Enclosure 1

Instructions for Sample Collection, Packaging, and Shipment EPA Sampling Program

The samples you will be colle cting are very important. The samples will be used by the U.S. Environmental Protection Agency (EPA ) for revising the effluent limitations guidelines and standards for the Steam Electric Power Generating Industry.

These instructions are bei ng provided to Wabash Valley Power Association’s Wabash River Power Station to aid in collecting, packaging, and shipping samples for this sampling program.

The plant must collect grab samples for all analytes at the sour water sampling points, and 24-hour composite samples for all analytes except mercury and cyanide at the vapor crystallizer (RCC) evaporator distillate stream sample point . At the vapor crystallizer (RCC) evaporator distillate sa mpling point, the plant must coll ect cyanide as a single grab sample and mercury must be collected as f our individual grab sa mples over the 24-hour period (i.e., a grab sample collected every six hours).

Samples must be collected Monday through Thursday during the week of January 31, 2011. If the plant has any questions regarding the timeline or the steps provided, please contact Mr. Ronald Jordan at ( 202) 566-1003 or jordan.ronald@epa.gov.

Equipment Needed

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

• Sample bottles, composite containers, and tubing sets (specially-cleaned according to EPA Method 1669);

• Automatic compositor;

• Powder-free gloves;

• Tyvek® coveralls or su itable alternative;

• Dust masks (for use while collecting mercury samples)

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

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

• Coolers;

• Garbage bags;

• Packing material;

• Strapping tape; and

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

The plant must collect samples Monday thr ough Thursday during the week of January 31, 2011 from each of the four sampling points spec ified below. Figure 1 identifies each of the sampling points for this sampling program. The following is a description of the four sampling points:

• Sour Water Feed to the Treatment System (SP-1) : This sampling point shall represent the combined c ondensate and chloride scrubber blowdown stream (D162 and E-166A/B) sour water feed to th e carbon filter beds (V-166A/B) and degassing column (C-270). The sample shall be collected at the sample tap prior

to the carbon filter beds.

• Sour Water Return from the Sulfur Recovery Unit (SP-2) . This sampling point shall represent the sour water return (V-241) from the sulfur recovery unit that is sent to the degassing column (C- 270). The sample shall be collected prior to it combining with the sour wa ter exiting filter beds V-167A/B.

• Sour Water Feed to the Vapor Crystallizer (RCC) Evaporator (SP-3) : This sampling point shall represen t the sour water following ammonia stripping for the

removal of NH 3 and trace compounds. To avoi d collecting a high temperature sample, this sample should be collected from the sample tap located immediately downstream of the E-271 heat exchanger.

• Vapor Crystallizer (RCC) Evap orator Distillate (SP-4) : This sampling point shall represent the distillate stream from the vapor crystallizer (RCC) evaporator system prior to any commingling with ot her plant water, such as cooling tower blowdown. This sample should be collected between the T-278 distillate tank and the P-278 pump.

Analytes

Table 1 contains the listing of all the analytes included in this sampling program, as well as the analytical methods that EPA will use to analyze the samples.Table 1. Analytes and Anal ytical Methods Included in the Sampling 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, ch romium, copper, lead, nickel, selenium, silver, thallium, and vanadium EPA 200.8 with collision

cell Aluminum, barium, beryllium, boron, calcium, cobalt, iron, magnesium, manganese, molybdenum, sodium, tin, titanium, and

zinc EPA 200.7Figure provided under separate correspondenceFigure 1. Wabash River Gasification Wastewater Treatment System Sampling PointsSample Bottles and Preservation

Table 2 identifies the sample bottles that ar e needed for collecting samples. The table also identifies the on-site preservation that is required for the samples. Please note that the number of sample bottles listed in Table 2 refers to the number of bottles that will need to be collected from each sampling point for each of the four sets of samples. For the Group II samples, the plant can either pres erve the samples with sulfuric acid after sample collection, or the plant can orde r pre-preserved sample bottles.

