# Final Sampling Plan Duke Energy Carolinas’
Belews Creek Steam Station Belews Creek, NC

Sampling Episode 6558

Prepared for:



## U.S. Environmental Protection Agency

Engineering and Analysis Division
Office of Water 1200 Pennsylvania Avenue, NW Washing ton, D.C. 20460

Prepared by:



### Eastern Research Group, Inc. 14555 Avion Parkway
Suite 200 Chantilly, VA 20151

May 27

, 20 10

EPA Contract No. 68

- C

- 02

- 095 Work Assignment 7

- 2 9i TABLE OF CONTENTS

Page

1. I NTRODUCTION

................................ ................................ ................................ ................. 1

- 1

1.1 Background

................................ ................................ ................................ .......... 1

- 1

1.2 Objectives and Scope

................................ ................................ ........................... 1

- 1

1.3 Plant Selection

................................ ................................ ................................ ..... 1

- 2

2. F ACILITY O VERVIEW

................................ ................................ ................................ ........ 2

- 1

2.1 FGD Scrubber Systems

................................ ................................ ........................ 2

- 1

2.2 FGD Wastewater Treatment System

................................ ................................ ... 2

- 2

3. S AMPLING P ROCEDURES

................................ ................................ ................................ ... 3

- 1

3.1 Sampling Point Selection

................................ ................................ ..................... 3

- 1

3.2 Analyte Selection

................................ ................................ ................................ . 3

- 1

3.3 Sample Collection Procedures

................................ ................................ ............. 3

- 2

3.3.1 Influent to FGD Wastewater Treatment System (SP

- 1)

.......................... 3

- 3

3.3.2 Influent to Bioreactor System (SP

- 2)

................................ ....................... 3

- 8

3.3.3 Effluent from Bioreactor System (SP

- 3)

................................ ................ 3

- 16

3.4 Sample Preservation, Shipping, and Analysis

................................ ................... 3

- 23

3.5 Field Measurements and Engineering Data C ollection

................................ ..... 3

- 24

3.6 Sample Labeling

................................ ................................ ................................ 3

- 25

3.7 Traffic Reports

................................ ................................ ................................ ... 3

- 25

3.8 Quality Assurance/Quality Control

................................ ................................ .... 3

- 26

3.9 Sample Splitting

................................ ................................ ................................ . 3

- 28

4. S AMPLING A CTIVITIES

................................ ................................ ................................ ...... 4

- 1

4.1 Sampling Team Organization

................................ ................................ .............. 4

- 1

4.2 Presampling Preparation

................................ ................................ ...................... 4

- 1

4.3 Field Sampling Activitie s

................................ ................................ .................... 4

- 1

4.4 Logistics

................................ ................................ ................................ ............... 4

- 2

4.4.1 Belews Creek Steam Station Contacts

................................ ..................... 4

- 2

4.4.2 EPA Contacts

................................ ................................ ........................... 4

- 2

4.4.3 Analytical Laboratories

................................ ................................ ............ 4

- 3

4.4.4 ERG Contacts

................................ ................................ ........................... 4

- 3

4.4.5 Freight Forwarders

................................ ................................ ................... 4

- 3

5. S AMPLE S HIPMENT

................................ ................................ ................................ ........... 5

- 1

5.1 Sample Set Preparation

................................ ................................ ........................ 5

- 1

5.2 Sample Packing

................................ ................................ ................................ .... 5

- 1

6. S ITE

- S PECIFIC H EALTH AND S AFETY P ROCEDURES

................................ .......................... 6

- 1

6.1 Emergency/ Medical Procedures

................................ ................................ .......... 6

- 1

6.1.1 First Aid 6

- 1

6.1.2 Site Evacuation/Emergency Response Plan

................................ ............. 6

- 1

6.1.3 Emergency Showers and Eye Washes

................................ ..................... 6

- 1

6.1.4 Local Hospital

................................ ................................ .......................... 6

- 1

6.2 ERG Health and Safety Respo nsibilities and Authority

................................ ...... 6

- 1TABLE OF CONTENTS (Continued)

Page

ii 6.2.1 Work Assignment Manager

................................ ................................ ..... 6

- 2

6.2.2 Crew Chief

................................ ................................ ............................... 6

- 2

6.2.3 Sampling Team Members

................................ ................................ ........ 6

- 2

6.3 Briefings

................................ ................................ ................................ ............... 6

- 2

6.3.1 Off

- Site Briefings

................................ ................................ ..................... 6

- 2

6.3.2 On

- Site Briefings

................................ ................................ ..................... 6

- 3

6.4 Safety Procedures

................................ ................................ ................................ . 6

- 3

6.4.1 Personal Protective Equipment (P PE)

................................ ..................... 6

- 3

6.4.2 Safety Practices

................................ ................................ ........................ 6

- 3

6.4.3 Safe Work Practices

................................ ................................ ................. 6

- 4

6.5 Sampling

- Point

- Specific Safety Procedures

................................ ........................ 6

- 4

6.5.1 Physical Hazards

................................ ................................ ...................... 6

- 4

6.5.2 Thermal Hazards

................................ ................................ ...................... 6

- 5

6.5.3 Chemical Hazards

................................ ................................ .................... 6

- 5

6.6 Temperature Extremes

................................ ................................ ......................... 6

- 5

6.6.1 Heat Stress

................................ ................................ ............................... 6

- 5

6.6.2 Heat Stress Monitoring

................................ ................................ ............ 6

- 6

6.7 First Aid

................................ ................................ ................................ ............... 6

- 7

6.8 Sample Preservation and Safety Considerations

................................ .................. 6

- 7

6.9 Training and Medical Monitoring Requirements

................................ ................ 6

- 8

6.10 Shift Work Protocol

................................ ................................ ............................. 6

- 9

7. R EFERENCES

................................ ................................ ................................ ..................... 7

- 1iii LIST OF TABLES

Page

3

- 1 Sample Collection at Belews Creek Steam Station

................................ ....................... 3

- 29

3

- 2 Analytical Methods

................................ ................................ ................................ ........ 3

- 30

3

- 3 Summary of Sample Container and Planned Preservation

................................ ............ 3

- 31

3

- 4 Sampling Point Field Measurements

................................ ................................ ............. 3

- 32

6

- 1 Sample

- Point

- Specific PPE and Potential Haz ards

................................ ....................... 6

- 10iv LIST OF FIGURES

Page

2

- 1 Simplified Diagram of the FGD Wastewater Treatment System, Belews Creek Steam

Station

................................ ................................ ................................ .............................. 2

- 6

2

- 2 Physical/Chemical Separation and Bi ological Reactor Portion of FGD Wastewater Treatment System, Belews Creek Steam Station

................................ ............................. 2

- 7

3

- 1 Sample Preservation Log Sheet

................................ ................................ ..................... 3

- 33

3

- 2 Field Sampling Log Sheet

................................ ................................ .............................. 3

- 34

3

- 3 Engineering Data Collection Sheet (Page 1 of 3)

................................ .......................... 3

- 35

3

- 4 Engineering Data Collection Sheet (Page 2 of 3)

................................ .......................... 3

- 36

3

- 5 Engineering Data Collection Sheet (Page 3 of 3)

................................ .......................... 3

- 37

3

- 6 Example Traffic Report

................................ ................................ ................................ . 3

- 381

- 1 1. I NTRODUCTION

The Engineering and Analysis Division (EAD) of the U.S. Environmental Protection Agency (EPA) is currently conducting a sampling program at steam electric power plants. T he sampling program will characterize raw wastewaters generated by coal

- fired steam electric power plants, as well as evaluate treatment technologies and best management practices used to reduce pollutant discharges. This sampling plan, developed for the D uke Energy Carolinas’ Belews Creek Steam Station (Belews Creek), provides plant

- specific sampling procedures and methods EPA and its contractors will follow when conducting sampling activities. Sampling will be performed by EPA’s technical contractor, East ern Research Group, Inc. (ERG), under

Contract No. 68

- C

- 02

- 095

. This document, in combination with the Generic Sampling and Analysis Plan for Coal

- Fired Steam Electric Power Plants [ 1 ], is intended to serve as a guide to the ERG field sampling crew, a revi ew mechanism for EPA personnel, and a source of procedural information for plant personnel.

1.1

During EPA’s recently completed detailed study of the steam electric industry, EPA identified metals and certain other constituents present in the was tewater discharges from steam electric power plants that are contributing the majority of the toxic loadings for the industry. Additionally, EPA determined that one of the waste streams contributing most of these toxic loadings are associated with wet flue gas desulfurization (FGD) systems present at coal

- fired power plants. Background

This sampling plan will focus on characterizing wastewaters and treatment system discharges at Belews Creek. For a general description of the steam electric process and the

wastewate rs 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 [ 2 ].

1.2

EPA is preparing to collect and analyze samples to characterize wastewater streams generated at coal

- fired steam electric power plants. This sampling plan describes the approach

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

tr eated FGD wastewater from the following types of FGD wastewater treatment systems: Objectives and Scope

**•** Chemical precipitation : Physical/chemical treatment for heavy metals removal using hydroxide or a combination of hydroxide and sulfide precipitation; and

**•** Biol ogical : B iolo gical treatment specifically designed for metals removal.1

- 2 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, pollutan t concentrations, flow rate/volume) of untreated FGD scrubber purge

wastewater?

**•** What are the effluent concentrations for pollutants present in treated FGD

wastewater?

**•** What are the pollutant loadings associated with discharges of FGD wastewater following treatment?

EPA conduct ed a one

- day pre

- sampling site visit at Belews Creek on March 12, 2008 as part of the detailed study

. EPA also collected samples from the FGD wastewater treatment

system at Belews Creek in October 2008 as part of the detailed study

. Data obtained from this sampling episode can be found in the Final Sampling Episode Report Duke Energy Carolinas’

Belews Creek Steam Station (DCN 06197 ). Because EPA had gathered all the information necessary in both the pre

- sampling site visit and sampli ng episode, EPA did not need to conduct another pre

- sampling site visit at Belews Creek for the purpose of this sampling episode

.

The sampling program will consist of four

- day sampling episodes at selected plants. The sampling will characterize the was tewaters 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 ele ctric power plants. In addition to sampling the wastewater , EPA will collect information regarding system design and day

- to

- day operation.

1.3

EPA expects to select up to seven coal

- fired steam electric plants for FGD wa stewater sampling, b as ing the plant selection on the process configurations and characteristics of the plants. Plant Selection

Belews Creek was selected by EPA for sampling based on the following site

characteristics:

**•** The plant is a coal

- fired power plant that burns e astern b ituminous coal in each of its two generating units;

**•** The plant operates limestone forced oxidation wet FGD systems on both units;1

- 3 **•** The plant operates a segregated FGD wastewater treatment system, which includes the following steps:

— Equalization,

— p H adjustment (lime addition),

— Ferric chloride addition,

— Polymer addition,

— Clarification,

— Filtration,

— Biological treatment (nitrogen and metals), and

**•** The plant operates selective catalytic reduction ( SCR ) systems on both units; and

**•** The plant produces a co mmercial

- grade gypsum by

- product.2

- 1 2. F ACILITY O VERVIEW

Belews Creek operates two steam electric units and each has a coal

- fired boiler. Belews Creek burns approximately 19,000 tons of e astern b ituminous coal per day. Units 1 and 2, whi ch came on line in 1974 and 1975, respectively, each have a capacity of 1,200 megawatts (MW). The Belews Creek plant and supporting facilities are located on approximately 700 acres in Belews Creek, NC, adjacent to Belews Lake. The plant owns approximately 7,000 a cres adjacent

to Belews Lake.

A pproximately two years ago, Belews Creek retrofitted both units with a wet FGD scrubber system to control the sulfur dioxide (SO 2 ) releases from the plant. The Unit 1 FGD system was installed in February 2008, and the Unit 2 FGD system was installed in May 2008. The wet FGD scrubbers are designed to remove more than 95 percent of SO 2 from the flue gas

. With the addition of the FGD scrubber systems, Belews Creek also installed an FGD wastewater

treatment system to co ntrol the discharges of the wastewater generated during the operation of

the FGD scrubbers. Sections 2.1 and 2.2 further discuss t he FGD scrubber systems and the FGD

wastewater treatment system , respectively.

