# 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 th e effluent limitations guidelines and standards for the Steam Electric Power Gen erating Industry.

These instructions are being provided to Allegheny Energy Supply Co, LLC’s Hatfield’s Ferry Power Station to aid in collecting, packaging, an d shipping samples for this sampling program.

The plant must collect grab samples for all analytes a t 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 tre atment sampling point. At the FGD wastewater treatment effluent, the plant must co llect 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 month s. 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 re garding the timeline or the steps provided, please contact Mr. Ronald Jordan at (202) 566-1003 or j ordan.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 (spe cially-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 labora tories);

• Preservation supplies (see the “Sample Bottles and Pr eservation” 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 fr om each of the two sampling points included in the EPA’s sampling episode. Figure 1 identifies e ach of the sampling points for this sampling program. The following is a description o f 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 pri or to any commingling with other wastewaters or treatment system recycle s treams. This sample should be collected from the sample tap located on the pipe th at 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 s ets, and secondary hydroclone overflow from Unit 3 for two of the sample se ts.

• 

### FGD wastewater treatment effluent (SP-2) : This sampling point shall represent the effluent from the FGD wastewater treatment syste m, prior to mixing with dilution water or other streams. This sampling point shou ld be collected from the sample tap that is located on the pipe downstream of th e effluent storage tank at a point where a sample can be collected regardless of whet her the effluent is being discharged or recirculated.

Analytes

The analytes included in this sampling program include all ana lytes from EPA’s sampling program, except for the dissolved metals analyses (which includes hexavalent chromium). Table 1 contains the listing of all the an alytes 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 Moni toring Program

Parameter Method Number

Classicals Biochemical oxygen demand (BOD 5 ) 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, ir on, magnesium, manganese, molybdenum, sodium, tin, and titani um EPA 200.7Figure 1.Hatfield’s Ferry FGD Wastewater Treatment System Monitoring Program Sampling PointsFGD Scrubber PurgeLimeReaction Tank 1SP-1.1Indicates a Sampling PointGravityFilterClarifier 1SludgeStorageTankFilter PressSumpGravityFilterSolids to Onsite LandfillWastewater FlowSludge FlowIntermittent Wastewater FlowClarifierSludgeClarifier 2Gravity FilterBackwashReactionTank 2Ferric ChlorideTreatedWastewaterStorageTankEqualizationTankEffluentRecycleMonongahelaRiverWastewaterfrom SumpSP-2EffluentRecyclePolymerHydrochloricAcidOrganosulfideSecondaryHydroclonefor Unit 1SecondaryHydroclonefor Unit 2SecondaryHydroclonefor Unit 3HydrocloneoverflowHydrocloneoverflowHydrocloneoverflowSP-1.2SP-1.3

### Sample Bottles and Preservation

Table 2 identifies the sample bottles that are needed fo r collecting samples. The table also identifies the on-site preservation that is requi red for the samples. Please note that the number of sample bottles listed in Table 2 refers t o 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-preserv ed 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 chl orine). 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 t he plant will need to add sodium arsenite until the chlorine is not detected by the potass ium 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

BOD 5 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 H 2 SO 4 to pH <2, ≤ 6 ° C

Total cyanide One 1-L HDPE

bottle Dilution until sulfide is not detected,

NaAsO 2 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/nit rite 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 i t 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 co ver the labels with clear tape to prevent tampering, abrasion, smearing, or loss during trans it. For metal and mercury samples, do not place labels directly on the sample bot tles because of the potential for contamination. Instead, place the label on the outer pl astic 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 Zi ploc bag after collection.

Table 3 provides the sampling point descriptions, sample numbe rs, and sampling episode number for the plant for this monitoring program. The info rmation 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 followi ng, 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 ef fluent laboratory composite samples. The bottles should be l abeled as Grab 1, Grab 2, Grab 3, and Grab 4 for the four respective collec tion times).

The “sample bottle type” should be shown on the label t he 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 bo ttle type” should be “250-mL glass bottle.” The “required on-site preservation” sh ould be shown on the label the same as the “On-Site Preservation” column in Table 2, exce pt that “(acid preserve at laboratory)” does not need to be included for the total me tals 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) Classicals 1



### 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 requi red.

Sample Collection

The plant must use clean sampling techniques when collecti ng the total metals and total mercury samples; therefore, the sampling team should fo llow the clean hands/dirty hands sampling techniques outlined in EPA Method 1669. Additionally, t he plant must try to avoid significant contamination during sample collection, especially from sources such as airborne particles, dirt, and corrosion particulates fr om piping, railing, etc.

### The plant must collect grab samples for all analytes a t the influent to the FGD wastewater

treatment system. The plant must collect 24-hour compo site samples for all analytes except cyanide and mercury at the FGD wastewater treatme nt effluent sampling point. The 24-hour composites must be set up to collect equal sam ple aliquots every hour over the 24-hour period. For mercury at the FGD wastewater tr eatment 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 th e FGD wastewater treatment effluent sampling point, the plant must collect a singl e 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 fo llow 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 th e composite pump-off procedures for the FGD wastewater treatment effluent sampling po int. 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 trea tment effluent sampling point has intermittent flows which may interfere with the autom atic composite collection, please contact TJ Finseth, (703) 633-1698 to discuss possible alterna tives.)

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 slightl y (touching only the outer part of the bag) so that clean hands can place h ands in the bag and open the bag completely.

4. Clean hands then uses the plastic bag to shroud the samp le tap (note that there should be no flow through the sample tap at this t ime). Clean hands will need to puncture a small hole in the bag using the ta p and dirty hands can cable tie the bag to the tap to prevent it from fall ing during sample

collection.

5. Dirty hands opens the outer bags of the field blank wat er and total mercury and total metals field blank sample bottles. Clean hand s opens the inner bag of the field blank water and unscrews the lid. Clean h ands then opens the inner bag of the total mercury and total metals field bl ank sample bottles. Clean hands pours the blank water into the fi eld blank sample bottles under the shrouding, caps the bottles, and closes the inner bags. Clean hands then places the total mercury and total met als bottles in the outer bags and dirty hands closes the outer bag.

6. Dirty hands then opens the valve to the sample tap and pur ges the tap for at least two minutes, then keeps the valve open until all sam ples have been

collected.

### 7. Dirty hands opens the outer bag for the total mercury s ample bottle. Clean hands takes the sample bottle and inner bag and holds the m under the shroud. Clean hands then opens the inner bag, opens the l id of the bottle and fills the total mercury sample bottle. Clean hands caps the sample bottle, closes the inner bag, and places the sample bo ttle in the outer bag. Dirty hands closes the outer bag. The samplers repea t 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 met als 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 samp les 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 prio r to shipment to the laboratories. Use the information provide d in the “Sample

Bottle and Preservation” section of these instruction f or the preservation steps. Additionally, the BOD, Group I, Group II, and tota l cyanide samples should be placed on ice immediately after sample coll ection/preservation.

Sample Packing and Shipment

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

laboratories.

1. Make sure that each sample bottle has a label, and tha t the label correctly specifies the sample point.

2. Tighten the lid on each filled sample bottle, being car eful not to overtighten the lid. If bottle threads are dirty to w here the lid is impeded from closing, clean the threads on the bottle being caref ul to not introduce contamination into the sample. Clean the sample bottl e 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 wr ap 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 th e coolers with proper end up, close the interior garbage bag by tying, or with a tw ist-tie.

7. Add ice to the cooler to keep samples cold during shipment. Ar range 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 l east 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 sec ond 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 diff erent cooler with proper end up, close the interior garbage bag by tying or wit h 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 w ould need to be chilled prior to packing them in the cooler with the clas sicals and ice

would need to be added to the cooler between the interior a nd 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 pac king material should be used so that the sample containers will not shi ft during shipment.

11. Fill out and print a traffic report form for the classi cals and metals samples (provided electronically by ERG). Seal the last two pages o f the traffic report form(s) in a plastic envelope secured to the insid e of the top of the cooler(s). NOTE: the top page of the traffic report mus t 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 o f the cooler(s). The classicals and metals samples should be shipped to TestAme rica 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 pe rpendicular to

the seal to ensure that the lid will remain closed if t he latch is accidentally released or damaged.

15. Place the mercury samples in the garbage bags in a separ ate 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 o f the cooler. NOTE: the top page of the traffic report must be sent to ERG a t the same address provided in step 11:

19. Close the cooler.

20. Place a completed laboratory address label on the lid o f 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 pe rpendicular to

the seal to ensure that the lid will remain closed if t he latch is accidentally released or damaged.

22. Fill out the necessary paperwork for FedEx or UPS to prepa re the shipment for pick up or drop off. NOTE: the samples must b e 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), pleas e contact TJ Finseth at (703) 633-1698, to notify him that the samples have b een 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 t o 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, th e plant must print the four pages in the file. The last two pages in the file must be placed in t he 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 operatio n of the plant and FGD systems during the sample collection period. Additionall y, 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 w ill 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 th e 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 s ample 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 pointPlant NameSampleCollectionNumberDate of SampleCollectionSample CollectionTime Temperature (°C)pH(S.U.)Set 1Set 2Set 3Set 4Plant NameSampleCollectionNumberUnit OverflowSampled atInfluent(7 or 8)Influent SamplesCollected as Grabs(Yes or No)Mercury and CyanideSamples Collected asGrabs(Yes or No)Effluent SamplesCollected as 24-Hour Composites(Yes or No)Tyvek Suitsused(Yes or No)Dust MasksUsed forMercury(Yes or No)Clean Hands/DirtyHands SamplingTechniques Used(Yes or No)Description of SampleCollection Technique (ifdifferent thaninstructions)Description of AbnormalConditions in FGD Systemor FGD WastewaterTreatment System that MayImpact ConcentrationsSet 1Set 2Set 3Set 4Complete the following tables based on the plant operating characteristics during each set of samplescollectedUnits OperatingDuring SamplingDayUnits Off-lineEntireSampling DaySCRs/SNCRsOperating onUnitsSet 1Set 2Set 3Set 4Flow Rate (gpm)DurationSet 1Set 2Set 3Set 4Lime Usage(tons)Ferric ChlorideUsage(Liters/day)Organosulfide Usage(Liters/day)Polymer Usage(Liters/day)Acid Usage(Liters/day)ChemicalPrecipitationSystem EffluentFlow Rate (gpd)Set 1Set 2Set 3Set 4Plant NameSampleCollectionNumberDate of SampleCollectionPlant Operation During Sample CollectionPlant NameSampleCollectionNumberDate of SampleCollectionPlant Operation During Sample CollectionScrubber Slurry Blowdown FlowRateScrubber SlurryPercent SolidsPercent HydrocloneOverflow RecycledBack to ScrubberFGD Wastewater Treatment Operation During Sample CollectionPlant NameSampleCollectionNumberDate of SampleCollectionScrubber PurgeFlow Rate DuringInfluent SampleCollection(gpm)Unit 1 Unit 2 Unit 3 Daily Power Generation (MW-hrs)

Plant Name Date Provide the daily power generation for each scrubbe d unit starting two weeks prior to the first set of samples through the last set of samplesFGD Wastewater Treatment System Flow

Rates (gpd) Chemical Precipitation Effluent Plant Name Date 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. Secti on 308 provides that, "Whenever required to carry out the objective of this Act, includi ng 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 requ ire the owner or operator of any point source to "establish and maintain such records, . . make s uch 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 informatio n are contained in 40 CFR Part 2, Subpart B. The manner of asserting such a claim is speci fied 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 informat ion 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 inf ormation 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 ma ke a determination as to whether or

not such information is entitled to confidential treatm ent. At that time, EPA will request that you substantiate any claim you have made that information is c onfidential. 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 t reatment (see 40 CFR 2.302).