For the total cyanide samples, the plant should test the wastewater from the sampling points with lead acetate paper (turns black in the presence of sulfide) and potassium iodide starch paper (turns blue/violet in the pr esence of chlorine). If sulfide is present, the plant will need to dilute the sample with blank water until the su lfide is not detected by the lead acetate paper. If chlorine is pr esent, then the plant w ill need to add sodium

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

dilution and/or sodium arsenite is added to th e sample, the plant will need to preserve the sample with sodium hydroxide until the samp le 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 the vapor crystallizer (RCC) evaporator

distillate Four 125-mL glass

bottles

Sour water samples (feed to treatment, return from sulfur recovery, and feed to RCC) and field blank samples Two 250-mL glass

bottles None (acid preserve at laboratory)

(a) Group I includes TSS, TD S, sulfate, and chloride. (b) Group II includes ammonia as nitrogen, COD, nitr ate/nitrite as nitrogen, TKN, and total phosphorus. NOTE: The number of sample bottles refers to the number of sample bottles needed for each sampling point for each of the four sets of samples.Sample Labeling

Label each bottle prior to collecting the sample so it can be identified by the laboratory. Each self-adhesive label must be complete d 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 plan t must revise the labe l using indelible ink. Once applied to the sample container, the plan t must cover the labels with clear tape to prevent tampering, abrasion, smearing, or loss during transit. For metals and mercury samples, do not place labels directly on the sample bottles because of the potential for contamination. Instead, place the label on the ou ter plastic bag of the sample bottle. To ensure that the sample label does not b ecome separated from the bottle, the doublebagged sample bottle should be placed in an additional Ziploc bag after collection. Please note however, that the labels can be placed directly on the metals and mercury sample bottles ONLY IF they are placed directly on the bottles in a clean laboratory environment. HOWEVER, any revisions to the labels by the plant must be made on a label placed on the outer plastic bag for the double-bagged sample bottle, and the changes noted in the traffic report.

Table 3 provides the sampling point descrip tions, sample numbers, and sampling episode number for the plant for this monitoring progr am. The information in the table should be provided on the sample bottle labels for the appropriate bottles. The “analysis to be performed” should be shown on the label as the following, depending on the specific analysis:

• BOD;

• Group I;

• Group II;

• Total Cyanide;

• Total Metals – 200.8 w/ CC;

• Total Metals – 200.7;

• Total Mercury (for sour water feed to treatment, sour water return from sulfur recovery, sour water feed to vapor crystallizer (RCC) evaporator, and field blank samples); and

• Total Mercury – Grab 1 (for vapor crys tallizer (RCC) evaporator distillate laboratory composite samples. The bo ttles should be labeled as Grab 1, Grab 2, Grab 3, and Grab 4 for the four respective collection times).The “sample bottle type” should be shown on the label the same as the “Sample Container and Volume” column in Table 2, except that the quantity should not be included. For example, for total mercury, the “sample bottle type” should be “250-mL glass bottle.” The “required on-site preservation” should be shown on the label the same

as the “On-Site Preservation” column in Table 2, except that “(acid preserve at laboratory)” does not need to be included for the total metals and total mercury sample

bottles.