Belews Creek retrofitted Units 1 and 2 with S CR systems in August 2003 and February 2004, respectively, to control nitrogen oxide (NO

x ) releases from the plant. Initially, Belews Creek was only operating the SCRs during ozone season, May through September; however, in January 2007, Belews Creek bega n operating the SCRs year

- round. Belews Creek personnel stated that the plant plans to continue operating the SCRs year

- round into the foreseeable future.

The electrostatic precipitators ( ESPs ) at Belews Creek are particulate control devices that

are des igned to remove 99.8 percent of the fly ash and other particulates from the flue gas. Belews Creek utilizes ESPs to remove the fly ash from both units. The fly ash and other particulates are collected in hoppers and typically are pneumatically transferred to fly ash silos. However, Belews Creek also has the capability of handl ing the fly ash wet by sluicing the fly ash in the hoppers and transferring the fly ash sluice water to the ash basin.

Units 1 and 2 have the following configuration:

**•** Boiler;

**•** Air p reheater;

**•** SCR system;

**•** ESP; and

**•** FGD scrubber system.

2.1

Belews Creek operates a wet FGD scrubber system on both Units 1 and 2, downstream of the ESP, to control the emission of sulfur dioxide from the unit. The plant uses limestone slurr y as the sorbent for sulfur dioxide absorption. Limestone and service water are fed to on

- site ball

mills , which pulverize the limestone to create the slurry

. From the ball mills, the slurry is transferred to hydroclones to collect limestone particles that are too large for use in the FGD

system. The underflow from the hydroclones is transferred to the reject tank and then sent back to the ball mill for additional processing. The overflow from the hydroclones, which is FGD Scrubber Systems2

- 2 approximately 27 to 30 percent solids (by weight), is transferred to the reagent tank for storage and then used as fresh limestone slurry in the absorber.

The fresh limestone slurry is fed to the reaction tank of the FGD system and the recycle pumps pump the slurry to the various levels of the FGD scrubber (typically three of four spray levels are operating at one time). The slurry is pressurized and sprayed downward into the scrubber vessel through spray nozzles. As the slurry falls downward and the flue gas flows

counter current to the slur ry, the spray droplets of the limestone slurry contact the flue gas and

absorb the SO 2 , which reacts with the limestone particles and produces calcium sulfite. The spray droplets continue to flow d ownward in the scrubber until they reach the reaction tank. Belews Creek bubbles air through the reaction tank to oxidize the calcium sulfite to calcium sulfate (i.e., gypsum).

Belews Creek intermittently blows down the gypsum slurry from the reaction tank to

control the solids concentration in the scrubbers aro und 15 percent solids. The chlorides concentration in the scrubbers is maintained between 8,000 and 10,000 parts per million ( ppm )

, with a design maximum chlorides concentration of 12,000 ppm. Belews Creek transfers the blowdown from the scrubber to the gy psum dewatering operations.

The gypsum slurry is pumped to the primary hydrocyclones where the solid gypsum is separated from the water by centrifugal force. The solid gypsum is forced outward to the walls of the hydrocyclones and falls downward, while the water exits the top of the hydrocyclones. The gypsum from the primary hydrocyclones is transferred to the filter feed tank, which is then transferred to the vacuum filter belts. The overflow from the primary hydrocyclones is transferred to a holding ta nk and then pumped to the secondary hydrocyclones. The underflow from the secondary hydrocyclones is returned to the scrubber or sent to the filter feed tank. The overflow from the secondary hydrocyclones is sent to the purge tank and then pumped to the

FG D wastewater treatment system.

Belews Creek washes the gypsum sent to the vacuum filter belts with service water, as it is poured onto the belts. The vacuum filter belts dry the gypsum to a moisture content of approximately 10 percent. Belews Creek trans fers the dry gypsum to an uncovered gypsum storage area and then trucks the gypsum to a wallboard manufacturer in Mount Holly, N orth

C arolina , approximately 105 miles from the plant. Belews Creek generates approximately 500,000 tons of gypsum per year; how ever, plant personnel stated that the gypsum production is dependent on the coal being burned and sulfur content of the coal.

2.2

The FGD wastewater treatment system is designed to receive intermittent transfers of

FGD wastewa ter from the purge tank, which contains secondary hydrocyclone overflow , at a flow rate varying from 350 to 600 gallons per minute ( gpm ) for approximately 18 hours per day, with a total daily flow rate of approximately 489,000 gallons per day ( gpd ) . Accord ing to Belews Creek personnel, the flow rate to the equalization tank varies depending on whether one or both of the scrubbers are purging. FGD Wastewater Treatment System

The plant operates the FGD wastewater treatment system 24 hours per day. Belews Creek

installed t he wastewater tr eatment system to treat the FGD scrubber purge wastewater to meet its2

- 3 permit limits, which include limits for total suspended solids (TSS) and selenium . The Belews Creek FGD wastewater treatment system contains the following treatment operations:

**•** Physical /Chemical Separation;

— Equalization,

— pH adjustment (lime addition),

— Ferric chloride addition,

— Polymer addition,

— Clarification,

— Filtration; and

**•** Biological Reactors;

— Cooling (heat extraction),

— Nutrient addition,

— First

- stage biological reaction,

— Nutrient addi tion, and

— Second

- stage biological reaction

.

Figures 2

- 1 and 2

- 2

, located at the end of this section, present process flow diagrams of the FGD wastewater treatment system, as well as the planned sampling locations for EPA’s sampling episode. Figure 2

- 1 is a simplified diagram of the FGD wastewater treatment system, showing different portions of the system. Figure 2

- 2 is a diagram of the chemical precipitation and biological reactor portions of the treatment system

.

The secondary hydrocyclone overflow fr om the scrubbers is transferred to the purge tank and then sent to the equalization tank at the start of the wastewater treatment system. This wastewater is expected to contain approximately 0.8 percent solids and have a pH of 6.5 to 7.0

S.U

. The equalizat ion tank also receives water from the filtrate sump (which includes filter press filtrate), gravity filter backwash reject, backflush waste from the biological treatment system,

and off

- specification biological treatment effluent.

From the equalization t ank, the wastewater enters three reaction tanks in series: reaction

tank 1

, in which lime is added to increase the pH to between 8.5 and 9.2 S.U. (target 8.8 S.U. );

reaction tank 2 , formerly used for organosulfide addition, but which is now used to provide additional mixing; and reaction tank 3, in which ferric chloride is added. From reaction tank 3, the wastewater flows to a mix chamber where polymer (Nalco 71307) is added.

From the mix chamber, the wastewater flow split s and enters two clarifiers in pa rallel. Each of the clarifiers is capable of handling 100 percent of the waste stream capacity. Typically both clarifiers are in operation. However, during the scheduled sampling event one clarifier will be out of service for preventative maintenance. The clarifiers are solids contact clarifiers that contain a sludge bed that attracts the solids in the wastewater. Hydrochloric acid is added to the wastewater at a point between the clarifiers and the sand filters to adjust the pH prior to the biological trea tment system. The target pH after hydrochloric acid addition is 6.8 S.U. After the hydrochloric acid addition, the overflow from the two clarifiers is split and sent through three sand filters in parallel. Each of the sand filters can handle 75 percent of the waste stream capacity. The target maximum TSS level for the sand filter effluent is 50 ppm; however, the plant tries to achieve an effluent TSS concentration below 20 ppm. The sand filters are2

- 4 continuous backwash gravity filters. The filter backwash is sent to a sump, and then transferred to the equalization tank.

The sludge from the clarifiers is transferred to a sludge storage tank. A portion of the clarifier sludge is recycled from the sludge storage tank to reaction tank 1, while the majority is

p umped to a filter press for dewatering . Belews Creek achieves a solids concentration of 15 percent in the sludge tank

. The filter press cake is transferred to the fly ash landfill and the filtrate is sent to the filtrate sump. Each filter press operation p roduces an average of 28,000 lbs

of filter cake. Belews Creek performs approximately 10 filter press operations per week.

In t he bioreactor portion of the treatment system , Belews Creek treats the wastewater in

two stages. Each stage contains eight bior eactor cells, which are operated in parallel. Each cell contains an activated carbon bed. Within the activated carbon bed, specialized microbes fill the voided areas and reduce the nitrogen and metals, specifically selenium, in the wastewater. The

microbes selected for the bioreactor system have the ability to reduce selenium to its elemental form, while other metals are precipitated as sulfide complexes. The wastewater from the sand filters is transferred to a holding tank prior to entering a heat exchange r to reduce the temperature from approximately 110 o F to 95 o F. As the wastewater flows from the heat exchanger to the first stage of bioreactor cells, Belews Creek adds nutrients (molasses

- based) , which provide a source

of carbon to feed the bacteria . The w astewater is divided evenly among the eight first

- stage cells. The flow to each cell is sent to 16 distribution pipes to create an even distribution of flow into the top of the cell. The water level in the cells is approximately three feet above the activa ted

carbon bed.

Belews Creek operates the bioreactors to achieve a negative oxidation reduction potential within the system, which provides the optimum environment to reduce selenium to its elemental form. This reduction potential is controlled by the am ount of nutrient that is fed to the system. The plant also controls the pH in the bioreactor cells to between 6.0 and 9.0 S.U. because extreme high or low pH levels could affect the performance of the microbe s and potentially

allow for non desirable microbe s to propagate.

The effluent from all eight of the first

- stage bioreactor cells is combined in the first

- stage effluent storage area. The wastewater is then transferred to the second

- stage bioreactor cells,

which are operated in parallel. Nutrients are a dded to the wastewater as feed for the microbes as the wastewater is transferred. As in the first stage, the wastewater is divided evenly among the eight second

- stage cells and each cell has 16 distributor pipes to evenly distribute the flow into

the cell.

Occasionally the bioreactor cells will need to be backflushed to remove accumulated solids. The plant pumps the effluent from the first

- stage bioreactor cells backwards through each cell and it overflows into a spillover chamber

. The plant then returns the backwash overflow to the equalization tank at the start of the FGD wastewater treatment system.

Because the first

- stage bioreactor cells denitrify the waste stream, they produce nitrogen and carbon dioxide gas. To remove the gas from the cells, the plant occasionally performs a degassing operation where water is sent backwards through the cells, like a backflush, but the flush is only long enough for the gas to “burp” out of the system. The second

- stage bioreactor2

- 5 cells are primarily anoxic and do no t produce as much gas as the first

- stage cells , requiring less frequent degassing than the first

- stage cells

.

F rom the second stage of the biological treatment system , wastewater is transferred to

two wetland supply t anks , which is then transferred dire ctly to the ash basin

. According to plant personnel, the treated FGD wastewater , excluding cooling water, represents approximately seven percent of the total flow discharge from the ash basin to the Dan River, via NPDES Outfall 003.

Figure 2

- 2 shows the planned sampling points for the sampling episode at Belews Creek. The influent sampling point at Belews Creek’s FGD wastewater treatment system is located downstream of the purge tank and upstream of the equalization tank. Thus, the influent sampling poin t is upstream of any chemical addition or treatment system recirculation flow streams . The

in

- process sampling point within Belews Creek’s FGD wastewater treatment system is located downstream of the sand filters and the holding tank. The biological reacto r effluent sampling point at Belews Creek’s FGD wastewater treatment system is located downstream of the second

stage effluent storage area and upstream of where the FGD wastewater treatment effluent is commingled with the heat exchanger cooling water

.2-6

Figure 2

- 1. Simplified Diagram of the FGD Wastewater Treatment System, Belews Creek Steam Station2-7 FGD Scrubber Purge ( from Purge Tank ) Lime

Polymer

Equalization

Tank Reaction Tank 1 Reaction

Tank 2 Reaction

Tank 3 SP

- 1

SP

- 2

Indicates a Sampling Point Ferric

Chloride

Filter

2 Holding

Tank

Clarifier 1

Sludge Storage

Tank Filter Press Sump Filter

Backwash Filter

1

Solids to Fly

Ash Landfill Wastewater Flow

Sludge Flow Intermittent Wastewater Flow Clarifier Sludge

Mix

Chamber

Clarifier 2 Filter

3 Cooling Water

Nutrient

First

- Stage

Bioreactors ( 8 ) First

- Stage

Effluent Storage Second

- Stage

Bioreactors ( 8 )

Second

- Stage

Effluent Storage To Ash Basin

Bio Reactor Backflush Hydrochloric

Acid

SP

- 3

Figure 2

- 2. Physical/Chemical Separa tion and Biological Reactor Portion of FGD Wastewater Treatment System, Belews

Creek Steam Station3

- 1 3. S AMPLING P ROCEDURES

This section discusses the planned sampling procedures to be followed during the sampling episode at Belews Creek. This section also pro vides the necessary information to plan for the logistics of this sampling episode. All tables and figures in this section are presented at

the end of the section.

