Enclosure 1 

Instructions for Sample Collection, Packaging, and Shipment 

EPA Sampling Program

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

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

guidelines and standards for the Steam Electric Power Generating Industry. 

These instructions are being provided to TECO Energy’s Polk 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 neutralized weak acid stream 

and the influent to the vapor compression evaporator sampling points and 24-hour 

composite samples for all analytes except mercury and cyanide at the vapor compression 

evaporator condensate and the forced circulation evaporator brine condensate sampling 

points. At the sampling points for the vapor compression evaporator condensate and 

forced circulation evaporator brine condensate, the plant must collect cyanide as a single 

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

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

Samples must be collected Monday through Thursday during the week of October 18, 

2010. If the plant has any questions regarding the timeline or the steps provided, please 

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

Equipment Needed

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

samples to the laboratories: 

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

according to EPA Method 1669); 

• Automatic compositor; 

• Powder-free gloves; 

• Tyvek® coveralls or suitable alternative; 

• Dust masks (for use while collecting mercury samples) 

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

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

• Coolers; 

• Garbage bags; 

• Packing material; 

• Strapping tape; and 

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

The plant must collect samples Monday through Thursday during the week of October 

18, 2010 from each of the four sampling points specified below. Figures 1 and 2 identify 

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

the four sampling points: 

• Neutralized Weak Acid Stream (SP-1): This sampling point shall represent the 

weak acid stream entering the Grey Water Surge Tank from the sulfuric acid 

plant. This sample should be collected from the sample tap that is located on the 

pipe that transfers the weak acid stream to the Grey Water Surge Tank. 

• Influent to the Vapor Compression Evaporator (SP-2): This sampling point 

shall represent the waste stream exiting the Grey Water Surge Tank for transfer to 

the vapor compression evaporator. This sample should be collected from the 

sample tap that is located on the pipe that transfers the water from the Grey Water 

Surge Tank to the vapor compression evaporator. [Note: This sample should not 

be collected directly from the Grey Water Surge Tank.] 

• Vapor Compression Evaporator Condensate (SP-3): This sampling point shall 

represent the condensate stream from the vapor compression evaporator. This 

sample should be collected from the sample tap that is located on the pipe exiting 

the Condensate Storage Tank and returning the condensate to pump seals, 

instrument tap flushes, and the slag screen. 

• Forced Circulation Evaporator Brine Condensate (SP-4): This sampling point 

shall represent the condensate stream from the forced circulation evaporator. 

This sample should be collected from the sample tap that is located on the pipe 

exiting the Forced Circulation Evaporator and returning the condensate to slurry 

preparation. 

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 Analytical Methods Included in the Sampling Program 

Parameter Method Number 

Classicals

Biochemical oxygen demand (BOD5) SM 5210 B 

Chemical oxygen demand (COD) EPA 410.4 

Total suspended solids (TSS) SM 2540 D 

Total dissolved solids (TDS) SM 2540 C 

Sulfate EPA 300.0 

Chloride EPA 300.0 

Ammonia as nitrogen EPA 350.1 

Nitrate/nitrate as nitrogen EPA 353.2 

Total Kjeldahl nitrogen (TKN) EPA 351.2 

Total phosphorus EPA 365.1 

Total cyanide SM 4500 CN E 

Total Metals

Total mercury EPA 1631E 

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

selenium, silver, thallium, and vanadium 

EPA 200.8 with collision 

cell 

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

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

zinc 

EPA 200.7 
Figure 1. Polk Grey Water Evaporator Sampling Points
Figure 2. Polk Forced Circulation Evaporator Sampling Points 
Sample Bottles and Preservation

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

cyanide. 

Table 2. Summary of Sample Container and Planned Preservation 

Parameter 

Sample Container 

and Volume On-Site Preservation 

BOD5 One 1-L HDPE bottle ≤6°C 

Group I a One 1-L HDPE bottle ≤6°C 

Group II b Two 1-L HDPE 

bottles 

H2SO4 to pH <2, ≤6°C 

Total cyanide One 1-L HDPE bottle Dilution until sulfide is not detected, 

NaAsO2 until total chlorine is not 

present, NaOH to pH >10, ≤6°C 

Total metals (EPA Method 200.8 with collision 

cell) 

One 500-mL HDPE 

bottle 

None 

(acid preserve at laboratory) 

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

bottle 

None 

(acid preserve at laboratory) 

Total mercury: 

Laboratory composite grab samples at the 

vapor compression evaporator condensate and 

forced circulation evaporator brine condensate

Four 125-mL glass 

bottles 

Neutralized weak acid stream and influent to 

the vapor compression evaporator samples 

and field blank samples 

Two 250-mL glass 

bottles 

None 

(acid preserve at laboratory) 

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

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

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

the four sets of samples. 
Sample Labeling

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

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

following information: 

• Sample number (see Table 3); 

• Sampling episode number (see Table 3); 

• Sampling point/description (see Table 3); 

• Date of sample collection; 

• Analysis to be performed; 

• Sample bottle type; and 

• Required on-site preservation. 