Table 3. Sampling Point Descriptions and Sample Numbers for Sampling Program

Sampling Point Description Sample Number Sampling Episode

Number

Sour Water Feed to Treatment - Set 1 72441 6574

Sour Water Feed to Treatment - Set 2 72442 6574

Sour Water Feed to Treatment - Set 3 72443 6574

Sour Water Feed to Treatment - Set 4 72444 6574

Sour Water Return from Sulfur Recovery - Set 1 72445 6574

Sour Water Return from Sulfur Recovery - Set 2 72446 6574

Sour Water Return from Sulfur Recovery - Set 3 72447 6574

Sour Water Return from Sulfur Recovery - Set 4 72448 6574

Sour Water Feed to the RCC Evaporator - Set 1 72449 6574

Sour Water Feed to the RCC Evaporator - Set 2 72450 6574

Sour Water Feed to the RCC Evaporator - Set 3 72451 6574

Sour Water Feed to the RCC Evaporator - Set 4 72452 6574

RCC Evaporator Distillate - Set 1 72453 6574

RCC Evaporator Distillate - Set 2 72454 6574

RCC Evaporator Distillate - Set 3 72455 6574

RCC Evaporator Distillate - Set 4 72456 6574

Sour Water Feed to Treatment Field Blank 72457 6574

Sour Water Return from Sulfur Recovery Field Blank 72458 6574

Sour Water Feed to the RCC Evaporator Field Blank 72459 6574

RCC Evaporator Distillate Field Blank - Set 1 72460 6574

RCC Evaporator Distillate Field Blank - Set 2 72461 6574

RCC Evaporator Distillate Field Blank - Set 3 72462 6574

RCC Evaporator Distillate Field Blank - Set 4 72463 6574

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

Sour Water Feed to the Treatment System Collected during one

of the four sets Collected during one

of the four sets No field blanks required

Sour Water Return from Sulfur Recovery Collected during one

of the four sets Collected during one

of the four sets No field blanks required

Sour Water Feed to the RCC Evaporator Collected during one

of the four sets Collected during one

of the four sets No field blanks required RCC Evaporator

Distillate Collected once during

each of the four sets Collected during one

of the four sets 2 No field blanks required

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

2 The field blank can be collected during any of the sa mple sets, but the plant must use the sample number and sampling point description associated with the correct sample set (e.g., RCC Evaporator Distillate Field Blank – Set 2 – sample number 72461 if the field is collected during set 2).

The laboratory will perform MS/MSD analyses on the total metals and total mercury analyses; however, no additional sample volume is required.

Sample Collection

The plant must use clean sampling techniques when collecting the total metals and total mercury samples; therefore, the sampling t eam should follow the clean hands/dirty hands sampling techniques outlined in EPA Method 166 9. Additionally, the plant must try to avoid significant contamination during sample collection, especially from sources such as airborne particles, dirt, and corrosion pa rticulates from pipi ng, railing, etc.

The plant must collect grab samples for all analytes at the sour water sample points (sour water feed to treatment, sour water return fr om sulfur recovery, and sour water feed to RCC evaporator). The plant must collect 24-hour composite samples for all analytes except cyanide and mercury at the RCC evaporat or distillate sampling point. The 24-hour composites must be set up to collect equal sample aliquots ever y hour over the 24-hour period. For mercury at the RCC evaporator distillate sampling point, the plant must collect four individual grab samples over the 24-hour period (i.e., one mercury grab collected every six hours). Fo r cyanide at the RCC evaporator distillate sampling point, the plant must collect a single grab sample after one of the mercury grab samples.

If the plant is able to collect the sample s from a valve or tap, the plant can use the instructions provided in this section to set up and collect the composite samples at the RCC evaporator distillate sampling point. This section also provides instructions to collect the grab samples at the sour water samp le points (sour water feed to treatment, sour water return from sulfur recovery, and sour water feed to RCC evaporator) and for the mercury and cyanide grab samples at the RCC evaporator distillate sampling point. Please note that the plant will need to install a tw o-way splitter on the tap for the RCC evaporator distillate sampling point to allow for the com posite tubing to be connected to the tap and also have a tap available for the grab sa mple collection of the cyanide and mercurysamples. If the pressure in the piping is not excessive, the composito r can be connected to backflush the composite sample tubing direc tly back into the pi ping. An alternative approach described below is also effective, and may be necessary if the pressure in the piping system is too high for the composito r to backflush the composite sample tubing into the piping. (NOTE: If the RCC evaporator distillate sampling point has intermittent flow which may interfere with the automa tic composite collection, please contact TJ Finseth, (703) 633-1698 to disc uss possible alternatives.)

Composite Sample Collection

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

2. Clean hands and dirty hands put on T yvek® suits and powder-free gloves.

3. Dirty hands opens the outer bag of the cleanbox and clean hands opens the clear inner bags and secures the cl eanbox open with the clips located

inside the box.