### Enclosure 3

Notice of Intent to Transfer Confidential Information to Sel ected 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), a nd 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 sampli ng program. Transfer of this information to these contractors is necessary in order for the cont ractors to assist EPA in performing technical, statistical, and environmental analyses to support the development of effluent limitations guidelines and standards for the Steam Electri c Power Generating industry.

The contractors and subcontractors that will be providi ng 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 analysi s 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, yo u 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 noti ce. 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 sig n the Certification Statement listed below. The certifying official must be a responsible co rporate 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/di rty hands sampling techniques described in EPA Method 1669), that qualified personnel gathered t he engineering data required, and that the sampling and engineering data provided are complete and ref lect 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 di d 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 jus tify 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 Numbe r 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 Sampl ing 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 P lant (Hatfield’s Ferry) located in Masontown, PA. ERG was on site for all sample colle ction activities that Hatfield’s Ferry conducted for the second set of the industry self-monitori ng 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 fr om the on-site review. A process flow diagram of the FGD wastewater treatment system at Ha tfield’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 Attachmen t 3.

During this set of the industry self-monitoring, Unit 2 st arted up on Monday, November 8, 2010. All of the units operated throughout the self-monito ring 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 th e secondary hydrocyclone overflow that is transferred to the equalization tank at the beg inning 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 F erry samplers sampled Unit 3’s secondary hydrocyclone overflow for Set 1. Hatfield’s Ferry pers onnel 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 it s sample collection.

### Memorandum

November 15, 2010 Page 2

Sample Collection

To collect the samples of the FGD wastewater treatm ent influent, Hatfield’s Ferry personnel followed EPA Method 1669 protocols and the EPA-provi ded instructions. Hatfield’s Ferry personnel attached one end of the specially-cleane d 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 sample rs let the sample flow from the tap for four minutes prior to collecting any samples. The sampler s then collected the samples underneath the shroud. At this sampling point, Hatfield’s Ferry coll ected 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 c ollected samples for EPA analyses. All samples were filled while the samplers held the bottle s under the shrouding.

Preservation

Hatfield’s Ferry personnel followed all method specificat ions when preserving the classical samples. The Group II samples were preserve d using H 2 

### SO 4 

### and the pH was confirmed to be below 2 S.U. The cyanide sample was checked for sul fides and chlorine using lead acetate paper and potassium iodide starch paper, respectively. The sa mplers did not detect sulfides or chlorine in the samples. The cyanide sample was then pre served using NaOH and the pH was confirmed to be above 10 S.U. The BOD, Group I, Group II, an d cyanide samples were all placed on ice after collection or preservation.

Field Measurements

Hatfield’s Ferry personnel used a pH probe and a thermomete r to measure the pH and temperature of the FGD wastewater influent samples. Hat field’s Ferry personnel filled a small bottle with sample after collecting the classical sa mples and inserted the thermometer and pH probe into the sample bottle. Hatfield’s Ferry person nel stated that they calibrated the pH probe on Tuesday, November 9, 2010; however, ERG did not observe th e 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 t he 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 colle cted during Set 1. Hatfield’s Ferry personnel followed all applicable procedures during the sample collect ion. The field pH measurement was made within 5 minutes of sample collection, but the temper ature 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 class ical 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 wa s 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 sampl es, except for the mercury and cyanide samples. For this sampling point, Hatfield’s Ferry coll ected the samples using the plant’s existing compliance monitoring point. Hatfield’s Ferry i nstalled a 2-way splitter using stainless steel tubing; one of the taps was used to collect the com posite 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 treatm ent effluent stream, Hatfield’s Ferry personnel followed EPA Method 1669 protocols and the EPA-provi ded 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 perpendicu lar end of a T-splitter and two longer pieces of silicone tubing attached to the other two ends o f 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 t he sampling configuration is included as Figure 4 in Attachment 3. The samplers programmed the compo sitor to collect 830 mL of sample every hour for a 24-hour period. After the 24-hour period, th e samplers pumped the sample into the individual sample bottles. Hatfield’s Ferry person nel used a short piece of Teflon® tubing connected to a length of silicone tubing and the pump to tran sfer 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 T eflon® end of the tubing was then inserted into the carboy and the tubing was purged with 0.5 lite rs of sample. A picture of the pump-off set up is included as Figure 5 in Attachment 3. Hatfiel d’s Ferry personnel collected all of the samples using a cleanbox and the multi-fill approac h for all of the samples.

Hatfield’s Ferry personnel also collected grab samples f or mercury every six hours during the sampling. The samplers collected the mercury sample s at this sampling point by shrouding one of their effluent sample taps with a clean plasti c bag and letting sample flow through the sample tap for two minutes prior to collecting any sample s. Hatfield’s Ferry personnel filled the mercury bottles directly from the tap, underneath the s hroud. The samplers collected the mercury samples as multi-fill splits. Hatfield’s Ferry perso nnel 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 incl uded as Figure 6 in Attachment 3.

### Memorandum

November 15, 2010 Page 4

Preservation

Hatfield’s Ferry personnel followed all method specificat ions when preserving the classicals samples, which are the same as those descr ibed 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 thermomete r to measure the pH and temperature of the FGD wastewater effluent samples, whi ch 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 eac h mercury grab was collected, which was every six hours. Hatfield’s Ferry samplers also coll ected 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 t he 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 thi s set. ERG also observed the Grab 1 and 2 mercury grab samples and the cyanide grab sample. Hat field’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 tubi ng 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 ve nted 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 coll ection the 20-liter carboy only

contained 11 L. ERG noted that the flow of the FGD waste water treatment effluent stream, measured with an in-line flow meter, varied from approxima tely 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 m ade because the samplers thought the probe was reading temperature; however, other s amplers indicated that the probe read 25°C because it adjusts the pH reading to standard tempera ture. Hatfield’s Ferry personnel used the correct techniques to preserve the classical sa mples; 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

ChecklistsAttachment 3Pictures from the On-Site ReviewFigure 1. FGD Wastewater Influent (SP-1) Sample Tap with ExtensionFigure 2. FGD Wastewater Influent (SP-1)Sample Tap Extension ConfigurationFigure 3. FGD Wastewater Effluent (SP-2) Sample TapsFigure 4. FGD Wastewater Effluent (SP-2) Composite Sample ConfigurationFigure 5. FGD Wastewater Effluent(SP-2) Pump-Off Configuration