3.1

EPA selected the following eight sampling points for the Belews C reek sampling episode (the three proposed sampling points for Belews Creek’s FGD wastewater treatment system as

well as the related Quality Assurance/Quality Control (QA/QC) samples) : Sampling Point Selection

**•** SP

- 1 Influent to FGD Wastewater Treatment System;

**•** SP

- 2 Influent to Bio reactor System ;

**•** SP

- 3 Effluent from Bioreactor System;

**•** SP

- 4 Duplicate of Influent to Bioreactor System (SP

- 2);

**•** SP

- 5 Duplicate of Effluent from Bioreactor System (SP

- 3);

**•** SP

- 6 Influent to FGD Wastewater Treatment System (SP

- 1) Field Blank ;

**•** SP

- 7 Influent to Bioreactor System (SP

- 2) Field Blank; and

**•** SP

- 8 Effluent from Bioreactor System (SP

- 3) Field Blank.

3.2

Analytes that will be included in EPA’s Belews Creek sampling episode include those in the following classes of pollutants: Analyte Selection

**•** Classica ls :

— Biochemical oxygen demand, 5

- day (BOD 5 ),

— 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

,

— Tot al c yanide ;3

- 2 **•** Total m etals:

— 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 zin c.

**•** Dissolved m etals:

— Same parameters as listed for total metals, plus hexavalent chromium

.

The analytes selected for analysis reflect the current understanding of coal

- fired power plant FGD wastewaters, including contributions from coal, scrubber sorben ts, treatment chemicals, and other sources. Table 3

- 1 lists the potential analytes for each sampling point, Table

3

- 2 lists the analytical methods that will be used, and Table 3

- 3 lists the sample container and volume and planned on

- site preservation for e ach parameter or parameter group.

3.3

To characterize the influent to FGD wastewater treatment system (SP

- 1), the influent to bioreactor system (SP

- 2), and the effluent from bioreactor system (SP

- 3) at Belews Creek, the sampling team will use varying methods to collect the samples depending on the sampling point and pollutant parameters. This section describes in detail the sample collection techniques. Sample Collection Procedures

Samples are collected as a series of “fractions,” or bottles designated fo r particular analyses requiring the same preservation. The comprehensive sample set consists of sample fractions for all pollutant classes listed in Section 3.2. Note that some sample fractions will be collected in the same sample bottle , such as Group I a nalytes (TSS, TDS, sulfate, and chloride) and Group II analytes (ammonia as nitrogen, COD, nitrate/nitrite as nitrogen, TKN, and total phosphorus).

In general, samplers will work in teams of 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, hard hats, and safety eyewear, and will observe precautions while collecting

s amples, remaining aware of their surroundings. Note that the use of masks is to prevent contamination of the mercury samples and not for respiratory protection.

Sample containers an d 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. For this sampling episode, ERG will collect 24

- hour composite samples at

the influent to and the effluent from the bioreactor sampling points for most analytes; however, mercury will be collected as four grab samples and cyanide will be collected as a single grab sample . ERG will collect individual grab samples at the influent to the FGD wastewater treatment system sampling point for all analytes

. ERG will collect one sample at each sampling point each day over four consecutive 24

- hour periods ( mercury will be collected as four grab samples each day for the influent to and the effluent from the bioreactor sampling points )

. 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 procedures3

- 3 described in EPA Method 1669. Samplers will use “clean hands / dirty hands” sample collecti on techniques when collecting metal sample fractions, as described in EPA Method 1669.

Sampl ers 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 and then placed into coolers containing bagged ice throughout sample storage, shipment, and receipt at the analytical laboratories.

3.3.1 Influent to FGD Wastewater Treatment System (SP

- 1)

The influent to FGD wastewater treatment system (SP

- 1) has a sample tap located on the wastewater piping downstream of the purge tank and u pstream of the equalization tank. ERG will collect the sample prior to the wastewater entering the equalization tank because the FGD scrubber purge is commingled with other waste streams in the equalization tank and, therefore, the sampling point upstream of the tank provides the best representation of the FGD scrubber purge from the Belews Creek FGD system. Because the flow from the purge tank to the equalization tank is not continuous, ERG will need to coordinate closely with Belews Creek personnel during the sampling episode to determine when grab samples can be collected (i.e.,

when wastewater is being transferred to the FGD wastewater treatment system ) . ERG will follow protocols described in EPA Method 1669 to collect metal sample fractions from SP

- 1.

ERG plans to collect split samples with Belews Creek (or its representative), where possible; therefore, ERG plans to attach a piece of silicone tubing to the sample tap with a “Y” splitter at the other end of the tubing to allow ERG and Belews Creek (or its representative) to collect samples simultaneously. I f problems occur during the collection of split samples (e.g., the splitters become clogged and the flow is split unevenly between the sampling crews), then EPA may stop the split sample collection an d offer instead to collect duplicate samples with Belews Creek or its representative. For all analyses (except dissolved metals and hexavalent chromium), the samplers will collect samples through the tubing directly into the specified containers. For

the d issolved metals (excluding mercury) and hexavalent chromium samples, the samplers will

fill one 10

- L container, allow the solids to settle for one hour, and then pump the aqueous portion of the sample through a 0.45

- μm filter and then through a “Y” splitter into the specified
containers; therefore, the dissolved metals and hexavalent chromium samples will be collected as split samples.

Due to the high suspended solids content ( typically 0.8 percent at Belews Creek, but has

been observed on the order of 1

- 5 percent at other plants ) of the samples collected at the influent to the FGD wastewater treatment system, EPA may analyze the samples as bi

- phasic samples. If

the TSS content of the sample is greater than one perc ent, the n the laboratory will separate the

aqueous and solid portion s 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 p hosphorus 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), BOD 5 , hexavalen t chromium, and dissolved metals (including mercury ) samples will not be analyzed as bi

- phasic samples. Scrubber purge samples with less than one percent TSS will not require bi

- phasic separation and analysis.3

- 4 The samples for the influent to the FGD was tewater treatment system (SP

- 1) will be

collected from a sample tap. 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 me tals samples);

**•** Masks (for mercury samples); and

**•** Sample containers.

All metals sampling equipment will be specially

- cleaned according to the procedures

described in EP A 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 samples 1

.

1. Samplers remove the bags containing the gloves and high

- density polyethylene ( HDPE ) plastic wrap from the c oolers or storage containers in which they are packed

. Samplers identify which coolers or boxes contain the double

- bagged sample bottles, precleaned tubing, blank water, and cleanbox

. Depending on the condition of the sample tap, sampl ers may need 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 H DPE plastic wrap and places the double

bagged 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 colle ction

, opens the cleanbox

, and secures it open with the clips located inside the box.

1 For the sample collection, the samples will be split with the plant (or the plant’s repres entative) 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 in thi s plan.3

- 5 4. “Dirty hands” opens the outer bag containing a length of precleaned silicone tubing

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

, removes the tubing , and pl aces 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 and attaches the funnel to the tubing.

6. “Dirty hands” opens the outer bags of the me rcury field blank water and tota l

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 shroudi ng 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

cl eanbox 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 a nd 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 samples 2

.

7. “Dirty hands” opens the outer bag for a precleaned 10

- L container. “Clean hands” opens the inne r 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 enoug h 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 li d 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

.

2 ERG will collect field blank samples at the influent to the FGD wastewater treatment system on Day 1 of the sampling episode. Additionally, ERG will collect the dissolved mercury sample using the same technique as the total mercury sample, but th e dissolved sample will be filtered at the laboratory. A dissolved mercury field blank sample will be analyzed by the laboratory to assess any mercury contamination from the filtering performed at the laboratory. Therefore, ERG does not need to collect a d issolved mercury field blank sample in the field.3

- 6 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 p iping 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 precleaned 10

- L container

. “Clean hands”

op e ns the inner bag and loosens the lid

. “Clean hands” holds the e nd 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 with sample to be analyzed for dissolved metals

and hex avalent chromium, which is required to be filtered for these analyses

. 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 th e 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 han ds” 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 oute r bag

. The samplers repeat this procedure

for the d issolved mercury and total metals samples.

12. “Dirty hands” p l aces 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

t o another sampling team member to measure the temperature and pH

.

14. Both samplers collect the BOD 5 , Group I, Group II , and total cyanide samples from the sample location. T he samplers need to test the total cyanide samples for

sulfides and oxidants and pre serve the sample s immediately after sample collection, according to the preservation protocol s outlined in Section 3.4.

Dissolved Metals Sample Collection

15. Samplers allow the 10

- L sample container to continue to settle if one hour has not elapsed since th e sample was collect ed

.

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.3

- 7 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

, 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 precleaned Teflon® tubing attached to a 5

- foot length of precleaned silicone tubing, a “Y” splitter, and two additional pieces of precleaned silicone tubing

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

, removes the tubing , and places a clean plastic bag over the end s 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 plas tic 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 pla ces 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 and then 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 2 1 to replace the filter 3

.

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 tu bing outside the cleanbox, with the plastic bag still covering the end of the tubing

. “Dirty hands”

3 ERG will collect field blank samples only at the influent to the FGD wastewater treatment system during one day of the sampling episode.3

- 8 starts the pump and passes approximately 7 50 mL through the tubing and filter

and then stops the pump.

25. “Dirty hands” opens the outer bag of the dissolved m etals 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 and then 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 di ssolved metals and hexavalent

chromium samples

.

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

EPA plans to collect samples at the influent to the wastewater treatment system (SP

- 1) on four consecutive days . T he sample collection setup and sampling technique for each day of sampling will be the same

.

3.3.2 Influent to Bioreactor System (SP

- 2)

The influent to the bioreactor system (SP

- 2) will be collected downstream of the sand filters after the wastewater from the three filters is commingled. Belews Creek has a sampl e tap located on the wastewater piping after the three sand filter effluent streams are commingled, downstream of the holding tank and upstream of the heat exchanger

. Belews Creek has agreed to

install a three

- way splitter on the sample tap that will have three separate taps to collect samples from the sampling point. ERG will follow protocols described in EPA Method 1669 to collect metal sample fractions at SP

- 2.

ERG will collect the influent from the bioreactor system composite samples using two

automa tic compositors which will be programmed to collect individual sample volumes into two large containers ( e.g. , two 20

- liter 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 pump o ff the specific sample volumes into the individual sample containers.

ERG will use one automatic compositor to collect sample volume for the metals analyses (excluding mercury) and another automatic compositor to collect sample volume for all classical analytes (i.e., BOD 5 , Group I, and Group II). In addition to collecting automatic composite samples for the analytes listed above, ERG will collect total and dissolved mercury grab samples every six hours during each compositing period. ERG will also colle ct one grab sample for cyanide during each compositing period.

ERG plans to collect split samples with Belews Creek (or its representative), where possible; therefore, when pump ing off the composite samples, a “Y” splitter will be used with two pieces o f silicone tubing attached to the “Y” splitter to allow ERG and Belews Creek (or its3

- 9 representative) to collect samples simultaneously. I f problems occur during the collection of split samples (e.g., the splitters become clogged and the flow is split uneve nly between the sampling crews), then EPA may stop the split sample collection and offer instead to collect duplicate samples with Belews Creek or its representative.

ERG will collect the total and dissolved mercury grab samples by shrouding one of the

t hree taps on the three

- way splitter (the other two taps are used for the two compositors) and collecting the samples directly from the tap. Because the samples are collected directly from the

tap, ERG will not be able to collect split samples with Belews C reek (or its representative); therefore, duplicate samples will be collected.

For all analytes, ERG will collect QC samples at the influent to the bioreactor system (SP

- 2 ) on Day 4 of the sampling episode . In addition, for all analytes, ERG will collect a duplicate sample of the influent from bioreactor system (SP

- 4) on Day 3 of the sampling episode

.

The samples for the influent to the bioreactor system (SP

- 2) will be collected from a sample tap. The sampling equipment will consist of the following:

**•** C olorless, electronic

- grade, non

- nitrile gloves;

**•** Peristaltic pump (automatic compositor

– battery powered);

**•** Large composite containers (e.g., 20

- liter containers);

**•** Funnel;

**•** “Y” splitter;

**•** “T” splitter;

**•** Teflon® tubing;

**•** Silicone tubing;

**•** 0.45

- um filter;

**•** Cleanbox ;

**•** Tyvek® suits (for metals samples);

**•** Masks (for mercury samples); and

**•** Sample containers.

All metals sampl ing equipment will be specially cleaned according to the procedures

described in EPA Method 1669. The supplier of the cleaned bottles, tubing, and c omposite containers will prepare and analyze bottle blanks and equipment blanks to evaluate possible

contamination. 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 samples 4

.