4. Dirty hands opens the outer bag contai ning a length of precleaned silicone tubing, a “T” splitter, and two additi onal pieces of silicone tubing. Clean hands takes the inner bag containing the tubing and moves it into the cleanbox. Clean hands opens the inner bag and removes the tubing. Clean hands places a clean plastic bag over each end of the silicone tubing. The tubing configuration will be set up such that one end will be connected to the sample tap, one end will be thre aded through the automatic compositor and connected to the large composite container, and one end will be placed next to a sump/drain near the sampling point. To collect the samples, the sample tap will be left open during the entire sample collection time period and will flow di rectly to the sump/drain; however, the automatic compositor will pull sample from the flowing stream as dictated by the sampling program. Additionally, the automatic compositor will be capable of purging the line back to the flowing stream between each individual sample aliquot.

5. Dirty hands threads one portion of the silicone tubing through the peristaltic pump portion of the automatic compositor.

6. Dirty hands opens the outer bag of th e metals field blank water and the field blank composite container. Clea n hands opens the inner bag for the field blank water, unscrews the lid and places it in the inner bag. Clean hands then places one end of the silicone tubing into the blank water. Clean hands also opens the inner bag for the field blank composite

container and loosens the lid. Clean hands holds the silicone tubing with the plastic bag covering the end out of the cleanbox and over a bucket and dirty hands operates the pump to pump blank water through the tubing. After the tubing has been purged with sufficient volume, clean hands holds the silicone tubing at the m outh of the field blank composite container and fills the composite container with sufficient volume to

collect the total metals field blank samples at the pump -off location. Dirty hands stops the pump. During the purgi ng of the tubing and collection ofthe field blank sample volume, di rty hands pinches a portion of the silicone tubing that will be placed by the sump/drain. Clean hands places the plastic bag over the end of the si licone tubing, replaces the lid on the field blank composite cont ainer, places the silicone tubing back in the cleanbox, and closes the inner bag of th e field blank composite container. Dirty hands closes the outer bag of th e field blank composite container.

7. Clean hands holds the end of the si licone tubing outside the cleanbox over a bucket, with the plastic bag still covering the end of the tubing. Dirty hands places the end of the silicone tubing near the sump/drain and opens the sample tap valve to allow the wa stewater to flow through the tubing. Dirty hands operates the pump to pur ge the pump portion of the tubing for

a minimum of 2 minutes.

8. Dirty hands programs the automatic co mpositor to collect the 20 liters of sample over a 24-hour time period in one-hour intervals (i.e., collect 830 mL of sample every hour). Dirty hand s calibrates the compositor to ensure that 830 mL is being collected for each individual grab.

9. Dirty hands opens the outer bag of th e large composite container. Clean hands opens the inner bag and connect s the silicone tubing to the port on the composite container, securing th e connection with a cable tie. Clean hands closes the inner bag around the composite bottle, and dirty hands closes the outer bag. The samplers put ice around the composite container to keep the samples cold during the compositing time period.

10. At the end of the composite sampling period, dirty hands stops each of the automatic compositors and opens the outer bag of each composite container. For each container, clean hands opens the inner bag and detaches the used tubing from the co mposite container and covers the port with a closed lid or small plastic ba g. The samplers transport each of the composite containers, including the fiel d blank composite container, to the pump-off area to pump off the samples into the specified sample

containers.

11. The samplers then repeat steps 1 th rough 10 (skipping step 6) to collect the composite samples for the next day of sample collection.

After the composite samples have been collected, the sampling team will then transfer the sample into the individual sample containers at the pump-off area.

Sample Pump-Off Procedures

12. Arrive at the pump-off location and prepare suppl ies and bottles for the sample collection.

13. Clean hands and dirty hands put on T yvek® suits and powder-free gloves.

14. Dirty hands opens the outer bag of the cleanbox and clean hands opens the clear inner bags and secures the cl eanbox open with the clips located

inside the box.

15. Dirty hands opens the opening on the pe ristaltic pump head so the tubing can be placed in the pump head. Dirty hands opens the outer bagcontaining a length of precleaned Teflon® tubing connected to a length of precleaned silicone tubing. Clean hands moves the tubing into the cleanbox and opens the inner bag and removes the tubing. Clean hands places a clean plastic bag over the end of the Teflon® and silicone tubing.

