatfield

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Classicals Ammonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 50 0.95 5 Nitrogen, Total Kjeldahl 351.2 mg/L 10 0.77 10 Biochemical Oxygen Demand 5210B mg/L 1 2.8 24 Chemical Oxygen Demand 410.4 mg/L 5 20 100 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 200 46 1,000 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 160 330 Total Suspended Solids 2540D mg/L 1 140 500 Phosphorus, Total 365.1 mg/L 5 0.025 0.25 Total MetalsAluminum 200.7 ug/L 50 240 5,000 1,Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 50 62 500 Beryllium 200.7 ug/L 5 1.8 5 Boron 200.7 ug/L 50 170 5,000 3Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 5,Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 50 29 500 Copper 200.8 ug/L 2 0.96 4 
B – Analyte was found in the blank and sample. 

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

Table G5-8. Influent to FGD Wastewater Treatment System, Set 3 Analytical Results, Hatfield

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Iron 200.7 ug/L 50 800 5,000 1,Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 5,Manganese 200.7 ug/L 50 13 500 1Mercury 1631E ng/L 20,000 4,970 10,400 4Molybdenum 200.7 ug/L 5 4 100 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 50 4,600 250,000 4Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 5 12 500 Titanium 200.7 ug/L 50 41 500 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 50 230 1,000 
B – Analyte was found in the blank and sample. 

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

Table G5-9. Influent to FGD Wastewater Treatment System, Set 4 Analytical Results, Hatfiel

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL C

Classicals Ammonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 Nitrogen, Total Kjeldahl 351.2 mg/L 10 3.8 50 Biochemical Oxygen Demand 5210B mg/L 1 2.8 24 Chemical Oxygen Demand 410.4 mg/L 5 20 100 5Chloride 300.0 mg/L 500 130 1,500 7Sulfate 300.0 mg/L 500 120 2,500 11Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0Total Dissolved Solids 2540C mg/L 1 240 500 31Total Suspended Solids 2540D mg/L 1 280 1,000 33Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.Total MetalsAluminum 200.7 ug/L 5 24 500 63Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 1Barium 200.7 ug/L 5 6.2 50 1Beryllium 200.7 ug/L 5 1.8 5 Boron 200.7 ug/L 50 170 5,000 29Cadmium 200.8 ug/L 2 1.2 4 4Calcium 200.7 ug/L 50 1,700 10,000 3,40Chromium 200.8 ug/L 2 3.3 8 3Cobalt 200.7 ug/L 5 2.9 50 5Copper 200.8 ug/L 2 0.96 4 1
B – Analyte was found in the blank and sample. 

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

Table G5-9. Influent to FGD Wastewater Treatment System, Set 4 Analytical Results, Hatfiel

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL C

Iron 200.7 ug/L 5 80 500 1,30Lead 200.8 ug/L 2 0.73 2 6Magnesium 200.7 ug/L 50 540 10,000 5,40Manganese 200.7 ug/L 50 13 500 14Mercury 1631E ng/L 400,000 96,500 202,000 28Molybdenum 200.7 ug/L 5 4 100 6Nickel 200.8 ug/L 2 0.89 4 2Selenium 200.8 ug/L 2 0.62 4 1Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 5 460 25,000 36Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 5 12 500 Titanium 200.7 ug/L 5 4.1 50 9Vanadium 200.8 ug/L 2 1.7 10 3Zinc 200.7 ug/L 5 23 100 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 G5-10. Effluent from FGD Wastewater Treatment System, Set 1 Analytical Results, Hatfi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL C

Classicals Ammonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 Biochemical Oxygen Demand 5210B mg/L 1 0.24 2 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 500 130 1,500 Sulfate 300.0 mg/L 500 120 2,500 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 NTotal Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 250 830 25,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 1Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 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 G5-10. Effluent from FGD Wastewater Treatment System, Set 1 Analytical Results, Hatfi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL C

Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 3Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 200 48.3 101 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 NTitanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 
ND – Not detected (number in parentheses is the quantitation limit). 

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

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

Table G5-11. Effluent from FGD Wastewater Treatment System, Set 2 Analytical Results, Hatfi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Classicals Ammonia 350.1 mg/L 1 0.055 1 Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 2 8.1 40 Chloride 300.0 mg/L 200 51 600 Sulfate 300.0 mg/L 200 46 1,000 Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 Total Dissolved Solids 2540C mg/L 1 47 100 Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 Total MetalsAluminum 200.7 ug/L 2 9.4 200 Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 Boron 200.7 ug/L 50 170 5,000 Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 
ND – Not detected (number in parentheses is the quantitation limit). 

