DRAFT 

Generic Sampling and Analysis Plan for 

Steam Electric Power Plants 

Prepared for:

U.S. Environmental Protection Agency

Engineering and Analysis Division 

Office of Water 

1200 Pennsylvania Avenue, NW 

Washington, D.C. 20460 

Prepared by: 

Eastern Research Group, Inc.

14555 Avion Parkway 

Suite 200 

Chantilly, VA 20151 

February 24, 2010 

EPA Contract No. 68-C-02-095 

Work Assignment 7-29
DRAFT 

i

TABLE OF CONTENTS 

Page 

1.0 INTRODUCTION ................................................................................................................ 1-1 

1.1 Background ........................................................................................................... 1-1 

1.2 Objectives and Scope ............................................................................................ 1-2 

1.3 Plant Selection ...................................................................................................... 1-3 

2.0 SAMPLING PROCEDURES .................................................................................................. 2-1 

2.1 Sampling Point Selection ...................................................................................... 2-1 

2.1.1 FGD Scrubber Purge .............................................................................. 2-1 

2.1.2 Mid-Point of FGD Wastewater Treatment ............................................. 2-3 

2.1.3 Effluent from FGD Wastewater Treatment ............................................ 2-3 

2.2 Analyte Selection .................................................................................................. 2-4 

2.3 Sample Fractions, Bottle Sets, and Sample Collection ......................................... 2-5 

2.4 Sample Collection Methodology .......................................................................... 2-5 

2.4.1 Composite Sample Collection ................................................................ 2-7 

2.4.2 Grab Sample Collection ....................................................................... 2-13 

2.4.2.1 Grab Sample Collection from Tap ....................................................... 2-13 

2.4.2.2 Grab Sample Collection from Basin (or Tank) .................................... 2-18 

2.5 Preservation, Shipping, and Analysis ................................................................. 2-21 

2.6 Field Measurements and Engineering Data Collection ...................................... 2-22 

2.7 Sample Labeling ................................................................................................. 2-23 

2.8 Traffic Reports .................................................................................................... 2-24 

2.9 Quality Assurance/Quality Control .................................................................... 2-24 

2.10 Sample Splitting .................................................................................................. 2-26 

3.0 SAMPLING ACTIVITIES ..................................................................................................... 3-1 

3.1 Sampling Team Organization ............................................................................... 3-1 

3.2 Pre-Sampling Preparation ..................................................................................... 3-1 

3.3 Field Sampling Activities ..................................................................................... 3-2 

3.4 Standard Logistics ................................................................................................. 3-3 

3.4.1 Plant Contacts ......................................................................................... 3-3 

3.4.2 EPA Contacts .......................................................................................... 3-3 

3.4.3 Analytical Laboratories .......................................................................... 3-4 

3.4.4 ERG Contacts ......................................................................................... 3-4 

3.4.5 Freight Forwarders ................................................................................. 3-4 

4.0 SAMPLE SHIPMENT .......................................................................................................... 4-1 

4.1 Sample Set Preparation ......................................................................................... 4-1 

4.2 Sample Packing ..................................................................................................... 4-2 

5.0 REFERENCES .................................................................................................................... 5-1 
DRAFT 

ii

LIST OF TABLES 

Page 

2-1 Sample Collection at Steam Electric Plants ....................................................................... 2-27 

2-3 Summary of Sample Container and Planned Preservation ................................................ 2-29 

2-4 Sampling Point Field Measurements ................................................................................. 2-30 
DRAFT 

iii

LIST OF FIGURES 

Page 

2-1 Sample Preservation Log Sheet ......................................................................................... 2-31 

2-2 Field Sampling Log Sheet .................................................................................................. 2-32 

2-3 Engineering Data Collection Sheet (Page 1 of 3) .............................................................. 2-33 

2-4 Engineering Data Collection Sheet (Page 2 of 2) .............................................................. 2-34 

2-5 Engineering Data Collection Sheet (Page 3 of 3) .............................................................. 2-35 

2-6 Example SCC Traffic Report ............................................................................................. 2-36 
DRAFT 

1-1

1.0 INTRODUCTION

 The Engineering and Analysis Division (EAD) of the U.S. Environmental 

Protection Agency (EPA) is planning to conduct a sampling program of up to seven steam 

electric power plants to 1) obtain wastewater characterization data and 2) obtain wastewater 

treatment technology performance data. EPA will use these data in combination with other 

industry-supplied data to evaluate wastewater discharges resulting from steam electric generating 

plants and to evaluate technology options for the handling and treatment of these wastewaters. 

This “generic” sampling plan provides general sampling procedures and methods to be followed 

when conducting sampling activities. Sampling will be performed either by EPA’s technical 

contractor, Eastern Research Group, Inc. (ERG) or by industry representatives. This document, 

in combination with plant-specific sampling plans, is intended to serve as a guide to the field 

sampling crew. The plan also provides a review mechanism for EPA personnel, and a source of 

procedural information for plant personnel. 

1.1 Background

 During EPA’s recently completed detailed study of the steam electric industry, 

EPA identified metals and certain other constituents present in the wastewater discharges from 

steam electric power plants are contributing the majority of the toxic loadings for the industry. 

Additionally, EPA determined that one of the waste streams contributing the majority of these 

toxic loadings are associated with wet flue gas desulfurization (FGD) systems present at coalfired power plants. 

 This sampling and analysis plan (SAP) will focus on characterizing treatment 

system discharges from coal-fired steam electric power plants. For a description of the steam 

electric process and the wastewaters generated during the operation of a coal-fired steam electric 

power plant, see Chapters 3 and 4 of the Steam Electric Power Generating Point Source 

Category: Final Detailed Study Report [1]. 
DRAFT 

1-2

1.2 Objectives and Scope

EPA is preparing to collect and analyze samples to characterize wastewater 

streams generated at coal-fired steam electric power plants. This SAP describes the approach 

EPA will use to collect and analyze samples to characterize untreated FGD scrubber purge and 

treated FGD wastewater from the following types of FGD wastewater treatment systems: 

 Chemical precipitation: Physical/chemical precipitation for heavy metals 

removal using hydroxide or a combination of hydroxide and sulfide 

precipitation; and 

 Biological: Biological treatment specifically designed for metals removal. 

Generally, the analytical results collected during this sampling program will 

support EPA in answering the following key questions: 

 What are the characteristics (i.e., pollutants present, pollutant 

concentrations, flow rate/volume) of untreated FGD scrubber purge 

wastewater? 

 What is the performance (e.g., effluent pollutant concentrations) of 

technologies for the treatment of FGD scrubber purge wastewater? 

 What are the average effluent concentrations for pollutants present in 

treated FGD wastewater? 

 What are the pollutant loadings associated with discharges of FGD 

wastewater following treatment? 

 EPA will conduct one-day pre-sampling site visits at the plants selected for the 

sampling program; however, if EPA previously visited the plant as part of the detailed study, a 

site visit may not be necessary. The objectives of the pre-sampling site visits are to: 

 Gather general information about the plant’s operations, including 

exisiting sampling data and results; 

 Gather process-specific information; 

 Gather information on pollution prevention and wastewater 

treatment/operations; 

 Gather plant-specific information to tailor sampling plans; and 

 Select and evaluate potential sampling points. 
DRAFT 

1-3

 The sampling program will consist of four-day sampling episodes at up to seven 

selected plants. The sampling will characterize the wastewaters generated by wet FGD scrubbers 

and the treatment performance of the systems used to treat the FGD scrubber purge wastewaters. 

EPA will also collect field quality control (QC) samples consisting of bottle blanks, field blanks, 

equipment blanks, and duplicate samples, and laboratory QC samples used for matrix 

spike/matrix spike duplicate analyses. 

 EPA’s sampling program will provide data to perform an engineering assessment 

of the design, operation, and performance of treatment systems at steam electric power plants. 

Specifically, EPA will collect information regarding system design and day-to-day operation. 

1.3 Plant Selection

 EPA expects to select up to seven coal-fired steam electric plants for wastewater 

sampling. EPA will base the plant selection on the process configurations and characteristics of 

the plants. The following primary criteria will be used to select the plants for the sampling 

program: 

 Coal-fired power plant: EPA expects that all of the plants selected for the 

sampling program will be coal-fired plants because the waste streams of 

interest for the sampling program data objectives are associated with coalfired power plants. 

 Wet FGD system: EPA will evaluate wastewaters generated from wet 

FGD systems and the treatment of these wastewaters. EPA will consider 

the following selection criteria regarding FGD systems: 

o Type of FGD wastewater treatment system: The primary factor for 

selection is the type of wastewater treatment system being operated 

for the treatment of FGD wastewater. EPA plans to select plants 

operating the following types of wastewater treatment systems: 

 Chemical precipitation – EPA will sample up to five plants 

operating chemical precipitation systems. 

 Biological – EPA will sample up to two plants operating 

biological systems that use an anaerobic/anoxic biological 

system specifically designed for the treatment of nitrates 

and selenium. 
DRAFT 

1-4

o Age of FGD wastewater treatment system: EPA does not intend to 

collect samples from a wastewater treatment system that has not 

reached steady state operation because the performance of the 

system may not be optimized. Generally, EPA plans to sample 

FGD wastewater treatment systems that have been operating for at 

least six months, or where data have shown the system to be at 

steady state. 

o Type of FGD system: EPA will consider the type of FGD system 

operated by the plant (e.g., limestone forced oxidation, lime 

inhibited oxidation) when selecting plants for sampling. Although 

EPA may sample different types of FGD systems, the plants 

operating the types of FGD wastewater treatment system of 

interest for the rulemaking are likely to operate limestone forced 

oxidation systems. The limestone forced oxidation system has the 

capability of producing wallboard-grade gypsum, but it typically 

requires a purge stream that needs to be treated prior to discharge. 

Plants operating most other types of FGD systems either reuse the 

FGD water stream or treat it in a settling pond (often commingled 

with other plant wastewaters, such as ash sluice water). 

 NOx controls: EPA will consider whether the plants operate a selective 

catalytic reduction (SCR) system or a selective non-catalytic reduction 

(SNCR) system when selecting plants for sampling. Although these NOx

control systems do not generate a specific wastewater stream, their 

operation can impact the FGD wastewater characteristics. 

 Power load cycling: EPA will consider a plant’s load cycling (i.e., 

baseload, cycling, peaking). EPA expects that most of the plants selected 

for sampling will be baseload plants; however, EPA will consider 

sampling a cycling plant. EPA does not believe that there are any coalfired peaking plants. 

 Type of Coal: EPA will consider the type of coal that the plant burns. 

EPA plans to select plants that burn different types of coal. EPA expects 

to sample at least two different types of coal. 

 EPA will consider the following characteristics as secondary factors to be 

considered in the selection of plants. Although these are not primary criteria for plant selection, 

these characteristics may be used as a determining factor where warranted. 

 Continuous versus batch operation of FGD wastewater treatment system 

(e.g., five days per week versus seven days per week); 
DRAFT 

1-5

 Use of advanced mercury control system and configuration; 

 Type of boiler; 

 Age of boiler and FGD unit (i.e., time of last upgrade); 

 Source of lime/limestone used in wet FGD system; 

 Plant location; and 

 Other plant conditions that may affect wastewater characteristics or 

sample collection, such as whether target waste streams are segregated or 

commingled. 

