## EPA COLLISION CELL ICP

- MS METHODS DEVELOPMENT STUDY

TOTAL RECOVERABLE TRACE METALS & MERCURY

IN FGD WASTE WATER GRAB SAMPLING INSTRUCTIONS

Introduction
The samples you will be collecting are very important . The samples will be used for a U.S.

Environment al Protection Agency (EPA) methods development study. The goal of the study is to develop analytical methods for accurately measuring metals in flue gas desulphurization (FGD) waste waters. EPA will not use these samples for any other purpose beyond the methods development study. Further, EPA will send facilities providing samples all analyses of these samples as soon as the laboratories involved have validated the data and provided the data to EPA or EPA’s Sample Control center staff.

It is crucial tha t the 7 or 8 one liter split samples you produce from this sampling be as identical as possible. The similarity of all the split samples is critical because the samples will be analyzed by many different laboratories to determine the most accurate metal s concentrations and to develop the best analytical method for making these measurements. Significant differences in composition among the 7 to 8 split samples will weaken the methods development study and possibly lead to erroneous conclusions. The “mu lti

- pour” approach used to produce very s imilar split samples is described in detail below. Please follow the “multi

- pour” split sampling instructions as carefully as possible. Your effort and attention to producing identical split samples is very import ant to the success of this EPA Study and is much appreciated. If you have any questions about sample collection please

contact Dr. Paul Boothe at Albion Environmental at any time (979

- 268

- 2677 or pboothe@albionenv.com)

.

It will NOT be necessary to use clean sampling techniques. However, it is important to avoid significant contamination during sample collection especially by metal

- rich particles such as dust, rust and corrosion particulates from piping, railings, etc . If metal

- rich particles get into the initial large volume (i.e. 10 or 20 liter carboy) sample or into spli t samples during sub

- sampling, then it will be impossibl e to produce identical split samples. To minimize the chance for such metal

- rich particulate contamination please follow the detailed sampling instructions below.



## Manual g rab sampling instructions

General Instructions

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 c arboys, 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.



### Collecting the large volume (composite) sample :

1

. Wear powder

- free gloves provided whenever performing any sample collection activities.

2

. Use the large volume plastic carboys provided to collect the composite FGD effluent sample s

. Use

a new plastic bucket and new plastic garbage can to collect the FGD influent sample as described

below.

4

. If submersi on grab sampling is possible (i.e. direct access to the surface of waste stream being sampled), then collect the large volume composite sam ple as follows:a. Loosen the cap on the carboy but do not remove it.

b. Submerge the carboy under the surface of the wastewater being sampled.

c. Uncap the carboy and allow it to fill to the neck of the carboy.

d. While still submerged, recap the carboy.

e. Remove the carboy from the waste stream and fully tighten the cap.

f. Rinse the outside of the capped carboy as needed with tap water. Avoid getting any water into the threads of the cap.

g. Place the carboy back in the original plastic bag in which i t came and take the carboy to the location where split sample sub

- sampling will be performed.

h. Be sure to record the unique sample ID number in your notes along with the sample collection information to be included in the sample shipment.

5

. If sampl ing from a valve or tap, then collect the large volume composite sample as follows :

a. 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 lab towel and distilled wat er. b. P urge the tap for several minutes to remove particulates from the inside of the tap line.

c. If there is any concern about particles falling into the carboy during filling, then shroud the tap with one of the Ziploc bags provided.

d

. Place the carb oy 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.

e. Remove the carboy from the flowing tap stream and fully tighten the cap.

f. Rinse the outside of the capped carboy as needed with tap water. Avoid getting any water into the threads of the cap.

g. 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

. h. Be sure to record the unique sample ID number in your notes along with the sample collection information to be included in the sample shipment.



### Sub

- sampling the large volume carboy to produce FGD EFFLUENT split samples:

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 minimum particles falling from the ceiling.

b. Wipe the bench or table with a damp lint

- free lab 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

. Line up the 7 or 8 one liter bottles on the cleaned bench or table surface with the caps loosened but

st ill in place.

4

. 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.

5

. 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 one liter split sample bottle

about 25% ful l with the homogenized sub

- sample.