16. Dirty hands threads the silicone tubi ng into the peristaltic pump head.

17. Dirty hands shakes the field blank co mposite container to mix the sample and then opens the outer bag of the field blank composite container and total metals field blank sample bottle. Clean hands removes the total metals field blank sample bottle and places it in the cleanbox. Clean hands opens the inner bag of the field blank composite container, removes the lid from the container, and places the end of the Teflon® tubing in the blank

water. Clean hands holds the end of the silicone tubing outside the cleanbox over a bucket, with the plastic bag still covering the end of the tubing and dirty hands operates the pump to pump about two liters of

blank water from the field blank com posite container. Clean hands places the end of the silicone tubing in th e cleanbox, opens the inner bag of the total metals field blank sample bottle, and removes the lid. Dirty hands operates the pump to collect the total metals field blank sample and then stops the pump. Clean hands closes the lid on the sample bottle and closes the inner bag. Clean hands places the i nner bag and bottle in the outer bag and dirty hands clos es the outer bag.

18. Dirty hands shakes the large composite container to mix the sample and then opens the outer bag of the larg e composite container for the metals samples and clean hands opens the in ner bag. Clean hands transfers the Teflon® tubing from the field blank composite container to the metals sample composite container. Clean ha nds holds the end of the silicone tubing outside the cleanbox over a buck et, with the plastic bag still covering the end of the tubing and dirt y hands operates the pump to pump about two liters of sample through the tubing and then stops the pump.

19. Dirty hands opens the outer bag of the total metals by EPA Method 200.8 sample bottle. Clean hands removes th e inner bag and bottle and places it in the cleanbox. Clean hands opens the inner bag and removes the lid. Dirty hands operates the pump to collect the total metals sample and then stops the pump. Clean hands closes the lid on the sample bottle and closes the inner bag. Clean hands places the i nner bag and bottle in the outer bag and dirty hands closes the outer bag. The samplers repeat the procedure to collect the total metals by EPA Method 200.7 sample.

20. The samplers operate the pump to collect the BOD 5 , Group I, and Group II samples. NOTE: The samplers do not need to use the cleanbox while collecting these samples.

Grab Sample Colletion

1. Arrive at the sampling point location and prepare supplies and bottles for the sample collection.2. Clean hands and dirty hands put on T yvek® suits, masks, and powder-free gloves.

3. Dirty hands gets a clear plastic bag and opens it slightly (touching only the outer part of the bag) so that clean hands can place hands in the bag and open the bag completely.

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

collection.

5. Dirty hands opens the outer bags of th e field blank water and total mercury and total metals field blank sample bottles. Clean hands opens the inner bag of the field blank water and unscrew s the lid. Clean hands then opens the inner bag of the total mercury an d total metals field blank sample bottles. Clean hands pours the blank water into the field blank sample bottles under the shrouding, caps the bottles, and clos es the inner bags. Clean hands then places the total mercury and total metals bottles in the outer bags and dirty hands closes the outer bags.

6. Dirty hands then opens the valve to th e sample tap and purges the tap for at least two minutes, then keeps the valv e open until all samples have been

collected.

7. Dirty hands opens the outer bag for the total mercury sample bottle. Clean hands takes the sample bottle and inner bag and holds them under the shroud. Clean hands then opens the i nner bag, opens the lid of the bottle and fills the total mercury sample bottle. Clean hands caps the sample bottle, closes the inner bag, and places the sample bottle in the outer bag. Dirty hands closes the outer bag. The samplers repeat this procedure for

the collection of the to tal metals samples (both EPA 200.8 with collision cell and EPA 200.7), unless the plant is collecting the metals samples as composite samples.

8. The samplers then collect the BOD, Group I, Group II, and total cyanide samples. NOTE: the samplers can collect these samples using the same technique as the mercury and metals samples, or they can remove the plastic bag shrouding and collect directly from the tap.