 
DRAFT 

2-1

2.0 SAMPLING PROCEDURES

 This section discusses the general sampling procedures to be followed during all 

sampling activities. This section also provides the necessary information to plan for the logistics 

of potential sampling activities. 

2.1 Sampling Point Selection

 In general, EPA plans to collect representative samples at the influent and effluent 

of the FGD wastewater treatment system that is operating under steady-state conditions. In 

addition, EPA may collect samples at a mid-point of the FGD treatment system (e.g., effluent 

from chemical precipitation system prior to biological treatment). EPA plans to collect 24-hour 

composite samples at the mid-point and effluent sampling points and grab samples at the influent 

sampling points of the wastewater treatment system. The proposed sampling points were selected 

by EPA to answer the questions that are the objective of the sampling program, which are 

presented in Section 1.2. The specific sampling points and locations, samples, and list of 

parameters selected for each plant will be described in the plant-specific sampling plans. 

2.1.1 FGD Scrubber Purge 

 EPA plans to collect samples of untreated FGD scrubber purge wastewater. The 

scrubber blowdown generated directly from the FGD system is expected to contain large 

amounts of solids (i.e., calcium sulfite or calcium sulfate (gypsum)); therefore, EPA will collect 

the FGD wastewater after initial solids removal, which represents the FGD scrubber purge waste 

stream. 

 Many of the FGD wastewater treatment systems that EPA has observed thus far 

contain a surge tank (or equalization tank) prior to the wastewater entering the treatment system. 

For some of these treatment systems, FGD scrubber purge is the only waste stream that enters 

the surge tank; however, for other systems, the FGD scrubber purge may be combined with 

recycle streams from the treatment system (e.g., filter backwash) within the surge tank. EPA 

will collect the FGD scrubber purge from the following locations depending on the set up of the 

influent to the FGD wastewater treatment system: 
DRAFT 

2-2

 No surge tank prior to treatment system: EPA will collect a sample of the 

FGD scrubber purge stream prior to it entering the first-stage of the 

treatment system; 

 Surge tank with only FGD scrubber purge prior to treatment system: EPA 

will collect a sample of the FGD scrubber purge either directly from the 

surge tank or from the effluent stream leaving the surge tank; and 

 Surge tank with other recycle streams prior to treatment system: EPA will 

collect a sample of the FGD scrubber purge prior to it entering the surge 

tank. 

 EPA will collect grab samples of the FGD scrubber purge. Because of the 

intermittent nature of the FGD scrubber purge waste stream, EPA anticipates working closely 

with the plants to determine the expected duration and frequency of purging the FGD wastewater 

to the treatment system. Based on this information, EPA will determine when to collect the grab 

samples. 

 EPA expects that the wastewater entering the FGD treatment system will contain 

high concentrations of certain parameters, including suspended and dissolved solids, chlorides, 

sulfates, and various cations. The high solids content of the samples may make it difficult to 

filter the samples for the dissolved metals analyses; therefore, EPA plans to allow the sample to 

settle for one hour prior to running the sample through the filter. 

 Due to the high suspended solids content (on the order of 1-5 percent) of the 

samples collected at the influent to the FGD wastewater treatment system, EPA may analyze the 

samples as bi-phasic samples. If the suspended solids content of the sample is greater than one 

percent, then the laboratory will separate the aqueous portion of the sample from the solid 

portion of the sample and analyze both for the analyte of interest. In this instance, Group I 

(chloride and sulfate only), Group II (ammonia as nitrogen, nitrate/nitrite as nitrogen, and total 

phosphorus only), and total metals (including mercury, but not hexavalent chromium because it 

is filtered in the field during sample collection) samples will be analyzed as bi-phasic samples. 

Group I (TSS and TDS only), Group II (COD only), BOD5, hexavalent chromium, and dissolved 

metals (including mercury) samples will not be analyzed as bi-phasic samples. Scrubber purge 
DRAFT 

2-3

samples with less than one percent suspended solids will not require bi-phasic separation and 

analysis. 

2.1.2 Intermediate Point of FGD Wastewater Treatment 

 EPA may collect samples at an intermediate point of the FGD wastewater 

treatment system. EPA expects to collect this sample after some initial treatment steps that could 

represent a wastewater treatment system of interest for the program. For example, some plants 

operate a chemical precipitation system followed by a biological treatment system. For this type 

of treatment system, EPA may consider collecting a sample after the chemical precipitation 

system to represent the effectiveness of the chemical precipitation portion of the system. 

 EPA expects that these samples will be collected either after a clarification step or 

after a filtration system, and will be collected from the effluent stream leaving the particular 

system before it enters the next stage of the treatment process. EPA will collect 24-hour 

composite samples of the intermediate point of the FGD wastewater treatment system, preferably 

using an automatic compositor. 

 EPA expects that the wastewater at an intermediate point in the FGD treatment 

system will contain high concentrations of certain parameters, such as chlorides, sulfates, and 

various cations. The suspended solids content of the sample is expected to be lower than at the 

influent; however, it may still be difficult to filter the samples for the dissolved metals analyses. 

2.1.3 Effluent from FGD Wastewater Treatment 

 EPA plans to collect samples of the effluent from the FGD wastewater treatment 

system. EPA expects to collect this sample from the waste stream that exits the wastewater 

treatment system; however, if EPA is unable to collect the sample from this location, then EPA 

will select a point within the system to represent the effluent. For example, if the wastewater is 

collected in an effluent tank prior to being transferred to additional treatment (e.g., an ash pond) 

and a sample cannot be collected from the wastewater piping leading to the additional treatment 

system, then it may be necessary to collect an effluent sample directly from the effluent tank. 
DRAFT 

2-4

 EPA does not expect to collect the influent and effluent samples from the FGD 

treatment system as “paired” samples because the primary objective of the sampling program is 

to collect effluent data to establish effluent limitations for the waste stream. Additionally, these 

treatment systems can have long residence times and therefore, could extend the amount of time 

required for EPA to be on site, which is a burden for the plant and unnecessary to achieve the 

sampling objectives. 

 EPA expects that the wastewater at the effluent from the FGD treatment system 

will still contain high concentrations of certain parameters, such as chlorides, sulfates, and 

various cations. The suspended solids content of the sample should be minimal (less than 0.01 

percent) and should not present any issues for filtering the sample for dissolved metals analyses. 

2.2 Analyte Selection

 Analytes that will be included in this EPA/EAD sampling program include those 

in the following classes of pollutants: 

 Classicals: 

— Biochemical oxygen demand, 5-day (BOD5), 

— Chemical oxygen demand (COD) 

— Total suspended solids (TSS), 

— Total dissolved solids (TDS), 

— Sulfate, 

— Chloride, 

— Total Kjeldahl nitrogen (TKN), 

— Ammonia as nitrogen, 

— Nitrate/nitrite as nitrogen, 

— Total phosphorus, 

— Total cyanide; 

 Total metals: 

— Aluminum, antimony, arsenic, barium, beryllium, boron, cadmium, 

calcium, chromium, cobalt, copper, iron, lead, magnesium, 

manganese, mercury, molybdenum, nickel, selenium, silver, 

sodium, thallium, tin, titanium, vanadium, and zinc. 

 Dissolved metals 

— Same parameters as listed for total metals, plus hexavalent 

chromium. 
DRAFT 

2-5

 The analytes selected for analysis reflect the current understanding of coal-fired 

power plant FGD wastewaters, including contributions from coal, scrubber sorbents, treatment 

chemicals, and other sources. Table 2-1 lists the potential analytes for each sampling point and 

Table 2-2 lists the analytical methods that will be used. In addition to these analytes, the 

sampling crew will conduct field measurements at all sampling points (see Section 2.6). The 

plant-specific sampling plans will specify the list of parameters and collection frequency for each 

sampling point. 

 

2.3 Sample Fractions, Bottle Sets, and Sample Collection

 Samples are collected as a series of “fractions” or bottles designated for particular 

analyses requiring the same preservation. A typical, comprehensive sample set consists of 

sample fractions for all pollutant classes listed in Section 2.2. Note that some sample fractions 

will be collected in the same sample bottle, such as Group I (TSS, TDS, sulfate, and chloride) 

and Group II (ammonia as nitrogen, COD, nitrate/nitrite, TKN, and total phosphorus). Table 2-3 

presents a summary of the parameters, bottle types, sample volume, and planned on-site 

preservation requirements. 

 Sample containers and bottles will be purchased pre-cleaned and certified and will 

not require rinsing with sample. The sample bottles for the metals analyses will be cleaned 

according to EPA Method 1669. 

 

2.4 Sample Collection Methodology

 To characterize the various waste streams expected to be sampled during the 

sampling program, the samplers may employ varying methods of sample collection depending 

on the sampling point, pollutant parameters, and the nature of the sample flow and composition 

at each sampling point. This section provides a general description of the anticipated sample 

collection techniques. Plant-specific sampling plans will contain detailed information regarding 

specific sampling points and locations, sampling methodologies, and analytes. 
DRAFT 

2-6

 In general, samplers will work in teams of at least two to ensure that proper 

sampling techniques are followed and adequate notes are taken at each sampling location. 

Samplers will wear disposable gloves, Tyvek® suits, masks (when sampling for mercury by 

EPA Method 1631E), steel-toed boots, and safety eyewear, and will observe precautions while 

collecting samples, remaining aware of his/her surroundings. Note that the use of masks is to 

prevent contamination of the mercury samples and not for respiratory protection. The plantspecific sampling plans will identify any sampling points that require additional precautions. 

 

 Samplers will take care not to touch the insides of bottles or lids/caps during 

sampling. Samples that require cooling to ≤6C for preservation will be cooled immediately in 

an ice-water bath to ≤6C and then placed into coolers containing bagged ice to maintain a 

sample temperature of ≤6C throughout sample storage, shipment, and receipt at the analytical 

laboratories. 

 Discharge practices vary from plant to plant and process to process. For example, 

some processes may generate wastewater continuously, while others may only generate 

wastewater when parameters reach a certain predetermined threshold and require blowdown 

from the process. Thus, the plant-specific sampling plan will outline the sample collection 

methodology that EPA plans to implement at each sampling point at a particular plant. 

 EPA will collect 24-hour composite samples at the intermediate point and effluent 

of the FGD wastewater treatment system sampling points and grab samples at the influent 

sampling point during the sampling episodes. Additionally, EPA will collect samples over four 

consecutive 24-hour periods. Each sampling point will be collected each day; therefore, EPA 

will collect four samples for each sampling point. ERG will follow protocols described in EPA 

Method 1669 to collect metal sample fractions. All sampling equipment (e.g., tubing) and 

sample bottles will be cleaned according to the procedures described in EPA Method 1669. 

Samplers will use “clean hands / dirty hands” sample collection techniques when collecting 

metal sample fractions, as described in EPA Method 1669. In addition to the differences 

between collecting grab or composite samples, ERG will also use two different techniques to 

collect samples from steam electric plants based on the location of the sampling point: collection 
DRAFT 

2-7

from a tank or basin and collection from a sample tap. Specific instructions for the potential 

sampling techniques are described below. 

2.4.1 Composite Sample Collection 

 The preferred approach for collecting the composite samples will use two 

automatic compositors which will be programmed to collect individual sample volumes into two 

large containers (e.g., two 20-liter HPDE containers). To collect sufficient sample volume, ERG 

will calculate the total volume required for ERG sample collection as well as plant split sample 

collection and also add additional volume for purging tubing and contingencies. The volume 

will then be programmed to be collected in one-hour intervals during the 24-hour composite 

period. Following the composite period, ERG will pour and/or pump-off the specific sample 

volumes into the individual sample containers. 