1. Sampl ers remove the bags containing the gloves and HDPE plastic wrap from the coolers or storage containers in which they are packed. Samplers identify which

4 For the sample collection, the samples will be split with the pla nt (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 sample s is not described in this plan.3

- 10 coolers or boxes contain the double

- bagged composite containers, precleaned tubing , blank water, and cl eanbox

. Depending on the condition of the sample tap, samplers may need to wipe the tap with a clean paper towel to remove any buildup 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 double

bagged composite containers within easy access on the covered surface.

3. “Dirty hands” opens the outer bag of the cleanbox and “clean hand s” opens the clear inner bag. “Clean hands” places the cleanbox at the point of sample

collection

, 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 composit or so the tubing can be added. “Dirty hands” opens the outer bag containing a length of pre cleaned silicone tubing, a “T” splitter, and two additional pieces of silicone tubing. “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 each end of the silicone tubing. The tubing configuration will be set up such that one end will be connected to the sample tap,

one end will b e threaded through the automatic compositor and connected to the large composite container, and one end will be placed next to a sump/drain near the sampling point. To collect the samples, the sample tap will be left open during the entire sample collectio n time period and will flow directly to the sump/drain; however, the automatic compositor will pull sample from the flow ing stream as dictated by the sampling program. Additionally, the automatic compositor will be capable of purging the line back to the f lowing stream between each individual sample aliquot.

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

6. Both samplers change gloves.

7. “D irty hands” opens the outer bag of the metal s 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

one end of the silicone 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 “ d irty hands” operates the pump to pump bl ank

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 sufficient volume to

collect the total and dissolved metals field blank samples at the pump

- off location

.3

- 11 “Dirty hands” stops the pump. During the purging of the tubing and collection of the field blank sample volume, “dirty hands” holds the end of the silicone tubing placed by the sump/drain above the composite container to prevent this portion of the tubing configuration from filling with blank water during the pumping

process. “Clean hands” places the plastic bag over the end of the silicone tubing, replaces the lid on the field blank compos ite container, places the silicon e tubing back in the cleanbox, and closes the inner bag of the field blank composite

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

container 5

.

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 en d of the silicone tubing outside the cleanbox over a bucket, with the plastic bag still covering the end of the tubing. “Dirty hands” places the end of the silicone tubing near the sump/drain and opens the sample tap

valve to allow the wastewater to flow t hrough the tubing. “Dirty hands” operates the pump to purge the pump portion of 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 temper ature 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 8 33 mL of sample every hour). “Dirty hands” calibrates the compositor to ensure that approxima tely 8 33 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. The samplers put ice around the composite container to keep the samples cold during the compositing time period.

14. Samplers repeat ste ps 1

- 1 3 to set up the automatic compositor for the classical analy t es (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 the compositing time per iod.

5 ERG will collect field blank samples for all metals at the influent to the bioreactor system during Day 1 of the sampling episode. Additionally, ERG will collect a total mercury field blank sample during one of the grab s amples for each day of sample collection at the influent to the bioreactor system.3

- 12 15. “Dirty hands” and “c lean hands” then work to collect the total mercury field blank sample. “Dirty hands” shrouds the sample tap with a clear plastic bag that covers the end of the sample tap and provides enough room for samplers to work in with

thei r hands. “Dirty hands” then opens the outer bag of the mercury field blank water and the total mercury field blank sample bottle. “Clean hands” opens the inner bag for the field blank water and the total mercury field blank sample bottle,

unscrews the lids and places each in their inner bags. “Clean hands” pours the field blank water into the field blank sample bottle, closes the lids, and closes the inner bags. “Clean hands” places the total mercury field blank sample bottle in the outer bag and “Dirty han ds” closes the outer bag.

16. “ Dirty hands” positions a bucket under the sample tap, opens the valve and purges the valve for at least one minute and then closes the tap. Dirty hands” then opens the outer bag of the total mercury sample bottle. “Clean hands” takes the bottles and positions himself/herself at the tap with the bottle under the shrouding and opens the inner bag. “Dirty hands” opens the sample tap and adjusts the flow. “Clean hands” open the lid of the total mercury sample bottle and places the bo ttle under the flowing stream to fill the bottle. “Clean hands” then closes the lid on the bottle and closes the inner bag. “Dirty hands” closes the sample tap. “Clean hands” places the bottle in the outer bag and “dirty hands” closes the outer bag.

The sa mplers repeat this procedure for the collection of the dissolved mercury sample

T he samplers will fill the bottle directly from the sample tap; therefore, the total and dissolved mercury samples will not be collected as split samples with Belews Creek (or its representative), but will be collected as duplicate samples.

17. The samplers will collect total and dissolved mercury grab samples every six hours during the compositing time period.

18. Samplers collect a total cyanide grab sample from the same sample tap used for the mercury sample collection . The samplers will fill the bottle directly from the

tap ; therefore, the cyanide sample will not be collected as a split sample with Belews Creek (or its representative). Immediately after collection, the samplers

ne ed to test for sulfides and oxidants and preserve the sample according to the preservation protocols outlined in Section 3.4.

19. The samplers will collect field measurement samples every six hours during the compositing time period

. The field measurement sam ples will be collected from

the sample tap used for the mercury collection

.

20. At the end of the composite sampling period, “dirty hands” stops each of the automatic compositors and opens the outer bag of each composite container. For each container, “clean hands” opens the inner bag and detaches the used tubing from the composite container and covers the port with a closed lid or small plastic bag. The s amplers transport each of the composite container s, including the field3

- 13 blank composite container, to the pump

- off area to pump off the sample s into the specified containers.

21. The samplers then repeat steps 1 through 20 to collect the composite samples for the next day of sample collection.

After the composite samples have been collected, the sampling team will then transfer the sample into the individual sample containers at the pump

- off area

. For this sampling point, ERG

will use a sample pump

- off approach to transfer the composite samples to the individual sample

bottles , because the samples are expected to have a low solids content. 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 t he dissolved metals fractions.

Sample Pump

- Off Procedures

22. S amplers 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

- b agged sample bottles

, pre cleaned tubing , and

cleanbox

.

23. 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 cove red surface.

24. “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

, opens the cleanbox

, and secures it open with the clips located inside

the box.

25. “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 con taining a length of

pre cleaned Teflon® tubing connected to a length of pre cleaned silicone tubing , a “Y” spli tter, 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.

26. “Dirty hands” th reads the silicone tubing into the peristaltic pump head.

27. Both samplers change gloves.

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

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

blank sample bottle and places it in the cleanbox. “C lean hands” opens the inner bag of the field blank composite container

, removes the lid from the container

,3

- 14 and places the end of the Teflon® tubing in the blank water. “Clean hands” holds

the end of the sili cone tubing outside the cleanbox over a bucket, with the plastic bag still covering the end of the tubing and “ d irty hands” operates the pump to pump about 75 0 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 and then 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.

29. “Dirty hands” opens the outer bag of a capsule filter. “Clean hands” opens the inner bag and removes the c apsule filter. “Clean hands” attaches the capsule filter to the silicone tubing just before the “Y” splitter

.

30. “Dirty hands” opens the outer bag of the dissolved me t als field blank sample

bottle. “Clean hands” removes the dissolved metals field blank sampl e 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 “ d irty hands” operates the pump to pump about 75 0 mL of blank

water from the field blank 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 to colle ct the dissolved metals field blank sample and then 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 sampl ers repeat this procedure for the dissolved metals and hexavalent chromium field blank samples 6

. “Clean hands” closes the inner bag of the field blank composite container and “dirty hands” closes the outer bag. Note:

75 0 mL of blank water does not need to be purge d for each sample, just at the beginning of each new filter. If a new filter is needed, “clean hands” removes the

used filt er and samplers follow step 2 9 to replace the filter

.

31. “Dirty hands” opens the outer bag of the large composite container fo r 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 cleanbo x over a bucket, with the plastic bag still covering the end of the tubing and “ d irty hands” operates the pump to pump about one liter of sample through the tubing and filter and then stops the pump.

6 ERG will collect field blank samples for all metals samples at the influent to the bioreactor system during Day 1 of the sampling episode. ERG will collect the dissolved m ercury 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 analyzed by the laboratory to assess any mercury contamination from the filtering perfo rmed at the laboratory. Therefore, ERG does not need to collect a dissolved mercury field blank sample in the field.3

- 15 32. “Dirty hands” opens the outer bag of the dissolved meta ls 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 and then stops the pump. “Clean ha nds” 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 sa mples. During Day 3 of the sampling episode, the samplers will collect additional sample volume for the duplicate samples and Day 4 of the sampling episode, the samplers will collect additional sample volume for the laboratory QC analyses.

33. “Clean hands” removes the capsule filter from the sample tubing configuration and reconnects the two pieces of tubing together.

34. “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 and then s tops the pump. “Clean hands” places the end of the silicone tubing back in the cleanbox.

35. “ Dirty hands” opens the outer bag of the total metals sample bottle. “Clean hands”

removes the inner ba g 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 metals sample and then 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. During Day

3 of the sampling episode, the samplers will collect additional sample volume for the duplicate samples and during Day 4 of the sam pling episode, the samplers will collect additional sample volume for the laboratory QC analyses

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

37. “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.

38. “Clean hands” hold s 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 and then stops the pump.

39. Both samplers collect the BOD 5 , Group I, and Group II samples

. During Day 3 of the sampling episode, the samplers will collect additional sample volume for the duplicate samples and during Day 4 of the sampling episode, the samplers will collect additional sample volume for the laboratory QC analyses.3

- 16 EPA pl ans to collect samples at the influent to the bioreactor system (SP

- 2) on four

consecutive days. The sample collection setup and sampling technique for each day of sampling

will be the same

.

3.3.3 Effluent from Bioreactor System (SP

- 3)

The effluent from biore actor system (SP

- 3) will be collected downstream of the second

stage effluent storage tank from the second

- stage bioreactor cells. Belews Creek has a sample tap located on the wastewater piping downstream of the second

- stage effluent storage tank. Belews

C reek has agreed to install a three

- way splitter on the sample tap that will have three separate taps to collect samples from the sampling point. ERG will follow protocols described in EPA Method 1669 to collect metal sample fractions from SP

- 3.

ERG will collect the effluent from the bioreactor system composite samples using two automatic compositors that will be programmed to collect individual sample volumes into two large containers (e. g. , two 20

- liter 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 du ring the 24

- hour composite period

. Following the composite period, ERG will 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 (excluding mer cury) and another automatic compositor to collect sample volume for all classical analytes (i.e., BOD 5 , Group I, and Group II). In addition to collecting automatic composite samples for the analytes listed above, ERG will collect total and dissolved mercur y samples every six hours during each compositing period. ERG will also collect one grab sample for cyanide during each compositing period.

ERG plans to collect split samples with Belews Creek (or its representative), where possible; therefore, when pum p ing off of the composite samples, a “Y” splitter will be used with two pieces of silicone tubing attached to the “Y” splitter to allow ERG and Belews Creek (or its representative) to collect samples simultaneously. I f problems occur during the collection of split samples (e.g., the splitters become clogged and the flow is split unevenly between the sampling crews), then EPA may stop the split sample collection and offer instead to collect duplicate samples with Belews Creek or its representative.

ERG wi ll collect the total and dissolved mercury grab samples by shrouding one of the three taps on the three

- way splitter (the other two taps are used for the two compositors) and collecting the samples directly from the tap. Because the samples are collected d irectly from the

tap, ERG will not be able to collect split samples with Belews Creek (or its representative); therefore, duplicate samples will be collected.