### Figure 6. FGD Wastewater Effluent (S P-2) Mercury Grab Configuration

## Section 3

Signed Certification Statement

## Section 4

Engineering DataTable G4-1. Field Measurements for Sample Collection at the Influent to FGD Wastewater Treatment System, Hatfield’s FerryEpisode NumberSample CollectionNumberDate of SampleCollectionSample CollectionTimeTemperature(°C)pH(S.U.)6571Set 1 - Grab 1 10/5/2010135839.66.256571Set 2 - Grab 1 11/10/20100925426.296571Set 3 - Grab 1 1/12/20110820475.86571Set 4 - Grab 1 2/9/20110753485.8Table G4-2. Field Measurements for SampleCollection at the Effluent from FGD Wastewater Treatment System, Hatfield’s FerryEpisode NumberSample CollectionNumberDate of SampleCollectionSample CollectionTimeTemperature(°C)pH(S.U.)6571Set 1 - Grab 1 10/4/20101722257.876571Set 1 - Grab 2 10/4/20102320267.86571Set 1 - Grab 3 10/5/20100522257.876571Set 1 - Grab 4 10/5/20101116247.526571Set 2 - Grab 1 11/9/20101211256.866571Set 2 - Grab 2 11/9/20101815256.716571Set 2 - Grab 3 11/10/20100015246.776571Set 2 - Grab 4 11/10/20100615277.056571Set 3 - Grab 1 1/11/20111200287.496571Set 3 - Grab 2 1/11/20111800307.556571Set 3 - Grab 3 1/12/20110002257.216571Set 3 - Grab 4 1/12/20110600297.216571Set 4 - Grab 1 2/8/2011120728.07.356571Set 4 - Grab 2 2/8/2011180028.57.376571Set 4 - Grab 3 2/9/2011000527.57.46571Set 4 - Grab 4 2/9/2011060227.07.35Table G4-3. SampleCollection Procedures Used during the Sampling EpisodeEpisodeNumberSampleCollectionNumberUnitOverflowSampledatInfluentInfluentSamplesCollected asGrabs(Yes or No)Mercuryand CyanideSamplesCollected asGrabs(Yes or No)Effluent SamplesCollected as 24-Hour Composites(Yes or No)CleanHands/DirtyHands SamplingTechniques Used(Yes or No)*Description ofSampleCollectionTechnique (ifdifferent thaninstructions)Description ofAbnormal Conditionsin FGD System or FGDWastewater TreatmentSystem that MayImpact Concentrations6571 Set 13Yes Yes Yes Yes None None6571 Set 22Yes Yes Yes Yes None None6571 Set 33Yes Yes Yes Yes None None6571 Set 41Yes Yes Yes Yes None 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 Operationat Time of Sampling, Hatfield’s FerryEpisode NumberSample CollectionNumberDate of SampleCollectionPlant Operation During Sample CollectionUnits OperatingDuring SamplingDayUnits Off-line EntireSampling DaySCRs/SNCRsOperating onUnits6571Set 110/5/2010Unit 3Units 1,2No6571Set 211/10/2010Units 1,2,3NoneNo6571Set 31/12/2010Units 1,2,3NoneNo6571Set 42/9/2010Units 1,2,3NoneNoTable G4-5. FGD Scrubber Slurry Information at Time of Sampling, Hatfield’s FerryEpisodeNumberSampleCollectionNumberDate of SampleCollectionPlant Operation During Sample CollectionScrubber Slurry BlowdownFlow RateScrubberSlurryPercentSolidsPercentHydrocloneOverflow RecycledBack to ScrubberFlow Rate(gpm)Duration6571 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 FerryEpisodeNumberSampleCollectionNumberDate of SampleCollectionScrubber PurgeFlow Rate DuringInfluent SampleCollection(gpm)FGD Wastewater Treatment Operation During Sample CollectionLimeUsage(tons)FerricChlorideUsage(Liters/day)OrganosulfideUsage(Liters/day)Polymer Usage(Liters/day)Acid Usage(Liters/day)6571 Set 110/5/2010 100 2.4 43 11 15 5256571 Set 211/10/2010 100 4 73 18 25 8756571 Set 31/12/2010 110 3.2 58 14 20 7006571 Set 42/9/2010 110 2.4 43 11 15 525Table G4-7. Daily Power Generation Du ring 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 0Table G4-7. Daily Power Generation Du ring 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 6,104Table G4-7. Daily Power Generation Du ring 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 12,519Table G4-8. FGD Wastewater Treatment Syst em 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 134,156Table G4-8. FGD Wastewater Treatment Syst em 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 170,133Table G4-8. FGD Wastewater Treatment Syst em 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 belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 quantitation limit, but at least oneresult 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 FerryAnalyteUnitsMethodInfluent to FGD Wastewater Treatment System (SP-1)Set 1Set 2Set 3Set 44-SetAverageClassicalsAmmonia mg/L 350.1 1.20 1.50 1.00 Est 1.90 B, Est 1.40Nitrate Nitrite as N mg/L 353.2 120 120 150 Est 100 Est 123Nitrogen, TotalKjeldahl mg/L 351.2 28.0 B 47.0 47.0 Est 130 B, Est 63.0Biochemical OxygenDemand mg/L 5210B NQ (2.50) s NQ (2.50) 45.0 70.0 < 29.4Chemical OxygenDemand mg/L 410.4 230 140 490 Est 500 Est 340Chloride mg/L 300.0 5,000 4,700 8,400 7,500 6,400Sulfate mg/L 300.0 8,700 6,500 7,700 11,000 8,480Cyanide, Total mg/L 4500 CN E ND (0.100) 0.360 2.70 0.480 < 0.898Total Dissolved Solids mg/L 2540C 34,000 B 23,000 28,000 31,000 29,000Total Suspended Solids mg/L 2540D 38,000 50,000 54,000 33,000 43,800Phosphorus, Total mg/L 365.1 NQ (0.0500) 0.700 B 2.60 B, Est NQ (0.0500) < 0.838Total MetalsAluminum ug/L 200.7 580,000 B,^ 470,000 1,100,000 B 630,000 B 695,000Antimony ug/L 200.8 18.0 20.0 8.60 29.0 18.9Arsenic ug/L 200.8 550 300 630 1,000 620Barium ug/L 200.7 460 3,000 830 1,300 B 1,400Beryllium ug/L 200.7 34.0 16.0 56.0 34.0 35.0Boron ug/L 200.7 280,000 160,000 B 320,000 B 290,000 B 263,000< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 quantitation limit, but at least oneresult 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 FerryAnalyteUnitsMethodInfluent to FGD Wastewater Treatment System (SP-1)Set 1Set 2Set 3Set 44-SetAverageCadmium ug/L 200.8 340 290 540 490 415Calcium ug/L 200.7 4,000,000 4,200,000 5,300,000 B 3,400,000 B 4,230,000Chromium ug/L 200.8 1,500 1,300 ^ 3,100 3,200 2,280Cobalt ug/L 200.7 330 250 800 550 483Copper ug/L 200.8 680 540 1,400 1,100 930Iron ug/L 200.7 710,000 540,000 1,400,000 1,300,000 988,000Lead ug/L 200.8 250 240 130 650 318Magnesium ug/L 200.7 4,400,000 3,600,000 5,400,000 B 5,400,000 B 4,700,000Manganese ug/L 200.7 66,000 39,000 100,000 B 140,000 B 86,300Mercury ng/L 1631E 247,000 184,000 413,000 289,000 283,000Molybdenum ug/L 200.7 530 230 760 620 535Nickel ug/L 200.8 2,100 1,400 2,200 2,200 1,980Selenium ug/L 200.8 1,400 1,100 510 1,200 1,050Silver ug/L 200.8 NQ (2.00) NQ (2.00) 5.50 4.70 < 3.05Sodium ug/L 200.7 490,000 350,000 430,000 B 360,000 B 408,000Thallium ug/L 200.8 43.0 24.0 100 70.0 59.3Tin ug/L 200.7 NQ (200) NQ (200) NQ (500) NQ (500) NQ (350)Titanium ug/L 200.7 9,900 6,700 22,000 9,900 12,100Vanadium ug/L 200.8 1,300 1,100 2,500 3,300 2,050Zinc ug/L 200.7 9,300 6,100 21,000 16,000 B 13,100< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 quantitation limit, but at least oneresult 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 FerryAnalyteUnitsMethodEffluent from FGD Wastewater Treatment System (SP-2)Set 1Set 2Set 3Set 44-SetAverageClassicalsAmmonia mg/L 350.1 NQ (1.00) NQ (1.00) NQ (1.00) 1.10 B < 0.650Nitrate Nitrite as N mg/L 353.2 130 86.0 150 Est 83.0 112Nitrogen, Total Kjeldahl mg/L 351.2 25.0 B 5.40 16.0 Est 28.0 B,4 18.6Biochemical OxygenDemand mg/L 5210B ND (2.00) NQ (2.50) 4.00 3.00 < 2.31Chemical OxygenDemand mg/L 410.4 250 130 460 Est 380 F 305Chloride mg/L 300.0 6,300 2,900 8,100 8,200 6,380Sulfate mg/L 300.0 5,200 3,800 4,700 4,500 4,550Cyanide, Total mg/L 4500 CN E ND (0.100) NQ (0.100) F 0.270 0.110 F < 0.120Total Dissolved Solids mg/L 2540C 20,000 B 10,000 19,000 18,000 16,800Total Suspended Solids mg/L 2540D 4.40 NQ (4.00) NQ (4.00) NQ (4.00) < 2.60Phosphorus, Total mg/L 365.1 NQ (0.0500) NQ (0.0500) B 0.0700 B,F, Est 0.0560 F, Est < 0.0440Total MetalsAluminum ug/L 200.7 480 B ND (200) ^ ND (200) ND (200) < 195Antimony ug/L 200.8 5.70 3.90 12.0 13.0 8.65Arsenic ug/L 200.8 NQ (4.00) NQ (4.00) 11.0 10.0 < 6.25Barium ug/L 200.7 110 88.0 170 220 B 147Beryllium ug/L 200.7 ND (2.00) ND (2.00) ND (2.00) ND (2.00) ND (2.00)Boron ug/L 200.7 160,000 80,000 B,4 240,000 B 220,000 B,4 175,000Cadmium ug/L 200.8 ND (4.00) NQ (4.00) NQ (4.00) 13.0 < 4.75< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 quantitation limit, but at least oneresult 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 FerryAnalyteUnitsMethodEffluent from FGD Wastewater Treatment System (SP-2)Set 1Set 2Set 3Set 44-SetAverageCalcium ug/L 200.7 1,400,000 1,000,000 4 1,500,000 B 1,600,000 B,4 1,380,000Chromium ug/L 200.8 14.0 18.0 ^ ND (8.00) ND (8.00) < 10.0Cobalt ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND (20.0) ND (20.0)Copper ug/L 200.8 NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.00) NQ (4.00)Iron ug/L 200.7 NQ (200) NQ (200) NQ (200) 260 < 140Lead ug/L 200.8 ND (2.00) ND (2.00) ND (2.00) ND (2.00) ND (2.00)Magnesium ug/L 200.7 3,100,000 1,600,000 4 3,100,000 B 3,200,000 B,4 2,750,000Manganese ug/L 200.7 800 NQ (20.0) 9,600 B 11,000 B,4 < 5,350Mercury ng/L 1631E 978 228 77.5 82.5 342Molybdenum ug/L 200.7 350 100 450 590 373Nickel ug/L 200.8 7.80 NQ (4.00) 6.50 5.50 < 5.45Selenium ug/L 200.8 750 610 4 880 580 4 705Silver ug/L 200.8 ND (2.00) ND (2.00) F ND (2.00) ND (2.00) F ND (2.00)Sodium ug/L 200.7 690,000 300,000 4 410,000 B 520,000 B,4 480,000Thallium ug/L 200.8 7.00 2.90 11.0 17.0 9.48Tin ug/L 200.7 ND (200) ND (200) ND (200) ND (200) ND (200)Titanium ug/L 200.7 ND (20.0) ND (20.0) ND (20.0) ND (20.0) ND (20.0)Vanadium ug/L 200.8 21.0 10.0 31.0 24.0 21.5Zinc ug/L 200.7 ND (40.0) NQ (40.0) ND (40.0) ND (40.0) NQ (40.0)< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).Table G5-3. Classical Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment System, HatieldsFerryAnalyteUnitMethodInfluent to FGDWastewater TreatmentSystem (SP-1)4-Set AverageEffluent from FGDWastewater TreatmentSystem (SP-2)4-Set AverageClassicalsAmmonia mg/L 350.1 1.40 < 0.650Nitrate Nitrite as N mg/L 353.2 123 112Nitrogen, Total Kjeldahl mg/L 351.2 63.0 18.6Biochemical Oxygen Demand mg/L 5210B < 29.4 < 2.31Chemical Oxygen Demand mg/L 410.4 340 305Chloride mg/L 300.0 6,400 6,380Sulfate mg/L 300.0 8,480 4,550Cyanide, Total mg/L 4500 CN E < 0.898 < 0.120Total Dissolved Solids mg/L 2540C 29,000 16,800Total Suspended Solids mg/L 2540D 43,800 < 2.60Phosphorus, Total mg/L 365.1 < 0.838 < 0.0440< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 quantitation limit, but at least oneresult is a J-value.Table G5-4. Metals Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment System,Hatfield’s FerryAnalyteUnitMethodInfluent to FGD WastewaterTreatment System (SP-1)4-Set AverageEffluent from FGD WastewaterTreatment System (SP-2)4-Set AverageTotal MetalsAluminum ug/L 200.7 695,000 < 195Antimony ug/L 200.8 18.9 8.65Arsenic ug/L 200.8 620 < 6.25Barium ug/L 200.7 1,400 147Beryllium ug/L 200.7 35.0 ND (2.00)Boron ug/L 200.7 263,000 175,000Cadmium ug/L 200.8 415 < 4.75Calcium ug/L 200.7 4,230,000 1,380,000Chromium ug/L 200.8 2,280 < 10.0Cobalt ug/L 200.7 483 ND (20.0)Copper ug/L 200.8 930 NQ (4.00)Iron ug/L 200.7 988,000 < 140Lead ug/L 200.8 318 ND (2.00)Magnesium ug/L 200.7 4,700,000 2,750,000Manganese ug/L 200.7 86,300 < 5,350Mercury ng/L 1631E 283,000 342Molybdenum ug/L 200.7 535 373Nickel ug/L 200.8 1,980 < 5.45Selenium ug/L 200.8 1,050 705Silver ug/L 200.8 < 3.05 ND (2.00)< - Average result includes at least one value measured belowthe quantitation limit. (Calculation uses 1⁄2 the quantitation limit for values below the quantitation limit).ND – Not detected (number in parentheses is the quantitation limit).NQ – Analyte was measured above the method detection limit, butbelow the quantitation limit (number shown in parentheses is the quantitation limit). The analytical result ispresented 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 quantitation limit, but at least oneresult is a J-value.Table G5-4. Metals Pollutants 4-Set Average Data Summary for FGD Wastewater Treatment System,Hatfield’s FerryAnalyteUnitMethodInfluent to FGD WastewaterTreatment System (SP-1)4-Set AverageEffluent from FGD WastewaterTreatment System (SP-2)4-Set AverageSodium ug/L 200.7 408,000 480,000Thallium ug/L 200.8 59.3 9.48Tin 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 21.5Zinc ug/L 200.7 13,100 NQ (40.0)