 ERG will use one automatic compositor to collect sample volume for the metals 

analyses and another automatic compositor to collect sample volume for all classical analytes 

(i.e., BOD5, Group I, and Group II). 

 

 ERG’s preferred approach is to collect sample volume from a basin (or tank), 

where the composite samplers will be located outside, positioned near the edge of the basin. If 

the collection point is a sample tap, the composite samplers may be outside, depending on the 

location of the tap, and will be near wastewater piping and equipment. ERG may have to 

engineer a basin that draws a slip stream from a sample tap if the collection point is located at 

pressurized piping. This basin would be level controlled and would draw volume continuously 

into the basin, with the overflow entering the plants sumps. In this case, ERG would set up the 

composite samplers to draw volume from the engineered basin. The field sampling personnel 

will use care when setting up the sample point to avoid any contamination from the 

surroundings. The sampling equipment will consist of the following: 

 Colorless, electronic-grade, non-nitrile gloves; 

 Peristaltic pump (automatic compositor – battery powered); 

 Large composite containers (e.g., 20-liter containers); 

 Funnel; 
DRAFT 

2-8

 “Y” splitter; 

 Teflon® tubing; 

 Silicone tubing; 

 0.45 um filter; 

 Cleanbox; 

 Tyvek® suits (for metals samples); 

 Masks (for mercury samples); and 

 Sample containers. 

 All metals sampling equipment will be specially-cleaned according to the 

procedures described in EPA Method 1669. ERG will follow protocols described in EPA 

Method 1669 to collect metal sample fractions. Two or more ERG samplers (“clean hands” and 

“dirty hands”) will follow the protocols described in the steps below to set up the sampling point, 

collect the field blank samples, and collect wastewater samples. This section describes the set up 

of the sample point and collection of the EPA samples1. 

1. Samplers remove the bags containing the gloves and HDPE plastic wrap from the 

coolers or storage containers in which they are packed. Samplers identify which 

coolers or boxes contain the double-bagged composite containers, pre-cleaned 

tubing, blank water, and cleanbox. 

2. Both samplers put on Tyvek® suits, masks, and gloves. “Dirty hands” covers 

work surfaces (ground or table) with HDPE plastic wrap and places the doublebagged composite containers within easy access on the covered surface. 

3. “Dirty hands” opens the outer bag of the cleanbox and “clean hands” opens the 

clear inner bag. “Clean hands” places the cleanbox at the point of sample 

collection. “Clean hands” opens the cleanbox and secures it open with the clips 

located inside the box. 

4. “Dirty hands” opens up the peristaltic pump portion of the automatic compositor 

so the tubing can be added. “Dirty hands” opens the outer bag containing a length 

of pre-cleaned Teflon® tubing attached to a 4-foot length of pre-cleaned silicone 

tubing, if sampling from a basin (or a length of pre-cleaned silicone tubing if 

sampling from a sample tap). “Clean hands” takes the inner bag containing the 

tubing and moves it into the cleanbox. “Clean hands” opens the inner bag and 

removes the tubing. “Clean hands” places a clean plastic bag over the end of the 

Teflon® and silicone tubing. 

 

1

 For the sample collection, EPA assumes that samples will be split with the plant (or the plant’s representative) and 

therefore, the sample set-up describes equipment needed for split samples. However, EPA is not responsible for the 

collection of the split samples collected by the plant and therefore, the collection of their samples is not described. 
DRAFT 

2-9

5. “Dirty hands” threads the silicone tubing through the peristaltic pump portion of 

the automatic compositor. 

6. Both samplers change gloves. 

7. “Dirty hands” opens the outer bag of the mercury and metals field blank water 

and the field blank composite container. “Clean hands” opens the inner bag for 

the field blank water, unscrews the lid and places it in the inner bag. “Clean 

hands” then places the Teflon® end of the tubing into the blank water. “Clean 

hands” also opens the inner bag for the field blank composite container and 

loosens the lid. “Clean hands” holds the silicone tubing with the plastic bag 

covering the end out of the cleanbox and over a bucket and “dirty hands” operates 

the pump to pump blank water through the tubing. After the tubing has been 

purged with sufficient volume, “clean hands” holds the silicone tubing at the 

mouth of the field blank composite container and fills the composite container 

with enough field blank water for the collection of the total and dissolved mercury 

and metals field blank samples collected for the specific sampling point. “Dirty 

hands” stops the pump. “Clean hands” places the plastic bag over the end of the 

silicone tubing, replaces the lid on the field blank composite container, places the 

silicone tubing back in the cleanbox, and closes the inner bag on the field blank 

composite container. “Dirty hands” closes the outer bag of the field blank 

composite container. 

8. Both samplers work together to move the sampling tubing, automatic compositor, 

and composite containers into position for the sample collection. Samplers will 

ensure that the tubing will stay in place during the 24-hour sample collection 

period. 

9. “Dirty hands” changes gloves. 

10. “Clean hands” holds the end of the silicone tubing outside the cleanbox over a 

bucket, with the plastic bag still covering the end of the tubing. “Dirty hands” 

operates the pump to purge the tubing for a minimum of 2 minutes. 

11. Samplers fill a 1-L jar for the field measurements. The samplers will give the jar 

to another sampling team member to measure the temperature and pH. 

12. “Dirty hands” programs the automatic compositor to collect the 20 liters of 

sample over a 24-hour time period in one-hour intervals (i.e., collect 800 mL of 

sample every hour). “Dirty hands” calibrates the compositor to ensure that 800 

mL is being collected for each individual grab. 

13. “Dirty hands” opens the outer bag of the large composite container. “Clean 

hands” opens the inner bag and connects the silicone tubing to the port on the 

composite container, securing the connection with a cable tie. “Clean hands” 

closes the inner bag around the composite bottle, and “dirty hands” closes the 

outer bag. 
DRAFT 

2-10

14. Samplers repeat steps 1-13 to set up the automatic compositor for the 

conventional analyses (skipping step 7). Samplers will use another composite 

container. The samplers will put the classicals composite container in ice to keep 

the samples cold during compositing time period. 

15. Samplers collect a total cyanide grab sample using a bottle dipper. NOTE: if 

sample collection is from a tap, the samplers will need a third tap to allow for the 

collection of total cyanide and field measurements. The samplers will attach the 

bottle to the bottle dipper and dip the bottle directly into the tank or basin. 

16. The samplers will collect field measurements and total cyanide samples every six 

hours during the compositing time period, which will result in a total of four total 

cyanide samples for each day of sampling. The four grab samples will be 

composited by the laboratory. 

17. At the end of the sampling period, “dirty hands” stops each of the automatic 

compositors and opens the outer bag of each composite container. For each 

container, “clean hands” detaches the used tubing from the composite container 

and covers the port with a lid or small plastic bag. Then samplers transport each 

of the composite containers, including the field blank composite container, to the 

pump–off area to pump off the samples into the specified containers. 

18. The samplers then repeat steps 1 through 17 to set up the composite containers for 

the next day of sample collection. 

After the composite samples have been collected, the sampling team then needs to 

transfer the sample into the individual sample containers. EPA will use a sample pump-off 

approach to transfer the sample volume to individual sample containers at the pump-off area. 

For this sample pump-off procedure, the dissolved metals samples will be collected before the 

total metals and classical samples to prevent cross-contamination within the tubing which could 

lead to greater concentrations in the dissolved metals fractions. 

Sample Pump–Off Procedure 

19. Samplers remove the bags containing the gloves and HDPE plastic wrap from the 

coolers or storage containers in which they are packed. Samplers identify which 

coolers or boxes contain the double-bagged sample bottles, pre-cleaned tubing, 

and cleanbox. 

20. Both samplers put on Tyvek® suits and gloves. “Dirty hands” covers work 

surfaces with HDPE plastic wrap and places the double-bagged sample bottles 

and pre-cleaned tubing within easy access on the covered surface. 
DRAFT 

2-11

21. “Dirty hands” opens the outer bag of the cleanbox and “clean hands” opens the 

clear inner bag. “Clean hands” places the cleanbox at the point of sample 

collection. “Clean hands” opens the cleanbox and secures it open with the clips 

located inside the box. 

22. “Dirty hands” opens the opening on the peristaltic pump head so the tubing can be 

placed in the pump head. “Dirty hands” opens the outer bag containing a length 

of pre-cleaned Teflon® tubing connected to a length of pre-cleaned silicone 

tubing, a “Y” splitter, and two additional pieces of silicone tubing. “Clean hands” 

moves the tubing into the cleanbox and opens the inner bag and removes the 

tubing. “Clean hands” places a clean plastic bag over the end of the Teflon® and 

silicone tubing. 

23. “Dirty hands” threads the silicone tubing into the peristaltic pump head. 

24. Both samplers change gloves. 

25. “Dirty hands” opens the outer bag of the field blank composite container and total 

metals field blank sample bottle. “Clean hands” removes the total metals field 

blank sample bottle and places it in the cleanbox. “Clean hands” opens the inner 

bag of the field blank composite container. “Clean hands” removes the lid from 

the field blank composite container and places the end of the Teflon® tubing in 

the blank water. “Clean hands” holds the end of the silicone tubing outside the 

cleanbox over a bucket, with the plastic bag still covering the end of the tubing 

and “dirty hands” operates the pump to pump about 750 mL of blank water from 

the field blank composite container. “Clean hands” places the end of the silicone 

tubing in the cleanbox, opens the inner bag of the total metals field blank sample 

bottle, and removes the lid. “Dirty hands” operates the pump to collect the total 

metals field blank sample. “Dirty hands” stops the pump. “Clean hands” closes 

the lid on the sample bottle and closes the inner bag. “Clean hands” places the 

inner bag and bottle in the outer bag and “dirty hands” closes the outer bag. The 

samplers repeat this procedure for the remaining total metals field blank samples 

(i.e., total metals and total mercury field blank samples). 

26. “Dirty hands” opens the outer bag of a capsule filter. “Clean hands” opens the 

inner bag and removes the capsule filter. “Clean hands” attaches the capsule filter 

to the silicone tubing just before the “Y” splitter. 

27. “Dirty hands” opens the outer bag of the dissolved metals field blank sample 

bottle. “Clean hands” removes the dissolved metals field blank sample bottle and 

places it in the cleanbox. “Clean hands” holds the end of the silicone tubing 

outside the cleanbox over a bucket, with the plastic bag still covering the end of 

the tubing and “dirty hands” operates the pump to pump about 750 mL of blank 

water from the field blank composite container. “Clean hands” places the end of 

the silicone tubing in the cleanbox, opens the inner bag of the dissolved metals 

field blank sample bottle, and removes the lid. “Dirty hands” operates the pump 
DRAFT 

2-12

to collect the dissolved metals field blank sample. “Dirty hands” stops the pump. 

“Clean hands” closes the lid on the sample bottle and closes the inner bag. “Clean 

hands” places the inner bag and bottle in the outer bag and “dirty hands” closes 

the outer bag. The samplers repeat this procedure for the remaining dissolved 

metals field blank samples (i.e., dissolved metals and hexavalent chromium field 

blank samples)2. “Clean hands” closes the inner bag of the field blank composite 

container and “dirty hands” closes the outer bag. Note: 750 mL of blank water 

does not need to be purged for each sample, just at the beginning of each new 

filter. If a new filter is needed, “clean hands” removes the used filter and 

samplers follow step 25 to replace the filter. 