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

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

prevent tampering, abrasion, smearing, or loss during transit. For 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 outer plastic bag of the sample bottle. To 

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

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 descriptions, sample numbers, and sampling episode 

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

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

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

analysis: 

• BOD; 

• Group I; 

• Group II; 

• Total Cyanide; 

• Total Metals – 200.8 w/ CC; 

• Total Metals – 200.7; 

• Total Mercury (for neutralized weak acid stream, influent to the vapor 

compression evaporator, and field blank samples); and 

• Total Mercury – Grab 1 (for vapor compression evaporator condensate 

and forced circulation evaporator brine condensate laboratory composite 

samples. The bottles should be labeled as Grab 1, Grab 2, Grab 3, and 

Grab 4 for the four respective collection times). 
The “sample bottle type” should be shown on the label the same as the “Sample 

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

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

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

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

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

bottles. 

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

 

Sampling Point Description 

Sample 

Number 

Sampling 

Episode Number

Neutralized Weak Acid Stream - Set 1 72391 6573 

Neutralized Weak Acid Stream - Set 2 72392 6573 

Neutralized Weak Acid Stream - Set 3 72393 6573 

Neutralized Weak Acid Stream - Set 4 72394 6573 

Influent to Vapor Compression Evaporator - Set 1 72395 6573 

Influent to Vapor Compression Evaporator - Set 2 72396 6573 

Influent to Vapor Compression Evaporator - Set 3 72397 6573 

Influent to Vapor Compression Evaporator - Set 4 72398 6573 

Vapor Compression Evaporator Condensate - Set 1 72399 6573 

Vapor Compression Evaporator Condensate - Set 2 72400 6573 

Vapor Compression Evaporator Condensate - Set 3 72401 6573 

Vapor Compression Evaporator Condensate - Set 4 72402 6573 

Forced Circulation Evaporator Brine Condensate - Set 1 72403 6573 

Forced Circulation Evaporator Brine Condensate - Set 2 72404 6573 

Forced Circulation Evaporator Brine Condensate - Set 3 72405 6573 

Forced Circulation Evaporator Brine Condensate - Set 4 72406 6573 

Neutralized Weak Acid Stream Field Blank 72407 6573 

Influent to Vapor Compression Evaporator Field Blank 72408 6573 

Vapor Compression Evaporator Condensate Field Blank - Set 1 72409 6573 

Vapor Compression Evaporator Condensate Field Blank - Set 2 72410 6573 

Vapor Compression Evaporator Condensate Field Blank - Set 3 72411 6573 

Vapor Compression Evaporator Condensate Field Blank - Set 4 72412 6573 

Forced Circulation Evaporator Brine Condensate Field Blank - Set 1 72413 6573 

Forced Circulation Evaporator Brine Condensate Field Blank - Set 2 72414 6573 

Forced Circulation Evaporator Brine Condensate Field Blank - Set 3 72415 6573 

Forced Circulation Evaporator Brine Condensate Field Blank - Set 4 72416 6573 

QC Samples

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

field blank samples should be collected at the frequency specified in Table 4. 
Table 4. Field Blank Collection Frequency 

Sampling Point Total Mercury 

Total Metals (200.8 

and 200.7) Classicals1 

Neutralized Weak Acid 

stream 

Collected during one 

of the four sets 

Collected during one 

of the four sets 

No field blanks 

required 

Influent to the Vapor 

Compression Evaporator 

Collected during one 

of the four sets 

Collected during one 

of the four sets 

No field blanks 

required 

Vapor Compression 

Evaporator Condensate 

Collected once during 

each of the four sets 

Collected during one 

of the four sets2 

No field blanks 

required 

Forced Circulation 

Evaporator Brine 

Condensate 

Collected once during 

each of the four sets 

Collected during one 

of the four sets2 

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 sample sets, but the plant must use the sample number 

and sampling point description associated with the correct sample set (e.g., Vapor Compression Evaporator 

Condensate Field Blank – Set 2 – sample number 72410 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 team should follow the clean hands/dirty hands 

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

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

airborne particles, dirt, and corrosion particulates from piping, railing, etc. 

The plant must collect grab samples for all analytes at the neutralized weak acid stream 

and influent to the vapor compression evaporator sampling points. The plant must collect 

24-hour composite samples for all analytes except cyanide and mercury at the vapor 

compression evaporator condensate and forced circulation evaporator brine condensate 

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

every hour over the 24-hour period. For mercury at the vapor compression evaporator 

condensate and forced circulation evaporator brine condensate sampling points, the plant 

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

collected every six hours). For cyanide at the vapor compression evaporator condensate 

and forced circulation evaporator brine condensate sampling points, the plant must collect 

a single grab sample after one of the mercury grab samples. 