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

d. Immediately after shaking, remove the carboy cab and fill the second one liter split sample

bottle about 25% full with the homogen ized sub

- sample.

e. Repeat the process of shaking (homogenizing) the large volume carboy sample and filling each one liter split sample bottle about 25% at a time and sequentially until all 7 or 8 one liter bottles are full. Depending on the number of one liter split samples, this procedure will take 28 or 32 shake and pour operations.

f. The “multi

- pour” sub

- sampling procedure is somewhat laborious but is necessary to produce identical split samples that are needed for the success of this EPA Study.6

. A fter the sub

- sampling is completed, make sure the cap of each one liter split sample is tightly closed. Place each one liter split sample bottle back in the original plastic bag in which it was supplied.

7

. Be sure to record the unique sample ID number in your notes along with the sample collection information to be included in the sample shipment.



### Special FGD influent sub

- sampling instructions :

1. A special sampling approach is recommended for collecting the liquid phase of the FGD influent

waste wate r for this study. For this sampling, it will be necessary for the plant to supply a new all plastic bucket and an all new ~ 30 gallon plastic garbage can. The bucket and garbage can should be washed out with tap water to remove dust and other particulate s prior to use.

2. Wear powder

- free gloves provided when performing the carboy sub

- sampling.

3

. FGD influent samples will be collected using the bucket and then transferred to the garbage can which should be covered with its plastic lid when not receiving FGD waste water samples. Fill the garbage can with approximately 20 gallons of FGD waste water. This approach is needed to allow the total suspended solids (TSS) to settle out (separate) from the liquid phase of the influent sample.

4. After collecting approximately 20 gallons of FGD influent as described above, take the garbage can with its plastic lid in place to the location where split sample sub

- sampling will be performed.

5. Allow the TSS in the garbage can to settle for 1

- 2 hours so that the uppe r part of the FGD waste water sample becomes fairly clear in the upper one foot of liquid sample.

6. After the TSS has settled, it will be possible to collect the sub

- sample splits as follows. Be careful to NOT stir up any TSS during the into the decant ed influent liquid phase sample :

a. Wear powder

- free gloves provided when performing the carboy sub

- sampling.

b. Use the same prepared sub

- sampling area as used for the effluent split sampling described

above.

c. Line up the 7 or 8 one liter bottles on th e cleaned bench or table surface with the caps loosened but still in place.

d. Have one person wearing gloves remove the cap from the first bottle and submerge the bottle into the cleared surface layer of the FGD influent sample in the 30 gallon garbage ca n. Let the bottle fill about 1/3 with the cleared liquid phase of the FGD influent sample. Remove the bottle and immediately replace the cap.

e. Repeat the same submerged sampling procedure using the second one liter split sample bottle. Again, fill the second bottle about 1/3 with the liquid phase.

f. Repeat the process of submerging and partially filling each one liter bottle about 1/3 at a time and sequentially until all 7 or 8 one liter bottles are full. Depending on the number of one liter split samples, this procedure will take 21 or 28 submerge and partially fill operations.

g. The “multi

- pour” sub

- sampling procedure is somewhat laborious but is necessary to produce identical split samples that are needed for the success of this EPA Study.

7. Be sure to record the unique sample ID number in your notes along with the sample collection information to be included in the sample shipment.



### One liter split sample handling

1. Do not preserve or ice the split samples at your facility or during ship ment.

2. Ship the one liter split samples as follows:

a. Seal five (5) one liter split samples in a single outer bag. (1) Ship the five (5) split samples to the analytical laboratory specified by the EPA.b. Seal three (3) one liter split samples i n a single outer bag. Ship the three (3) split samples to

Albion Environmental as follows:

Albion Environmental 4505 Boyett Street Bryan , TX 778 01

- 4614

ATTN: Dr. Paul Boothe (979

- 268

- 2677)



### Returning Used Carboys

1. Please accumulate all used and unus ed carboys in the Albion Environmental (AE) 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. R eturn all used and unused carboys to AE for poss ible recycling as follows:

Albion Environmental 4505 Boyett Street Bryan , TX 778 01

- 4614

ATTN: Dr. Paul Boothe (979

- 268

- 2677)



### Any questions please contact Dr. Paul Boothe at Albion Environmental (979

- 268

- 2 6 77 or pboothe@albionenv.com ) at any time.