28. “Dirty hands” opens the outer bag of the large composite container for the metals 

samples and “clean hands” opens the inner bag. “Clean hands” transfers the 

Teflon® tubing from the field blank composite container to the metals sample 

composite container. “Clean hands” holds the end of the silicone tubing outside 

the cleanbox over a bucket, with the plastic bag still covering the end of the 

tubing and “dirty hands” operates the pump to pump about one liter of sample 

through the tubing and filter. “Dirty hands” stops the pump. 

29. “Dirty hands” opens the outer bag of the dissolved metals sample bottle. “Clean 

hands” removes the inner bag and bottle and places it in the cleanbox. “Clean 

hands” opens the inner bag and removes the lid. “Dirty hands” operates the pump 

to collect the dissolved metals sample. “Dirty hands” stops the pump. “Clean 

hands” closes the lid on the sample bottle and closes the inner bag. “Clean hands” 

places the inner bag and bottle in the outer bag and “dirty hands” closes the outer 

bag. The samplers repeat this procedure for the dissolved metals and hexavalent 

chromium samples. During one day of the sampling episode, the samplers will 

collect additional sample volume for the duplicate samples and laboratory QC 

analyses. 

30. “Clean hands” removes the capsule filter from the sample tubing configuration 

and reconnects the two pieces of tubing together. 

31. “Clean hands” holds the silicone tubing outside the cleanbox over a bucket, with 

the plastic bag covering the end of the tubing. “Dirty hands” pumps about one 

liter of sample through the tubing. “Dirty hands” stops the pump. “Clean hands” 

places the end of the silicone tubing back in the cleanbox. 

32. “Dirty hands” opens the outer bag of the total mercury sample bottle. “Clean 

hands” removes the inner bag and bottle and places it in the cleanbox. “Clean 

hands” opens the inner bag and removes the lid. “Dirty hands” operates the pump 

to collect the total mercury sample. “Dirty hands” stops the pump. “Clean 

 

2

 ERG only plans to collect field blank samples at each sampling point for one day of sampling episode. ERG will 

collect the dissolved mercury sample using the same technique as the total mercury sample, but the dissolved sample 

will be filtered at the laboratory. A dissolved mercury field blank will be performed by the laboratory to assess any 

mercury contamination from the filtering performed at the laboratory. Therefore, ERG does not need to collect a 

dissolved mercury field blank sample in the field. 
DRAFT 

2-13

hands” closes the lid on the sample bottle and closes the inner bag. “Clean hands” 

places the inner bag and bottle in the outer bag and “dirty hands” closes the outer 

bag. The samplers repeat this procedure for the dissolved mercury and total 

metals samples. During one day of the sampling episode, the samplers will collect 

additional sample volume for the duplicate samples and laboratory QC analyses. 

33. “Dirty hands” places an ERG label on the outer bags of the sample bottles. 

34. “Dirty hands” shakes the large composite containers for the classical analytes to 

mix the sample. “Dirty hands” opens the outer bag for the composite container. 

“Clean hands” opens the inner bag and transfers the Teflon® tubing from the 

metals composite container to the composite container for the classical analytes. 

35. “Clean hands” holds the silicone tubing outside the cleanbox over a bucket, with 

the plastic bag covering the end of the tubing. “Dirty hands” pumps about one 

liter of sample through the tubing. “Dirty hands” stops the pump. 

36. Both samplers collect the BOD5, Group I, and Group II samples. During one day 

of the sampling episode, the samplers will collect additional sample volume for 

the duplicate samples and laboratory QC analyses. 

2.4.2 Grab Sample Collection 

 ERG will collect the grab samples from the FGD scrubber purge, which is 

expected to contain a significant amount of suspended solids. ERG will collect samples directly 

into individual sample containers for all samples that are not required to be filtered in the field. 

For the samples that will to be filtered in the field, ERG will collect a large volume of sample 

into a large container (e.g., 10-L HDPE container) and then pump off the specific sample 

volumes into the individual sample containers. 

 The grab sample collection technique can vary significantly depending on the 

specific sampling point location (e.g., collection from a basin (or tank) compared to collection 

from a sample tap. The following two subsections describe the specific collection techniques 

that will be used to collect grab samples from the differing sampling point locations. 

2.4.2.1 Grab Sample Collection from Tap 

 For grab samples that are collected from a sample tap, ERG will set up the 

sampling equipment near the sample tap that represents the FGD scrubber purge sample. The 
DRAFT 

2-14

field sampling personnel will use care when setting up the sample point to avoid any 

contamination from the surroundings. The sampling equipment will consist of the following: 

 Colorless, electronic-grade, non-nitrile gloves; 

 Silicone tubing with “Y” splitter; 

 10-L containers; 

 Teflon® tubing; 

 Silicone tubing; 

 0.45 um filter; 

 Funnel; 

 Peristaltic pump; 

 Small table; 

 Cleanbox; 

 Tyvek® suits (for metals samples); 

 Masks (for mercury samples); and 

 Sample containers. 

 All metals sampling equipment will be specially-cleaned according to the 

procedures described in EPA Method 1669. ERG will follow protocols described in EPA 

Method 1669 to collect metal sample fractions. Two or more ERG samplers (“clean hands” and 

“dirty hands”) will follow the protocols described in the steps below to set up the sampling point, 

collect the field blank samples, and collect wastewater samples. This section describes the set up 

of the sample point and collection of the EPA samples3. 

 

1. Samplers remove the bags containing the gloves and HDPE plastic wrap from the 

coolers or storage containers in which they are packed. Samplers identify which 

coolers or boxes contain the double-bagged sample bottles, pre-cleaned tubing, 

blank water, and cleanbox. Depending on the condition of the sample tap, it may 

be necessary to wipe the tap with a clean paper towel to remove any build up on 

the tap that could potentially fall in the sample bottles during sample collection. 

2. Both samplers put on Tyvek® suits, masks, and gloves. “Dirty hands” covers 

work surfaces (ground or table) with HDPE plastic wrap and places the doublebagged sample bottles within easy access on the covered surface. 

3. “Dirty hands” opens the outer bag of the cleanbox and “clean hands” opens the 

inner bag. “Clean hands” places the cleanbox at the point of sample collection. 

“Clean hands” opens the cleanbox and secures it open with the clips located 

inside the box. 

 

3

 For the sample collection, EPA assumes that samples will be split with the plant (or the plant’s representative) and 

therefore, the sample set-up describes equipment needed for split samples. However, EPA is not responsible for the 

collection of the split samples collected by the plant and therefore, the collection of their samples is not described. 
DRAFT 

2-15

4. “Dirty hands” opens the outer bag containing a length of pre-cleaned silicone 

tubing. “Clean hands” opens the inner bag inside of the cleanbox and removes the 

tubing. “Clean hands” places clean plastic bags over the ends of the silicone 

tubing. 

5. “Dirty hands” opens the outer bag of the funnel and “clean hands” opens the inner 

bag inside of the cleanbox. “Clean hands” attaches the funnel to the tubing. 

6. “Dirty hands” opens the outer bags of the mercury field blank water and total 

mercury field blank sample bottles. “Clean hands” opens the inner bag for the 

field blank water, unscrews the lid and places it in the inner bag. “Clean hands” 

passes the funnel end of the tubing with a plastic bag shrouding the funnel to 

another “clean hands” person to hold outside the cleanbox. “Clean hands” 

removes the inner bag for the total mercury field blank sample bottle and places it 

in the cleanbox. “Clean hands” holds the end of the silicone tubing outside the 

cleanbox over a bucket, with the plastic bag still covering the end of the tubing. 

“Dirty hands” pours field blank water through the funnel and tubing. After the 

tubing has been purged with sufficient volume, “clean hands” places the silicone 

tubing back in the cleanbox. Working inside the cleanbox, “clean hands” 

unscrews the lid of the field blank sample bottle, removes the tubing from the 

plastic bag, and prepares to fill the field blank sample bottle. “Dirty hands” pours 

field blank water into the funnel and tubing, and “clean hands” fills the total 

mercury field blank sample bottle. “Clean hands” places the end of the silicone 

tubing into the plastic bag, replaces the lid on the sample bottle, and closes the 

inner bag. “Clean hands” removes the bottle from the cleanbox and places it in the 

outer bag. “Dirty hands” closes the outer bag. The samplers repeat this procedure 

for the total metals field blank samples4

. 

7. “Dirty hands” opens the outer bag for a pre-cleaned 10-L container. “Clean 

hands” opens the inner bag and loosens the lid. “Clean hands” holds the end of 

the silicone tubing at the mouth of the 10-L container and removes the lid. “Dirty 

hands” pours field blank water through the funnel and tubing, and “clean hands” 

fills the 10-L container with enough field blank water to collect the dissolved 

metals field blank samples. “Clean hands” places the lid back on the 10-L 

container, places the plastic bag over the end of the silicone tubing, and places the 

tubing in the cleanbox. “Clean hands” screws the lid on the 10-L container and 

closes the inner bag. “Dirty hands” closes the outer bag of the 10-L container. 

8. After collecting the field blank samples, “clean hands” removes the funnel from 

the tubing. “Clean hands” and “dirty hands” work to attach the end of the silicone 

tubing to the sample tap. 

 

4

 ERG only plans to collect field blank samples at each sampling point for one day of sampling episode. ERG will 

collect the dissolved mercury sample using the same technique as the total mercury sample, but the dissolved sample 

will be filtered at the laboratory. A dissolved mercury field blank will be performed by the laboratory to assess any 

mercury contamination from the filtering performed at the laboratory. Therefore, ERG does not need to collect a 

dissolved mercury field blank sample in the field. 
DRAFT 

2-16

9. “Clean hands” holds the opposite end of the silicone tubing outside the cleanbox 

over a bucket, with the plastic bag covering the end of the tubing. “Dirty hands” 

opens the valve to the sample tap to purge the piping for a minimum of 2 minutes. 

“Clean hands” places the end of the silicone tubing back in the cleanbox. 

10. “Dirty hands” opens the outer bag for a pre-cleaned 10-L container. “Clean 

hands” opens the inner bag and loosens the lid. “Clean hands” holds the end of the 

silicone tubing at the mouth of the 10-L container and removes the lid. “Dirty 

hands” opens the sample valve to allow sample to flow into the 10-L container. 

Samplers fill the 10-L container for the collection of dissolved metals and 

hexavalent chromium, which are all required to be filtered. The samplers will 

allow the solids to settle for one hour while collecting the remaining samples. 

“Clean hands” places the lid back on the 10-L container, places the plastic bag 

over the end of the silicone tubing, and places the tubing into the cleanbox. 

”Clean hands” screws the lid on the 10-L container and closes the inner bag. 

“Dirty hands” closes the outer bag of the 10-Liter container. Both samplers 

change their gloves. 

 

11. “Dirty hands” opens the outer bag for the total mercury sample bottle. “Clean 

hands” removes the inner bag and bottle and places it in the cleanbox. “Clean 

hands” opens the inner bag and bottle lid. “Clean hands” removes the plastic bag 

from the tubing and fills the sample bottle. “Clean hands” places the tubing back 

in the plastic bag, replaces the lid on the sample bottle and closes the inner bag. 