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

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

Table G5-11. Effluent from FGD Wastewater Treatment System, Set 2 Analytical Results, Hatfi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL 

Chromium 200.8 ug/L 2 3.3 8 Cobalt 200.7 ug/L 2 1.1 20 Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 Magnesium 200.7 ug/L 50 540 10,000 Manganese 200.7 ug/L 2 0.51 20 Mercury 1631E ng/L 100 24.4 51 Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 Sodium 200.7 ug/L 2 180 10,000 Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 Titanium 200.7 ug/L 2 1.6 20 Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 
ND – Not detected (number in parentheses is the quantitation limit). 

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

Table G5-12. Effluent from FGD Wastewater Treatment System, Set 3 Analytical Results, Hatfi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL C

Classicals Ammonia 350.1 mg/L 1 0.055 1 0Nitrate Nitrite as N 353.2 mg/L 50 0.95 5 Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 5 20 100 Chloride 300.0 mg/L 200 51 600 8Sulfate 300.0 mg/L 200 46 1,000 4Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0Total Dissolved Solids 2540C mg/L 1 94 200 19Total Suspended Solids 2540D mg/L 1 1.1 4 Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 Beryllium 200.7 ug/L 2 0.71 2 NBoron 200.7 ug/L 50 170 5,000 24Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 1,5Chromium 200.8 ug/L 2 3.3 8 N
ND – Not detected (number in parentheses is the quantitation limit). 

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

Table G5-12. Effluent from FGD Wastewater Treatment System, Set 3 Analytical Results, Hatfi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL C

Cobalt 200.7 ug/L 2 1.1 20 ND Copper 200.8 ug/L 2 0.96 4 Iron 200.7 ug/L 2 32 200 Lead 200.8 ug/L 2 0.73 2 NMagnesium 200.7 ug/L 50 540 10,000 3,1Manganese 200.7 ug/L 2 0.51 20 9Mercury 1631E ng/L 100 24.8 52 7Molybdenum 200.7 ug/L 2 1.6 40 Nickel 200.8 ug/L 2 0.89 4 Selenium 200.8 ug/L 2 0.62 4 Silver 200.8 ug/L 2 0.59 2 NSodium 200.7 ug/L 2 180 10,000 41Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 ND Titanium 200.7 ug/L 2 1.6 20 ND Vanadium 200.8 ug/L 2 1.7 10 Zinc 200.7 ug/L 2 9.1 40 ND 
ND – Not detected (number in parentheses is the quantitation limit). 

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

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

Table G5-13. Effluent from FGD Wastewater Treatment System, Set 4 Analytical Results, Hatfi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Co

Classicals Ammonia 350.1 mg/L 1 0.055 1 1Nitrate Nitrite as N 353.2 mg/L 10 0.19 1 8Nitrogen, Total Kjeldahl 351.2 mg/L 10 0.77 10 2Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 Chemical Oxygen Demand 410.4 mg/L 5 20 100 3Chloride 300.0 mg/L 200 51 600 8,Sulfate 300.0 mg/L 200 46 1,000 4,Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0Total Dissolved Solids 2540C mg/L 1 94 200 18Total Suspended Solids 2540D mg/L 1 1.1 4 1Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND Antimony 200.8 ug/L 2 0.72 2 Arsenic 200.8 ug/L 2 1.2 4 Barium 200.7 ug/L 2 2.5 20 2Beryllium 200.7 ug/L 2 0.71 2 ND Boron 200.7 ug/L 50 170 5,000 220Cadmium 200.8 ug/L 2 1.2 4 Calcium 200.7 ug/L 50 1,700 10,000 1,60
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. Est – Estimated value. F – MS and/or MSD not within laboratory control limits. J – Result measured above the MDL, but less than the quantitation limit. U – Result below the MDL. (Number shown in parentheses is the quantitation limit). 

Table G5-13. Effluent from FGD Wastewater Treatment System, Set 4 Analytical Results, Hatfi

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Co

Chromium 200.8 ug/L 2 3.3 8 ND Cobalt 200.7 ug/L 2 1.1 20 ND Copper 200.8 ug/L 2 0.96 4 1Iron 200.7 ug/L 2 32 200 2Lead 200.8 ug/L 2 0.73 2 ND Magnesium 200.7 ug/L 50 540 10,000 3,20Manganese 200.7 ug/L 2 0.51 20 11Mercury 1631E ng/L 100 24.8 52 8Molybdenum 200.7 ug/L 2 1.6 40 5Nickel 200.8 ug/L 2 0.89 4 5Selenium 200.8 ug/L 2 0.62 4 5Silver 200.8 ug/L 2 0.59 2 ND Sodium 200.7 ug/L 2 180 10,000 520Thallium 200.8 ug/L 2 0.47 2 Tin 200.7 ug/L 2 4.8 200 ND Titanium 200.7 ug/L 2 1.6 20 ND Vanadium 200.8 ug/L 2 1.7 10 2Zinc 200.7 ug/L 2 9.1 40 ND 
ND – Not detected (number in parentheses is the quantitation limit). 