9. The Group II and total cyanide samples must be preserved prior to shipment to the laboratories. Use th e information provided in the “Sample

Bottles and Preservation” section of th ese instruction for the preservation steps. Additionally, the BOD, Group I, Group II, and total cyanide samples should be placed on ice immediately afte r sample collection/preservation.

Sample Packing and Shipment

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

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

2. Tighten the lid on each filled sample bottle, being careful not to overtighten the lid. If bo ttle threads are dirty to where the lid is impeded from closing, clean the threads on th e bottle being careful to not introduce contamination into the sample. Clean the sample bottle with a cloth rag or paper towel.

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

into an ice chest with wet ice to cool.

4. When each sample requiring ≤ 6°C preservation has reached the desired temperature, wrap each glass sample bottle with two layers of “bubble wrap” (or place bottle in two “bubble bags”). The bubble wrap must fit snugly and completely cover the sa mple bottle. Enclose each “bubblewrapped” container and pl astic container in an in dividual sealable plastic freezer bag.

5. Place two garbage bags inside each ot her in each of the coolers used to ship samples to the laboratories.

6. Place the classicals samples in the garb age bags in the coolers with proper end up, close the interior garbage ba g by tying, or with a twist-tie.

7. Add ice to the cooler to keep sample s cold during shipment. Arrange blue ice or sealed plastic freezer bags fill ed 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 fre ezer bags. Put at least 4 × 1⁄2 gallons of ice (4 × 2.5 pounds of ice) in each large cooler and 2 × 1⁄2 gallons of ice (2 × 2.5 pounds of ice) in each small cooler. Use more ice when ambient temperatures are very high. Place the ice inside the second garbage bag.

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

9. Place the metals samples in the garbage bags in a different cooler with proper end up, close the interior garbag e bag by tying or with a twist-tie. Close the second garbage bag by tying, or with a twist-tie. NOTE: the metals samples are not required to be cooled; however, because the metals and classicals are being analyzed by the same laboratory, the metals can be shipped with the classicals, but th e metals samples would need to be chilled prior to packing them in the cooler with the classicals and ice

would need to be added to the cool er between the interior and outer garbage bags to keep the samples cold.

10. Fill in any free space aro und the bottles in the metals and classicals coolers with additional cushioning mate rial. Sufficient packing material should be used so that the sample containers will not shift during shipment.

11. Fill out and print a traffic report form for the classicals and metals samples (provided electronically by ERG). Seal the last two pages of the traffic report form(s) in a plastic envelope secu red to the inside of the top of the cooler(s). NOTE: the top page of the tr affic report must be sent to ERG at the following address:Eastern Research Group 14555 Avion Parkway, Suite 200 Chantilly, VA 20151

Attn: TJ Finseth (703) 633-1698

12. Close the cooler(s).

13. Place a completed laboratory address labe l on the lid of the cooler(s). The classicals and metals samples shoul d be shipped to TestAmerica as

follows:

TestAmerica

4955 Yarrow Street Arvada, CO 80002 Attn: Elizabeth Eichelberger (303) 736-0100

14. Make several wraps with strapping tape around the cooler perpendicular to the seal to ensure that the lid will remain closed if the latch is accidentally released or damaged.

15. Place the mercury samples in the garbage bags in a separate cooler with proper end up, close the interior garbag e 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 bot tles 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 in side of the top of the cooler. NOTE: the top page of the traffic report must be sent to ERG at the same address provided in step 11:

19. Close the cooler.

20. Place a completed laboratory address la bel on the lid of the cooler. The mercury samples should be shipped to Frontier as follows:

Frontier GeoSciences

414 Pontius Ave. North Seattle, WA 98109

Attn: Patrick Garcia-Strickland (206) 957-1428

21. Make several wraps with strapping tape around the cooler perpendicular to the seal to ensure that the lid will remain closed if the latch is accidentally released or damaged.22. Fill out the necessary paperwork for FedEx or UPS to prepare the shipment for pick up or drop off. NOTE: the samples must be shipped priority overnight to arri ve at the laboratories the following morning. Ship

the coolers to the laboratories.

