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 We Energies’ Pleasant Prairie Power Plant to aid in the sample collection, packaging, 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 regarding the t im eline 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 samp les to the
laboratories :

Items Provided by EPA in
Cooler Items Provided by Albion
Environmental

**•** Gloves Additional Items Needed

**•** 10

- L carboy (2 ) **•** Paper towels

**•** 1

- L plastic bottles (pre

labeled) (16 ) **•** 20

- L carboy (1) **•** Clean, plastic 5

- gallon bucket (if a samp le 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 complete) **•** Traffic re port (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 each of the fol lowing 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 treatment syste m 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 the stream enter ing the equalization tank.

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

Sampling Points, Sample Containers, and Sample Volumes

Sampling Point Sample Container and Volume

FGD wastewater treatment influent 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 bottles from the c ooler 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 clean sampling tech niques 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 piping, railing, e tc. 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 be come 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, samp le 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 activity 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 results will be com pared. To collect 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 t reatment 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 usedto collect the sample in the large composite container. The specific i nstructions are
described below.

Collecting the L arge Volume Composite Sample for 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 availab le 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 one of the 10

- L plastic carboys provided to collect the com posite FGD

wastewater treatment effluent samples. NOTE: Do not use the 20

- L plastic carboy for the effluent sample s . The 20

- L carboy will be used to collect 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 and distilled water. ( i.e., FGD scrubber

p urge )

.

4. Purge the tap for several minutes to remove particulates from the inside of the t ap 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 the 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 of the capped carboy as needed with tap water. Avoid getting any water into the threads of the cap.

9. P lace 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.

Collecting the Large Volume Composite Sample for FGD Wastewater Treatment
Influent :

A special sampli ng approach is recommended for collecting the liquid phase of the FGD
wastewater treatment influent waste water for the optimization study , due to the potential 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 col lection 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. Take 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 performing any sampling activities.
5. Slowly decant the liquid in the 20

- L carboy into a clean 10

- L carbo y 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 Comp osite into Eight 1

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

- L equivalent splits. The following steps should be carefully 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 prepare the sub

- sampling area as follows:

a. Locate a lab or office area with mi nimal blowing dust and mi nimal 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 you are concerned about the cleanliness of
the bench or table surface.

3. Remove the eight 1

- L bottles fr om 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 one person wearing gloves who can remove the cap from each bottle to receive the sequential sub

- sample s. 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 the large volume carboy as follows:

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

- L split sample bottle about 1/3 full

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

- sample.

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

- L split sample bottle about 1/3 full

e. Repeat the process of shaking (homogenizing) 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

. with the homogenized sub

- sample.

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 Z iploc bag in which it was supplied8. 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, 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. Make sure that each sample bottle is sealed in a Ziploc bag.

4. Separate the bottles labeled as E PA 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 inside each other in each of the coolers used to ship samples to the laboratories.

6. For the EPA samples, p lace the 10 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 the second garbage bag by tying, or with a twist

- tie.

8. Fill in any free space around the bottles with a dditional cushioning
material (some provided) . Sufficient packing material should be used so that the sample containers will not shift during shipment.

9. Locate the provided Traffic Report form (partially completed by EPA) and fill out any remaining detail s 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 cool er (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 t o 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 tag 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 the 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 cooler.
15. Close the cooler and place a completed laboratory address label on the lid of the cooler (prov ided by Albion).

16. Ship these samples to Albion Environmental (using a cooler provided by Albion Environmental):

Albion Environmental 4505 Boyett Street Bryan, TX 77801

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

- 2677

17. Seal the cooler with strapping tape to secur e the lid. Locate the FedEx airbill provided by Albion and fill out any remaining details in the airbill (e.g., date). Please the FedEx airbill in the plastic sleeve on top of the cooler. Ship the coolers via FedEx.

18. After both the EPA and UWAG coolers h ave 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 no tify 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 the 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