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

Table G5-14. Influent to FGD Wastewater Treatment System Field Blank, Set 1 Analytical R

Hatfield’s Ferry 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Concen

Total MetalsAluminum 200.7 ug/L 2 9.4 200 12 Antimony 200.8 ug/L 2 0.72 2 ND (2) Arsenic 200.8 ug/L 2 1.2 4 ND (4) Barium 200.7 ug/L 2 2.5 20 ND (20) Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 2 6.7 200 14 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 ND (400Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 ND (4) Iron 200.7 ug/L 2 32 200 ND (200Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 2 21 400 61 Manganese 200.7 ug/L 2 0.51 20 0.98 Mercury 1631E ng/L 1 0.24 0.5 0.65 Molybdenum 200.7 ug/L 2 1.6 40 ND (40) Nickel 200.8 ug/L 2 0.89 4 ND (4) Selenium 200.8 ug/L 2 0.62 4 ND (4) Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 ND (10,00
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 G5-14. Influent to FGD Wastewater Treatment System Field Blank, Set 1 Analytical R

Hatfield’s Ferry 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Concen

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 ND (20) Vanadium 200.8 ug/L 2 1.7 10 ND (10) 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. 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 G5-15. Effluent from FGD Wastewater Treatment System Field Blank, Set 1 Analy

Results, Hatfield’s Ferry 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Concentra

Total MetalsAluminum 200.7 ug/L 2 9.4 200 16 Antimony 200.8 ug/L 2 0.72 2 ND (2) Arsenic 200.8 ug/L 2 1.2 4 ND (4) Barium 200.7 ug/L 2 2.5 20 ND (20) Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 2 6.7 200 19 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 ND (400) Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 ND (4) Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 2 21 400 49 Manganese 200.7 ug/L 2 0.51 20 ND (20) Mercury 1631E ng/L 1 0.24 0.5 ND (0.5) Molybdenum 200.7 ug/L 2 1.6 40 ND (40) Nickel 200.8 ug/L 2 0.89 4 ND (4) Selenium 200.8 ug/L 2 0.62 4 ND (4) Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 ND (10,000) 
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 G5-15. Effluent from FGD Wastewater Treatment System Field Blank, Set 1 Analy

Results, Hatfield’s Ferry 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Concentra

Thallium 200.8 ug/L 2 0.47 2 ND (2) Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 ND (10) 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. 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 G5-16. Effluent from FGD Wastewater Treatment System Field Blank, Set 2 Analy

Results, Hatfield’s Ferry 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Concentra

Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) Antimony 200.8 ug/L 2 0.72 2 ND (2) Arsenic 200.8 ug/L 2 1.2 4 ND (4) Barium 200.7 ug/L 2 2.5 20 ND (20) Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 2 6.7 200 22 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 ND (400) Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 ND (4) Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 2 21 400 25 Manganese 200.7 ug/L 2 0.51 20 ND (20) Mercury 1631E ng/L 1 0.24 0.5 ND (0.5) Molybdenum 200.7 ug/L 2 1.6 40 ND (40) Nickel 200.8 ug/L 2 0.89 4 ND (4) Selenium 200.8 ug/L 2 0.62 4 ND (4) Silver 200.8 ug/L 2 0.59 2 1.3 Sodium 200.7 ug/L 2 180 10,000 ND (10,000) 
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 G5-16. Effluent from FGD Wastewater Treatment System Field Blank, Set 2 Analy

Results, Hatfield’s Ferry 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Concentra

Thallium 200.8 ug/L 2 0.47 2 ND (2) Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 ND (10) 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 G5-17. Effluent from FGD Wastewater Treatment System Field Blank, Set 3 Analy

Results, Hatfield’s Ferry 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Concent

Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200Antimony 200.8 ug/L 2 0.72 2 ND (2) Arsenic 200.8 ug/L 2 1.2 4 ND (4) Barium 200.7 ug/L 2 2.5 20 ND (20) Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 2 6.7 200 35 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 75 Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 ND (4) Iron 200.7 ug/L 2 32 200 ND (200Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 2 21 400 61 Manganese 200.7 ug/L 2 0.51 20 1.3 Mercury 1631E ng/L 1 0.24 0.5 ND (0.5Molybdenum 200.7 ug/L 2 1.6 40 ND (40) Nickel 200.8 ug/L 2 0.89 4 ND (4) Selenium 200.8 ug/L 2 0.62 4 ND (4) Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 ND (10,00
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 G5-17. Effluent from FGD Wastewater Treatment System Field Blank, Set 3 Analy

Results, Hatfield’s Ferry 

Analyte Method Unit

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Concent

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 ND (20) Vanadium 200.8 ug/L 2 1.7 10 ND (10) 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 G5-18. Effluent from FGD Wastewater Treatment System Field Blank, Set 4 Analy

Results, Hatfield’s Ferry 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Concentra