“Clean hands” removes the sample bottle from the cleanbox and places it in the 

outer bag. “Dirty hands” closes the outer bag. The samplers repeat this procedure 

for the dissolved mercury and total metals samples. 

12. “Dirty hands” places an ERG label on the outer bags of the sample bottles. 

13. Samplers fill a 1-L jar for the field measurements. The samplers will give the jar 

to another sampling team member to measure the temperature and pH. 

14. Both samplers collect the BOD5, Group I, Group II, and total cyanide samples 

from the sample location. 

Dissolved Metals Sample Collection 

15. Samplers allow the 10-L sample container to continue to settle if one hour has not 

elapsed since the collection of the sample. 

 

16. “Dirty hands” covers the work surfaces (ground or table) with HDPE plastic wrap 

and places the double-bagged sample bottles within easy access on the covered 

surface. 

17. “Dirty hands” opens the outer bag of the clean box and “Clean hands” opens the 

inner bag. “Clean hands” places the cleanbox at the point of sample collection. 
DRAFT 

2-17

“Clean hands” opens the cleanbox and secures it open with the clips located 

inside the box. 

18. “Dirty hands” opens the opening on the peristaltic pump head so the tubing can be 

placed in the pump head. “Dirty hands” opens the outer bag containing a length of 

pre-cleaned Teflon® tubing attached to a 5-foot length of pre-cleaned silicone 

tubing, a “Y” splitter, and two additional pieces of pre-cleaned silicone tubing. 

“Clean hands” moves the tubing into the cleanbox, opens the inner bag, and 

removes the tubing. “Clean hands” places a clean plastic bag over the end of the 

Teflon® and silicone tubing. 

19. “Dirty hands” threads the silicone tubing into the peristaltic pump head. 

20. Both samplers change gloves. 

21. “Dirty hands” opens the outer bag of a capsule filter. “Clean hands” opens the 

inner bag and removes the capsule filter. “Clean hands” attaches the capsule filter 

to the silicone tubing just before the “Y” splitter. 

22. “Dirty hands” opens the outer bag of the 10-L container that was used to collect 

the field blank water for the dissolved metals fractions. “Clean hands” opens the 

inner bag of the 10-L container. “Clean hands” removes the Teflon® tubing from 

the cleanbox, opens the lid of the 10-L plastic container, removes the plastic bag 

from the Teflon® tubing, and places the Teflon® into the 10-L container. “Dirty 

hands” opens the dissolved metals field blank sample bottle. “Clean hands” 

removes the dissolved metals field blank sample bottle and places it in the 

cleanbox. “Clean hands” holds the end of the silicone tubing outside the cleanbox 

over a bucket, with the plastic bag still covering the end of the tubing and “dirty 

hands” operates the pump to pump about 750 mL of blank water from the field 

blank water bottle. “Clean hands” places the end of the silicone tubing in the 

cleanbox, opens the inner bag of the dissolved metals field blank sample bottle, 

and removes the lid. “Dirty hands” operates the pump to collect the dissolved 

metals field blank sample. “Dirty hands” stops the pump. The samplers repeat the 

procedure for the dissolved metals and hexavalent chromium field blank samples. 

If a new filter is needed, “clean hands” removes the used filter and samplers 

following step 22 to replace the filter. 

23. Both samplers change gloves. 

24. “Dirty hands” opens the outer bag of one of the 10-L containers. “Clean hands” 

opens the inner bag, removes the lid, and places the end of the Teflon® tubing 

into the container. “Clean hands” holds the end of the silicone tubing outside the 

cleanbox, with the plastic bag still covering the end of the tubing. “Dirty hands” 

starts the pump and passes approximately 750 mL through the tubing and filter. 

“Dirty hands” stops the pump. 
DRAFT 

2-18

25. “Dirty hands” opens the outer bag of the dissolved metals sample bottle. “Clean 

hands” removes the inner bag and bottle and places it in the cleanbox. “Clean 

hands” opens the inner bag and removes the lid. “Dirty hands” operates the pump 

to collect the dissolved metals sample. “Dirty hands” stops the pump. “Clean 

hands” closes the lid on the sample bottle and closes the inner bag. “Clean hands” 

places the inner bag and bottle in the outer bag and “dirty hands” closes the outer 

bag. The samplers repeat this procedure for the dissolved metals and hexavalent 

chromium samples. 

26. “Dirty hands” places an ERG label on the outer bags of the sample bottles. 

2.4.2.2 Grab Sample Collection from Basin (or Tank) 

 For grab samples that are collected from a basin (or tank), ERG will set up the 

sampling equipment near the basin that represents the FGD scrubber purge sample. The field 

sampling personnel will use care when setting up the sample point to avoid any contamination 

from the surroundings. The sampling equipment will consist of the following: 

 Peristalic pump; 

 Colorless, electronic-grade, non-nitrile gloves; 

 PVC piping; 

 0.45 um filter; 

 Teflon® tubing; 

 Silicone tubing; 

 “Y” splitter; 

 Small table; 

 Cleanbox; 

 Tyvek® suits (for metals samples); 

 Masks (for mercury samples); and 

 Sample containers. 

 All metals sampling equipment will be specially-cleaned according to the 

procedures described in EPA Method 1669. ERG will follow protocols described in EPA 

Method 1669 to collect metal sample fractions. Two or more ERG samplers (“clean hands” and 

“dirty hands”) will follow the protocols described in the steps below to set up the sampling point, 

collect the field blank samples, and collect wastewater samples. This section describes the set up 

of the sample point and collection of the EPA samples5

. 

 

5

 For the sample collection, EPA assumes that samples will be split with the plant (or the plant’s representative) and 

therefore, the sample set-up describes equipment needed for split samples. However, EPA is not responsible for the 

collection of the split samples collected by the plant and therefore, the collection of their samples is not described. 
DRAFT 

2-19

1. Samplers remove the bags containing the gloves and HDPE plastic wrap from the 

coolers or storage containers in which they are packed. Samplers identify which 

coolers or boxes contain the double-bagged sample bottles, pre-cleaned tubing, 

and cleanbox. 

2. Both samplers put on Tyvek® suits, gloves, and masks. “Dirty hands” covers 

work surfaces (tables and platform) with HDPE plastic wrap and places the 

double-bagged sample bottles and Teflon® tubing within easy access on the 

covered surface. 

3. “Dirty hands” opens the outer bag of the cleanbox and “clean hands” opens the 

inner bag. “Clean hands” places the cleanbox at the point of sample collection. 

“Clean hands” opens the cleanbox and secures it open with the clips located 

inside the box. 

4. “Dirty hands” opens the opening on the peristaltic pump head so the tubing can be 

placed in the pump head. “Dirty hands” opens the outer bag containing a length 

of pre-cleaned Teflon® tubing attached to a 5-foot length of pre-cleaned silicone 

tubing with a “Y” splitter and two separate pieces of silicone tubing attached to 

the “Y” splitter. “Clean hands” moves the tubing into the cleanbox, opens the 

inner bag, and removes the tubing. “Clean hands” places a clean plastic bag over 

the end of the Teflon® and silicone tubing and places the end of the tubing in the 

cleanbox. 

5. “Dirty hands” threads the silicone tubing into the peristaltic pump head. 

6. Both samplers change gloves. 

7. “Dirty hands” opens the outer bags of the mercury field blank water and total 

mercury field blank sample bottles. “Clean hands” opens the inner bag for the 

field blank water, unscrews the lid and places it in the inner bag. “Clean hands” 

then places the Teflon® end of the tubing into the blank water. “Clean hands” 

moves the total mercury sample bottle into the cleanbox and opens the inner bag. 

Working inside the cleanbox, “clean hands” unscrews the lid. “Clean hands” 

holds the end of the silicone tubing outside the cleanbox over a bucket, with the 

plastic bag still covering the end of the tubing. “Dirty hands” operates the pump 

to pump blank water through the tubing. After the tubing has been purged with 

sufficient volume, “clean hands” places the silicone tubing back in the cleanbox, 

removes the plastic bag, and fills the total mercury field blank sample bottle. 

“Dirty hands” stops the pump. “Clean hands” places the plastic bag over the end 

of the silicone tubing, replaces the lid on the sample bottle, and closes the inner 

bag. “Clean hands” removes the bottle from the cleanbox and places it in the 

outer bag. “Dirty hands” closes the outer bag. The samplers repeat this procedure 

for the total metals field blank samples6

. 

 

6

 ERG only plans to collect field blank samples at each sampling point for one day of sampling episode. ERG will 

collect the dissolved mercury sample using the same technique as the total mercury sample, but the dissolved sample 

will be filtered at the laboratory. A dissolved mercury field blank will be performed by the laboratory to assess any 
DRAFT 

2-20

8. “Dirty hands” opens the outer bag of a capsule filter. “Clean hands” opens the 

inner bag and removes the capsule filter. “Clean hands” attaches the capsule filter 

to the end of the silicone tubing, prior to the “Y” splitter. 

9. “Dirty hands” opens the outer bag of the dissolved metals field blank water and 

dissolved metals by field blank sample bottle. “Clean hands” moves the dissolved 

metals field blank sample bottle to the cleanbox. “Clean hands” opens the inner 

bag of the field blank water. “Clean hands” removes the lid from the dissolved 

metals field blank water, places it in the inner bag, and places the end of the 

Teflon® tubing in the blank water. “Clean hands” holds the end of the silicone 

tubing outside the cleanbox over a bucket, with the plastic bag still covering the 

end of the tubing and “dirty hands” operates the pump to purge about 750 mL of 

blank water from the field blank water bottle through the tubing and filter. “Clean 

hands” places the end of the silicone tubing in the cleanbox, opens the inner bag 

of the dissolved metals field blank sample bottle, and removes the lid. “Clean 

hands” holds the silicone tubing over the bottle and “dirty hands” operates the 

pump to collect the dissolved metals field blank sample. “Dirty hands” stops the 

pump. “Clean hands” closes the lid on the sample bottle and closes the inner bag. 

“Clean hands” places the inner bag and bottle in the outer bag and “dirty hands” 

closes the outer bag. The samplers repeat this procedure for the dissolved metals 

and hexavalent chromium field blank samples. Note: 750 mL of blank water 

does not need to be purged into the waste bottle for each sample, just at the 

beginning of each new filter. If a new filter is needed, “clean hands” removes the 

used filter and samplers follow step 8 to replace the filter. 

10. Both samplers change gloves. 

11. After collecting all of the total and dissolved metals field blank samples, “clean 

hands” and “dirty hands” work together to place the Teflon® end of the tubing 

into the sample water, taking care that the end of the tubing does not touch 

anything other than the sample water. The samplers will secure the Teflon® 

tubing to a piece of PVC piping so the samplers can easily control the position of 

the tubing in the basin/tank. 

12. “Clean hands” holds the end of the silicone tubing outside the cleanbox over a 

bucket, with the plastic bag still covering the end of the tubing and “dirty hands” 

operates the pump to purge the tubing for a minimum of 2 minutes. After the 

tubing is purged, “Dirty hands” turns off the pump. “Clean hands” places the end 

of the silicone tubing back in the cleanbox. . 

