Instructions for Sample Collection, Packaging, and Shipping EPA Method Study

The samples you will be collecting are very important. The samples will be used for a U.S. Environmental Protection Agency (EPA) study of several methods that measure metals in flue gas desulphurization (FGD) wastewaters

.
These instructions are being provided to the Progress Energy Carolinas’ Roxboro Steam Electric Plant to aid in the sample collection, packa ging, and shipping of samples col lected for EPA ’s method optimization study . Step

- by

- step instructions are provided below to aid the sampl ing team in the preparation of the samples.

The samples should be collected and shipped to the laborator ies no later than Thursday, November 1 9 , 2009

. I f the plant has any questions r egarding the ti meline or the steps provided, please contact TJ Finseth

, at Eastern Research Group (technical contractor to the EPA) at (703) 633

- 1698 or Thomas.Finseth@erg.com

.
Equipment Needed

The following equipment will be needed to collect, pack , and ship the samples to the laboratories :

Items Provided by EPA in Cooler Items Provided by Albion Environmental

**•** Gloves Additional Items Needed

**•** 10

- L carboy (3) **•** Paper towels

**•** 1

- L plastic bottles (pre

labeled) (24) **•** 20

- L carboy (1) **•** Clean, plastic 5

- gallon buc ket (if a sample tap is not available) **•** Shipping cooler

**•** Garbage bags (4) **•** Garbage bags (4)

**•** Packing material **•** Packing material **•** Clean Funnel (if a sample tap is not available and if needed) **•** Strapping tape **•** Strapping tape

**•** Traffic report (partially comple te) **•** Traffic report (partially complete)

**•** Laboratory address label **•** Albion address label

**•** FedEx airbill (partially complete) **•** FedEx airbill (partially complete)

**•** FedEx pouch

Sampling Overview

The plant should collect a total of eight 1

- L bottles for e ach of the following sampling points for the FGD wastewater treatment system:

**•** FGD wastewater treatment influent ( FGD scrubber purge ) : This sampling point should represent the FGD purge stream (e.g., hydroclone overflow) transferred to the FGD wastewater t reatment system prior to any commingling with other wastewaters. Note: if the plant operates an equalization tank thatreceives recycle streams from the treatment system (e.g., filter press filtrate), then collect the FGD scrubber purge sample prior to th e stream entering the equalization tank.

**•** FGD wastewater treatment mid point : This sampling point should represent the effluent from the settling pond system and the influent to the biological treatment system (prior to nutrient addition).

**•** FGD wastewater treatment effluent : This sampling point should represent the effluent from the biological treatment system.

Sampling Points, Sample Containers, and Sample Volumes

Sampling Point Sample Container and Volume
FGD wastewater treatment influent Eight 1

- L p lastic bottles FGD wastewater treatment mid point Eight 1

- L plastic bottles
FGD wastewater treatment effluent Eight 1

- L plastic bottles

Sample Labeling

The bottles provided for the sample collection are already pre

- labeled. Please remove the sample b ottles from the cooler and organize by the sampling point specified on the label. The bottles can be filled directly with sample, no preparation (e.g.

, rinsing) is needed.



## Sample Collection Instructions

General Instructions It is NOT necessary to use cl ean sampling techniques when collecting the samples for the optimization study; however, the sampling team should try to avoid significant contamination during sample collection, especially from sources such as dust, rust, and corrosion particulates from p iping, railing, etc. Use the following techniques to minimize contamination during sample collection.

1. Wear a new pair of powder

- free gloves whenever you are involved in sample collection or sub

- sampling activities. Change the gloves whenever you feel they may have become contaminated with particulates, etc. Be sure clothing of the sampling team is free of loose dust, etc. Remove all jewelry, watches and other metallic items from your hands and arms before handling any sampling equipment. 2. Keep all carboys, sample bottles and equipment inside the plastic bags provided to minimize dust and other particulate contamination. 3. Uncap sample bottles only long enough to receive the sample. Re

- cap the bottle immediately after the sample collection acti vity is completed.

EPA is requesting that the samples be collected as split samples to produce eight samples that are as similar as possible. The samples need to be similar in composition because they will be analyzed by different laboratories and the re sults will be compared. Tocollect the split samples, the FGD wastewater will first be collected into a large composite container (i.e., carboy ) and then sub

- sampled into the individual 1

- L sample bottles

. There is a modified technique for collecting the FGD wastewater treatment influent samples which is described in the step by step instructions. However, the same sub

- sampling technique should be used for all samples, regardless of the technique used to collect the sample in the large composite containe r. The specific instructions are described below.