Total MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) Antimony 200.8 ug/L 2 0.72 2 ND (2) Arsenic 200.8 ug/L 2 1.2 4 ND (4) Barium 200.7 ug/L 2 2.5 20 ND (20) Beryllium 200.7 ug/L 2 0.71 2 ND (2) Boron 200.7 ug/L 2 6.7 200 37 Cadmium 200.8 ug/L 2 1.2 4 ND (4) Calcium 200.7 ug/L 2 69 400 ND (400) Chromium 200.8 ug/L 2 3.3 8 ND (8) Cobalt 200.7 ug/L 2 1.1 20 ND (20) Copper 200.8 ug/L 2 0.96 4 ND (4) Iron 200.7 ug/L 2 32 200 ND (200) Lead 200.8 ug/L 2 0.73 2 ND (2) Magnesium 200.7 ug/L 2 21 400 ND (400) Manganese 200.7 ug/L 2 0.51 20 ND (20) Mercury 1631E ng/L 1 0.24 0.5 ND (0.5) Molybdenum 200.7 ug/L 2 1.6 40 ND (40) Nickel 200.8 ug/L 2 0.89 4 ND (4) Selenium 200.8 ug/L 2 0.62 4 ND (4) Silver 200.8 ug/L 2 0.59 2 ND (2) Sodium 200.7 ug/L 2 180 10,000 ND (10,000) 
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 G5-18. Effluent from FGD Wastewater Treatment System Field Blank, Set 4 Analy

Results, Hatfield’s Ferry 

Analyte Method Unit 

Dilution 

Factor 

SampleSpecific MDL Sample- Specific QL Concentra

Thallium 200.8 ug/L 2 0.47 2 ND (2) Tin 200.7 ug/L 2 4.8 200 ND (200) Titanium 200.7 ug/L 2 1.6 20 ND (20) Vanadium 200.8 ug/L 2 1.7 10 ND (10) Zinc 200.7 ug/L 2 9.1 40 ND (40) 
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 2.2 mg/L 

71991 TDS EXCLUDE Dilution factor cannot be 

confirmed 

XXX mg/L 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

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

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Donna Tedder, ERG 

Date: 2/9/2012

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

Month 2 (Part 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 three samples (excluding laboratory prep blanks) FGS extracted 

and analyzed for total mercury. 

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

EPA 

Sample # 

Lab Sample 

ID # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72292 1011118-01 Aqueous FGD Influent, Set 2 11/10/2010 

72296 1011118-06 Aqueous FGD Effluent, Set 2 11/10/2010

72301 1011118-07 Aqueous FGD Effluent Field Blank, Set 2 11/9/2010

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. 
2

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 this sampling episode. A sample from 

another work order was analyzed in duplicate at the laboratory with these samples. The 

RPD was 6.33%. 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 (MS/MSD) 

The matrix spike (MS) and matrix spike duplicate (MSD) was performed on Effluent 

sample 72296. An MS/MSD was also performed on a sample from another work order. 

The MS/MSD samples for 72296 had recoveries of 82.6% and 96.8%, respectively, with 

an RPD of 7.94%. The MS/MSD samples from another work order had recoveries of 

100% and 85.2%, respectively, with an RPD of 8.85%. All MS/MSD samples met the 

method specified recovery criteria of 71-125% and the RPD criteria of less than or equal 

to 24%. 

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 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 2 (Part 2) Total Metals – Sample 

Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72292 FGD Influent, Set 2 280-9642-1 Aqueous 11/10/2010 11/11/2010

72296 FGD Effluent, Set 2 280-9642-2 Aqueous 11/10/2010 11/11/2010

72301 FGD Effluent Field Blank, 

Set 2 

280-9642-3 Aqueous 11/10/2010 11/11/2010

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

silver for sample 72296 failed the EPA Method 200.8 control limits of 70-130%. 
2

• The post digestion spike (PDS) recoveries for silver for sample 72296 failed 

TestAmerica’s control limits of 85–115%. 

INTERNAL STANDARDIZATION 

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

INITIAL CALIBRATION 

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

calibration for the ICP-MS analysis consisted of a blank and four calibration standards. 

INITIAL AND CONTINUING CALIBRATION VERIFICATION (ICV/CCV) 

The initial calibration verifications (ICV) and continuing calibration verifications (CCV) 

performed by TestAmerica all had recoveries within the method criteria. 

METHOD/INSTRUMENT BLANKS 

All the method blanks were less than the reporting limit (RL); however, some elements 

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

required for method blanks. 

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

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

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

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. 
3

The ICSA solution for the method 200.8 analysis exceeded the acceptance limits for 

Chromium in analytical batch 280-41398. The lab has confirmed with the vendor that 

Chromium is a trace impurity in the ICSA solution. Therefore, corrective action was 

deemed unnecessary; the associated data have been flagged “^”. 