13. “Dirty hands” opens the outer bag of the dissolved metals sample bottle. “Clean 

hands” removes the inner bag and bottle and places it in the cleanbox. “Clean 

hands” opens the inner bag and removes the lid. “Clean hands” holds the silicone 

 mercury contamination from the filtering performed at the laboratory. Therefore, ERG does not need to collect a 

dissolved mercury field blank sample in the field. 
DRAFT 

2-21

tubing over the bottle and “dirty hands” operates the pump to collect the dissolved 

metals sample. “Clean hands” closes the lid on the sample bottle and closes the 

inner bag. “Clean hands” places the inner bag and bottle in the outer bag and 

“dirty hands” closes the outer bag. The samplers repeat this procedure for the 

dissolved metals and hexavalent chromium samples. 

14. Both samplers change gloves. 

15. “Clean hands” removes the capsule filter from the silicone tubing and reattaches 

the tubing to the “Y” splitter. 

16. “Clean hands” holds the end of the silicone tubing outside the cleanbox over a 

bucket, with the plastic bag still covering the end of the tubing. “Dirty hands” 

operates the pump to purge the tubing for at least 2 minutes. 

17. “Dirty hands” opens the outer bag for the total mercury sample bottle. “Clean 

hands” removes the inner bag and bottle and places it in the cleanbox. “Clean 

hands” opens the inner bag and bottle lid. “Clean hands” removes the plastic bag 

from the tubing and fills the sample bottle. “Clean hands” places the tubing back 

in the plastic bag, replaces the lid on the sample bottle and closes the inner bag. 

“Clean hands” removes the sample bottle from the cleanbox and places it in the 

outer bag. “Dirty hands” closes the outer bag. The samplers repeat this for the 

dissolved mercury and total metals samples. 

18. “Dirty hands” places an ERG label on the outer bags of the sample bottles. 

19. Samplers fill a 1-L jar for the field measurements. The samplers will give the jar 

to another sampling team member to measure the temperature and pH. 

20. Both samplers collect the BOD5, Group I, Group II, and total cyanide samples 

from the sample location. Samples will be pumped directly into sample bottles. 

2.5 Preservation, Shipping, and Analysis

 All samples will be maintained on ice immediately upon collection (except the 

total and dissolved metals and the total and dissolved mercury samples, which do not require 

cooling). In addition, all samples will follow the on-site preservation requirements specified in 

40 CFR 136 method-specified protocols, including hexavalent chromium. The dissolved metals 

(not including mercury) and hexavalent chromium samples will be filtered in the field. The 

dissolved mercury samples will be filtered upon receipt at the laboratory. Samplers will filter 

samples within 15 minutes of the completion of the compositing period (or as soon thereafter as 

possible). For the FGD influent, filtration of dissolved samples will occur approximately one 

hour after the compositing period (or after the large sample volume is collected during the grab 
DRAFT 

2-22

sample collection) to allow for solids settling because it has a high suspended solids content that 

would clog the filter. 

 The total cyanide samples will be preserved according to the method-specific 

protocols. The samplers will first adjust the pH of the sample to >10 S.U. using sodium 

hydroxide. The samplers will then test the sample for the presence of sulfide using lead acetate 

test strips. If sulfide is present, the samplers will dilute the sample by pouring some of the 

sample into another sample bottle containing a measured amount of blank reagent water (e.g., 

add 50 mL of sample to 200 mL of blank reagent water). The samplers will then test the diluted 

sample for the presence of sulfide. If sulfide is still present, the samplers will create a more 

diluted sample and retest for sulfide until sulfide is not present in the sample. The samplers will 

then test the sample for the presence of total chlorine using potassium-iodide starch paper. If 

total chlorine is present, the samplers will add sodium arsenite in small increments until total 

chlorine is no longer present in the sample. The samplers will then readjust the pH to >10 S.U. 

using sodium hydroxide, if necessary, and place the sample on ice. 

 Table 2-3 lists the parameters, required sample and QC volume, bottle types, and 

on-site preservation requirements for each type of analysis. The type and amount of preservation 

used will be recorded on sample preservation log sheets (Figure 2-1). Preservation will be 

discontinued and noted on the traffic report if 10 percent of the sample volume is added and the 

required pH is not achieved. The wastewater samples, except certain metals samples, will be 

packed in ice chests with a sufficient quantity of ice to maintain a temperature of ≤6C. All 

samples will be prepared for overnight shipment via Federal Express to laboratories. 

2.6 Field Measurements and Engineering Data Collection

 Temperature and pH will be measured and recorded by the sampling crew at each 

sampling point when the automatic composite samplers are set up (and every six hours after the 

composite set up) or during the grab sample collection. A 1-liter glass jar will be filled prior to 

connecting the sample tubing to the composite containers for field measurements. Temperature 

and pH will be measured immediately after the collection of the field measurement aliquot. 

Table 2-4 summarizes the field measurements, the method to be used for the measurement, and 
DRAFT 

2-23

the detection range of each field test instrument. In addition, EPA will collect flow rate data for 

all waste streams. 

 Field sampling log sheets (Figure 2-2) will be completed at each sampling point. 

This sheet will record the sampling methodology, names of the samplers, sample collection time, 

field measurements, and any notes and observations. 

 During each sampling episode, engineering information will be collected with 

regard to design and operation of the plant being sampled. For example, information such as 

coal usage, plant capacity, wastewater flow rates, sludge generation rates (if applicable), and 

retention times in wastewater treatment process stages. Engineering data collection sheets 

(Figures 2-3, 2-4, and 2-5) will be completed for each plant. This information will be used to 

determine if the specific design or operational criteria of the steam electric operations affect the 

wastewater characteristics. 

2.7 Sample Labeling

 Each sample will be coded with a unique sample number and labeled at the time 

of collection. Typically, labels are printed prior to arrival in the field, though they may also be 

completed by hand. Each self-adhesive label is completed in indelible ink and contains the 

following information: 

 Sample number; 

 Sampling episode number; 

 Sampling point/description; 

 Date of sample collection; 

 Analysis to be performed; 

 Sample bottle type; and 

 Required preservation. 

If any of the pre-printed information is incorrect, it will be revised using indelible ink. In 

particular, if a required preservation is not used, it will be marked out (additional preservation 

details will be noted on the traffic report). Once applied to the sample container, labels are 

covered with clear tape to prevent tampering, abrasion, smearing, or loss during transit. 
DRAFT 

2-24

2.8 Traffic Reports

 To maintain a record of sample collection, transfer between personnel, shipment, 

and receipt by the laboratory, a traffic report is completed for each sample set at each sampling 

location. These forms are used to document sample custody transfer from the field to the 

laboratory. Traffic report forms are completed for all samples sent to all laboratories. Figure 2-6 

includes an example traffic report. At the time of sample shipment, a copy of the traffic report is 

sent to ERG, another copy is kept by sampling personnel, and two copies are transmitted with the 

samples to the analytical laboratory. 

 In addition to the transfer of custody, the traffic report provides information to the 

analytical laboratory on the sample number, type of water sample (in-line process, untreated 

wastewater, treated effluent), sample description, whether the sample is preserved, pH of the 

sample after preservation, type of sample (grab, composite), sample collection date and time, and 

the analyses requested. The comment section is used to provide special notes or instructions to 

the laboratory, such as how to composite separate samples prior to analysis. The sampling team 

will also comment if sample bottles are not completely filled (i.e., less than 75 percent full). In 

addition, the comments section will be used to note deviations from standard sampling protocols 

(for example, if a sample could not be acid-preserved because of excessive buffering). 

2.9 Quality Assurance/Quality Control

 Quality assurance/quality control (QA/QC) procedures applicable to this project 

are outlined in the Quality Assurance Project Plan for the Steam Electric Effluent Guidelines 

Rulemaking [2]. The QA/QC program for sample collection at steam electric plants will include 

the following: 

 Documentation for samples through laboratory traffic reports; 

 Collection of duplicate samples; 

 Collection of field blank(s) for total metals, dissolved metals, total 

mercury, dissolved mercury, and hexavalent chromium samples. 

 Analysis of bottle blank(s) for metals by the clean-equipment supplier; 
DRAFT 

2-25

 Analysis of equipment blank(s) for metals by the clean-equipment 

supplier; 

 Collection of laboratory QC samples for matrix spike/matrix spike 

duplicate analyses. 

 Duplicate sample sets will be collected as part of the quality assurance program 

for sampling. Duplicate samples are collected as separate aliquots in the field. EPA will collect 

one duplicate sample for every ten samples collected at a sampling event, excluding field blank 

samples. For example, EPA will collect four samples from each sampling point selected at a 

plant; therefore, if the EPA collects samples from two sample points at a plant (total of 8 

samples), only one duplicate sample will be collected, but if EPA collects samples from three 

sample points at a plant (total of 12 samples), then two duplicate samples will be collected. The 

field blank samples associated with the sampling points will not be included in the count of the 

total samples collected. Results of the duplicate analyses will be used to evaluate precision, 

including variability in sample collection, handling, preparation, and analysis. 

 Bottle blanks are used to evaluate possible contamination from the sample bottles. 

The bottle blank will consist of an analyte-free matrix (Ultra Pure Blank Water DI+TM) poured 

into the appropriate sample bottles (250-mL plastic bottle for metals by) and stored for several 

days prior to shipment to the laboratory. The supplier of the cleaned metals bottles will prepare 

and analyze the bottle blanks prior to shipping the equipment to the sampling episode. 

 Field blanks will be used to evaluate possible contamination caused by sampling 

equipment or by sampling equipment decontamination procedures. Field blanks will be 

prepared in the field prior to sample collection and analyzed for all sampling equipment, other 

than sample bottles, that come into direct contact with samples. Examples of sampling 

equipment are: 

 On-site sampling devices or piping installed for sample collection; and 

 Pumps, tubing, bottle dippers, buckets, and other equipment used to 

collect samples from less accessible sampling locations. 
DRAFT 

2-26

 For all metals samples (i.e., total mercury, total and dissolved metals, and 

hexavalent chromium), EPA will prepare a field blank at each sampling point for one day of the 

sample episode 7. 

 Equipment blanks will be used to evaluate possible contamination of metals 

caused by the sampling equipment. The supplier of the equipment used for metals sample 

collection will prepare and analyze the equipment blanks for metals. 

 As part of standard laboratory quality control, matrix effects on analytical 

performance are assessed through the analysis of matrix spikes and laboratory duplicates. 

Consequently, additional sample volume must be collected for these QC analyses. The ERG 

sampling team will be responsible for collecting, labeling, and shipping the laboratory QC 

volumes. Laboratory QC volumes will be collected as duplicate samples collected immediately 

after the original sample aliquot. For metals and classical analyses, EPA will collect one QC 

sample volume (i.e., MS/MSD sample) for every ten samples collected at a sampling event, 

excluding field blank samples. For example, EPA will collect four samples from each sampling 

point selected at a plant; therefore, if EPA collects samples from two sample points at a plant 

(total of 8 samples), only one QC sample volume will be collected, but if EPA collects samples 

from three sample points at a plant (total of 12 samples), then two QC sample volumes will be 

collected. The field blank samples associated with the sampling points will not be included in 

the count of the total samples collected. 

2.10 Sample Splitting

 The plant being sampled has the option to collect split or duplicate samples at 

each of the sampling points. If this option is exercised, the plant will supply all of the personnel, 

equipment, glassware, and reagents required to collect the samples and to coordinate the analysis 

of samples. 