Collecting the L arge Volume Composite Sample for FGD Wastewater Treatment Mid

- Point and FGD Wastewater Treatment Effluent :

If sampling from a valve or tap, collect the large vol ume composite sample as follows : (NOTE: If a sample tap or valve is not available to collect this sample, please contact TJ Finseth, (703) 633

- 1698 to discuss possible alternatives .)

1. Wear powder

- free gloves provided whenever performing any sample collection activities. 2. Use the 10

- L plastic carboys provided to collect the composite FGD wastewater treatment mid

- point and FGD wastewater treatmen t effluent samples. NOTE: Do

not use the 20

- L plastic carboy for the mid

- point or effluent sample s . The 20

- L carboy will be used to coll ect the large volume composite sample for the FGD

wastewater treatment influent 3. Be sure the sampling tap or other sampling location is clean and free from loose particulates. If necessary clean the tap with a lint

- free towel a nd distilled water. ( i.e., FGD scrubber purge )

.

4. Purge the tap for several minutes to remove particulates from the inside of the tap line. 5. If there is any concern about particles falling into the carboy during filling, then shroud the tap with one of the Ziploc bags provided.
6. Place th e carboy under the shrouded tap, remove the cap (put the cap into the original bag during filling to avoid contamination) and fill the carboy from the flowing tap.
7. Remove the carboy from the flowing tap stream and fully tighten the cap. 8. Rinse the outside o f the capped carboy as needed with tap water. Avoid getting any water into the threads of the cap. 9. Place the carboy back in the original plastic bag in which it came and take the carboy to the location where split sample sub

- sampling will be performed.

C ollecting the Large Volume Composite Sample for FGD Wastewater Treatment Influent :

A special sampling approach is recommended for collecting the liquid phase of the FGD wastewater treatment influent waste water for the optimization study , due to the poten tial of higher solids in this wastestream. For the collection of the FGD influent sample, the large volume composite sample should be collected as follows:(NOTE: If a sample tap or valve is not available to collect this sample, please contact TJ Finseth , (703) 633

- 1698, to discuss possible alternatives.)

1. Follow the same steps as described for the collection of the FGD wastewater treatment effluent, except f ill the 20

- L plastic carboy with FGD wastewater

treatment influent rather than the 10

- L carboy. 2. T ake the carboy to the location where split sample sub

- sampling will be performed

. 3. Allow the solids in the 20

- L carboy to settle for 1

- 2 hours so that the upper part of the FGD wastewater sample becomes fairly clear. 4. Wear powder

- free gloves provided when pe rforming any sampling activities. 5. Slowly decant the liquid in the 20

- L carboy into a clean 10

- L carboy and fill to the neck , taking special car e to not disrupt the solids that may have settled in the bottom of the 20

- L carboy

. NOTE: a clean, plastic funnel can be used to transfer the sample to the 10

- L carboy, if available.

Sub

- Sampling Large Volume Composite into Eight 1

- L Bottles : Each large volume composite sample must be subdivided into eight 1

- L equivalent splits. The following steps should be carefu lly conducted on each large volume sample

. Take care to use the appropriate bottles (e.g., split the large volume of “effluent” into the bottles labeled “effluent”).

1. Wear powder

- free gloves provided when performing the carboy sub

- sampling. 2. Locate and p repare the sub

- sampling area as follows:

a. Locate a lab or office area with mi nimal blowing dust and minimal particles falling from the ceiling. b. Wipe the bench or table with a damp lint

- free towel to remove any particulates.

c. Work on top of a plastic bag if y ou are concerned about the cleanliness of the bench or table surface. 3. Remove the eight 1

- L bottles from the Ziploc bags and line them up on the cleaned bench or table surface with the caps loosened but still in place

. 4. Record the start time and date

. 5. Have o ne person wearing gloves who can remove the cap from each bottle to receive the sequential sub

- samples. Uncap the bottle only long enough to receive each “multi

- pour” sub

- sample and then immediately replace the cap.
6. Perform the “multi

- pour” split using th e large volume carboy as follows:

a. Thoroughly shake the carboy to completely homogenize the large volume sample. b. Immediately after shaking, remove the carboy cap and fill the first 1