If the plant is able to collect the samples 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 

vapor compression evaporator condensate and forced circulation evaporator brine 

condensate sampling points. This section also provides instructions to collect the grab 

samples at the neutralized weak acid stream and influent to the vapor compression 

evaporator sampling points and for the mercury and cyanide grab samples at the vapor 
compression evaporator condensate and forced circulation evaporator brine condensate 

sampling points. Please note that the plant will need to install a two-way splitter on the 

tap to allow for the composite tubing to be connected to the tap and also have a tap 

available for the grab sample collection of the cyanide and mercury samples. 

Additionally, the description below assumes that the sample lines are pressurized and 

therefore would not allow the compositor to backflush the composite tubing directly into 

the sample line (NOTE: If a sample tap or valve is not available to collect these samples or 

if the vapor compression evaporator condensate and forced circulation evaporator brine 

condensate sampling points have intermittent flows which may interfere with the 

automatic composite collection, please contact TJ Finseth, (703) 633-1698 to discuss 

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 Tyvek® 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 cleanbox open with the clips located 

inside the box. 

4. Dirty hands opens the outer bag containing a length of precleaned silicone 

tubing, a “T” splitter, and two additional 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 threaded 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 directly 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 the metals field blank water and the 

field blank composite container. Clean 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 mouth 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 purging of the tubing and collection of 

the field blank sample volume, dirty 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 silicone tubing, replaces the lid on the 

field blank composite container, places the silicone tubing back in the 

cleanbox, and closes the inner bag of the field blank composite container. 

Dirty hands closes the outer bag of the field blank composite container. 

7. 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. Dirty 

hands places the end of the silicone tubing near the sump/drain and opens 

the sample tap valve to allow the wastewater to flow through the tubing. 

Dirty hands operates the pump to purge the pump portion of the tubing for 

a minimum of 2 minutes. 

8. Dirty hands programs the automatic compositor 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 hands calibrates the compositor to ensure 

that 830 mL is being collected for each individual grab. 

9. Dirty hands opens the outer bag of the large composite container. Clean 

hands opens the inner bag and connects the silicone tubing to the port on 

the composite container, securing the 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 composite container and covers the port 

with a closed lid or small plastic bag. The samplers transport each of the 

composite containers, including the field 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 through 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 supplies and bottles for the 

sample collection. 

13. Clean hands and dirty hands put on Tyvek® 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 cleanbox open with the clips located 

inside the box. 

15. Dirty hands opens the opening on the peristaltic pump head so the tubing 

can be placed in the pump head. Dirty hands opens the outer bag 

containing 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 tubing into the peristaltic pump head. 

17. Dirty hands shakes the field blank composite 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 composite container. Clean hands places 

the end of the silicone tubing in the 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 inner bag and bottle in the outer bag 

and dirty hands closes the outer bag. 

18. Dirty hands shakes the large composite container to mix the sample and 

then opens the outer bag of the large composite container for the metals 

samples and clean hands opens the inner bag. Clean hands transfers the 

Teflon® tubing from the field blank composite container to the metals 

sample composite container. 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 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 the 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 inner 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 BOD5, 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 Tyvek® suits, masks, and powder-free 

gloves. 

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

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

open the bag completely. 

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

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

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

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

collection. 

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

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

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

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

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

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

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

outer bags and dirty hands closes the outer bags. 

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

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

collected. 

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

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

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

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

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

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

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

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

composite samples. 

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

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

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

plastic bag shrouding and collect directly from the tap. 

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

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

Bottles and Preservation” section of these instruction for the preservation 

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

should be placed on ice immediately after sample collection/preservation. 
Sample Packing and Shipment

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

laboratories. 

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

specifies the sample point. 

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

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

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

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

paper towel. 

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

into an ice chest with wet ice to cool. 

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

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

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

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

freezer bag. 

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

ship samples to the laboratories. 

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

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

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

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

bottles (if samples require ≤6°C preservation). If using wet ice, place the 

ice inside two one-gallon sealable freezer bags. Put at least 4 × 1⁄2 gallons 

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

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

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

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

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

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

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

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

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

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

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

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

garbage bags to keep the samples cold. 

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

coolers with additional cushioning material. Sufficient packing material 

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

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

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

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

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

the following address: 

 Eastern Research Group 

 14555 Avion Parkway, Suite 200 

 Chantilly, VA 20151 

 Attn: TJ Finseth 

 (703) 633-1698 

12. Close the cooler(s). 

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

classicals and metals samples should be shipped to TestAmerica as 

follows: 

 TestAmerica 

 4955 Yarrow Street 

 Arvada, CO 80002 

 Attn: Elizabeth Eichelberger 

 (303) 736-0100 

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

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

released or damaged. 