For all analytes, ERG will collect QC samples at the effluent from the bioreactor system (SP

- 3) on Day 3 of the sampling episode . In addition, for all analytes, ERG will collect a duplicate sample of the effluent from bioreactor system (SP

- 5 ) on Day 2 of the sampling episode

.3

- 17 The sample of the effluent from the bioreactor system (SP

- 3) will be col lected from a sample tap. 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;

**•** “Y” splitter;

**•** “T” splitter;

**•** Teflon® tubing;

**•** Silicone tubing;

**•** 0.45

- um filter;

**•** Cleanbox;

**•** Tyvek® suits (for metals samples);

**•** Masks (for mercury samples); and

**•** Sample containers.

All metals sampl ing equipment will be specially cleaned according to the procedure s described in EPA Method 1669. The supplier of the cleaned bottles, tubing, and composite containers will prepare and analyze bottle blanks and equipment blanks to evaluate possible

contamination. 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 de scribes the set up of the sample point and collection of the EPA samples 7

.

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 cont ain 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 double

bagged compo site 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 silicone tubing , a “T” splitter, and two additional pieces of silicone

7 For the sample collection, the samples will be split with the plant (or the plant’s representative) and therefore, the sample set

- up desc ribes 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.3

- 18 tubing

. “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 each end of the silicone tubing. The tubing configuration will be set up such that one end will be connected to the sample tap, one end will be threaded through the automatic compositor and connected to the large composite container, and one end will be placed next to a sump/drain near the sampling point. To collect the samples, the sample tap will be left open during the entire sample collection time period and will flow directly to the sump/drain; however, the automatic compositor will pull sample from the fl ow ing stream as dictated by the sampling program. Additionally, the automatic compositor will be capable of purging the line back to the flowing stream between each individual sample aliquot.

5. “Dirty hands” threads one portion of the silicone tubing throug h the peristaltic pump portion of the automatic compositor.

6. Both samplers change gloves.

7. “D irty hands” opens the outer bag of the metals field blank water and the field

blank composite container

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

wate r, unscrews the lid and places it in the inner bag. “Clean hands” then places

the one end of the silicone 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 t he silicone tubing with the plastic bag covering the end out of the

cleanbox and over a bucket and “ d irty hands” operates the pump to pump blank

water through the tubing

. After the tubing has been purged with sufficient volume, “clean hands” holds the sili cone tubing at the mouth of the field blank composite container and fills the composite container with sufficient volume to the collect the total and dissolved metals field blank samples at the pump

- off

location. “Dirty hands” stops the pump. During the pu rging of the tubing and collection of the field blank sample volume, “dirty hands” holds the end of the silicone tubing that will be placed by the sump/drain above the composite container to prevent this portion of the tubing configuration from filling wit h blank water during the pumping process. “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

of the fi eld blank composite container. “ Dirty hands” closes the outer bag of the field blank composite container 8

.

8. Both samplers work together to move the sampling tubing, automatic compositor, and composite containers into position for the sample collection. Sa mplers will ensure that the tubing will stay in place during the 24

- hour sample collection period.

8 ERG will collect field blank samples for all metals samples at the effluent from the bioreactor system during Day 1 of the sampling episode. Additionally, ERG will collect a total mercury field blank sample during one of the grab samples for each day of sample collection at the effluent from the bioreactor system.3

- 19 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 t he end of the tubing. “Dirty hands” places the end of the silicone tubing near the sump/drain and opens the sample tap valve to allow the wastewater to flow through the tubing. “Dirty hands” operates the pump to purge the pump portion of the tubing for a m inimum 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 8 33 mL of sample every hour)

. “Dirty hands” calibrates the compositor to ensure that approximately 8 33 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 hand s” closes the outer bag. The samplers put ice around the composite container to keep the samples cold during the compositing time period.

14. Samplers repeat steps 1

- 1 3 to set up the automatic compositor for the classical analy t es (skipping step s 7 and 8 ). Sa mplers will use another composite container.

15. “Dirty hands” and “Clean hands” then work to collect the total mercury field blank sample. “Dirty hands” shrouds the sample tap with a clear plastic bag that covers the end of the sample tap and provides enough room for samplers to work in with their hands. “Dirty hands” then opens the outer bag of the mercury field blank water and the total mercury field blank sample bottle. “Clean hands” opens the inner bag for the field blank water and the total mercury field blank sample bottle, unscrews the lids and places each in their inner bags. “Clean hands” pours the field blank water into the field blank sample bottle, closes the lids, and closes the inner bags. “Clean hands” places the total mercury sample bottle in t he outer bag and “Dirty hands” closes the outer bag

16. “ Dirty hands” positions a bucket under the sample tap, opens the valve and purges the valve for at least one minute and then closes the tap. Dirty hands” then opens the outer bag of the total mercury sam ple bottle. “Clean hands” takes the bottles and positions himself/herself at the tap with the bottle under the shrouding and opens the inner bag. “Dirty hands” opens the sample tap and adjusts the flow. “Clean hands” open the lid of the total mercury sampl e bottle and places the bottle under the flowing stream to fill the bottle. “Clean hands” then closes the lid on the bottle and closes the inner bag. “Dirty hands” closes the sample tap. “Clean hands” places the bottle in the outer bag and “dirty hands” cl oses the outer bag.3

- 20 The samplers repeat this procedure for the collection of the dissolved mercury sample.

The samplers will fill the bottle directly from the sample tap; therefore, the total and dissolved mercury samples will not be collected as split s amples with Belews Creek (or its representative), but will be collected as duplicate samples.

17. The samplers will collect total and dissolved mercury grab samples every six hours during the compositing time period.

18. Samplers collect a total cyanide grab sa mple from the same sample tap used for the mercury sample collection. The samplers will fill the bottle directly from the

tap ; therefore, the cyanide sample will not be collected as a split sample with Belews Creek (or its representative). Immediately afte r collection, the samplers need to test for sulfides and oxidants and preserve the sample according to the preservation protocols outlined in Section 3.4.

19. The samplers will collect field measurements samples every six hours during the compositing time per iod. The field measurement samples will be collected from

the sample tap used for the mercury collection

.

20. At the end of the composite sampling period, “dirty hands” stops each of the automatic compositors and opens the outer bag of each composite contain er. For each container, “clean hands” opens the inner bag and detaches the used tubing from the composite container and covers the port with a closed lid or small plastic bag. The s amplers transport each of the composite containers, including the field

bla nk composite container, to the pump

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

21. The samplers then repeat steps 1 through 20 to collect the composite samples for the next day of sample collection.

After the composite samples have bee n collected, the sampling team will then transfer the sample into the individual sample containers at the pump

- off area

. For this sampling point, ERG

will use a sample pump

- off approach to transfer the composite samples to the individual sample

bottles , be cause the samples are expected to have a low solids content. 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 Procedures

22. S amplers remove the bags containing the gloves and HDPE plastic wrap from the coolers or storage containers in which they are packed. Samplers identify which

cooler s or boxes contain the double

- bagged sample bottles

, precleaned tubing , and

cleanbox

.3

- 21 23. 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.

24. “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

, opens the cleanbox

, and secures it open with th e clips located inside

the box.

25. “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 con taining a length of

pre cleaned Teflon® tubing connected to a length of pre clea ned 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 sil icone tubing.

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

27. Both samplers change gloves.

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

me t als field blank sample bottle. “Clean hands” remov es the total metals field blank sample bottle and places it in the cleanbox. “C lean hands” opens the inner bag of the field blank composite container

, removes the lid from the container

, and places the end of the Teflon® tubing in the blank water. “Clean h ands” 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 “ d irty hands” operates the pump to pump about 75 0 mL of blank water from the field blank composite container

. “Clea n 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 and then 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.

29. “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

.

30. “Dirty hands” opens the outer bag of the dissolved me t als field blank sample

bottle. “Clean hands” removes the dis solved 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 “ d irty hands” operates the pump to p ump about 75 0 mL of blank

water from the field blank field blank composite container

. “Clean hands” places the end of the silicone tubing in the cleanbox, opens the inner bag of the dissolved3

- 22 metals field blank sample bottle, and removes the lid. “Dirty ha nds” operates the pump to collect the dissolved metals field blank sample and then 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 9

. “Clean hands” closes the inner bag of the field blank composite container and “dirty hands” closes the outer bag. Note:

75 0 mL o f blank water does not need to be purge d for each sample, just at the beginning of each new filter. If a new filter is needed, “clean hands” removes the

used filt er and samplers follow step 2 9 to replace the filter

.

31. “Dirty hands” opens the outer bag of th e 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 silic one tubing outside the cleanbox over a bucket, with the plastic bag still covering the end of the tubing and “ d irty hands” operates the pump to pump about one liter of sample through the tubing and filter and then stops the pump.

32. “Dirty hands” opens the o uter 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 and then 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 met als and hexavalent chromium samples. During Day 2 of the sampling episode, the samplers will collect additional sample volume for the duplicate samples and during Day 3 of the sampling episode, the samplers will collect additional sample volume for the

lab oratory QC analyses.

33. “Clean hands” removes the capsule filter from the sample tubing configuration and reconnects the two pieces of tubing together.

34. “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 and then stops the pump. “Clean hands” places the end of the silicone tubing back in the cleanbox.

35. “ Dirty hands” opens the outer bag of the total 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

9 ERG will collect field blank samples for all metals samples at the effluent from the bioreactor system during Day 1 of the sampling episode. ERG will collect the dissolved mercury sample using the same technique as the total mercury sample, but t he 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 dissol ved mercury field blank sample in the field.3

- 23 collect the total metals sample and then 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. During Day

2 of the sampling episode, the samplers will collect additional sample volume for the duplicate samples and during Day 3 of the sampling episode, the samplers will collect additional sample volume for the laboratory QC analyses.

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

37. “Dirty hands” shakes the large composite cont ainers 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 c lassical analytes.

38. “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.

39. Both sampl es collect the BOD 5 , Group I, and Group II samples. During Day 2 of the sampling episode, the samplers will collect additional sample volume for the duplicate samples and during Day 3 of the sampling episode, the samplers will collect additional sample vol ume for the laboratory QC analyses.

EPA plans to collect samples at the effluent from the bioreactor system (SP

- 3) on four

consecutive days. The sample collection setup and sampling technique for each day of sampling

will be the same

.

3.4

All samples will be maintained on ice immediately upon collection (except metals samples that do not require cooling). Because the classical and hexavalent chromium samples are required to be cooled, all c omposite containers will be maintained on ice. After pumping off the composite samples into the individual sample containers, the classical and hexavalent chromium samples will be put in an ice

- water bath; however, the other metals samples, which do not

re quire cooling, will Sample Preservation, Shipping, and Analysis

not be placed on ice. The classical and hexavalent chromium grab samples collected at the FGD influent sampling point will also be placed on ice immediately after

collection.

The dissolved metals ( excluding mercury) and hexavalent ch romium samples will be

filtered in the field. The dissolved mercury samples will be filtered upon receipt at the laboratory. All metals samples, except he xavalent chromium, will be acid

- preserved prior to extraction at the laboratory. H exavalent chromium s amples will be preserved on site, according

to the method

- specified protocols. Samplers will filter samples within 15 minutes after the compositing period ends (or as soon thereafter as possible). The dissolved samples of the FGD

influent will be filtered approximately one hour after they are collected t o allow for solids settling because the samples’ high solids content that would clog the filter.3

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

- specific protocols immediately foll owing collection

. Prior to sample collection, the samplers will test the

wastewater at each sampling point for sulfide using lead acetate test strips. If sulfide is present, the samplers will use the procedure identified in Section 3.5 to determine the min imal amount of dilution necessary to reduce sulfide to a nondetectable concentration. After determining this

minimal dilution factor for the sampling point, the samplers will dilute all samples collected at this sampling point using blank water . After dilu tion, the samplers will retest the sample for

sulfides. If sulfides are still detected, the sample will be diluted further using the same technique

as identified in Section 3.5 to ensure that the sample is not over

- diluted. The samplers will then

test the diluted sample for the presence of oxidants (i.e., chlorine) using potassium

- iodide starch

paper. If total chlorine is present, the samplers will add sodium arsenite in small increments until the oxidants are at nondetectable concentrations in the sample

. The samplers will then carefully adjust the pH to >10 S.U. using sodium hydroxide and place the sample on ice. The preservation, including the amount of dilution, will be reported to the lab oratory on the traffic reports.

Table 3

- 3 lists the parameters, bottle types, sample volume, 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 3

- 1). With the exception of total cyanide samples, if 10 perce nt of the sample volume is added and the required pH is not achieved

, ERG

will stop diluting the sample s by discontinuing preservation and noting it on the traffic report. The wastewater samples, except metals samples that do not require cooling , will be p acked 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

.