SERIAL DILUTION 

The serial dilution performed on sample 72296 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) 

The MS and MSD was performed on sample 72296. The total selenium results in the 

MSD sample for sample 72296 failed the 70-130% recovery method control limits and 

were flagged with a “4” qualifier indicating concentrations in the parent samples were 

greater than four times the spike amounts. This result was considered acceptable based on 

the LCS passing the method control limits. 

The total silver results in the MS and MSD samples for sample 72296 failed the 70-130% 

recovery method control limits and were flagged with an “F” qualifier. The poor 

recovery of silver is likely due to 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 relative percent difference (RPD) passed the FGD ICP/MS SOP control 

limits of ±20% for all analytes. No additional data qualifiers were required for MS/MSD 

samples. 

POST DIGESTION SPIKES (PDS) 

The PDS performed on sample 72296 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. An additional qualifier is required as shown in 

Table 2. 

DETECTION LIMITS 
4

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 

72296 Silver 

(total) 

Matrix 

Interference 

PDS Failed 85-

115% Recovery 

ND 
1

MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD 

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

 Deb Bartram, ERG 

 TJ Finseth, ERG 

From: Randy Mercurio, ERG 

Date: 2/9/2012 

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

Monitoring: Month 2 (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 2 (Part 2) Total Metals – Sample Identification 

EPA 

Sample # 

EPA Sample Description Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72292 FGD Influent, Set 2 280-9642-1 Aqueous 11/10/2010 11/11/2010

72296 FGD Effluent, Set 2 280-9642-2 Aqueous 11/10/2010 11/11/2010

72301 FGD Effluent Field Blank, Set 2 280-9642-3 Aqueous 11/10/2010 11/11/2010

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. 

• An initial calibration verification (ICV) had a recovery for aluminum above the 

upper control limit. Aluminum values for all samples associated with this ICV 

were non-detects and were reported by TestAmerica. 

• The matrix spike (MS)/matrix spike duplicate (MSD) relative percent difference 

(RPD) for boron, calcium, and magnesium for sample 72296 failed TestAmerica’s 

SOP requirement of ± 20%. 
2

• The post digestion spike (PDS) for barium for sample 72296 failed TestAmerica’s 

control limits of 85-115% recovery. 

SAMPLE RECEIPT, HANDLING AND STORAGE ISSUES 

There were no sample receipt issues in this data package. 

INTERNAL STANDARDIZATION 

While the internal standard (ISTD) yttrium was used for these analyses, no checks for the 

ISTD recoveries within the ±30% criterion of the calibration blank as per Section 9.11 of 

the SOP were seen. All ISTD were within the control limits. 

INITIAL CALIBRATION 

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

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

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS 

All ICVs had recoveries within the method criteria with the exception of aluminum, 

which recovered above the upper control limit. Aluminum values of samples associated 

with this ICV were non-detects and were reported by TestAmerica. 

All continuing calibration verifications (CCV) 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) 

The CRI sample passed TestAmerica’s SOP control limits of 50–150% recovery. 

LABORATORY CONTROL SAMPLES (LCS) 

The LCS passed the method control limits of 85–115% recovery. 
3

INTERFERENCE CHECK SOLUTIONS 

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

data quality objectives met TestAmerica’s SOP criteria.

SERIAL DILUTION (SRD) 

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

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

FIELD DUPLICATES 

No field duplicate samples were collected with these sampling episodes. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

An MS and MSD were performed on the total sample 72296. 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. Otherwise, 

all MS/MSD spike recoveries were within the method control criteria of 70-130%. The 

MS/MSD RPD for boron, calcium, and magnesium for sample 72296 failed 

TestAmerica’s SOP requirement of ± 20%. These elements were flagged with an “F” 

qualifier. No additional qualifiers are needed. 

POST DIGESTION SPIKE (PDS) 

The PDS performed on sample 72296 passed TestAmerica’s control limits of 85-115% 

recovery for all analytes except barium, which was qualified with a “W”. Barium passed 

the MS/MSD recovery and serial dilution control limits demonstrating no significant 

matrix interference. No additional qualifiers are needed.

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 2) 

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for these long-term monitoring samples. 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 two samples that TestAmerica analyzed for the above analytes. 

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

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72292 Water FGD Influent, Set 2 11/10/10

72296 Water FGD Effluent, Set 2 11/10/10
2 

SUMMARY 

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

samples were preserved appropriately. 

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. 

As described below, the analyte of interest was detected above the method detection limit 

(MDL) in some laboratory reagent blanks (LRB). However, the analyte of interest was 

never detected above the reporting limit (RL) in the LRBs. If required by the method, all 

laboratory fortified blanks (LFB) met the criteria specified in the method unless specified 

below. 

If required by the method, a matrix spike (MS) sample was analyzed on sample 72296 for 

each analyte to check for matrix interferences. MS samples analyzed met the criteria 

specified in the method unless described below. 

DATA NOTES/ISSUES 

Ammonia 

No issues were identified by the data reviewer. 