### Table G5-5. Field Blank Analyt ical 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 0.650ND – 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, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1 mg/L 1 0.055 1 1.2Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 120Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.38 5 28 BBiochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 2.2 J,sChemical Oxygen Demand 410.4 mg/L 2 8.1 40 230Chloride 300.0 mg/L 200 51 600 5,000Sulfate 300.0 mg/L 500 120 2,500 8,700Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 ND (0.1) UTotal Dissolved Solids 2540C mg/L 1 160 330 34,000 BTotal Suspended Solids 2540D mg/L 1 140 500 38,000Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.015 JTotal MetalsAluminum 200.7 ug/L 2 9.4 200 580,000 B,^Antimony 200.8 ug/L 2 0.72 2 18Arsenic 200.8 ug/L 10 6.1 20 550Barium 200.7 ug/L 2 2.5 20 460Beryllium 200.7 ug/L 2 0.71 2 34Boron 200.7 ug/L 250 830 25,000 280,000Cadmium 200.8 ug/L 2 1.2 4 340Calcium 200.7 ug/L 50 1,700 10,000 4,000,000Chromium 200.8 ug/L 2 3.3 8 1,500ND – 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, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCobalt 200.7 ug/L 2 1.1 20 330Copper 200.8 ug/L 2 0.96 4 680Iron 200.7 ug/L 2 32 200 710,000Lead 200.8 ug/L 2 0.73 2 250Magnesium 200.7 ug/L 50 540 10,000 4,400,000Manganese 200.7 ug/L 50 13 500 66,000Mercury 1631E ng/L 10,000 2,410 5,050 247,000Molybdenum 200.7 ug/L 2 1.6 40 530Nickel 200.8 ug/L 2 0.89 4 2,100Selenium 200.8 ug/L 10 3.1 20 1,400Silver 200.8 ug/L 2 0.59 2 1.7 JSodium 200.7 ug/L 2 180 10,000 490,000Thallium 200.8 ug/L 2 0.47 2 43Tin 200.7 ug/L 2 4.8 200 98 JTitanium 200.7 ug/L 2 1.6 20 9,900Vanadium 200.8 ug/L 2 1.7 10 1,300Zinc 200.7 ug/L 2 9.1 40 9,300^ - 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, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1 mg/L 1 0.055 1 1.5Nitrate Nitrite as N 353.2 mg/L 20 0.38 2 120Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 47Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 2 JChemical Oxygen Demand 410.4 mg/L 2 8.1 40 140Chloride 300.0 mg/L 200 51 600 4,700Sulfate 300.0 mg/L 200 46 1,000 6,500Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.36Total Dissolved Solids 2540C mg/L 1 470 1,000 23,000Total Suspended Solids 2540D mg/L 1 140 500 50,000Phosphorus, Total 365.1 mg/L 5 0.025 0.25 0.7 BTotal MetalsAluminum 200.7 ug/L 50 240 5,000 470,000Antimony 200.8 ug/L 2 0.72 2 20Arsenic 200.8 ug/L 5 3.1 10 300Barium 200.7 ug/L 2 2.5 20 3,000Beryllium 200.7 ug/L 2 0.71 2 16Boron 200.7 ug/L 50 170 5,000 160,000 BCadmium 200.8 ug/L 2 1.2 4 290Calcium 200.7 ug/L 50 1,700 10,000 4,200,000Chromium 200.8 ug/L 2 3.3 8 1,300 ^Cobalt 200.7 ug/L 2 1.1 20 250Copper 200.8 ug/L 2 0.96 4 540^ - 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, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationIron 200.7 ug/L 50 800 5,000 540,000Lead 200.8 ug/L 2 0.73 2 240Magnesium 200.7 ug/L 50 540 10,000 3,600,000Manganese 200.7 ug/L 2 0.51 20 39,000Mercury 1631E ng/L 40,000 9,940 20,800 184,000Molybdenum 200.7 ug/L 2 1.6 40 230Nickel 200.8 ug/L 2 0.89 4 1,400Selenium 200.8 ug/L 5 1.6 10 1,100Silver 200.8 ug/L 2 0.59 2 1.3 JSodium 200.7 ug/L 2 180 10,000 350,000Thallium 200.8 ug/L 2 0.47 2 24Tin 200.7 ug/L 2 4.8 200 38 JTitanium 200.7 ug/L 2 1.6 20 6,700Vanadium 200.8 ug/L 2 1.7 10 1,100Zinc 200.7 ug/L 2 9.1 40 6,100B – 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’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1 mg/L 1 0.055 1 1 EstNitrate Nitrite as N 353.2 mg/L 50 0.95 5 150 EstNitrogen, Total Kjeldahl 351.2 mg/L 10 0.77 10 47 EstBiochemical Oxygen Demand 5210B mg/L 1 2.8 24 45Chemical Oxygen Demand 410.4 mg/L 5 20 100 490 EstChloride 300.0 mg/L 200 51 600 8,400Sulfate 300.0 mg/L 200 46 1,000 7,700Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 2.7Total Dissolved Solids 2540C mg/L 1 160 330 28,000Total Suspended Solids 2540D mg/L 1 140 500 54,000Phosphorus, Total 365.1 mg/L 5 0.025 0.25 2.6 B, EstTotal MetalsAluminum 200.7 ug/L 50 240 5,000 1,100,000 BAntimony 200.8 ug/L 2 0.72 2 8.6Arsenic 200.8 ug/L 2 1.2 4 630Barium 200.7 ug/L 50 62 500 830Beryllium 200.7 ug/L 5 1.8 5 56Boron 200.7 ug/L 50 170 5,000 320,000 BCadmium 200.8 ug/L 2 1.2 4 540Calcium 200.7 ug/L 50 1,700 10,000 5,300,000 BChromium 200.8 ug/L 2 3.3 8 3,100Cobalt 200.7 ug/L 50 29 500 800Copper 200.8 ug/L 2 0.96 4 1,400B – 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’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationIron 200.7 ug/L 50 800 5,000 1,400,000Lead 200.8 ug/L 2 0.73 2 130Magnesium 200.7 ug/L 50 540 10,000 5,400,000 BManganese 200.7 ug/L 50 13 500 100,000 BMercury 1631E ng/L 20,000 4,970 10,400 413,000Molybdenum 200.7 ug/L 5 4 100 760Nickel 200.8 ug/L 2 0.89 4 2,200Selenium 200.8 ug/L 2 0.62 4 510Silver 200.8 ug/L 2 0.59 2 5.5Sodium 200.7 ug/L 50 4,600 250,000 430,000 BThallium 200.8 ug/L 2 0.47 2 100Tin 200.7 ug/L 5 12 500 150 JTitanium 200.7 ug/L 50 41 500 22,000Vanadium 200.8 ug/L 2 1.7 10 2,500Zinc 200.7 ug/L 50 230 1,000 21,000B – 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, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1 mg/L 1 0.055 1 1.9 B, EstNitrate Nitrite as N 353.2 mg/L 20 0.38 2 100 EstNitrogen, Total Kjeldahl 351.2 mg/L 10 3.8 50 130 B, EstBiochemical Oxygen Demand 5210B mg/L 1 2.8 24 70Chemical Oxygen Demand 410.4 mg/L 5 20 100 500 EstChloride 300.0 mg/L 500 130 1,500 7,500Sulfate 300.0 mg/L 500 120 2,500 11,000Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.48Total Dissolved Solids 2540C mg/L 1 240 500 31,000Total Suspended Solids 2540D mg/L 1 280 1,000 33,000Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.0076 JTotal MetalsAluminum 200.7 ug/L 5 24 500 630,000 BAntimony 200.8 ug/L 2 0.72 2 29Arsenic 200.8 ug/L 2 1.2 4 1,000Barium 200.7 ug/L 5 6.2 50 1,300 BBeryllium 200.7 ug/L 5 1.8 5 34Boron 200.7 ug/L 50 170 5,000 290,000 BCadmium 200.8 ug/L 2 1.2 4 490Calcium 200.7 ug/L 50 1,700 10,000 3,400,000 BChromium 200.8 ug/L 2 3.3 8 3,200Cobalt 200.7 ug/L 5 2.9 50 550Copper 200.8 ug/L 2 0.96 4 1,100B – 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, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationIron 200.7 ug/L 5 80 500 1,300,000Lead 200.8 ug/L 2 0.73 2 650Magnesium 200.7 ug/L 50 540 10,000 5,400,000 BManganese 200.7 ug/L 50 13 500 140,000 BMercury 1631E ng/L 400,000 96,500 202,000 289,000Molybdenum 200.7 ug/L 5 4 100 620Nickel 200.8 ug/L 2 0.89 4 2,200Selenium 200.8 ug/L 2 0.62 4 1,200Silver 200.8 ug/L 2 0.59 2 4.7Sodium 200.7 ug/L 5 460 25,000 360,000 BThallium 200.8 ug/L 2 0.47 2 70Tin 200.7 ug/L 5 12 500 110 JTitanium 200.7 ug/L 5 4.1 50 9,900Vanadium 200.8 ug/L 2 1.7 10 3,300Zinc 200.7 ug/L 5 23 100 16,000 BND – 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 TreatmentSystem, Set 1 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1 mg/L 1 0.055 1 0.85 JNitrate Nitrite as N 353.2 mg/L 20 0.38 2 130Nitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 25 BBiochemical Oxygen Demand 5210B mg/L 1 0.24 2 ND (2) UChemical Oxygen Demand 410.4 mg/L 2 8.1 40 250Chloride 300.0 mg/L 500 130 1,500 6,300Sulfate 300.0 mg/L 500 120 2,500 5,200Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 ND (0.1) UTotal Dissolved Solids 2540C mg/L 1 47 100 20,000 BTotal Suspended Solids 2540D mg/L 1 1.1 4 4.4Phosphorus, Total 365.1 mg/L 1 0.005 0.05 0.033 JTotal MetalsAluminum 200.7 ug/L 2 9.4 200 480 BAntimony 200.8 ug/L 2 0.72 2 5.7Arsenic 200.8 ug/L 2 1.2 4 3.9 JBarium 200.7 ug/L 2 2.5 20 110Beryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 250 830 25,000 160,000Cadmium 200.8 ug/L 2 1.2 4 ND (4) UCalcium 200.7 ug/L 50 1,700 10,000 1,400,000Chromium 200.8 ug/L 2 3.3 8 14Cobalt 200.7 ug/L 2 1.1 20 ND (20) UND – 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 TreatmentSystem, Set 1 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCopper 200.8 ug/L 2 0.96 4 1.4 JIron 200.7 ug/L 2 32 200 160 JLead 200.8 ug/L 2 0.73 2 ND (2) UMagnesium 200.7 ug/L 50 540 10,000 3,100,000Manganese 200.7 ug/L 2 0.51 20 800Mercury 1631E ng/L 200 48.3 101 978Molybdenum 200.7 ug/L 2 1.6 40 350Nickel 200.8 ug/L 2 0.89 4 7.8Selenium 200.8 ug/L 2 0.62 4 750Silver 200.8 ug/L 2 0.59 2 ND (2) USodium 200.7 ug/L 2 180 10,000 690,000Thallium 200.8 ug/L 2 0.47 2 7Tin 200.7 ug/L 2 4.8 200 ND (200) UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 21Zinc 200.7 ug/L 2 9.1 40 ND (40) UND – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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 TreatmentSystem, Set 2 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1 mg/L 1 0.055 1 0.94 JNitrate Nitrite as N 353.2 mg/L 10 0.19 1 86Nitrogen, Total Kjeldahl 351.2 mg/L 1 0.077 1 5.4Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 2.1 JChemical Oxygen Demand 410.4 mg/L 2 8.1 40 130Chloride 300.0 mg/L 200 51 600 2,900Sulfate 300.0 mg/L 200 46 1,000 3,800Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.082 J,FTotal Dissolved Solids 2540C mg/L 1 47 100 10,000Total Suspended Solids 2540D mg/L 1 1.1 4 2.8 JPhosphorus, Total 365.1 mg/L 1 0.005 0.05 0.006 J,BTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) U,^Antimony 200.8 ug/L 2 0.72 2 3.9Arsenic 200.8 ug/L 2 1.2 4 2.8 JBarium 200.7 ug/L 2 2.5 20 88Beryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 50 170 5,000 80,000 B,4Cadmium 200.8 ug/L 2 1.2 4 1.5 JCalcium 200.7 ug/L 50 1,700 10,000 1,000,000 4ND – 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 laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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 TreatmentSystem, Set 2 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationChromium 200.8 ug/L 2 3.3 8 18 ^Cobalt 200.7 ug/L 2 1.1 20 ND (20) UCopper 200.8 ug/L 2 0.96 4 1.1 JIron 200.7 ug/L 2 32 200 33 JLead 200.8 ug/L 2 0.73 2 ND (2) UMagnesium 200.7 ug/L 50 540 10,000 1,600,000 4Manganese 200.7 ug/L 2 0.51 20 8.4 JMercury 1631E ng/L 100 24.4 51 228Molybdenum 200.7 ug/L 2 1.6 