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 Duke Energy Carolinas’ Belews Creek 

Steam Station to aid in the sample collection, packaging, and shipping of samples 

collected for EPA’s method optimization study. Step-by-step instructions are provided

below to aid the sampling team in the preparation of the samples.

The samples should be collected and shipped to the laboratories no later than Thursday, 

November 19, 2009. If the plant has any questions regarding the timeline 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 (prelabeled) (24)• 20-L carboy (1) • Clean, plastic 5-gallon 

bucket (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 

complete)

• 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 each 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 treatment system prior to any commingling 

with other wastewaters. Note: if the plant operates an equalization tank that 
receives recycle streams from the treatment system (e.g., filter press filtrate), then 

collect the FGD scrubber purge sample prior to the stream entering the 

equalization tank.

• FGD wastewater treatment mid point: This sampling point should represent the 

effluent from the chemical precipitation 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 plastic 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 bottles 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 clean 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 piping, 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 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 compared. 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 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 container. The specific instructions are 

described below. 

Collecting the Large Volume Composite Sample for FGD Wastewater Treatment 

Mid-Point and FGD Wastewater Treatment Effluent:

If sampling from a valve or tap, collect the large volume 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 treatment effluent samples. NOTE: Do 

not use the 20-L plastic carboy for the mid-point or effluent samples. 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 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 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. 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.

Collecting 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 wastewater 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 collection of the FGD wastewater 

treatment effluent, except fill 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 carboy and fill to the 

neck, taking special care 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 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 minimal 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 you 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 one 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 the 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. Recap 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 (homogenizing) the large volume carboy 

sample and filling each 1-L split sample bottle about 1/3 each time 

sequentially 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 when packing and shipping the samples to the 

laboratories. NOTE: The samples do NOT need to be preserved 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 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 inside each other in each of the coolers used to 

ship samples to the laboratories.

6. For the EPA samples, place the 15 EPA sample bottles in the garbage bags 

in the coolers 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 additional 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 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 EPA). The samples should be shipped to TestAmerica as 

follows:

TestAmerica

4955 Yarrow Street

Arvada, CO 80002

Attn: Richard Burrows

(303) 736-0100

12. 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.

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 (provided 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 secure the lid. Locate the FedEx 

airbill provided by Albion and fill out any remaining details in the airbill 

(e.g., date). Place 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 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 19th 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 19th. 
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