23. After the coolers have been dropped o ff (or picked up), please contact TJ Finseth at (703) 633-1698, to notify him that the samples have been shipped to the laboratories.

Traffic Reports

An example traffic report will be provided to the plant by ERG for the first grab sample collection event. The plant will need to make changes to the traffic report electronically for the other three sample collection events. Some information, such as the date and sample collection times must be entered by the plant after the sample collection and therefore, will not be included in the example provided by ERG.

After the traffic report is completed by the plant, the plant must print the four pages in the file. The last two pages in the file must be placed in the cooler for shipment to the laboratories and the first page must be sent to ERG. The plant can keep the second page of the traffic report.

Engineering Data and Process Flow Diagram

The plant must provide engi neering data regarding the operation of the plant and gasification wastewater tr eatment system during the sample collection period. Additionally, the plant must ma ke some field measurements when samples are collected, including pH, temperature, and visual observa tions, and provide the data to EPA after the sample collection period. The engineering da ta and field measurement data requirements are in an Excel® spreadsheet titled “Monitori ng Program Engineering Data Tables.” The

tables are also included at the end of this enclosure. The plant must also submit a detailed process flow diagram for the sour water and vapor crystallizer (RCC) systems, annotated to indicate the location of each sampling point . The process flow diagram must present sufficient detail to depict each process flow stream (influent, effluent, and recycle streams) associated with or contributing direct ly or indirectly to the sour water stream and the evaporator distillate streams. The plan t must complete the engineering data sheets

and field measurement sheets in the Excel® file and e-mail the completed forms, along with the process flow diagram, to TJ Finseth at thomas.finseth@erg.com . Note that any

information claimed as confidential business information (CBI) must not be sent by email and must instead be sent via U.S. posta l service or by courier (e.g., Federal Express).

Certification Statement

The individual responsible for directing a nd supervising the sample collection and the engineering data preparation must sign the ce rtification statement (provided in Enclosure 4) and submit it upon the completion of the sampling program. The signed certificationstatement 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 1 - Grab 1Set 1 - Grab 2Set 1 - Grab 3Set 1 - Grab 4Set 2 - Grab 1Set 2 - Grab 2Set 2 - Grab 3Set 2 - Grab 4Set 3 - Grab 1Set 3 - Grab 2Set 3 - Grab 3Set 3 - Grab 4Set 4 - Grab 1Set 4 - Grab 2Set 4 - Grab 3Set 4 - Grab 4NOTE: For influent (sour water) samples, only the grab 1 row needs to be completed.Plant NameSampleCollectionNumberSour WaterSamplesCollected asGrabs(Yes or No)Mercury and CyanideSamples Collected asGrabs(Yes or No)RCC DistillateSamples (ExceptMercury & Cyanide)Collected as 24-HourComposites(Yes or No)Tyvek Suits used(Yes or No)Dust MasksUsed forMercury(Yes or No)CleanHands/DirtyHandsSamplingTechniquesUsed(Yes or No)Description ofSample CollectionTechnique (ifdifferent thaninstructions)Description ofAbnormal Conditions inGasifier, Sour Water, orVapor Crystallizer (RCC)Systems that MayImpactProcess/WastewaterCharacteristicsSet 1Set 2Set 3Set 4Daily Power Generation (MW-hrs)

Plant Name Date Provide the daily power generation for the IGCC unit starting two weeks prior to the first set of samples through the last set of samplesSour Water Feed toTreatment(D-162)Sour Water Feed toTreatment(E-166A/B)Sour Water Returnfrom Sulfur Recovery(V-241)Sour Water Feed toSulfur Recovery(C-240)Sour Water Feed toVapor Crystallizer(RCC) Evaporator(E-277)Sour Water toSlurry Makeup(T-100)Brine from BrineCollection Tank T279 to Drum DryerRCC EvaporatorDistillateProvide the average flow rate in the Gasification 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 samplesBrine SolidsOutput from DrumDryer (tons/day)Plant Name DateSour Water & Treatment System Flow Rates(gpd)Enclosure 2

Authority

This request for information is made under auth ority provided by Secti on 308 of the Federal Water Pollution Control Act, as amended, 33 US C 1318. Section 308 provides that, "Whenever required to carry out the objective of this Act, including but not limited to . . . developing or assisting in the development of any effluent limita tion . . . pretreatment standard, or standard of performance under this Act," the Administrator shall require the owner or operator of any point source to "establish and maintain such records, . . make such reports, . . install, use, and maintain such monitoring equipment . . . sample such efflue nt . . . and provide such other information as he may reasonably require."