40 100Nickel 200.8 ug/L 2 0.89 4 3.9 JSelenium 200.8 ug/L 2 0.62 4 610 4Silver 200.8 ug/L 2 0.59 2 ND (2) U,FSodium 200.7 ug/L 2 180 10,000 300,000 4Thallium 200.8 ug/L 2 0.47 2 2.9Tin 200.7 ug/L 2 4.8 200 ND (200) UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 10Zinc 200.7 ug/L 2 9.1 40 11 JND – 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 TreatmentSystem, Set 3 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1 mg/L 1 0.055 1 0.37 JNitrate Nitrite as N 353.2 mg/L 50 0.95 5 150 EstNitrogen, Total Kjeldahl 351.2 mg/L 5 0.38 5 16 EstBiochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 4Chemical Oxygen Demand 410.4 mg/L 5 20 100 460 EstChloride 300.0 mg/L 200 51 600 8,100Sulfate 300.0 mg/L 200 46 1,000 4,700Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.27Total Dissolved Solids 2540C mg/L 1 94 200 19,000Total Suspended Solids 2540D mg/L 1 1.1 4 2.8 JPhosphorus, Total 365.1 mg/L 1 0.005 0.05 0.07 B,F, EstTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) UAntimony 200.8 ug/L 2 0.72 2 12Arsenic 200.8 ug/L 2 1.2 4 11Barium 200.7 ug/L 2 2.5 20 170Beryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 50 170 5,000 240,000 BCadmium 200.8 ug/L 2 1.2 4 1.4 JCalcium 200.7 ug/L 50 1,700 10,000 1,500,000 BChromium 200.8 ug/L 2 3.3 8 ND (8) UND – 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 TreatmentSystem, Set 3 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationCobalt 200.7 ug/L 2 1.1 20 ND (20) UCopper 200.8 ug/L 2 0.96 4 1.7 JIron 200.7 ug/L 2 32 200 58 JLead 200.8 ug/L 2 0.73 2 ND (2) UMagnesium 200.7 ug/L 50 540 10,000 3,100,000 BManganese 200.7 ug/L 2 0.51 20 9,600 BMercury 1631E ng/L 100 24.8 52 77.5Molybdenum 200.7 ug/L 2 1.6 40 450Nickel 200.8 ug/L 2 0.89 4 6.5Selenium 200.8 ug/L 2 0.62 4 880Silver 200.8 ug/L 2 0.59 2 ND (2) USodium 200.7 ug/L 2 180 10,000 410,000 BThallium 200.8 ug/L 2 0.47 2 11Tin 200.7 ug/L 2 4.8 200 ND (200) UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 31Zinc 200.7 ug/L 2 9.1 40 ND (40) UND – Not detected (number in parentheses is the quantitation limit).4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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 TreatmentSystem, Set 4 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationClassicalsAmmonia 350.1 mg/L 1 0.055 1 1.1 BNitrate Nitrite as N 353.2 mg/L 10 0.19 1 83Nitrogen, Total Kjeldahl 351.2 mg/L 10 0.77 10 28 B,4Biochemical Oxygen Demand 5210B mg/L 1 0.3 2.5 3Chemical Oxygen Demand 410.4 mg/L 5 20 100 380 FChloride 300.0 mg/L 200 51 600 8,200Sulfate 300.0 mg/L 200 46 1,000 4,500Cyanide, Total 4500 CN E mg/L 1 0.02 0.1 0.11 FTotal Dissolved Solids 2540C mg/L 1 94 200 18,000Total Suspended Solids 2540D mg/L 1 1.1 4 1.6 JPhosphorus, Total 365.1 mg/L 1 0.005 0.05 0.056 F, EstTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) UAntimony 200.8 ug/L 2 0.72 2 13Arsenic 200.8 ug/L 2 1.2 4 10Barium 200.7 ug/L 2 2.5 20 220 BBeryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 50 170 5,000 220,000 B,4Cadmium 200.8 ug/L 2 1.2 4 13Calcium 200.7 ug/L 50 1,700 10,000 1,600,000 B,4ND – Not detected (number in parentheses is the quantitation limit).4 – MS and/or MSD did not meet laboratorycriteria, but sample concentration is fourtimes greater thanthe matrix spike amount, so control limits are not applicable.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 TreatmentSystem, Set 4 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationChromium 200.8 ug/L 2 3.3 8 ND (8) UCobalt 200.7 ug/L 2 1.1 20 ND (20) UCopper 200.8 ug/L 2 0.96 4 1.6 JIron 200.7 ug/L 2 32 200 260Lead 200.8 ug/L 2 0.73 2 ND (2) UMagnesium 200.7 ug/L 50 540 10,000 3,200,000 B,4Manganese 200.7 ug/L 2 0.51 20 11,000 B,4Mercury 1631E ng/L 100 24.8 52 82.5Molybdenum 200.7 ug/L 2 1.6 40 590Nickel 200.8 ug/L 2 0.89 4 5.5Selenium 200.8 ug/L 2 0.62 4 580 4Silver 200.8 ug/L 2 0.59 2 ND (2) U,FSodium 200.7 ug/L 2 180 10,000 520,000 B,4Thallium 200.8 ug/L 2 0.47 2 17Tin 200.7 ug/L 2 4.8 200 ND (200) UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 24Zinc 200.7 ug/L 2 9.1 40 ND (40) UND – 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 TreatmentSystem Field Blank, Set1 Analytical Results,Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 12 J,B,^Antimony 200.8 ug/L 2 0.72 2 ND (2) UArsenic 200.8 ug/L 2 1.2 4 ND (4) UBarium 200.7 ug/L 2 2.5 20 ND (20) UBeryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 2 6.7 200 14 JCadmium 200.8 ug/L 2 1.2 4 ND (4) UCalcium 200.7 ug/L 2 69 400 ND (400) UChromium 200.8 ug/L 2 3.3 8 ND (8) UCobalt 200.7 ug/L 2 1.1 20 ND (20) UCopper 200.8 ug/L 2 0.96 4 ND (4) UIron 200.7 ug/L 2 32 200 ND (200) ULead 200.8 ug/L 2 0.73 2 ND (2) UMagnesium 200.7 ug/L 2 21 400 61 JManganese 200.7 ug/L 2 0.51 20 0.98 JMercury 1631E ng/L 1 0.24 0.5 0.65Molybdenum 200.7 ug/L 2 1.6 40 ND (40) UNickel 200.8 ug/L 2 0.89 4 ND (4) USelenium 200.8 ug/L 2 0.62 4 ND (4) USilver 200.8 ug/L 2 0.59 2 ND (2) USodium 200.7 ug/L 2 180 10,000 ND (10,000) UND – 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 TreatmentSystem Field Blank, Set1 Analytical Results,Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationThallium 200.8 ug/L 2 0.47 2 ND (2) UTin 200.7 ug/L 2 4.8 200 ND (200) UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 ND (10) UZinc 200.7 ug/L 2 9.1 40 ND (40) U.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 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 16 J,B,^Antimony 200.8 ug/L 2 0.72 2 ND (2) UArsenic 200.8 ug/L 2 1.2 4 ND (4) UBarium 200.7 ug/L 2 2.5 20 ND (20) UBeryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 2 6.7 200 19 JCadmium 200.8 ug/L 2 1.2 4 ND (4) UCalcium 200.7 ug/L 2 69 400 ND (400) UChromium 200.8 ug/L 2 3.3 8 ND (8) UCobalt 200.7 ug/L 2 1.1 20 ND (20) UCopper 200.8 ug/L 2 0.96 4 ND (4) UIron 200.7 ug/L 2 32 200 ND (200) ULead 200.8 ug/L 2 0.73 2 ND (2) UMagnesium 200.7 ug/L 2 21 400 49 JManganese 200.7 ug/L 2 0.51 20 ND (20) UMercury 1631E ng/L 1 0.24 0.5 ND (0.5) UMolybdenum 200.7 ug/L 2 1.6 40 ND (40) UNickel 200.8 ug/L 2 0.89 4 ND (4) USelenium 200.8 ug/L 2 0.62 4 ND (4) USilver 200.8 ug/L 2 0.59 2 ND (2) USodium 200.7 ug/L 2 180 10,000 ND (10,000) UND – 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 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationThallium 200.8 ug/L 2 0.47 2 ND (2) UTin 200.7 ug/L 2 4.8 200 ND (200) UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 ND (10) UZinc 200.7 ug/L 2 9.1 40 ND (40) UND – 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 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) U,^Antimony 200.8 ug/L 2 0.72 2 ND (2) UArsenic 200.8 ug/L 2 1.2 4 ND (4) UBarium 200.7 ug/L 2 2.5 20 ND (20) UBeryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 2 6.7 200 22 J,BCadmium 200.8 ug/L 2 1.2 4 ND (4) UCalcium 200.7 ug/L 2 69 400 ND (400) UChromium 200.8 ug/L 2 3.3 8 ND (8) U,^Cobalt 200.7 ug/L 2 1.1 20 ND (20) UCopper 200.8 ug/L 2 0.96 4 ND (4) UIron 200.7 ug/L 2 32 200 ND (200) ULead 200.8 ug/L 2 0.73 2 ND (2) UMagnesium 200.7 ug/L 2 21 400 25 JManganese 200.7 ug/L 2 0.51 20 ND (20) UMercury 1631E ng/L 1 0.24 0.5 ND (0.5) UMolybdenum 200.7 ug/L 2 1.6 40 ND (40) UNickel 200.8 ug/L 2 0.89 4 ND (4) USelenium 200.8 ug/L 2 0.62 4 ND (4) USilver 200.8 ug/L 2 0.59 2 1.3 JSodium 200.7 ug/L 2 180 10,000 ND (10,000) UND – 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 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationThallium 200.8 ug/L 2 0.47 2 ND (2) UTin 200.7 ug/L 2 4.8 200 ND (200) UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 ND (10) UZinc 200.7 ug/L 2 9.1 40 ND (40) UND – 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 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) UAntimony 200.8 ug/L 2 0.72 2 ND (2) UArsenic 200.8 ug/L 2 1.2 4 ND (4) UBarium 200.7 ug/L 2 2.5 20 ND (20) UBeryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 2 6.7 200 35 J,BCadmium 200.8 ug/L 2 1.2 4 ND (4) UCalcium 200.7 ug/L 2 69 400 75 J,BChromium 200.8 ug/L 2 3.3 8 ND (8) UCobalt 200.7 ug/L 2 1.1 20 ND (20) UCopper 200.8 ug/L 2 0.96 4 ND (4) UIron 200.7 ug/L 2 32 200 ND (200) ULead 200.8 ug/L 2 0.73 2 ND (2) UMagnesium 200.7 ug/L 2 21 400 61 J,BManganese 200.7 ug/L 2 0.51 20 1.3 J,BMercury 1631E ng/L 1 0.24 0.5 ND (0.5) UMolybdenum 200.7 ug/L 2 1.6 40 ND (40) UNickel 200.8 ug/L 2 0.89 4 ND (4) USelenium 200.8 ug/L 2 0.62 4 ND (4) USilver 200.8 ug/L 2 0.59 2 ND (2) USodium 200.7 ug/L 2 180 10,000 ND (10,000) UND – 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 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationThallium 200.8 ug/L 2 0.47 2 ND (2) UTin 200.7 ug/L 2 4.8 200 ND (200) UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 ND (10) UZinc 200.7 ug/L 2 9.1 40 ND (40) UND – 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 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationTotal MetalsAluminum 200.7 ug/L 2 9.4 200 ND (200) UAntimony 200.8 ug/L 2 0.72 2 ND (2) UArsenic 200.8 ug/L 2 1.2 4 ND (4) UBarium 200.7 ug/L 2 2.5 20 ND (20) UBeryllium 200.7 ug/L 2 0.71 2 ND (2) UBoron 200.7 ug/L 2 6.7 200 37 J,BCadmium 200.8 ug/L 2 1.2 4 ND (4) UCalcium 200.7 ug/L 2 69 400 ND (400) UChromium 200.8 ug/L 2 3.3 8 ND (8) UCobalt 200.7 ug/L 2 1.1 20 ND (20) UCopper 200.8 ug/L 2 0.96 4 ND (4) UIron 200.7 ug/L 2 32 200 ND (200) ULead 200.8 ug/L 2 0.73 2 ND (2) UMagnesium 200.7 ug/L 2 21 400 ND (400) UManganese 200.7 ug/L 2 0.51 20 ND (20) UMercury 1631E ng/L 1 0.24 0.5 ND (0.5) UMolybdenum 200.7 ug/L 2 1.6 40 ND (40) UNickel 200.8 ug/L 2 0.89 4 ND (4) USelenium 200.8 ug/L 2 0.62 4 ND (4) USilver 200.8 ug/L 2 0.59 2 ND (2) USodium 200.7 ug/L 2 180 10,000 ND (10,000) UND – 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 AnalyticalResults, Hatfield’s FerryAnalyteMethodUnitDilutionFactorSampleSpecific MDLSample-Specific QLConcentrationThallium 200.8 ug/L 2 0.47 2 ND (2) UTin 200.7 ug/L 2 4.8 200 ND (200) UTitanium 200.7 ug/L 2 1.6 20 ND (20) UVanadium 200.8 ug/L 2 1.7 10 ND (10) UZinc 200.7 ug/L 2 9.1 40 ND (40) U