- L split sample bottle about 1/3 full

c. Reca p the carboy and thoroughly shake and homogenize the large volume sample again. with the homogenized sub

- sample.

d. Immediately after shaking, remove the carboy cap and fill the second 1

- L split sample bottle about 1/3 full with the homogenized sub

- sample.e. Repeat the process of shaking (homo genizing) the large volume carboy sample and filling each 1

- L split sample bottle about 1/3 each time

s equentially until all eight 1

- L bottles are full. This procedure will take 24 shake and pour operations

. 7. After the sub

- sampling is completed, make sure the cap of each 1

- L split sample is tightly closed. Place each 1

- L split sample bottle back in the Ziploc bag in which it was supplied 8. Note the time that the last bottle was filled.

After the eight 1

- L sample bottles have been filled from the first 10

- L carboy, these steps will need to be followed again to sub

- sample the next large volume sample into eight 1

- L bottles.

Sample Packing and Shipment

The following steps should be used whe n packing and shipping the samples to the laboratories. NOTE: T he samples do NOT need to be preserve d or put in ice at the plant or during shipment 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, be ing 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. Make sure that each sample bottle is sealed in a Ziploc bag. 4. Separate the bottles labeled as EPA samples from the bottles labeled as UWAG samples . NOTE: There are five EPA bottles and three UWAG bottles per sample point. 5. Place two garbage bags insi de each other in each of the coolers used to ship samples to the laboratories.
6. For the EPA samples, p lace the 1 5 EPA sample bottles in the garbage bags in the cooler s with proper end up, close the interior garbage bag by tying, or with a twist

- tie.
7. Close t he second garbage bag by tying, or with a twist

- tie. 8. Fill in any free space around the bottles with additional cushioning material (some provided) . Sufficient packing material should be used so that the sample containers will not shift during shipment. 9. L ocate the provided Traffic Report form (partially completed by EPA) and fill out any remaining details in the form (e.g., sample collection date and time, date shipped). Seal the Traffic Report form in the plastic envelope secured to the inside of the top of the cooler

. 10. Close the cooler.11. Place a completed laboratory address label on the lid of the cooler (provided by E PA ). The samples should be shipped to TestAmerica as follows:

Test America 4955 Yarrow Street Arvada, CO 80002 Attn: Richard Burrows ( 303) 736

- 0100

12. Make several wraps with strapping tape a round the cooler perpendicular to the seal to ensure that the lid will remain closed if the latch is accidentally released or damaged. 13. Locate a FedEx pouch (provided) and place it on the large white ta g on the handle of the cooler. Locate the provided FedEx airbill (partially completed by EPA) and fill out any remaining details in the airbill (e.g., date). Place the FedEx airbill in the pouch on the large white tag. Ship the coolers via FedEx. 14. For th e UWAG samples, locate the provided Traffic Report (partially completed) and fill out any remaining details in the form (e.g., date, time, and date shipped). Seal the Traffic Report in the plastic envelope and secure it to the inside of the top of the coo ler. 15. Close the cooler and place a completed laboratory address label on the lid of the cooler (provided by Albion). 16. Ship these samples to Albion Environmental (using a cooler provided by Albion Environmental):

Albion Environmental 4505 Boyett Street Brya n, TX 77801

- 4614 Attn: Dr. Paul Boothe (979) 268

- 2677

17. Seal the cooler with strapping tape to secure the lid. Locate the FedEx airbill provided by Albion and fill out any remaining details in t he airbill (e.g., date). Place the FedEx airbill in the plast ic sleeve on top of the cooler. Ship the coolers via FedEx. 18. After both the EPA and UWAG 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. 19. Note : If the shipment does not meet the Thursday, November 1 9 th drop off for FedEx Express, please notify TJ Finseth at (703) 633

- 1698 because if the samples are not shipped until Friday, they will need to be marked for Saturday delivery. Please notify TJ as early as possible if the samples will not be shipped until after November 1 9 th

.Returning Used Carboys

Please accumulate all used and unused carboys in the Albion Environmental coolers used to ship the equipment to you. If possible please rinse out th e carboys with tap water after all sampling and sub

- sampling activities are completed. Return all used and unused carboys to Albion Environmental for possible recycling as follows:

Albion Environmental 4505 Boyett Street Bryan, TX 77801

- 4614 ATTN: Dr. Paul Boothe (979 ) 268

- 2677