Confidentiality

A business ("you") may not withhold informa tion from EPA on the grounds that it is confidential. You may, however, if you desire, assert a busine ss confidentiality claim covering part or all of the informati on that you furnish to EPA.

EPA regulations concerning confidential business information are contained in 40 CFR Part 2, Subpart B. The manner of asserting such a clai m is specified in 40 CFR 2.203(b). Information covered by such a claim will be disclosed by EPA only to the extent, and by means of the procedures, set forth in Subpart B.

If you wish to claim as confidential any of th e information covered by the enclosed request, you must do so at the time you submit the information to EPA. If no such claim accompanies the information when EPA receives it, EPA may make the information available to the public without further notice to you.

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

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

not such information is entitled to confidential tr eatment. At that time, EPA will request that you substantiate any claim you have ma de that information is confiden tial. Therefore, we encourage you to consult 40 CFR Part 2, and to claim as c onfidential only those item s that you truly believe satisfy the criteria for confidentiality.

Note that effluent data ar e not eligible for confiden tial treatment (see 40 CFR 2.302).Enclosure 3

Notice of Intent to Transfer Confidential Information to Selected EPA Contractors

EPA intends to grant access to confidential information collected under this wastewater sampling program to selected EPA contractors.

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

allow those contractors identif ied below access to all data (i ncluding data claimed to be confidential) collected as part of the sampling 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 Stea m Electric Power Generating industry.

The contractors and subcontractor s that will be providing suppor t to EPA during the development of these regulations are listed below:

EPA Office

Receiving

Support Contractor Name EPA Contract

No. Type of Support

Eastern Research Group,

Inc. 68-C-02-095 Engineering analysis Office of Water/

Office of

Science & Technology/ Engineering & Analysis

Division Westat EP-C-10-023 Statistical analysis

EPA has determined that it is necessary to tr ansfer the information described above to the designated contractors and subcont ractors in order that they ma y 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 regulati ons, you are entitled to provide comments to EPA regarding this notice of contempl ated disclosure. Any such co mments must be received by EPA in writing within 10 days of your receipt of this notice. Please send such comments to:

Ronald Jordan USEPA Headquarters Ariel Rios Building 1200 Pennsylvania Ave., N.W.

Mail Code: 4303T Washington, DC 20460 jordan.ronald@epa.govEnclosure 4

Certification Statement

The individual responsible for di recting or supervising the sample collection and engineering data preparation for the sampling program must read a nd sign the Certification Statement listed below. The certifying official must be a responsible corporate official or his/her authorized representative.

Certification Statement

I certify under penalty of law that the samples collected for the sampling program were collected under my direction or supervis ion, that qualified personnel colle cted the samples following the procedures described in the in structions (including the use of clean hands/dirty hands sampling techniques described in EPA Me thod 1669), that qualified pers onnel gathered the engineering data required, and that the sampling and engineeri ng data provided are complete and reflect normal operations for this plant. The engineer ing data submitted are, to the best of my knowledge and belief, accurate and complete. In those cases where we did not possess direct measurement, we provided best estimates. We ha ve to the best of our ab ility indicated what we believe to be company confiden tial business information as de fined under 40 CFR Part 2, Subpart B. We understand that we may be required at a later time to just ify 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 possibili ty of fines and imprisonment as explained in Section 308 of the Clean Water Act.

Signature of Certifying Official Date

( ) Printed Name of Certifying Official Telephone Number of Certifying Official

Title of Certifying Official

Company Name