BOD5 

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

greater than 2.0 mg/L for samples 72292 and 72296; however the duplicate of sample 

72292 did not have a DO depletion greater than 2.0 mg/L. Therefore, BOD5 was reported 

as not detected for the duplicate. 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. 
3 

The seed correction factor was lower than 0.6 mg/L, at 0.464 mg/L. 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. 

All glucose-glutamic acid standards and laboratory duplicates were analyzed 

appropriately and met the criteria specified in SM 5210B. 

Chloride and Sulfate 

No issues were identified by the data reviewer.

COD 

No other issues were identified by data reviewer.

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 72292 and 72296 had results ≥ 20 ug/L; 

but were not diluted further because they were within the calibration performed. 

A MS/MSD was performed using sample 72296. The percent recovery for both the MS 

and MSD was 49%, which is below the control limit of 90% and therefore, the MS/MSD 

results were flagged with the “F” qualifier. Based on the LFB and LFBD recoveries being 

within the method control limits, the samples were not qualified. The MS/MSD results 

did exceed the calibration range and were not diluted. If reported, these MS/MSD results 

will be additionally qualified as estimated values. 

Nitrate/Nitrite 

The MS/MSD results for samples 72296 were above the calibration curve. TestAmerica 

did not reanalyze these MS/MSDs with a higher dilution factor, but the MS/MSD 

samples were flagged with “E” qualifier because the results exceeded calibration range. 

The percent recovery for the MS/MSD were within the control limits. 

Phosphorus 

The LRB was greater than the MDL at 0.0111 mg/L, but less than the RL; therefore, the 

LRB results were flagged with a “J” qualifier and the concentration is an approximate 

value. No further qualifiers are needed. All samples that contained the analyte were also 

flagged with “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 “J” qualifier meaning the sample result was an estimated 

value. 
4 

Sample 72296 and the LRB had results that were lower than the lowest calibration 

standard. Each of these results were greater than the MDL, but less than the RL and 

therefore, were flagged with a “J” qualifier. No further qualifiers are needed. 

The percent recoveries for the MS/MSD analysis of sample 72296 was not within the 

control limits of 90-110% specified in EPA Method 365.1. However the MS/MSD of 

sample 72296 were within the laboratory control limits of 71-128%. The percent 

recoveries of the MS and MSD samples were 79% and 76%, respectively. Because the 

MS/MSD of sample 72296 met laboratory control limits it was not flagged by the lab. If 

the MS/MSD results are reported, they should be flagged with an “F” qualifier. 

TDS 

Constant weight was not achieved after 3 drying cycles for the samples. The weight did 

not go up from first to second or second to third, so hygroscopy is not an issue. 

The RPD for laboratory duplicates from sample 72296 was 13%, which is not less than 

10% as required by SM 2540C; the sample was not qualified by the laboratory. Sample 

72296 was qualified as an estimated value. 

TKN 

A LFB (LCS) and a LFB duplicate (LCSD) were performed with a percent recovery of 

90% and 88%, respectively. The LFBD recovery was below the method control limit of 

90-110% recovery and was flagged with “*” qualifier. The samples were qualified as 

minimum values due to the low LFBD recovery. 

TestAmerica performed MS/MSD analyses on sample 72296. The percent recoveries for 

the MS and MSD sample 72296 were 93% and 85%, respectively. The MSD did not meet 

the method control limits of 90-110%, but it did meet the laboratory control limits of 54-

131% and therefore, was not flagged by the laboratory. If reported, the MSD of sample 

72296 should be flagged with an “F” qualifier. 

TSS 

The RPD for the laboratory duplicate performed on sample 72296 was 25%, which is 

greater than the method control criteria of 10 percent. Sample 72296 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. 
5 

Table 2. Data Review Summary Table 

Sample Analyte Qualifier/ 

Action 

Reason Level Detected

72292 BOD Minimum 

Value, s 

SCB recovery low 2.0 mg/L 

72296 BOD Minimum 

Value, s 

SCB recovery low 2.1 mg/L 

72296 TDS Estimated 

Value 

Lab duplicate RPD > 

method-specified 

criteria 

Sample-10000 

mg/L 

Dup-12000 

mg/L 

72292 TKN Minimum 

Value 

LFBD % 

Recovery<method 

47 mg/L

72296 TKN Minimum 

Value 

LFBD % 

Recovery<method 

5.4 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 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 1 mg/L 

72293 COD Estimated 

Value 

Received at neutral pH 490 mg/L 

72297 COD Estimated 

Value 

Received at neutral pH 460 mg/L 

72293 Nitrate/Nitrite Estimated 

Value 

Received at neutral pH 150 mg/L 

72297 Nitrate/Nitrite Estimated 

Value 

Received at neutral pH 150 mg/L 

72293 Phosphorus Estimated 

Value 

Received at neutral pH 2.6 mg/L 

72297 Phosphorus Estimated 

Value 

Received at neutral pH 0.07 mg/L 

72293 TKN Estimated 

Value 

Received at neutral pH 47 mg/L

72297 TKN Estimated 

Value 

Received at neutral pH 16 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: Randy Mercurio, ERG 