## 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 M onitoring Month 1 (Part 2)

Frontier Global Sciences (FGS) generated analytical da ta for total mercury. FGS analyzed the samples according to EPA Method 1631E for merc ury by Cold Vapor Atomic Fluorescence Spectrometry (CVAFS) analysis.

Table 1 summarizes the 20 samples (excluding laboratory pre p 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 a dditional 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 analysi s day. The initial calibration for the CVAFS analysis consisted of a blank and five calibrat ion standards with a correlation

coefficient ≥ 0.995. All method-specified criteria were met.

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

All initial and continuing calibration verifications (I CVs, CCVs) met method-specified

criteria.

BLANKS

All the preparation blanks or laboratory reagent blanks (L RBs) 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 sa mpling episodes. One sample was analyzed in duplicate at the laboratory, sample 71999. The r elative percent difference (RPD) for sample 71999 was 1.31%. The laboratory’s RPD cr iteria between analytical duplicates is 24%.

LABORATORY CONTROL SAMPLES

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

and 24% RPD.

### 3

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

Matrix spikes (MS) and matrix spike duplicates (MSD) we re 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, EP A 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, thalliumand vanadium) for these longterm monitoring samples. The samples were analyzed accor ding to EPA Method 200.8.

Table 1 summarizes the samples TestAmerica extracted a nd 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 accor ding to TestAmerica’s “FGD ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Elements Analysis in Flue Gas Desulfurization Wastewaters,” date d October 6, 2010, based on EPA Method 200.8, by ICP/MS analysis.

Any significant findings are summarized below. No addition al data qualifiers were required.

• The post digestion spike (PDS) recoveries for the follo wing analytes failed TestAmerica’s control limits of 85–115%: arsenic, antimony, and vanadium.

INTERNAL STANDARDIZATION

All internal standards used by TestAmerica were within th e method criteria.

INITIAL CALIBRATION

TestAmerica performed the initial calibrations on each analysis day. The initial calibration for the ICP-MS analysis consisted of a bla nk and four calibration standards.

INITIAL AND CONTINUING CALIBRATION VERIFICATION (IC V/CCV)

The initial calibration verifications (ICV) and continu ing calibration verifications (CCV) performed by TestAmerica all had recoveries within the m ethod 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 element s 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 limi ts of 50–150% recovery.

LABORATORY CONTROL SAMPLES (LCS)

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

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION

Based on TestAmerica’s SOP, all interference check sa mple 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 sp ikes recovered within

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

SERIAL DILUTION

The serial dilution performed on sample 72149 passed TestAmer ica’s criteria of ±10%

difference.

FIELD DUPLICATES

No field duplicate samples were collected with these sa mpling episodes.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

Matrix spikes (MS) and matrix spike duplicates (MSD) we re performed on samples 72149 and 72241. All MS/MSD spike recoveries were within the me thod control criteria of 70-130% for all analytes. The relative percent differenc e (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 cont rol limits of 85–115% recovery for all analytes, except for arsenic, antimo ny, and vanadium, which were flagged with a “W”. No additional data qualifiers were require d for PDS samples.

### 4

DETECTION LIMITS

The laboratory performed an MDL study in the synthetic F GD wastewater matrix, instead of reagent water.

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A 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 a nd 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

7 199 1 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

7 2003 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 Ef fluent Field Blank, Set 1 280

- 8194

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

7 214 1 FGD Influent, Set 1 280

- 8061

- 1 Aqueous 10/5 /2010 10/6 /2010

721 4 5 FGD Bioreactor Influent, Set 1 280

- 8061

- 2 Aqueous 10/5 /2010 10/6 /2010

7 214 9 FGD Bioreactor Effluent, Set 1 280

- 8061

- 3 Aqueous 10/5 /2010 10/6 /2010

7 215 3 FGD Influent Field Blank 2 80

- 8061

- 6 Aqueous 10/5 /2010 10/6 /2010

7 215 4 FGD Bioreactor Influent Field

Blank, Set 1 280

- 8061

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

7 215 8 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 Ef fluent, 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

7 2295 FGD Effluent, Set 1 280

- 8058

- 2 Aqueous 10/5 /2010 10/6 /2010

7 2299 FGD Influent Field Blank, Set 1 280

- 8058

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

7 2300 FGD Ef

fluent Field Blank

, Set 1 280

- 8058

- 3 Aqueous 10/5 /2010 10/6 /2010



### SUMMARY

The samples were prepared for total metals analysis acc ording to TestAmerica’s SOP for ICP Analysis for Trace Metals by Method 200.7. Any signific ant findings are summarized below. No additional data qualifiers were requir ed.

• The serial dilution for cobalt, iron, molybdenum, sodium , and titanium for sample 72241 failed TestAmerica’s SOP control limit of percent di fferences less than

10%.

• The matrix spike (MS) and matrix spike duplicate (MSD) r ecoveries 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 co balt 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 TestAme rica’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 calibra tion 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 an d one calibration standard.

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

The initial calibration verifications (ICV) and continu ing calibration verifications (CCV) performed by TestAmerica all had recoveries within the m ethod 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 f lagged with the “J” qualifier.

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank (CCB)) were less than the RL; however, some element s were above the MDL and were flagged with the “J” qualifier.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

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

LABORATORY CONTROL SAMPLES (LCS)

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

INTERFERENCE CHECK SOLUTIONS

Interference checks were performed using the synthetic m atrix 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 TestAmeric a’s SOP, except for cobalt, iron, molybdenum, sodium, and titanium for Sample 72241.

FIELD DUPLICATES

No field duplicate samples were collected with these sa mpling 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 magnes ium 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 concentra tion 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 con trol limits.

The MS/MSD recoveries of sample 72241 failed the method sp ike 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 Metho d 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 perf ormed on sample 72241 failed the method criteria of 85–115% recovery for cobalt a nd tin, which were qualified with a “W”. No additional data qualifiers were required.

DETECTION LIMITS

The laboratory performed an MDL study in the synthetic F GD 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 Ana lyses – Long-Term Monitoring: Month 1 (Part 2)

TestAmerica Denver Laboratory generated analytical data f or classical wet chemistry analyses for these long-term monitoring samples. All s amples were tested for the following analytes:

• Ammonia by EPA method 350.1,

• Biochemical Oxygen Demand – 5 day (BOD 5 

### ) 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 TestAmer ica 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 specif ied in 40 CFR 136 Table II unless otherwise noted below. All samples were preserved a ppropriately unless otherwise specified below.

Field duplicate samples were not collected for these ep isodes. Depending on the method, a laboratory duplicate was analyzed, instead. The Relati ve Percent Difference (RPD) between the sample and its duplicate was less than 20% unl ess 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 t o 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, a ll calibration blanks and calibration verification samples met the criteria sp ecified in the method.

If required by the method, the quality control sample (QC S), a secondary source standard used to verify calibration, was always within the cont rol limits specified by the method.

As described below, the analyte of interest was detecte d 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 spec ified 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 so me 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 sa mples 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 s ample 71999 were above the calibration range. Only one set of MS/MSD are required pe r the method; therefore, the results from sample 72149 meet the requirements. No further action is required.

### 3

BOD 5



### The traffic reports for the following samples did not ind icate 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 greate r than 6°C.

TestAmerica analyzed five dilutions; the dilutions had d issolved 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 o f the results for all dilutions with a DO depletion greater than 2.0 mg/L and a final DO greater t han 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 see d correction blank (SCB) recovery was low. This low seed correction factor suggest s 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 c riteria; however, for sample 71999, the MS/MSD results for sulfate exceeded the calibra tion range and for sample 72149, the MS/MSD results for chloride exceeded the calibra tion range. These MS/MSD results were qualified as estimated values. No further a ction 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 cont rol criteria. The percent recoveries for the MS and MSD for sample 71999 were 25% an d 44%, respectively,

which are outside the method control criteria of 90-110% and t herefore, the MS/MSD results were flagged with “F” qualifiers. The LCS/LCSD results were acceptable for this sample indicating the analytical system was operating w ithin control.

Cyanide

Because of the nature of the sample matrix, all of th e samples in this sampling episode used a lower volume, which resulted in elevated RLs being ca lculated 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 outs ide 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 f or sample 72149 were 89% and

### 4

88%, respectively, which are outside the method control c riteria and therefore, the MS and MSD results were flagged with “F” qualifiers. The LCS /LCSD results were acceptable for these samples indicating the analytical s ystem was operating within control. Additionally, there is no method requirement f or 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 cont rol criteria. The percent recoveries for the MS and MSD for sample 72149 were 77% an d 79%, respectively, which are outside the method control criteria, but did m eet 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 s ystem was operating within

control.

TDS

The method blank associated with one of the batches detec ted TDS at a level greater than the MDL, but less than the RL. All affected samples w ere flagged with a “B” qualifier, which includes samples 72141, 72145, 72149, 72291, and 72295.

Because of the nature of the sample matrix, some of t he samples in this sampling episode used a lower volume, which resulted in elevated RLs being c alculated 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 wo rksheets indicates that constant weight was achieved for all thr ee 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, TestAm erica reviewed the analyses and determined that the sample should have been run with a di lution factor of 10 or 20, but was run with a dilution of one. The laboratory has n o 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 da ta set.

### 5

TKN

Method blank results associated with one of the batches w ere 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 t he samples in this sampling episode used a lower volume, which resulted in elevated RLs being c alculated 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 M onitoring: Month 2 (Part 2)

Frontier Global Sciences (FGS) generated analytical da ta for total mercury. FGS analyzed the samples according to EPA Method 1631E for merc ury by Cold Vapor Atomic Fluorescence Spectrometry (CVAFS) analysis.

Table 1 summarizes the three samples (excluding labora tory 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 a dditional 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 analysi s day. The initial calibration for the CVAFS analysis consisted of a blank and five calibrat ion standards with a correlation

coefficient ≥ 0.995. All method-specified criteria were met.

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

All initial and continuing calibration verifications (I CVs, CCVs) met method-specified

criteria.

BLANKS

All the preparation blanks or laboratory reagent blanks (L RBs) and the continuing calibration blanks (CCBs) met the method-specified crite ria. Because all of the blank results were less than the RL, no samples were quali fied based on these preparation blank

results.

DUPLICATES

No field duplicate samples were collected with this samp ling episode. A sample from another work order was analyzed in duplicate at the labor atory with these samples. The RPD was 6.33%. The laboratory’s RPD criteria between a nalytical duplicates is 24%.

LABORATORY CONTROL SAMPLES

All laboratory control samples were within FGS’s contr ol 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) w as performed on Effluent sample 72296. An MS/MSD was also performed on a sample fro m 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 o rder had recoveries of 100% and 85.2%, respectively, with an RPD of 8.85%. All MS/M SD samples met the method specified recovery criteria of 71-125% and the RPD cr iteria 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, EP A 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, thalliumand vanadium) for these longterm monitoring samples. The samples were analyzed accor ding to EPA Method 200.8.