 

7

 ERG will collect the dissolved mercury sample using the same technique as the total mercury sample, but the 

dissolved sample will be filtered at the laboratory. A dissolved mercury field blank will be performed by the 

laboratory to assess any mercury contamination from the filtering performed at the laboratory. Therefore, ERG does 

not need to collect a dissolved mercury field blank sample in the field. 
DRAFT 

2-27

Table 2-1. Sample Collection at Steam Electric Plants 

Analytical Parameter

Influent to FGD 

Wastewater 

Treatment

Intermediate Point 

in FGD Wastewater 

Treatment 

Effluent from FGD 

Wastewater 

Treatment

BOD5 X X X 

Total Cyanide X X X 

Group I (a) X X X 

Group II (b) X X X 

Total Metals X X X 

 

Dissolved Metals X X X 

Total Mercury X X X 

Dissolved Mercury X X X 

Hexavalent Chromium X X X 

(a) Group I includes TSS, TDS, sulfate, and chloride. 

(b) Group II includes ammonia as nitrogen, COD, nitrate/nitrite as nitrogen, TKN, and total phosphorus. 

(c) Actual sample location and specific pollutants will be defined in the plant-specific sampling plan. 
DRAFT 

2-28

Table 2-2. Analytical Methods 

Parameter Method Number 

Classicals

Biochemical Oxygen Demand (BOD5) SM 5210 B (or other 40 CFR Part 136-approved method 

Chemical Oxygen Demand (COD) EPA 410.3 (or other 40 CFR Part 136-approved method) 

Total Suspended Solids (TSS) SM 2540 D (or other 40 CFR Part 136-approved method) 

Total Dissolved Solids (TDS) SM 2540 C (or other 40 CFR Part 136-approved method) 

Sulfate ASTM D516-90 (or other 40 CFR Part 136-approved 

method) 

Chloride SM 4500–Cl–C (or other 40 CFR Part 136-approved 

method) 

Ammonia as Nitrogen SM 4500—NH3 B, F (or other 40 CFR Part 136-approved 

method) 

Nitrate/Nitrate as Nitrogen SM 4500—NO3 -H (or other 40 CFR Part 136-approved 

method) 

Total Kjeldahl Nitrogen (TKN) SM 4500—NH3 B or C, F (or other 40 CFR Part 136-

approved method) 

Total Phosphorus EPA 365.3 (or other 40 CFR Part 136-approved method) 

Total Cyanide EPA 335.4 (or other 40 CFR Part 136-approved method) 

Total and Dissolved Metals

Mercury EPA 1631E 

Hexavalent Chromium (dissolved only) EPA 218.6 (or other 40 CFR Part 136-approved method) 

 

Aluminum, antimony, arsenic, 

barium, beryllium, boron, 

cadmium, calcium, chromium, 

cobalt, copper, iron, lead, 

magnesium, manganese, 

molybdenum, nickel, selenium, 

silver, sodium, thallium, tin, 

titanium, vanadium, and zinc

EPA 200.7, EPA 200.8 (Note: EPA 200.8 may include the 

use of collision cell or dynamic reaction cell 

instrumentation for selected analytes.) 
DRAFT 

2-29

Table 2-3. Summary of Sample Container and Planned Preservation 

Parameter 

Sample 

Container and 

Volume 

QC Sample 

Container and 

Volume On-Site Preservation 

Classicals 

BOD5 One 1-L plastic 

bottle 

One 1-L plastic 

bottle 

≤6C 

Group I a Two 1-L plastic 

bottle 

Two 1-L plastic 

bottle 

≤6C 

Group II b Two 1-L plastic 

bottle 

Three 1-L 

plastic bottle 

H2SO4 to pH <2, ≤6C 

Total cyanide One 1-L plastic 

bottle 

Two 1-L plastic 

bottle 

NaOH to pH >10, dilution until 

sulfide is not present, NaAsO2 until 

total chlorine is not present, ≤6C 

Metals 

Total metals (except mercury) One 250-mL 

plastic bottle 

One 250-mL 

plastic bottle 

None 

(acid preserve at laboratory) 

 

Dissolved metals (except mercury and 

hexavalent chromium) 

One 250-mL 

plastic bottle 

One 250-mL 

plastic bottle 

0.45 μm filter (performed in field) 

(acid preserve at laboratory) 

 

Total mercury One 250-mL 

glass 

(ultraclean), 

fluoropolymer 

lined caps 

One 250-mL 

glass 

(ultraclean), 

fluoropolymer 

lined caps 

None 

(acid preserve at laboratory) 

Dissolved mercury Two 250-mL 

glass 

(ultraclean), 

fluoropolymer 

lined caps 

Two 250-mL 

glass 

(ultraclean), 

fluoropolymer 

lined caps 

None 

(filter and acid preserve at 

laboratory) 

Hexavalent chromium One 250-mL 

plastic bottle 

One 250-mL 

plastic bottle 

0.45 μm filter (performed in field) 

Ammonium sulfate buffer to 

pH 9.3 – 9.7, ≤6oC 

(a) Group I includes TSS, TDS, sulfate, and chloride. 

(b) Group II includes ammonia as nitrogen, COD, nitrate/nitrite as nitrogen, TKN, and total phosphorus. 

 
DRAFT 

2-30

Table 2-4. Sampling Point Field Measurements 

Field Measurements Method Detection Range (or Gradation of 

Scale) 

Temperature Thermometer -20 to 150 ± 1 oC 

pH (Standard Units) Four color indicator strip 

pH meter 

0 to 12 ± 1 pH S.U. 

-1.0 to 15.0 ± 0.1 pH S.U. 
DRAFT 

2-31

Sampling Episode ________ 

Preservation Chemicals - List Strength of Solution from Bottle 

H2SO4 ______________________ NH4SO4 ____________________ 

NaOH ______________________ 

Sample 

Number Analysis Date Name Chemical Initial pH Final pH

Number of 

Drops

 

Figure 2-1. Sample Preservation Log Sheet 
DRAFT 

2-32

Sampling Episode: _________________________________ 

Sampling Point: ___________________________________ 

Sample Numbers: __________________________________ 

Date: ____________________________________________ 

Manual Composite □ Grab □

Automatic Composite □

Time of Sample Collection: 

 Start Time □ AM □ PM 

 End Time □ AM □ PM 

Equipment Used: _________________________________________________ 

Samplers’ Names: ________________________________________________ 

Sample 

Point Time

Temp 

°C 

Thermometer / Meter 

pH 

(S.U.) 

Meter / Strips

Waste Stream 

Flow Rate 

(GPM)

1 

2 

3 

4 

5 

6 

7 

Notes: (include observations of odor and color of each aliquot, take pictures if necessary) 

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________ 

Figure 2-2. Field Sampling Log Sheet 
2-33 

DRAFT 

Plant Name: ____________________________________________________________________________ Plant Contact: ____________________________________________________________________________ Dates of Sample Collection: ___________________________________________________________________ Data Collected by: __________________________________________________________________________ Instructions: In the tables below, fill out information on the generating units and FGD systems operating at the plant based on all four depisode. Note any changes in operation that occur during the four-day period. Provide actual data if possible. If actual data are not availfor the specific information. Some of the data requested may not be susceptible to estimation. Enter “URE” for “unable to reasonably especify whether data provided are actual or estimated by writing in “ACT” or EST” wherever appropriate. 

Generating Unit Operating Characteristics During Sample Collection 

Unit 

ID Boiler Type 

Capacity 

(MW) 

Electricity 

Production 

(or Percent 

Capacity) 

SCR 

(No, On, 

Off) 

Particulate 

Control System 

(HS/CS ESP, or 

BH) 

FGD System Operating Characteristics During Sample Collection 

Unit 

ID 

Wet FGD 

System 

(Yes/No) 

Type of 

Scrubber 

Forced 

Oxidation 

(Yes/No) Sorbent 

Additives 

(DBA, formic 

acid, etc.) 

FGD Makeup Water 

Source 

SO2

Removal 

Percentage 

Typ

So

Sepa

Note changes in operation over the past month (e.g., turned off SCRs on October 1 or burned 5% petroleum coke previous week):

Figure 2-3. Engineering Data Collection Sheet (Page 1 of 3) 
DRAFT 

2-34

Plant Name: ____________________________________________________________________________ 

Plant Contact: ____________________________________________________________________________ 

Dates of Sample Collection: ___________________________________________________________________ 

Data Collected by: __________________________________________________________________________ 

Instructions: In the tables below, provide information on the coal burned and FGD scrubber slurry at the plant for 

each day of the sampling episode. Provide actual data if possible. If actual data are not available, provide estimates 

for the specific information. Some of the data requested may not be susceptible to estimation. Enter “URE” for 

“unable to reasonably estimate.” Otherwise, specify whether data provided are actual or estimated by writing in 

“ACT” or EST” wherever appropriate. 

Coal Information 

Day of 

Sampling Unit ID Coal Type 

Amount of 

Coal Used 

During 

Day of 

Sampling 

Source of 

Coal (Coal 

Region 

and/or 

State) 

Percent 

Sulfur in 

Coal 

Chlorine 

Content of 

Coal 

1 

 

2 

3 

4 

 

 

Note changes in operation over the past month (e.g., turned off SCRs on October 1 or burned 5% petroleum coke 

previous week) as well as conditions and changes during the sampling episode: 

Scrubber Slurry Information 

Day of 

Sampling 

FGD 

System ID 

Associated 

Unit IDs 

Scrubber Slurry 

Blowdown Flow Rate 

Scrubber 

Slurry 

Percent 

Solids 

Time of 

Dewatering 

During 

Sampling Day 

Percent 

Filtrate 

Recycled 

Back to 

Scrubber 

Flow Rate 

(gpm) Duration 

1 

 

 

2 

3 

4 

Figure 2-4. Engineering Data Collection Sheet (Page 2 of 2)
DRAFT 

2-35

Plant Name: ____________________________________________________________________________ Plant Contact: ____________________________________________________________________________ Dates of Sample Collection: ___________________________________________________________________ Data Collected by: __________________________________________________________________________ Instructions: In the table below, provide information on the FGD wastewater treatment system for each day of the sampling episode and wastewater treatment system tanks and reactors. If possible, provide the name of the acid and polymer used during the sampling episod

possible. If actual data are not available, provide estimates for the specific information. Some of the data requested may not be suscepti“URE” for “unable to reasonably estimate.” Otherwise, specify whether data provided are actual or estimated by writing in “ACT” or E

appropriate. 

FGD Wastewater Treatment System Operation Information 

Day of 

Sampling 

Scrubber Purge 

Chemical Usage 

(specify units) 

Flow Rate 

(gpm) Duration Lime 

Ferric 

Chloride 

Organo-sulfide 

_________ 

(specify type) 

Polymer: 

_________ 

(specify type) 

A

___

(spec

1 2 3 4 

Volume of equalization tank ________________ Volume of reaction tanks: 1) ________________ 2) ________________ 3) ________________ Volume of clarifiers 1) ________________ 2) ________________ Volume of first-stage bioreactors ________________ Volume of second-stage bioreactors ________________ 

Figure 2-5. Engineering Data Collection Sheet (Page 3 of 3)
DRAFT 

2-36

Figure 2-6. Example Traffic Report 

EPISODE NO:

RANGE OF SAMPLE NOS:

Return completed form to:

FOR LAB USE ONLY

NAME: SHIP TO: DATE REC'D:

CITY: ATTN: REC'D BY:

STATE: CARRIER: SAMPLE CONDITION ON RECEIPT:

INDUSTRIAL CATEGORY: AIRBILL:

DATE SHIPPED:

CONFIDENTIAL (Y/N): SAMPLING OFFICE/SAMPLER:

SAMPLE 

NUMBER SOURCE WATER

(city, river, well)

IN LINE PROCESS

UNREATED EFFLUENT

(raw

wastewater)

TREATED EFFLUENT

OTHER

(specify)

ADDITIONAL 

SAMPLE 

DESCRIPTION PH LEVEL

PRESERVED (Y/N)

G=GRAB / C=CO

MPOSITE

SAMPLE COLLECT OI N

TIME / DATE

Comments:

EPA Form 7500-50 (Rev 6-94) Previous editions are obselete.