Date: 2/9/2012 

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

Monitoring: Month 5 

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 5 Total Metals – Sample Identification 

EPA 

Sample # EPA Sample Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72294 FGD Influent, Set 4 280-12365-1 Aqueous 2/9/2011 2/10/2011

72298 FGD Effluent, Set 4 280-12365-2 Aqueous 2/9/2011 2/10/2011

72303 FGD Effluent Field Blank, Set 4 280-12365-3 Aqueous 2/9/2011 2/10/2011

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 matrix spike duplicate (MSD) recovery for total silver for sample 72298 

failed the EPA Method 200.8 control limits of 70–130%. 

• The matrix spike (MS)/MSD relative percent difference (RPD) for total silver for 

sample 72298 failed the FGD ICP/MS SOP control limits of ±20%. 
2

• The post digestion spike (PDS) recoveries for selenium and silver for sample 

72298 failed TestAmerica’s control limits of 85–115%. 

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). 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. 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. 
3

SERIAL DILUTION 

The serial dilution performed on sample 72298 passed TestAmerica’s criteria of ±10% 

difference for all analytes except selenium, which was qualified with a “V” qualifier. 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) 

The MS and MSD were performed on sample 72298. The MSD of sample 72298 failed 

the method control limits of 70–130% recovery for silver at 45%, which was flagged with 

an “F” qualifier. This silver failure is 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/LCSD were acceptable. The RPD for the 

MS/MSD of sample 72298 also failed the FGD ICP/MS SOP ±20% control limits for 

silver at 47%. 

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 72298 passed TestAmerica’s control limits of 85–115% 

recovery for all analytes, except for selenium and silver, which were flagged with “W” 

qualifiers. The selenium and silver recoveries in the associated LCS/LCSD were 

acceptable. 

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 5 

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 5 Total Metals – Sample Identification 

EPA 

Sample # 

EPA Sample 

Description 

Lab Sample 

ID # 

Sample 

Matrix 

Sampling 

Date 

Receipt 

Date 

72294 FGD Influent, Set 4 280-12365-1 Aqueous 2/9/2011 2/10/2011

72298 FGD Effluent, Set 4 280-12365-2 Aqueous 2/9/2011 2/10/2011

72303 FGD Effluent Field Blank, 

Set 4 

280-12365-3 Aqueous 2/9/2011 2/10/2011

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. 

SAMPLE RECEIPT, HANDLING AND STORAGE ISSUES 

There were no sample receipt issues in this data package. 
2

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 before each analysis. 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. 
3

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD) 

A matrix spike (MS) and matrix spike duplicate (MSD) was performed on the total 

sample of 72298. 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. No additional data qualifiers 

were needed. 

POST DIGESTION SPIKE (PDS) 

The PDS of total sample 72298 failed the method criteria of 85–115% for boron and 

manganese; however, these results were not qualified with a “W” because their sample 

concentrations were greater than 4 times the spike amount. 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: Ariel Atkinson, ERG 

Date: 2/9/2012 

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

Monitoring: Month 5 

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for these long-term monitoring samples. 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 two samples that TestAmerica analyzed for the above analytes. 

Table 1. Long Term Monitoring Set 2 Episodes 6571 Classical Analytes – Sample 

Identification 

EPA 

Sample # 

Sample 

Matrix Sample Description 

Sampling 

Date 

72294 Water FGD Influent, Set 4 2/9/11

72298 Water FGD Effluent, Set 4 2/9/11

SUMMARY 

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

samples were preserved appropriately unless otherwise specified. Sample 72294 for 

Group II analytes was received at the laboratory at a neutral pH. The laboratory preserved 

the volume and proceeded with the requested analyses. No Collection date and time was 
2 

recorded on the traffic reports, so the laboratory set the collection date as 2/9/11 0:00; the 

date the samples were relinquished. 

 

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. 

As described below, the analyte of interest was detected above the method detection limit 

(MDL) in some laboratory reagent blanks (LRB). However, the analyte of interest was 

never detected above the reporting limit (RL) in the LRBs. If required by the method, all 

laboratory fortified blanks (LFB) met the criteria specified in the method unless specified 

below. 

If required by the method, a matrix spike (MS) sample was analyzed on sample 72298 for 

each analyte to check for matrix interferences. MS samples analyzed met the criteria 

specified in the method unless described below. 

DATA NOTES/ISSUES 

Ammonia 

Ammonia was detected in the method blank, at 0.106 mg/L. The results were greater than 

the MDL (0.055 mg/L), but less than the RL (1.0 mg/L) and therefore, was flagged with a 

“J” qualifier. The samples were also flagged with a “B” qualifier because the compound 

was found in the blank and the samples. 