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

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

16. Do not add ice to the mercury cooler; simply close the second garbage bag 

by tying, or with a twist-tie. 

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

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

containers will not shift during shipment. 

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

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

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

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

provided in step 11: 

19. Close the cooler. 

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

mercury samples should be shipped to Frontier as follows: 
 Frontier GeoSciences 

 414 Pontius Ave. North 

 Seattle, WA 98109 

 Attn: Patrick Garcia-Strickland 

 (206) 957-1428 

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

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

released or damaged. 

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

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

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

the coolers to the laboratories. 

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

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

shipped to the laboratories. 

Traffic Reports

An example traffic report will be provided to the plant by ERG for the first 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 engineering data regarding the operation of the plant and 

evaporator systems during the sample collection period. Additionally, the plant must 

make some field measurements when samples are collected, including pH, temperature, 

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

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

spreadsheet titled “Monitoring Program Engineering Data Tables.” The tables are also 

included at the end of this enclosure. The plant must also submit a detailed process flow 

diagram for the grey water and treatment 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 directly or indirectly to the grey water stream and the evaporator condensate 

streams. The plant 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 e-mail and must instead be 

sent via U.S. postal service or by courier (e.g., Federal Express). 

Certification Statement 

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

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

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

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

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

Plant Name

Sample 

Collection 

Number

Date of Sample 

Collection

Sample Collection 

Time Temperature (°C)

pH

(S.U.)

Set 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 4

NOTE: For influent samples, only the grab 1 row needs to be completed.

Plant Name

Sample 

Collection 

Number

Weak Acid and 

Grey Water 

Samples 

Collected as 

Grabs

(Yes or No)

Mercury and Cyanide 

Samples Collected as 

Grabs

(Yes or No)

Condensate Samples 

(Except Mercury & 

Cyanide) Collected as 

24-Hour Composites

(Yes or No)

Tyvek Suits used

(Yes or No)

Dust Masks 

Used for 

Mercury 

(Yes or No)

Clean 

Hands/Dirty 

Hands 

Sampling 

Techniques 

Used

(Yes or No)

Descript

Sample Co

Techniq

different 

instruct

Set 1Set 2Set 3Set 4
Daily Power Generation (MW-hrs)

Plant Name Date Unit 1

Provide the daily power generation for the IGCC unit starting two weeks prior to the first set of 

samples through the last set of samples
Neutralized 

Weak Acid 

Stream to Grey 

Water Surge 

Tank

Condensate to 

Grey Water 

Surge Tank 

from Vacuum 

Flash Overhead 

Condenser

Settler Overflow 

to Grey Water 

Surge Tank

Grey Water 

Surge Tank 

Feed to Vapor 

Compression 

Evaporator

Grey Water 

Surge Tank 

Feed to Syngas 

Scrubbers

Concentrated 

Brine Feed to 

Forced 

Circulation 

Evaporator 

(from Vapor 

Compression 

Evap)

Condensate 

from Vapor 

Compression 

Evaporator

Plant Name Date 

Provide the average flow rate in the gasification/wastewater treatment system for each stream included in the table starting two weeks prior to the first through the last set of samples

Gasification/Wastewater Treatment System Flow Rates

(gpd)
Enclosure 2 

Authority

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

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

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

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

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

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

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

he may reasonably require." 

Confidentiality

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

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

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

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

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

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

procedures, set forth in Subpart B. 

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

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

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

without further notice to you. 

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

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

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

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

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

satisfy the criteria for confidentiality. 

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

Notice of Intent to Transfer Confidential Information to Selected EPA Contractors

EPA intends to grant access to confidential information collected under 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 identified below access to all data (including 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 contractors to assist EPA in performing technical, 

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

guidelines and standards for the Steam Electric Power Generating industry. 

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

of these regulations are listed below: 

EPA Office 

Receiving 

Support 

Contractor Name EPA Contract 

No. Type of Support 

Eastern Research Group, 

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

Science & 

Technology/ 

Engineering & 

Analysis 

Division 

Westat EP-C-10-023 Statistical analysis 

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

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

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

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

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

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

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

Ronald Jordan 

USEPA Headquarters 

Ariel Rios Building 

1200 Pennsylvania Ave., N.W. 

Mail Code: 4303T 

Washington, DC 20460 

jordan.ronald@epa.gov
Enclosure 4 

Certification Statement 

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

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

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

representative. 

Certification Statement 

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

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

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

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

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

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

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

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

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

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

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

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

Section 308 of the Clean Water Act.

 

Signature of Certifying Official Date 

( ) 

Printed Name of Certifying Official Telephone Number of Certifying Official 

 

Title of Certifying Official 

Company Name