Page 1: SCC Copy Page 2: Lab Copy

Copy of Page 1: Sampler Copy Copy of Page 2: Lab Copy for return to SCC

United States

EPA Environmental Protection Agency

Washington, DC 20460

TRAFFIC REPORT P.O. BOX 1407

USEPA ENGINEERING AND ANALYSIS DIVISION ALEXANDRIA, VA 22313

SAMPLE CONTROL CENTER (703) 519-1140

INDUSTRIAL FIRM SAMPLED SHIPPING & INFORMATION

SAMPLE POINT DESCRIPTION SAMPLE ANALYSES
DRAFT 

3-1

3.0 SAMPLING ACTIVITIES

 This section discusses the sampling team organization, site visit preparation, and 

sampling activities. 

3.1 Sampling Team Organization

 The sampling crew will consist of a crew chief from ERG, crew members from 

ERG, and EPA representative(s). The actual number of ERG crew members will be determined 

based on the number of sampling points at the plant. The crew chief will be responsible for all 

health and safety, sample collection, preservation, and shipping activities on site. After 

completion of the visit, the analytical results from each laboratory will be collated. This 

information will be summarized and transmitted in a trip report to EPA. After EPA review, the 

report will be forwarded to the plant for their review. 

3.2 Pre-Sampling Preparation

 EPA will conduct a pre-sampling site visit at each selected plant prior to 

sampling, unless EPA has already visited the plant previously. The site visits will provide EPA 

with site-specific process information such as: 

 Types of wastewater streams generated by the steam electric operations; 

 Feasibility of sampling FGD wastewater streams prior to commingling 

with other wastewater; 

 Locations of potential sampling points; 

 Conditions at potential sampling points (e.g. temperature and pH); and 

 Type of discharge at each sampling point (e.g. continuous or intermittent); 

and 

 Health and safety concerns at each potential sampling point. 
DRAFT 

3-2

 EPA will use this information to select sampling points and plan the sampling 

episode. Prior to the sampling episode, the ERG crew chief will prepare a plant-specific 

sampling plan outlining the descriptions of sampling points (including any information on flow 

rate, temperature, solids content, and pollutant concentrations provided by the facility contact), 

equipment needed (e.g., bottle clamp, dipper, and pole), anticipated health and safety 

requirements and procedures, the sample team organization, plant names and contacts, location 

of the local Federal Express office, and the names and addresses of analytical laboratories. The 

ERG Health and Safety Coordinator (HSC), Kevin Sikora, will identify the plant-specific health 

and safety requirements. 

 The ERG crew chief will distribute the plant-specific sampling plan to each team 

member and make sure they are completely familiar with the plant-specific health and safety 

requirements. Plant personnel will be given copies of the generic sampling plan, generic health 

and safety plan, and plant-specific sampling plan prior to the start of sampling. 

 The ERG crew chief will also coordinate the procurement and shipment of all 

necessary sampling and health and safety equipment. 

3.3 Field Sampling Activities

 At each site, the ERG crew chief, in conjunction with the EPA Work Assignment 

Manager (WAM), will meet with plant personnel to determine whether samples can be collected 

at each of the planned sampling points. Upon making the decision to collect samples, the ERG 

crew chief will update the descriptions of the proposed sampling points, if necessary, in 

consultation with EPA and plant personnel. If necessary, additional equipment and glassware 

will be obtained. The revised description shall include: 

 A sample point description and collection procedure for each sample 

point; 

 A list of the sample fractions to be collected at each point; 

 A list of potential physical hazards (such as pH, temperature, and 

potentially hazardous equipment); 
DRAFT 

3-3

 A list of potential chemical hazards associated with each sample point; 

and 

 A list of proposed health and safety procedures. 

 Prior to sampling, the ERG crew chief will also notify the ERG HSC of any 

revised sampling activity descriptions along with recommended revisions to the proposed health 

and safety procedures. Together, the crew chief and HSC will review the proposed health and 

safety procedures. The crew chief will incorporate any plant-specific changes indicated by the 

HSC, and gain approval for sampling from the HSC before proceeding with sampling activities. 

 All sample bottles will be labeled, collected, and preserved, according to method 

protocols. Sample fractions requiring ≤6C preservation will be placed on ice until desired 

temperature is reached. Sample fractions will then be sealed, and placed in coolers for shipment 

to the laboratory. The Traffic Report forms will be completed and placed in plastic sleeves 

inside the coolers. The coolers will then be taken to the nearest Federal Express office and 

shipped to the analytical laboratories. At the conclusion of the sampling episode, the sampling 

equipment will be prepared for return shipping. 

 

3.4 Standard Logistics

 This section of the sampling plan summarizes plant contacts, analytical laboratory 

contacts and addresses, and sampling team personnel and support functions. 

3.4.1 Plant Contacts 

 To be determined prior to sampling. 

3.4.2 EPA Contacts 

Ron Jordan 

 Engineering and Analysis Division 

 U.S. Environmental Protection Agency 
DRAFT 

3-4

 1200 Pennsylvania Avenue, NW (4303T) 

 Washington, D.C. 20460 

 (202) 566-1003 

Jezebele Alicea 

Engineering and Analysis Division 

U.S. Environmental Protection Agency 

1200 Pennsylvania Avenue, NW (4303T) 

Washington, D.C. 20460 

(202) 566-1755 

3.4.3 Analytical Laboratories 

To be determined prior to sampling. 

3.4.4 ERG Contacts 

Deb Bartram (ERG Work Assignment Manager) 

 Eastern Research Group, Inc. 

 14555 Avion Parkway, Suite 200 

 Chantilly, VA 20151 

 (703) 633-1669 

 TJ Finseth (Sampling Program Lead) 

 Eastern Research Group, Inc. 

 14555 Avion Parkway, Suite 200 

 Chantilly, VA 20151 

 (703) 633-1698 

3.4.5 Freight Forwarders 

 Federal Express 

 General Information (800) 463-3339 

 Specific location to be determined for each sampling trip. 
DRAFT 

4-1

4.0 SAMPLE SHIPMENT

 All sample containers will be labeled with ERG's standard address labels. All 

samples will be tracked using Traffic Report forms. Custody will be maintained by the sampling 

crew chief from sample collection until samples are delivered to Federal Express. 

 All samples will be packaged and shipped in accordance with DOT or IATA 

regulations. The general IATA packaging requirements for air shipment are as follows: 

 “Inner packaging must be so packed, secured or cushioned as to prevent their 

breakage or leakage and so as to control their movement within the outer 

packaging during normal conditions of transport. Cushioning material must not 

react dangerously with the contents of the inner packaging. Any leakage of the 

contents must not substantially impair the protective properties of the cushioning 

material. Unless otherwise provided in this paragraph or in the Packing 

Instructions, liquids in Classes, 3, 4, 5, 6, or 8 of Packing Groups I or II in glass or 

earthenware inner packaging, must be packaged using material capable of 

absorbing the liquid. Absorbent material must not react dangerously with the 

liquid. Absorbent material is not required...” (IATA Dangerous Goods 

Regulations, 5.0.16). 

 “When filling receptacles for liquids, sufficient ullage (outage) must be left to 

ensure that neither leakage nor permanent distortion of the receptacle will occur 

as a result of an expansion of the liquid caused by temperatures likely to prevail 

during transport. Liquids must not completely fill a receptacle at a temperature of 

55°C (130°F).” (IATA Dangerous Goods Regulations, 5.0.12). 

 The packing and labeling procedures in the following subsections may be used for 

nonhazardous samples. Hazardous samples will be identified based on consultation with the 

hazardous shipments contact, and appropriate hazardous shipping procedures will be followed. 

Based on process considerations, samples collected are not expected to be classified as IATA 

dangerous goods. 

4.1 Sample Set Preparation

 Samples are collected as a series of “fractions,” or bottles designated for 

particular analyses requiring the same preservation. The comprehensive water sample set 

consists of sample fractions for all pollutants listed in Section 2.2, collected as 24-hour 

composite samples and transferred into the individual sample bottles. 
DRAFT 

4-2

4.2 Sample Packing

 All dilute samples from the plant will be packed according to the following 

guidelines (there is no limit on the amount of liquid each sample container may contain): 

1. Label each sample bottle. If a required preservation is not used, cross it off with 

indelible ink. Cover the label with clear tape to protect this information. Metals 

sample bottles will not be labeled; instead, the outer plastic bag for each bottle 

will be labeled. 

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. The bottle threads will not 

be cleaned for the mercury sample bottles. 

3. Place each sample bottle requiring ≤6C preservation into an ice chest with wet 

ice prior to packaging to cool. 

4. When each sample requiring ≤6C preservation has reached the desired 

temperature, wrap each glass sample bottle with two layers of “bubble wrap” (or 

place bottle in two “bubble bags”). The bubble wrap must fit snugly and 

completely cover the sample bottle. Each “bubble-wrapped” container and plastic 

container must then be enclosed in an individual sealable plastic freezer bag. 

5. Place two garbage bags inside each other in the cooler. 

6. Place sample bottles in garbage bags in the cooler with proper end up, close the 

interior garbage bag by tying, or with a twist-tie. 

7. Add ice to cooler to keep samples cold during shipment. Arrange blue ice or 

sealed plastic freezer bags filled with wet ice on top of the sample bottles (if 

samples require ≤6C preservation). If using wet ice, place the ice inside two onegallon sealable freezer bags. Put at least 4 × 1⁄2 gallons of ice (4 × 2.5 lbs of ice) in 

each large cooler and 2 × 1⁄2 gallons of ice (2 × 2.5 lbs of ice) in each small cooler. 

More ice should be used when ambient temperatures are very high. The ice should 

be placed inside the second garbage bag. Close the second garbage bag with a 

twist-tie. 

8. Fill in around the bottles and any free space with additional cushioning material. 

Sufficient packing material should be used so that the sample containers will not 

shift during shipment. 

9. Seal the Traffic Report form in a plastic zip-lock bag and tape securely to the 

inside of the cooler lid. 
DRAFT 

4-3

10. Place a "Return to ..." label on the inside of the cooler lid. 

11. Close cooler. 

12. Make several wraps with 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. Tape the cooler drain plug so it will not open. 

14. Place a completed address label on the lid of the cooler including name, address, 

and telephone number of the receiving laboratory and the return address and 

telephone number of the shipper. 
DRAFT 

5-1

5.0 REFERENCES

U.S. EPA. 2009. Steam Electric Power Generating Point Source Category: Final Detailed Study 

Report. EPA 821-R-09-008. Washington, DC. (October). Available online at: 

http://www.epa.gov/guide/steam/finalreport.pdf. DCN SE00003. 

Eastern Research Group, Inc. 2009. Quality Assurance Project Plan for the Steam Electric 

Effluent Guidelines Rulemaking. (September). DCN SE00058.