EPA COLLISION CELL ICP-MS METHODS DEVELOPMENT STUDY

TOTAL RECOVERABLE TRACE METALS & MERCURY

IN FGD WASTEWATER GRAB SAMPLING INSTRUCTIONS

Introduction

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

Environmental 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 that 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 metals 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 “multi-pour” approach used to produce very similar 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 important 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 split samples during sub-sampling, then it will be 

impossible to produce identical split samples. To minimize the chance for such metal-rich particulate 

contamination please follow the detailed sampling instructions below.

Manual grab sampling instructions

General Instructions

1. Wear a new pair of powder-free gloves whenever you are involved in sample collection or subsampling 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.

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 samples. Use 

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

below.

4. If submersion grab sampling is possible (i.e. direct access to the surface of waste stream being 

sampled), then collect the large volume composite sample 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 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. 

5. If sampling 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 water. 

b. Purge 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 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. 

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 EFFLUENTsplit 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 

still 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% full 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 homogenized 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. After 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 water 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 particulates 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 upper 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 decanted 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 the 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 can. 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 shipment.

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 in a single outer bag. Ship the three (3) split samples to 

Albion Environmental as follows:

Albion Environmental

4505 Boyett Street

Bryan, TX 77801-4614

ATTN: Dr. Paul Boothe

(979-268-2677)

Returning Used Carboys

1. Please accumulate all used and unused 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. Return all used and unused carboys to AE for possible 

recycling as follows:

Albion Environmental

4505 Boyett Street

Bryan, TX 77801-4614

ATTN: Dr. Paul Boothe

(979-268-2677)

Any questions please contact Dr. Paul Boothe at Albion Environmental (979-268-2677 or 

pboothe@albionenv.com) at any time.