Table 1 summarizes the samples TestAmerica extracted a nd 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 accor ding to TestAmerica’s “FGD ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Elements Analysis in Flue Gas Desulfurization Wastewaters,” date d October 6, 2010, based on EPA Method 200.8, by ICP/MS analysis.

Any significant findings are summarized below. No addition al data qualifiers were required.

• The matrix spike (MS) and matrix spike duplicate (MSD) rec overies for total silver for sample 72296 failed the EPA Method 200.8 control li mits 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 th e method criteria.

INITIAL CALIBRATION

TestAmerica performed the initial calibrations on each analysis day. The initial calibration for the ICP-MS analysis consisted of a bla nk and four calibration standards.

INITIAL AND CONTINUING CALIBRATION VERIFICATION (IC V/CCV)

The initial calibration verifications (ICV) and continu ing calibration verifications (CCV) performed by TestAmerica all had recoveries within the m ethod 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 element s 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 limi ts of 50–150% recovery.

LABORATORY CONTROL SAMPLES (LCS)

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

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION

Based on TestAmerica’s SOP, all interference check sa mple 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 sp ikes recovered within

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

### 3

The ICSA solution for the method 200.8 analysis exceeded t he acceptance limits for Chromium in analytical batch 280-41398. The lab has confirmed w ith the vendor that Chromium is a trace impurity in the ICSA solution. Ther efore, corrective action was deemed unnecessary; the associated data have been flagged “ ^”.

SERIAL DILUTION

The serial dilution performed on sample 72296 passed TestAmer ica’s criteria of ±10%

difference.

FIELD DUPLICATES

No field duplicate samples were collected with these sa mpling episodes.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

The MS and MSD was performed on sample 72296. The total se lenium 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 a n “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 qualif iers were required for MS/MSD samples.

POST DIGESTION SPIKES (PDS)

The PDS performed on sample 72296 passed TestAmerica’s cont rol limits of 85–115% recovery for all analytes, except for silver, which wa s 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 sul fate. The silver recoveries in the associated LCS/LCSD were acceptable. An additional quali fier is required as shown in

Table 2.

DETECTION LIMITS

### 4

The laboratory performed an MDL study in the synthetic F GD 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, EP A 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 a nd 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

7 2 292 FGD Influent, Set 2 280

- 9642

- 1 Aqueous 11/10 /2010 11 / 11 /2010

7 229 6 FGD Ef fluent, Set 2 280

- 9642

- 2 Aqueous 11/10 /2010 11/11 /2010

7 2 301 FGD E f

fluent Field Blank , Set 2 280

- 9642

- 3 Aqueous 11/10 /2010 11/11 /2010



### SUMMARY

The samples were prepared for total metals analysis acc ording to TestAmerica’s SOP for ICP Analysis for Trace Metals by Method 200.7. Any signific ant findings are summarized below. No additional data qualifiers were require d for this data set.

• An initial calibration verification (ICV) had a recov ery for aluminum above the upper control limit. Aluminum values for all samples ass ociated with this ICV were non-detects and were reported by TestAmerica.

• The matrix spike (MS)/matrix spike duplicate (MSD) rel ative percent difference (RPD) for boron, calcium, and magnesium for sample 722 96 failed TestAmerica’s SOP requirement of ± 20%.

### 2

• The post digestion spike (PDS) for barium for sample 722 96 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 calibra tion 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 an d 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 va lues of samples associated with this ICV were non-detects and were reported by Test America.

All continuing calibration verifications (CCV) had reco veries 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 f lagged with the “J” qualifier.

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank (CCB)) were less than the RL; however, some element s were above the MDL and were flagged with the “J” qualifier.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

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

LABORATORY CONTROL SAMPLES (LCS)

The LCS passed the method control limits of 85–115% recover y.

### 3

INTERFERENCE CHECK SOLUTIONS

Interference checks were performed using the synthetic m atrix 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 sa mpling 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 co ncentration 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 cont rol criteria of 70-130%. The MS/MSD RPD for boron, calcium, and magnesium for samp le 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 contr ol limits of 85-115% recovery for all analytes except barium, which was qual ified with a “W”. Barium passed the MS/MSD recovery and serial dilution control limit s demonstrating no significant matrix interference. No additional qualifiers are needed.

DETECTION LIMITS

The laboratory performed an MDL study in the synthetic F GD wastewater matrix, instead of reagent water.

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A EAD Deb Bartram, ERG TJ Finseth, ERG

From: Ariel Atkinson, ERG

Date: 2/9/2012 Subject: TestAmerica Data Review Narrative for Classicals Ana lyses – Long-Term Monitoring: Month 2 (Part 2)

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry analyses for these long-term monitoring samples. Sampl es were tested for the following analytes:

• Ammonia by EPA method 350.1,

• Biochemical Oxygen Demand – 5 day (BOD 5 

### ) 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 an alyzed 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 specif ied in 40 CFR 136 Table II. All samples were preserved appropriately.

Field duplicate samples were not collected for these ep isodes. Depending on the method, a laboratory duplicate was analyzed, instead. The Relati ve Percent Difference (RPD) between the sample and its duplicate was less than 20% unl ess 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 t o create the curve, the sample was diluted and reanalyzed, unless otherwise specified below. A ll 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 (QC S), a secondary source standard used to verify calibration, was always within the cont rol limits specified by the method.

As described below, the analyte of interest was detecte d 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 spec ified in the method unless specified

below.

If required by the method, a matrix spike (MS) sample wa s analyzed on sample 72296 for each analyte to check for matrix interferences. MS sam ples analyzed met the criteria specified in the method unless described below.

DATA NOTES/ISSUES

Ammonia

No issues were identified by the data reviewer.

BOD 5



### 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 dupli cate of sample 72292 did not have a DO depletion greater than 2.0 mg/L. There fore, BOD 5 

### was reported as not detected for the duplicate. As required in the met hod, 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 resu lts may be biased low.

All glucose-glutamic acid standards and laboratory duplicat es 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 s tandard 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 c alibration performed.

A MS/MSD was performed using sample 72296. The percent recover y for both the MS and MSD was 49%, which is below the control limit of 90% a nd 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 cali bration 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 resul ts exceeded calibration range. The percent recovery for the MS/MSD were within the c ontrol 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 conc entration 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 th e 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 s ample result was an estimated

value.

### 4

Sample 72296 and the LRB had results that were lower tha n 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 sam ple 72296 was not within the control limits of 90-110% specified in EPA Method 365.1. Howev er 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%, re spectively. 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 flagge d 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 hygros copy 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 l aboratory. 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 t he method control limit of 90-110% recovery and was flagged with “*” qualifier. The sampl es 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 l aboratory 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 samp le 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 t hat 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 M onitoring:

Month 4 and 5

Frontier Global Sciences (FGS) generated analytical da ta for total mercury. FGS analyzed the samples according to EPA Method 1631E for merc ury by Cold Vapor Atomic Fluorescence Spectrometry (CVAFS) analysis.

Table 1 summarizes the 30 samples (excluding laboratory pre p 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 a dditional qualifiers in this dataset. The following summarizes the findings from the data review:

• The sample number for Sample 72157 was labeled incorrectly o n the traffic
report.

• The sample description for Sample 72148 was entered incorrec tly 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 tra ffic report submitted to the laboratory. The error was identified and correct ed during the data review based on the sample description. FGS incorrectly labeled Sampl e 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 analysi s day. The initial calibration for the CVAFS analysis consisted of a blank and five calibrat ion standards with a correlation

coefficient ≥ 0.995. All method-specified criteria were met.

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

All initial and continuing calibration verifications (I CVs, CCVs) met method-specified

criteria.

BLANKS

All the preparation blanks or laboratory reagent blanks (L RBs) and the continuing calibration blanks (CCBs) met the method-specified crite ria. Because all of the blank results were less than the RL, no samples were quali fied based on these preparation blank

results.

DUPLICATES

No field duplicate samples were collected with these sa mpling episodes. Four samples were analyzed in duplicate at the laboratory, Influent s amples 72144 and 71994 and Effluent samples 72048 and 72298. The relative percent differenc e (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 RPD s of 13.3%, 22.4%, and 3.03%. The laboratory’s RPD criteria between analytica l 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 metho d-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, EP A 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, thalliumand vanadium) for these longterm monitoring samples. The samples were analyzed accor ding to EPA Method 200.8.

Table 1 summarizes the samples TestAmerica extracted a nd 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 accor ding to TestAmerica’s “FGD ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Elements Analysis in Flue Gas Desulfurization Wastewaters,” date d October 6, 2010, based on EPA Method 200.8, by ICP/MS analysis.

Any significant findings are summarized below. No addition al data qualifiers were required.

• The sample for FGD Effluent, Set 3 associated with Epi sode 6571 was incorrectly labeled as sample 72295 on the traffic report. The correc t sample number (72297) was found on the sample bottle label and confirmed with E RG prior to analysis.

• The matrix spike (MS) and matrix spike duplicate (MSD) rec overies for total silver for sample 72248 failed the EPA Method 200.8 control lim its of 70-130%. The MSD recovery for total silver for sample 72201 also fa iled the method

control limits.

• The MS/MSD relative percent difference (RPD) for tota l 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 th e 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 bla nk and four calibration standards.

INITIAL AND CONTINUING CALIBRATION VERIFICATION (IC V/CCV)

The initial calibration verifications (ICV) and continu ing calibration verifications (CCV) performed by TestAmerica all had recoveries within the m ethod 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 element s 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 limi ts of 50–150% recovery.

LABORATORY CONTROL SAMPLES (LCS)

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

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION

Based on TestAmerica’s SOP, all interference check sa mple 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 sp ikes 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 Te stAmerica’s criteria

of ±10% difference.

FIELD DUPLICATES

No field duplicate samples were collected with these sa mpling 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% recover y for silver at 61%, which was flagged with an “F” qualifier. The MS/MSD of sam ple 72248 failed the method control limits of 70–130% recovery for silver at 66% a nd 45% respectively, which were flagged with an “F” qualifier. These silver fa ilures 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 th e 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 b oth PDS samples, which were flagged with a “W” qualifier. Additional data qualifiers wo uld be required; however silver was not detected in these samples.

DETECTION LIMITS

The laboratory performed an MDL study in the synthetic F GD wastewater matrix, instead of reagent water.

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A 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 a nd 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 /201 1

72098 FGD Effluent , Set 4 280

- 11635

- 2 Aqueous 1/14/2011 1/15 /201 1

72103 FGD Effluent Field Blank, Set 4 280

- 11635

- 3 Aqueous 1/14/2011 1/15 /201 1

7 2144 FGD Influent, Set 4 280

- 11555

- 1 Aqueous 1/12 /201 1 1/13 /201 1

7 2148 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 /201 1 1/13 /201 1

7 2197 FGD SBR Influent, Set 3 280

- 11552

- 2 Aqueous 1/12 /201 1 1/13 /201 1

7 2201 FGD SBR Effluent, Set 3 280

- 11552

- 3 Aqueous 1/12 /201 1 1/13 /201 1

### 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

72 206 FGD SBR Influent Field Blank,

Set 3 280

- 11552

- 4 Aqueous 1/12 /201 1 1/13 /201 1

7 2210 FGD SBR Effluent Field Blank,

Set 3 280

- 11552

- 5 Aqueous 1/12 /201 1 1/13 /201 1

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

7 2293 FGD Influent, Set 3 280

- 11553

- 1 Aqueous 1/12 /201 1 1/13 /201 1

7 2297 FGD Effluent, Set 3 280

- 11553

- 3 Aqueous 1/12 /201 1 1/13 /201 1

7 2302 FGD Ef

fluent Field Blank, Set 3 2 80

- 11553

- 4 Aqueous 1/12 /201 1 1/13 /201 1



### SUMMARY

The samples were prepared for total metals analysis acc ording to TestAmerica’s SOP for ICP Analysis for Trace Metals by Method 200.7. Any signific ant findings are summarized below. No additional data qualifiers were require d for this set of data.