Sample 72294 was received at the laboratory at neutral pH. The method requires that the 

sample pH be adjusted to <2 at the time of collection; therefore, the sample result was 

qualified as an estimated value. 

BOD5 

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

greater than 2.0 mg/L for samples 72294 and 72298. 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. 
3 

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 for chloride for sample 72298 were above the calibration curve. 

TestAmerica did not reanalyze these MS/MSDs with a higher dilution factor, because the 

percent recoveries and RPD met the method criteria. The MS/MSD results for chloride 

for sample 72298 were flagged with an “E” qualifier because the results exceeded the 

calibration range.

COD 

Sample 72294 was received at the laboratory at neutral pH. Method 410.4 requires that 

the sample pH be adjusted to <2 at the time of collection. The sample result was 

qualified as an estimated value as shown in Table 2. 

The percent recovery of the MS for sample 72298 did not meet method criteria, at 66% 

recovery. Test America did flag the MS results with an “F” qualifier and no further 

qualifications were needed.

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. 

A MS/MSD was performed using sample 72298. The percent recovery for the MS and 

MSD were 84% and 83%, respectively, which is below the control limit of 90% and as a 

result, the MS/MSD results were flagged with an “F” qualifier. 

Nitrate/Nitrite 

The MS/MSD results for samples 72298 were above the calibration curve. TestAmerica 

did not reanalyze these MS/MSDs with a higher dilution factor, but the MS/MSD results 

were flagged with “E” qualifier. The percent recovery for the MS and MSD were within 

the laboratory control limits, but not within the method control limits, at 87% and 84%, 

respectively. These results were not flagged with an “F” qualifier. If the MS/MSD results 

are reported, they should be qualified with an “F” qualifier. 

Sample 72294 was received at the laboratory at neutral pH. The method requires that the 

sample pH be adjusted to <2 at the time of collection; therefore, the sample result was 

qualified as an estimated value. 
4 

Phosphorus 

The final CCB was greater than the MDL at 0.0212 mg/L, however the result was less 

than the RL; therefore, the CCB result was flagged with a “J” qualifier. No further 

qualifiers are needed. All samples that contained the analyte were also flagged with “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 “J” qualifier.

Sample 72294 and 72298 had results that were lower than the lowest calibration standard. 

Sample 72294 was flagged with a “J” qualifier because the result was less than the RL 

but greater than or equal to the MDL. Sample 72298 was above the RL and not flagged 

with a “J” qualifier; therefore, this result should be considered an estimated value. 

Sample 72294 was received at the laboratory at neutral pH. The method requires that the 

sample pH be adjusted to <2 at the time of collection. The sample result should be 

considered an estimated value, and since it already has the “J” qualifier, no further 

qualification is needed for this sample. 

The percent recoveries for the MS and MSD for sample 72298 were not within the 

control limits of 90-110% specified in EPA Method 365.1. The percent recoveries of the 

MS and MSD samples were 27% and 32%, respectively. Because the MS/MSD of 

sample 72298 did not meet control limits it was flagged with an “F” qualifier. 

TDS 

Constant weight was not achieved after 3 drying cycles for the samples. The weight did 

not go up from first to second or second to third, so hygroscopy is not an issue. No 

further issues were identified. 

TKN 

TKN was detected in the initial calibration blank and method blank, at 0.378 mg/L and 

0.389 mg/L, respectively. These results were flagged with a “J” qualifier because the 

results were above the MDL but below the RL; all associated samples were flagged with 

a “B” qualifier. 

Sample 72294 was received at the laboratory at neutral pH. The method requires that the 

sample pH be adjusted to <2 at the time of collection; therefore, the sample result was 

qualified as an estimated value. 

TestAmerica performed MS and MSD analyses on sample 72298. The percent recoveries 

for the MS and MSD for sample 72298 were 146% and -8%, respectively, the RPD was 

16%. The MS/MSD were flagged with the “4” qualifier because the analyte present in the 

original sample is four times greater than the matrix spike concentration; therefore, 

control limits are not applicable. No further qualification is necessary. 
5 

TSS 

The RPD for the laboratory duplicates performed on sample 72294 was 40%, which is 

greater than the method control criteria of 10 percent. Sample 72294 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. 

Table 2. Data Review Summary Table 

Sample Analyte 

Qualifier/ 

Action Reason Level Detected

72294 Ammonia Estimated 

Value 

Neutral pH at receipt 1.9 mg/L

72294 COD Estimated 

Value 

Neutral pH at receipt 500 mg/L

72294 Nitrate/Nitrite Estimated 

Value 

Neutral pH at receipt 100 mg/L

72298 Phosphorus Estimated 

Value 

Result<calibration 

curve 

0.0506 mg/L

72294 TKN Estimated 

Value 

Neutral pH at receipt 130 mg/L