3.5

Te mperature

, pH , sulfide , and oxidants will be measured and recorded by the sampling crew at each sampling point (SP

- 1, SP

- 2, and SP

- 3)

. The samplers will measure temperature and pH when the automatic composite samplers are initially set up and every six hou rs during the compositing period. The samplers will test the wastewater for sulfide and oxidants at the time the total cyanide grab sample is collected. For temperature and pH, the samplers will fill a 1

- liter glass jar with sample and test the wastewater immediately after collecting the aliquot. For sulfide and oxidants, the samplers will fill the cyanide sample bottle directly and test for sulfide and oxidants using test strips immediately after sample collection. Field Measurements and Engineering Data Collection

During a pre

- sampling set

- up day (i.e. , the day before the sampling episode begins), t he samplers will test the wastewater at each sampling point for sulfide using lead acetate test strips to determine if preservation is needed for cyanide

. The presence of sulfide will be determined using lead acetate test strips. If sulfide is present, the samplers should determine the minimal amount of dilution necessary to reduce the sulfide concentration to below detection by the lead acetate test strips. T o identify the minimal amount of dilution, the samp lers will dilute the sample by a factor of two (1:1) and retest for sulfides. If sulfide is still detected, the samplers will dilute the original sample by a factor of 3 (2:1). This process will be continued until sulfide is not detected in the sample. Aft er this minimal dilution factor is determined for the sampling point, the samplers will use this minimal dilution factor to dilu te all samples collected at the sampling point. The samplers will also test both the original (i.e., non

- diluted ) and diluted sa mple for the3

- 25 presence of oxidants (e.g., chlorine ) during the pre

- sampling set

- up day using potassium

- iodide starch paper.

Samplers will follow applicable test kit calibration procedures specified by the

manufacturer. Table 3

- 4 summarizes the field meas urements, the method to be used for the measurement, and the detection range of each field test instrument. In addition, EPA will collect flow rate data for each sampled waste stream. The flow rates for all the sampling points will be collected from the pl ant’s existing flow recorders.

Field sampling log sheets (Figure 3

- 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 observa tions.

Samplers will also collect e ngineering information with regard to design and operation of the plant. For example, they will collect 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 3

- 3, 3

- 4, and 3

- 5) will be completed for the plant. This information will be used to determine if the specific design or operational criteria of the steam electric operations affect the wastewater characteristics.

3.6

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, al t hough they may also be completed by hand. Each self

- adhesive label is completed in indelible ink and contains the following information: Sample Labeling

**•** Sample number;

**•** Sampling episode number;

**•** Sampling point/description;

**•** Date of sample collection;

**•** Analysis to be performe d;

**•** Sample bottle type; and

**•** Required preservation.

If any of the preprinted 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 wil l 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. For metal samples, the samplers will not label the sample bottles, but will label the outer plastic bag of the sample bottle.

3.7

To maintain a record of sample collection, transfer between personnel, shipment, and receipt by the laboratory, samplers will complete a traffic report for each sample set at each sampling location. These forms are used to document sample custody transfer from the field to Traffic Reports3

- 26 the laboratory. T raffic report forms will be completed for all samples sent to all laboratories. Figure 3

- 6 includes an example of a traffic report. At th e time of sample shipment, a copy of the traffic report will be sent to ERG , another copy will be kept by sampling personnel, and two copies will be transmitted with the samples to the analytical laboratory.

In addition to the transfer of custody, the tr affic 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, t ype of sample (grab, composite), sample collection date and time, and the analyses requested. Samplers will use the comment section to provide special notes or instructions to the laboratory, such as whether samples have been filtered on site or how to

com posite 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).

3.8

The QA/QC program for sample collection at Belews Creek will include the following: Quality Assurance/Quality Control

**•** Documentation for samples through laboratory traffic reports;

**•** Collection of duplicate samples for all analytes ;

**•** Collection of bottle blank(s) for metals;

**•** Collection of field blank(s) for metals;

**•** Collection of equipment blank(s) for metals; and

**•** Collection of laboratory QC samp les for matrix spike/matrix spike duplicate analyses.

Duplicate sample sets will be collected as part of the quality assurance program for sampling. During Day 3 of the sampling episode, ERG will collect one duplicate sample (SP

- 4)

of the influent to th e bioreactor system (SP

- 2) and during Day 2 of the sampling episode, ERG

will collect one duplicate sample (SP

- 5) of the effluent from the bioreactor system (SP

- 3). The duplicate samples will be collected as separate aliquots in the field. Results of the d uplicate analyses will be used to evaluate precision, including variability in sample collection, handling, preparation, and analysis.

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

The bottle blank will consist o f an analyte

- free matrix (Ultra Pure Blank Water DI+ TM ) poured into the appropriate sample bottles ( e.g., 250

- mL plastic bottle for metals ) and stored for several days prior to shipment to the laboratory . The supplier of the cleaned metals bottles will pre pare and analyze the bottle blanks prior to shipping the equipment to the sampling episode.3

- 27 Field blanks will be used to evaluate possible contamination caused by sampling equipment or by sampling equipment decontamination procedures. Field blanks will b e 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 (e.g., tubing or filters).

ERG will prepare field blanks for each of the total and dissolve d metals analyses at each of the three sampling points during Day 1 of the sampling episode 10

. Additionally, ERG will collect total mercury field blanks at the influent to the bioreactor and the effluent from the bioreactor sampling points during the collec tion of one of the grab samples each day of the sampling episode. ERG samplers will use “clean hands / dirty hands” sampling techniques to prepare the metals field bla nks, as discussed in more detail in Section 3.3. The total metals field

blanks (including mercury) at the influent to the FGD wastewater treatment system will be prepared by gravity

- feeding ASTM Type 1 water through the silicone tubing into the sample

bottles. The total metals field blanks (excluding mercury) at the influent to and effluent fr om the bioreactor system sampling points will be prepared by pumping ASTM Type 1 water through the composite tubing set into a large composite container where it will be held for the 24

- hour compositing period, then pumping the ASTM Type 1 water from the l arge composite container through the Teflon® and silicone tubing and into the sample bottles. The total mercury field blanks at the influent to and effluent from the bioreactor sampling points will be prepared by pouring ASTM Type 1 water directly into the sample bottles. The dissolved metals field blanks

at the influent to the FGD wastewater treatment system will be prepared by pumping the ASTM Type 1 water through the silicone tubing into a 1 0

- L composite container and then pumping the ASTM Type 1 water f rom the 10

- L container through the Teflon® and silicone tubing, through a

0.45

- um filter, and into the sample bottles. The dissolved metals field blanks at the influent to and effluent from the bioreactor system sampling points will be prepared by pumping ASTM Type 1 water through the composite tubing set into a large composite container where it will be

held for the 24

- hour compositing period, then pumping the ASTM Type 1 water from the large composite container through the Teflon® and silicone tubing, thr ough a 0.45

- um filter, and into the sample bottles. The field blanks will determine if there is any contamination from the sampling equipment, atmospheric contamination

, or other contamination from the surroundings.

EPA Method 1669 requires that equipmen t blanks also be prepared and analyzed for

metals to evaluate possible contamination of metals caused by the sampling equipment

. The supplier of the tubing and composite containers will prepare and analyze these equipment blanks and provide a report certif ying the equipment as clean.

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 sampling team will collect, label, and ship the necessary laboratory QC volumes. L aboratory QC volumes (i.e., MS/MSD sample) will be collected for every 10 samples collected at a sampling event, excluding field blank samples. For all analytes requiring laboratory QC volumes , the sampling team will collect QC sample volume from the influent to the bioreactor system (SP

- 2 ) during

10 ERG will not collect a field blank for dissolved mercury because a filter blank will be prepared and analyzed for by the laboratory.3

- 28 Day 4 of the sampling episode and from t he effluent from the bioreactor system (SP

- 3) during Day 3 of th e sampling episode

.

3.9

Belews Creek or its representative has elected to collect split samples at each of the sampling points. Belews Creek or its representative will supply all of the personnel, equipment, glassware, and reagents required to collect the split samples and to coordinate the analysis of samples. For each of the sampling points, the sampling crew will attempt to collect split samples with Belews Creek or its representative as described in this plan; howev er, if problems occur (e.g., the splitters become clogged and the flow is split unevenly between the sampling crews), then EPA may stop the split sample collection and offer instead to collect duplicate samples with Belews Creek or its representative. Sample Splitting3-29 T able 3

- 1

. Sample Collection at Belews Creek Steam Station

Sampling

Point Number Sampling Point NameTotal Metals(EPA Method 200.8 withcollision cell)Total Metals(EPA Method 200.7)DissolvedMetals(EPA Method 200.8 withcollision cell)DissolvedMetals(EPA Method 200.7)Total MercuryDissolved MercuryHexavalent ChromiumBOD5Group IaGroup IIbTotal Cyanide

SP

- 1 Influent to FGD Wastewater Treatment System 4 4 4 4 4 4 4 4 4 4 4

SP

- 2 Influent to Bioreactor System 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC 4+1QC

SP

- 3 Effluent from Bioreactor System 4 +1QC 4 +1QC 4 +1QC 4 +1QC 4 +1QC 4 +1QC 4 +1QC 4 +1QC 4 +1QC 4 +1QC 4 +1QC

SP

- 4 Duplicate of Influent to Bioreactor Sy stem 1 1 1 1 1 1 1 1 1 1 1

SP

- 5 Duplicate of Effluent from Bioreactor System 1 1 1 1 1 1 1 1 1 1 1

SP

- 6 Influent to FGD Wastewater Treatment System Field Blank 1 1 1 1 1 1

SP

- 7 Influent to Bioreactor System Field Blank 1 1 1 1 4 1

SP

- 8 Efflu ent from Bioreactor System Field

Blank 1 1 1 1 4 1

Total Number of Samples 17 +2QC 17 +2QC 17 +2QC 17 +2QC 23 +2QC 14 +2QC 17 +2QC 14 + 2 QC 14 + 2 QC 14 + 2 QC 14 + 2 QC

a

– Group I includes total suspended solids (TSS), total dissolved solids (TDS), sulfate

, and c hloride.

b

– Group II includes ammonia as nitrogen, nitrate/nitrite as nitrogen, total Kjeldahl nitrogen (TKN), chemical oxygen demand (CO D), and total phosphorus.3

- 30 Table 3

- 2

. Analytical Methods

Parameter Me thod Number

Classicals

Biochemical o xygen d emand (BOD 5 ) SM 5210 B

Chemical o xygen d emand (COD) EPA 410. 4

Total s uspended s olids (TSS) SM 2540 D

Total d issolved s olids (TDS) SM 2540 C

Sulfate EPA 300.0

Chloride EPA 300.0

Ammonia as n itrogen EPA 3 50.1

Nitrate/ n itrate as n itrogen EPA 353.2 Total Kjeldahl n itrogen (TKN) EPA 351.2

Total p hosphorus EPA 365. 1

Total c yanide SM 4500 CN E

Total and Dissolved Metals Mercury EPA 1631 E

Hexavalent c hromium (dissolved only) EPA 218.6

A ntimony, a rsenic, cadmium, chromium, copper, lead, manganese, nickel, selenium, silver, thallium, vanadium, and zinc EPA 200.8 with collision cell

Aluminum, barium, beryllium, boron, calcium, cobalt, iron, magnesium, molybdenum, sodium, tin, and titanium EPA 200.73

- 31 Ta ble 3

- 3

. Summary of Sample Container and Planned Preservation

Parameter Sample

Container and

Volume QC Sample

Container and

Volume On

- Site Preservation

Classicals

BOD 5 One 1

- L plastic

bottle One 1

- L plasti c bottle ≤6 **°** C

Group I a One 1

- L plastic

bottle s One 1

- L plastic

bottle s ≤6 **°** C

Group II b Two 1

- L plastic

bottle s Two 1

- L plastic

bottle s H 2 SO 4 to pH <2, ≤6 **°** C

Total c yanide One 1

- L plastic

bottle One 1

- L plastic

bottle s D ilution until sulfide is not detec ted

, NaAsO 2 until total chlorine is not

present, NaOH to pH >10, ≤6 **°** C

Metals

T otal metals (EPA Method 200.8 with collision cell) One 5 0 0

- mL plastic bottle No additional

volume needed None (acid preserve at laboratory)

T otal metals (EPA Method 200.7) On e 5 0 0

- mL plastic bottle No additional

volume needed None (acid preserve at laboratory)

D issolved metals ( EPA Method 200.8

with collision cell ) One 5 0 0

- mL plastic bottle No additional

volume needed 0.45

- μm filter (performed in field) (acid preserve at labo ratory)

D issolved metals (EPA Method 200.7) One 5 0 0

- mL plastic bottle No additional

volume needed 0.45

- μm filter (performed in field) (acid preserve at laboratory)

T otal mercury : None (acid preserve at laboratory) Manual composite grab samples Four 1 25

- mL glass bottle No additional

volume needed

Influent samples and field blank samples Two 250

- mL glass bottle No additional

volume needed

D issolved mercury : None ( filter and acid preserve at laboratory) Manual composite grab samples Four 125

- mL glass bottle No additional

volume needed

Influent samples One 250

- mL glass bottle No additional

volume needed

Hexavalent chromium One 2 50

- mL plastic bottle No additional

volume needed 0.45

- μm filter (performed in field)

Ammonium sulfate buffer to
pH 9.3

– 9.7

, ≤6 **°** C

(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.3

- 32 Table 3

- 4. Sampling Point Field Measurements

Field Meas urements Method Detection Range (or Gradation of Scale)

Temperature Thermometer

- 20 to 150 ± 1oC

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.