• Several samples did not have the date and time of sampl e 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 fai led 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 n ot have a sample date or time on the traffic report or s ample labels.

Samples associated with Episode 6571 (72293, 72297, and 72302) did not hav e a sample date or time on the traffic report or sample labels. Add itionally, a field sampler name was not present on the traffic report. The sample FGD Ef fluent, Set3 was listed on the traffic report as sample 72295, which is incorrect; however, the sam ple 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 dat e 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 calibra tion 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 an d one calibration standard.

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

The initial calibration verifications (ICV) and continu ing calibration verifications (CCV) performed by TestAmerica all had recoveries within the m ethod 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 f lagged with the “J” qualifier.

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank (CCB)) were less than the RL; however, some element s were above the MDL and were flagged with the “J” qualifier.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

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

LABORATORY CONTROL SAMPLES (LCS)

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

INTERFERENCE CHECK SOLUTIONS

Interference checks were performed using the synthetic m atrix 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 sa mpling episodes.

### 4

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

Matrix spikes (MS) and matrix spike duplicates (MSD) w ere performed on the total samples of 72201, 72248, and 72002. Some elements with high concent rations failed the EPA 200.7 Method spike recovery control limits of 70–130% but w ere flagged with a “4” qualifier indicating that the concentration in the paren t 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. Othe rwise, 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 TestAme rica’s ± 20% requirement, except for magnesium for sample 72095. No additional data quali fiers 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 amoun t.

The PDS performed on sample 72002 failed the method criteria of 85–115% recovery for boron, magnesium and manganese; however, these result s 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 F GD wastewater matrix, instead of reagent water.

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A 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 Ana lyses – Long-Term Monitoring: Month 4

TestAmerica Denver Laboratory generated analytical data f or classical wet chemistry analyses for these long-term monitoring samples. All s amples were tested for the following analytes:

• Ammonia by EPA method 350.1,

• Biochemical Oxygen Demand – 5 day (BOD 5 

### ) 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 anal yzed 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 specif ied in 40 CFR 136 Table II unless otherwise noted below. All samples were preserve d appropriately unless otherwise specified. Group II samples 72293 and 72297 were receiv ed 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 epis ode. 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% unl ess 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 t o 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, a ll calibration blanks and calibration verification samples met the criteria sp ecified in the method.

If required by the method, the quality control sample (QC S), a secondary source standard used to verify calibration, was always within the cont rol limits specified by the method.

As described below, the analyte of interest was detecte d 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 spec ified 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 crite ria specified in the method unless

described below.

### 3

DATA NOTES/ISSUES

Ammonia

Samples 72293 and 72297 were received by the laboratory at a neutra l pH. Sample 72293 was qualified as an estimated, as shown in Table 2. Samp le 72297 had a result greater than the MDL, but less than the RL, so the re sult 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 cri teria. 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 qualificatio n is needed.

BOD 5



### No issues were identified by the data reviewer.

Chloride and Sulfate

MS and MSD were performed on samples 72002, 72094, and 72201. The perce nt
recoveries for the MS and MSD for all chloride and sul fate 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 f or 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% an d 88%, respectively.

Both the MSD results are outside the method control c riteria. 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 analyti cal system was operating within control. Additionally, there is no method requirement f or 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 detec ted phosphorus at levels greater than the MDL, but less than the RL. All affec ted 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 withi n 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 fl agged 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 crite ria. 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 chemist ry worksheets indicates that constant weight was achieve d for all. No further action was

necessary.

The analytical duplicate performed on sample 72002 exceeded t he recovery criteria. The duplicate result was flagged with an “F” qualifier. Becaus e an analytical duplicate was not required by the method, no further corrective action i s 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 withi n 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 cri teria. There results were flagged with “F” qualifiers. The LCS/LCSD recoveries fo r this batch were acceptable, indicating that the analytical system was operating wit hin control.

TSS

Because of the nature of the sample matrix, some of t he samples in this sampling episode used a lower volume, which resulted in elevated RLs being c alculated and reported by TestAmerica with the sample results.

The analytical duplicate performed on sample 72248 exceeded t he recovery criteria. Because the sample result is below the RL, further qual ification 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, EP A 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, thalliumand vanadium) for these longterm monitoring samples. The samples were analyzed accor ding to EPA Method 200.8.

Table 1 summarizes the samples TestAmerica extracted a nd 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 accor ding to TestAmerica’s “FGD ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Elements Analysis in Flue Gas Desulfurization Wastewaters,” date d October 6, 2010, based on EPA Method 200.8, by ICP/MS analysis.

Any significant findings are summarized below. No addition al data qualifiers were required.

• The matrix spike duplicate (MSD) recovery for total sil ver 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 a nd silver for sample

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

INTERNAL STANDARDIZATION

All internal standards used by TestAmerica were within th e method criteria.

INITIAL CALIBRATION

TestAmerica performed the initial calibrations on each analysis day. The initial calibration for the ICP-MS analysis consisted of a bla nk and four calibration standards.

INITIAL AND CONTINUING CALIBRATION VERIFICATION (IC V/CCV)

The initial calibration verifications (ICV) and continu ing calibration verifications (CCV) performed by TestAmerica all had recoveries within the m ethod 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 limi ts of 50–150% recovery.

LABORATORY CONTROL SAMPLES (LCS)

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

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION

Based on TestAmerica’s SOP, all interference check sa mple 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 sp ikes recovered within

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

### 3

SERIAL DILUTION

The serial dilution performed on sample 72298 passed TestAmer ica’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 dilutio n.

FIELD DUPLICATES

No field duplicate samples were collected with these sa mpling episodes.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

The MS and MSD were performed on sample 72298. The MSD o f 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 matr ix interference from the high concentration of sulfates, which can form insoluble si lver 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 th e 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 cont rol limits of 85–115% recovery for all analytes, except for selenium and sil ver, which were flagged with “W” qualifiers. The selenium and silver recoveries in the a ssociated LCS/LCSD were acceptable.

DETECTION LIMITS

The laboratory performed an MDL study in the synthetic F GD wastewater matrix, instead of reagent water.

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A 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 a nd 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

7 2 294 FGD Influent, Set 4 280

- 12365

- 1 Aqueous 2/9 /201 1 2 / 10 /201 1

7 2298 FGD Ef

fluent, Set 4 280

- 12365

- 2 Aqueous 2/9 /201 1 2/10 /201 1

7 2303 FGD Effluent Field Blank

,

Set 4 280

- 12365

- 3 Aqueous 2/9 /201 1 2/10 /201 1



### SUMMARY

The samples were prepared for total metals analysis acc ording to TestAmerica’s SOP for ICP Analysis for Trace Metals by Method 200.7. Any signific ant findings are summarized below. No additional data qualifiers were require d.

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 calibra tion 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 an d one calibration standard.

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS

The initial calibration verifications (ICV) and continu ing calibration verifications (CCV) performed by TestAmerica all had recoveries within the m ethod 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 f lagged with the “J” qualifier.

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank (CCB)) were less than the RL; however, some element s were above the MDL and were flagged with the “J” qualifier.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

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

LABORATORY CONTROL SAMPLES (LCS)

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

INTERFERENCE CHECK SOLUTIONS

Interference checks were performed using the synthetic m atrix 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 sa mpling 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 wit h a “4” qualifier indicating that the concentration in the parent sample was greate r 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/MS D spike recoveries were within the method control criteria of 70-130%. The relative perce nt 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 wi th a “W” because their sample concentrations were greater than 4 times the spike amoun t. 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 F GD wastewater matrix, instead of reagent water.

### 1



## MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD

CC: Jezebele Alicea, Alternate Work Assignment Manager, EP A EAD Deb Bartram, ERG TJ Finseth, ERG

From: Ariel Atkinson, ERG

Date: 2/9/2012 Subject: TestAmerica Data Review Narrative for Classicals Ana lyses – Long Term Monitoring: Month 5

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry analyses for these long-term monitoring samples. Sampl es were tested for the following analytes:

• Ammonia by EPA method 350.1,

• Biochemical Oxygen Demand – 5 day (BOD 5 

### ) 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 an alyzed for the above analytes.

Table 1. Long Term Monitoring Set 2 Episodes 6571 Classical Analyt es – 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 specif ied in 40 CFR 136 Table II. All samples were preserved appropriately unless otherwise speci fied. 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 C ollection date and time was

### 2

recorded on the traffic reports, so the laboratory se t the collection date as 2/9/11 0:00; the date the samples were relinquished.

Field duplicate samples were not collected for these ep isodes. Depending on the method, a laboratory duplicate was analyzed, instead. The Relati ve Percent Difference (RPD) between the sample and its duplicate was less than 20% unl ess 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 t o create the curve, the sample was diluted and reanalyzed, unless otherwise specified below. A ll 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 (QC S), a secondary source standard used to verify calibration, was always within the cont rol limits specified by the method.

As described below, the analyte of interest was detecte d 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 spec ified in the method unless specified

below.

If required by the method, a matrix spike (MS) sample wa s analyzed on sample 72298 for each analyte to check for matrix interferences. MS sam ples 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 re sults were greater than the MDL (0.055 mg/L), but less than the RL (1.0 mg/L) and the refore, was flagged with a “J” qualifier. The samples were also flagged with a “B” qua lifier 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; th erefore, the sample result was qualified as an estimated value.

BOD 5



### TestAmerica analyzed five dilutions; the dilutions had a d issolved oxygen (DO) depletion greater than 2.0 mg/L for samples 72294 and 72298. As required in t he method, the final result was calculated by taking the average of the resul ts 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 duplicat es were analyzed appropriately and met the criteria specified in SM 5210B.

Chloride and Sulfate

The MS/MSD results for chloride for sample 72298 were abo ve the calibration curve. TestAmerica did not reanalyze these MS/MSDs with a hi gher dilution factor, because the percent recoveries and RPD met the method criteria. Th e 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. M ethod 410.4 requires that the sample pH be adjusted to <2 at the time of collect ion. 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 m eet 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 s tandard concentrations for this method are between 5 ppb and 20 ppb.

A MS/MSD was performed using sample 72298. The percent recover y for the MS and MSD were 84% and 83%, respectively, which is below the cont rol limit of 90% and as a result, the MS/MSD results were flagged with an “F” qual ifier.

Nitrate/Nitrite

The MS/MSD results for samples 72298 were above the cali bration 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 fo r the MS and MSD were within the laboratory control limits, but not within the metho d 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” qualifie r.

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; th erefore, the sample result was qualified as an estimated value.

### 4

Phosphorus

The final CCB was greater than the MDL at 0.0212 mg/L, ho wever the result was less than the RL; therefore, the CCB result was flagged w ith a “J” qualifier. No further qualifiers are needed. All samples that contained the an alyte were also flagged with “B” qualifier because the compound was found in the blank and th e sample. All calibration

blank results were also above the MDL but less than th e RL, and therefore are also flagged with “J” qualifier.

Sample 72294 and 72298 had results that were lower than the low est 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 abov e 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 th e “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 per cent recoveries of the MS and MSD samples were 27% and 32%, respectively. Becaus e 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 hygro scopy is not an issue. No

further issues were identified.

TKN

TKN was detected in the initial calibration blank and met hod 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 ass ociated 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; th erefore, the sample result was qualified as an estimated value.

TestAmerica performed MS and MSD analyses on sample 72298. T he percent recoveries for the MS and MSD for sample 72298 were 146% and -8%, respec tively, 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 s pike concentration; therefore, control limits are not applicable. No further qualificatio n is necessary.

### 5

TSS

The RPD for the laboratory duplicates performed on sam ple 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 t hat 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