Sulfide L ead acetate test strip >50 mg/L sulfide (S 2

- )

Oxidants (i.e., chlorine) P otassium

- iodide starch paper > 1 mg/L free chlorine ( Cl 2 )3

- 33 Sampling Episode

____________

Preservation Chemicals

– List Strength of Solution from Bottle and Lot Number

H 2 SO 4

_____________________ NH 4 SO 4

________________________

NaOH

_____________________

Sample

Numbe r Analysis Date Time Name Chemical Initial pH Final pH Number of Drops

Figure 3

- 1. Sample Preservation Log Sheet3

- 34 Sampling Episode:

________________________________ __

Sampling Point :

________________________________ ____

Sample Numbers :

________________________________ __

Date :

Manual Composite 

## □ Grab 

## □

Automatic Composite 

## □

Time of Grab Sample Collection:

Start Time 

## □ AM 

## □ PM

End Time 

## □ AM 

## □ PM

Time of Automatic Sample Collection:

Start Time 

## □ AM 

## □ PM

End Time 

## □ AM 

## □ PM

Equipment Used: _____________________________________

____________

Samplers’ Names: ________________________________________________

Grab Sample Time Temp

° C pH (S.U.) meter / strips Waste Stream Flow Rate (MGD)

1

2

3

4

Notes: (include observations of odor and color of each a liquot, take pictures if necessary)

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________ Figure 3

- 2. Field Sampling Log Sheet3-35 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 pl ant based on all four days of the sampling episode. Note any changes in operation that occur during the four

- day period. Provide actual data if possible. If actual data are not available, provide estimates for the specific information. Some of the data req uested 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.

Generating Unit Operating Characteristics Duri ng Sample Collection

Unit

ID Boiler Type Capacity (MW) Electricity

Production

(MW) (or Percent Capacity % ) a SCR (No, On,

Off) Particulate Control System (HS/CS ESP, or BH)

a The electricity production should be measured on a daily basis from midnight of the 1 st day of sample collection to midnight of the last day of sample collection.

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 Make

up Water

Source SO 2 Removal Percentage Type of

Solids Separation

Note changes in operation over the past month (e.g., turned off SCRs on October 1 or b urned 5 percent petroleum coke previous week):

Figure 3

- 3

. Engineering Data Collection Sheet (Page 1 of 3)3

- 36 Plant Name:

________________________________ ________________________________ ________________ Plant Contact:

________________________________ ________________________________ ______________ Dates of Sample Collection:

________________________________ ________________________________ ___ Data Collected by:

________________________________ ________________________________ ___________

Instructions: In the tables below, provi de 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 n ot 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 T ype Amount of

Coal Used

During Day of Sampling Source of Coal ( Coal

Region

and/or

S tate) 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 ID s Scrubber Slurry

Blowdown Flow Rate Scrubber

S lurr y P ercent
S olids Time of Dewatering

During Sampling Day Percent

Filtrate Recycled

Back to

S crubber Flow Rate

(gpm) Duration

1

2

3

4

Figure 3

- 4. Engineering Data Collection She et (Page 2 of 3 )3-37 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 epi sode a nd the volumes of the FGD wastewater treatment system tanks and reactors. If possible, provide the name of the acid and polymer used during the samplin g episode. Provide actual data if possible. If actual data are not available, provide estimates for the s pecific 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.

FGD W astewater Treatment System Operation Information

Day of Sampling Scrubber Purge Chemical Usage (specify units)

Flow Rate

(gpm) Duration Lime Ferric

Chloride Organosulfide

_________ (specify product ) Polymer:

_________ (specify product ) Acid:

_________ ( specify product )

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 3

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

- 38 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

NUMBERSOURCE WATER(city, river, well)IN LINE PROCESSUNREATED EFFLUENT(raw wastewater)TREATED EFFLUENTOTHER(specify) ADDITIONAL

SAMPLE

DESCRIPTIONPH LEVELPRESERVED (Y/N)G=GRAB / C=COMPOSITESAMPLE COLLECTIONTIME / DATE

Comments: 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 Eastern Research Group, Inc. 14555 Avion Parkway, Suite 200 Chantilly, VA 20151

Figure 3

- 6. Example Traffic Report4

- 1 4. S AMPLING A CTIVITIES

Th is section discusses the sampling team organization, sampling preparation, and sampling activities.

4.1

The sampling crew will consist of a crew chief and four crew members from ERG, and two EPA representatives. The crew chief will be responsible for all health and safety, sample collection, preservation, and shipping activities while at Belews Creek. Following the sampling episode, ERG will collate the analytical results from each laboratory and summarize and transmit

t his informat ion in a trip report to EPA. After EPA review, the report will be forwarded to

Belews Creek for review. Sampling Team Organization

4.2

On March 12, 2008, ERG and EPA conducted a site visit at Belews Creek. Additionally,

EPA conduct ed a sampling episode at Belew s Creek between October 20 , 200 8 and October 23,

2008. T he focus of this sampling episode was to characterize the purge stream entering the F GD wastewater treatment system and the influent to and effluent from the FGD bioreactor treatment

system

. The site visit and previous sampling effort provided ERG and EPA the necessary information to prepare for th is sampling episode. The information collected during the site visit

and previous sampling episode was used to create this sampling plan. Pres ampling Preparation

As part of prepa ring the team for the sampling episode at Belews Creek, the ERG crew chief will distribute this sampling plan to each team member and ensure they are completely familiar with the sampling plan and the health and safety requirements specific to Belews Creek

. The crew chief will also give copies of this sampling plan to Belews Creek personnel before sampling begins.

The ERG crew chief will also coordinate the procurement and shipment of all necessary sampling and health and safety equipment.

4.3

Upon arrival at Belews Creek, the ERG crew chief, in conjunction with the EPA representatives, will meet with Belews Creek personnel to determine whether samples can be collected as planned at each of the planned sampli ng points. Upon confirming the methods to collect samples, the ERG crew chief will update the descriptions of the proposed sampling points, if necessary, in consultation with EPA and Belews Creek personnel. If necessary, the

crew chief will obtain addition al equipment. The revised sampling description will include: Field Sampling Activities

**•** A sampling point description and collection procedure for each sampling point;

**•** A list of the sample fractions to be collected at each point ;

**•** A list of potential physical hazards (e.g., pH, tempe rature, and potentially hazardous equipment);

**•** A list of potential chemical hazards associated with each sampling point; and

**•** A list of proposed health and safety procedures.4

- 2 Prior to sampling, the ERG crew chief will notify the ERG Health and Safety

Coor dinator (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 incorpora te any plant

specific changes indicated by the HSC and receive 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 re quiring ≤6 o C preservation will be placed on ice. 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.

4.4

This subsection summarizes Belews Creek contacts, analytical laboratory contacts and addresses, and sampling team personnel and support functions. Logistics

4.4.1 Belews Creek Steam Station Contacts

Robert Wylie Duke Energy Carolinas

526 S. Church Street Charlotte, NC 28201 (704) 382

- 4669

Melo nie Martin Duke Energy Carolinas

Belews Creek Steam Station

3195 Pine Hall Road Belews Creek, NC 27009 (336) 445

- 0610

4.4.2 EPA Contacts

Ron Jordan Engineering and Analysis Division U.S. Environmental Protection Agency 1200 Pennsylvania Avenue, NW (43 03T) Washington, D.C. 20460 (202) 566

- 10034

- 3 Jezebele Alicea Engineering and Analysis Division U.S. Environmental Protection Agency 1200 Pennsylvania Avenue, NW (4303T) Washington, D.C. 20460 (202) 566

- 1 755

4.4.3 Analytical Laboratories

Classicals and Metals by 200.7 and 200.8 with Collision Cell TestAmerica, Inc. :

4955 Yarrow Street Arvada, CO 80002 Phone: (303) 736

- 0138 Contact: Elizabeth Eichelberger

Frontier GeoSciences, Inc. Mercury and Dissolved Hexavalent Chromium :

414 Pontius Ave. North Seattle, WA 9810 9 Phone: (206) 957

- 1428

Contact: Patrick Garcia

- Strickland

4.4.4 ERG Contacts

TJ Finseth (Crew Chief) Eastern Research Group, Inc. 14555 Avion Parkway, Suite 200 Chantilly, VA 20151 (703) 633

- 1698

Deborah Bartram (Work Assignment Manager)

Eastern Research Grou p, Inc. 14555 Avion Parkway, Suite 200 Chantilly, VA 20151 (703) 633

- 1669

4.4.5 Freight Forwarders

Federal Express (FedEx) General Information (800) 463

- 3339

FedEx Office Print & Ship Center ( 16 miles from plant) 3731 Battleground Ave

Greensboro

, NC 27 4 10

Ho urs of Operation: Mon.

– Fri.: 7 :00 a .m. to 11 : 0 0 p.m.

Last Express Drop

- off: Mon.

– Fri.: 6 : 3 0 p.m.4

- 4 FedEx Express Ship Center (15 miles from plant) 100 Progress Court Winston Salem, NC 27105 Hours of Operation: Mon.

– Fri.: 8:00 a.m. to 8:00 p.m.

L ast Express Drop

- off: Mon.

– Fri.: 8:00 p.m.5

- 1 5. S AMPLE S HIPMENT

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 samp le collection until samples are delivered to Federal Express.

All samples will be packaged and shipped in accordance with Department of Transportation ( DOT ) or International Air Transport Association ( IATA ) regulations. The general IATA packaging require ments 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 materi al 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

Instructio ns, 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 i s 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 sub sections 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 collect ed at Belews Creek will not be classified as IATA dangerous goods.

5.1

Samples are collected as a series of “fractions,” or bottles designated for particular analyses requiring the same preservation. The comprehen sive water sample set consists of sample fractions for all pollutants listed in Section 3.2, collected as grab samples directly into the individual sample containers or composite samples that are transferred to individual sample containers using a pump

- off approach

. Sample Set Preparation

5.2

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): Sample Packing5

- 2 1. Label each sample bottle. If a required preservation is not u sed, cross it off with indelible ink. Cover the label with clear tape to protect this information. Do not

label m etal sample bottles , but , the outer plastic bag for each bottle instead

.

2. Tighten the lid on each filled sample bottle, being careful not to ov ertighten 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. Do not clean t he bottle

threads for the metals sample bottles.

3. Prior to packaging, p lace each sample bottle requiring ≤6 ° C preservation into an

ice chest with wet ice 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 “bub ble bags”). The bubble wrap must fit snugly and completely cover the sample bottle. Enclose e ach “bubble

- wrapped” container and plastic container in an individual sealable plastic freezer bag. Place VOA vials in VOA bricks in a freezer bag.

5. Place two garb age 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

seal ed 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 one

gallon sealable freezer bags. Put at least 4 × 1⁄2 gallons of ice (4 × 2.5 pounds of ice) in each large cooler and 2 × 1⁄2 gallons of ice (2 × 2.5 pounds of ice) in each

small cooler. Use m ore ice when ambient temperatures are very high. Place t he ice inside the second garbage bag and c lose the second garbage bag with a twist

tie.

8. Fill in around the bot tles and any free space with additional cushioning material.

Use s ufficient packing material so that the sample containers will not shift during shipment.

9. Seal the Traffic Report form in a plastic zip

- lock bag and tape it securely to the

inside of the co oler lid.

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.5

- 3 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.6

- 1 6. S ITE

- S PECIFIC H EALTH AND S AFETY P ROCEDURES

This section specifies the health and safety procedures and practices to be used by the sampling team during sampling at Belews Creek. This section provides general health and safety information for this sampling episode. The sampling team is obligated to follow all safety procedures specified in this section.

6.1

The following procedures will be followed in the event of a medical or other emergency

situation. Emergency/Medical Procedures

6.1.1 First Aid

Belews Creek has first aid kits available throughout the plant. In addition, ERG will also bring a first aid kit. Additionally, Belews Creek has a first responder team, which is available for EPA/ERG in the event of an emergency

. Belews Creek personnel request t hat any emergencies be handled through the wastewater treatment system’s control room so they can direct the responders to the correct location

.

6.1.2 Site Evacuation/Emergency Response Plan

The sampling team will be informed of the Belews Creek evacuation pr ocedures and routes by plant personnel.

6.1.3 Emergency Showers and Eye Washes

Emergency showers and eye wash stations are located throughout the plant. Before collecting samples at any point, sampling team members will locate the nearest operating safety

sho wer and eye wash station.

6.1.4 Local Hospital

The nearest hospital is Stokes

- Reynolds Memorial Hospital, located in Danbury, NC , and is approximately 13 miles from Belews Creek Steam Station. The hospital address is:

Stokes

- Reynolds Memorial Hospital

1570 NC 8 & 89 Hwy North Danbury, NC 27106

The local emergency phone number in Belews Creek, NC is 911.

6.2

The ERG Work Assignment Manager (WAM), crew chief, and sampling team members have different responsibi lities to maintain a safe sampling environment. These responsibilities

are described below. ERG Health and Safety Responsibilities and Authority6

- 2 6.2.1 Work Assignment Manager

The ERG WAM, Deborah Bartram, has the overall responsibility to ensure that th ese health and safety procedures are developed and implement ed in accordance with regulations and corporate guidelines, that proper health and safety procedures have been initiated, and that all ERG activities are conducted in accordance with the health and safety plan. The ERG WAM will also ensure that proper reso urces are allocated so that the project is conducted in a safe manner, and that the crew chief is competent in his ability to oversee health and safety during the sampling episode.

6.2.2 Crew Chief

The ERG crew chief, TJ Finseth, is responsible for ensuring th at ERG sampling team members adhere to this plan. The ERG crew chief and ERG night crew chief are responsible for overseeing all a ctivities. The crew chief s must report any accident, near miss, or injury to any sampling team member to the ERG Chantilly Off ice Health and Safety Coordinator (HSC), Kevin Sikora, verbally within eight hours, or sooner. The HSC will investigate the incident to identify the cause of the accident, near miss, or injury. If sufficient cause exists, ERG’s general health and safety pl an and in

- house training program will be modified to avoid similar accidents

in the future.

At the start of the sampling visit, the crew chief s will inspect all sampling points and review sample collection procedures with the Belews Creek personnel to en sure that all potential

hazards have been identified.

The crew chief s ha ve the authority to enforce ERG’s health and safety requirements contained in this plan, and any facility

- specific requirements. Changes to this plan can be made if

the crew chief s
, the Chantilly HSC , and EPA representative agree that the changes are appropriate.

6.2.3 Sampling Team Members

All field personnel are responsible for following the requirements of this plan, for adhering to plant

- specific health and safety procedures, and donn ing required/recommended personal protective equipment ( PPE ) . They are also responsible for bringing health and safety

issues to the attention of the crew chief s

.

6.3

ERG sampling team personnel will attend on

- and off

- site health and safety briefi ngs. Briefings

6.3.1 Off

- Site Briefings

Prior to arriving on site, all members of the sampling team will receive a copy of this sampling plan and attend a presampling meeting to review th e sampling plan and the proposed sample collection activities

. Everyone at this mee ting will receive a copy of th e sampling plan. All ERG employees will be required to sign a health and safety sign

- off sheet stating that they have read, understood, and agree with this health and safety plan prior to participating in field sampling activi ties.6

- 3 6.3.2 On

- Site Briefings

ERG sampling team personnel must attend a one

- to two

- hour safety course given by Belews Creek personnel prior to conducting sampling activities at Belews Creek. This safety course will review plant

- specific health and safety proc edures, including:

**•** Locating on

- site first aid/emergency medical procedures;

**•** Required PPE;

**•** High hazard areas and other specific areas or hazards of concern;

**•** Emergency alarms and evacuation procedures; and

**•** Other site safety requirements and procedures that ERG personnel must follow.

6.4

ERG personnel will follow general safety procedures, which include wearing PPE and engaging in safe work practices. Safety Procedures

6.4.1 Personal Protective Equipment (PPE)

The PPE listed below will be worn by ERG personnel at all times while inside the premises of Belews Creek:

**•** Steel

- toed safety shoes;

**•** Long sleeves (when sampling) and pants;

**•** Hard hat, where required by Belews Creek;

**•** Hearing protection, where needed;

**•** Nitrile or non

- colored, electronic grade gloves, when collect ing or preserving; and

**•** Safety glasses with side shields or chemical splash goggles, when collecting or preserving samples.

For all phases of sample collection, disposable PPE will be used, so decontamination of the PPE may not be necessary . If gloves bec ome torn or degraded, they will be thrown away and replaced with a new pair. Disposable PPE, including gloves, will be removed, bagged, and left at

the site in a controlled manner.

6.4.2 Safety Practices

ERG personnel will conduct themsel ves at all times in a manner judged to be safe by site supervisors.

All sample collection will be scheduled so that no ERG employee collects samples alone. Each worker will maintain visual contact with at least one other worker at all times. This buddy system will ensure against an employee becoming injured or contamina ted with chemicals

without a co worker being aware of his or her condition. Workers should “watch out” for each other while working close to potential chemical and physical hazards. A Belew s Creek or EPA employee may be used as a buddy by ERG personnel. This arrangement will be agreed to and acknowledged by the employee.6

- 4 ERG employees will not enter any permit

- required confined space areas.

6.4.3 Safe Work Practices

ERG samplers will obey t he following safety rules while working in the facility:

**•** Wearing PPE, where required;

**•** Staying within designated areas;

**•** Not wearing loose clothing or jewelry;

**•** Keeping long hair in hard hat or tied back;

**•** Not eating in the sampling o r staging areas; and

**•** Not smoking in the sampling or staging areas.

6.5

All sampling team members will be advised of any sampling

- point

- specific safety protocols during the on

- site health and safety briefing. Table 6

- 1 su mmarizes all potential sampling

- point

- specific safety hazards as well as the PPE required at each sampling point. During the day shift, t he sampling team health and safety officer (HSO) for this sampling episode is the crew chief, TJ Finseth (ERG). Dur ing the night shift, the HSO for this sampling episode is the ERG night crew chief (to be determined at a later date). The HSO and the sampling team will inspect each sampling point area to identify unique or additional hazards not already covered in this plan or during the formal health and safety briefing. If additional hazards are found, the sampling team will be informed of each hazard and required control measures prior to the start of work. Where identified hazards may affect the plant’s personnel, th e HSO will notify the appropriate Belews Creek personnel. Sampling

- Point

- Specific Safety Procedures

6.5.1 Physical Hazards

ERG personnel will be alert for all physical hazards present while on site. Physical hazards may arise from using catwalks, hitting low

- hanging overhead piping, and working

around moving equipment or vehicles. ERG personnel will be aware of the potential splash

hazards at SP

- 1, SP

- 2, and SP

- 3 due to the location of the sample taps. To prevent splashing, ERG personnel will ensure that the sample tubing is connected securely to the s ample tap and will open the sample valve slowly when collecting samples. Other potential hazards may include falling hazards during sample collection, tripping on metal grates, or operation of large trucks and machinery in the vicinity of the sample collec tion area. See Table 6

- 1 for potential hazards that may be associated with specific sampling points.

Noise may be a hazard in certain areas of the facility. The sampling team will use h earing protection w here required by the plant, when they a re having t rouble hearing or being heard when standing three feet or less away from another person, or when deemed necessary by the Belews Creek personnel or ERG crew chief.6

- 5 6.5.2 Thermal Hazards

Heat stress may be a concern during the sampling episode. Samplers may be suited in Tyvek® and temperatures could reach extremes. Of particular concern is SP

- 1, which is located outside. The sampling team members will consume plenty of fluids prior to the start of sampling, and will monitor each other for symptoms of heat stress

.

Wastewater sampling points are not expected to be too hot for safe handling using typical PPE. Thicker nitrile gloves may be used during sampling if sample bottles are too hot to hold. Samplers will handle extremely hot samples with heat

- resistant glo ves.

6.5.3 Chemical Hazards

The only chemical hazards expected are chemicals used to preserve samples. All sampling team members will be advised of any potential chemical hazards at each sampling point as well as any special PPE recommendations during the form al health and safety briefing. If the sample tap (i.e., the point from which the wastewater flows) is above waist height, a face shield or goggles must be worn during sample collection. To avoid ingesting chemicals, sampling team members will be required t o wash hands thoroughly before eating or drinking. ERG personnel will not be permitted to enter areas where the facility has determined that respiratory protection equipment is necessary to protect against inhalation hazards.

6.6

Extrem ely hot temperatures can be a health and safety hazard for this sampling episode. ERG personnel will take precautions to avoid injuries due to extreme temperatures. Temperature Extremes

6.6.1 Heat Stress

Heat stress is not only a concern in hot/humid outdoor environments; it is a concern due to the thermal or radiant heat generated by equipment and/or processes. Sampling team personnel will monitor each other for the following symptoms:

**•** Heat rash that may result from continuous exposure to heat or humid air.

Treatment: Wear cotton clothing under coveralls or Tyvek®.

**•** Heat cramps that are caused by heavy sweating and inadequate electrolyte replacement. Many times, cramps may not occur until after work or until the worker is sleeping. Signs and symptoms include m uscle spasms and p ain in the hands, feet, and abdomen

Treatment: Gently stretch and massage muscles and replace fluids. Have worker

r est in a cool shaded area.

**•** Heat exhaustion that occurs from increased stress on various body organs including inadequate blood circulation due to cardiovascular insufficiency or dehydration. Signs and symptoms include:6

- 6 — Pale, cool, moist, clammy skin

— Heavy sweating

— Headache and dizziness

— Nausea

— Fainting or fatigue

— Elevated pulse rate (above 150)

Treatment: Replace fluids, pour cool water over face, neck, hands, arms, and legs.

Place worker in cool air and seek medical care.

**•** Heat stroke is the most serious form of heat stress. Temperature regulation fails and the body temperature rises to critical levels. Immediate action m ust be taken to cool the body before serious injury and death occur. Competent medical help

must be obtained. Signs and symptoms are:

— Red, hot, usually dry skin, body core temperature 108 ° F (oral)

— Lack of or reduced perspiration

— Nausea

— Headache, dizziness , and confusion

— Strong, rapid pulse

— Coma

Treatment: Remove worker to cool area, saturate clothes with cold water, wrap worker in wet cold sheets (if possible), monitor ABC (airway, breathing, circulation), treat for shock, and call emergency services for basic life support (BLS) or advanced life support (ALS).

6.6.2 Heat Stress Monitoring

A worker who exhibits any of the above symptoms will be immediately relieved of responsibilities and requested to consume electrolyte fluid or cool water while resting in a s haded area. The individual should not return to work until symptoms are no longer recognizable. If symptoms appear critical, persist, or get worse, the crew chief will seek immediate medical attention for the employee. If the individual does resume work, h e/she will be monitored for any

increase in heart rate for the remainder of his/her shift. In addition, the worker will be requested to consume electrolyte fluid or cool water every hour.

The crew chief will visually monitor workers hourly when:

**•** Symptom s of heat stress are reported or observed;

**•** Ambient temperatures exceed 70 ° F and workers are dressed in impervious clothing; or

**•** Ambient temperatures exceed 90 ° F and workers are dressed in normal clothing.

For sampling on this project, work periods will be considered to be approximately two hours in length.6

- 7 At ambient temperatures of 87 ° F and above, workers will be monitored for heat stress conditions by measuring the heart rate (HR) by radial (wrist) pulse for 30 seconds after one

minute of rest. The H R after one minute of rest should not exceed 110 beats per minute. If the

heart beat is higher, the next work period will be shortened by 33 percent, while the length of rest period remains the same. If the pulse rate is still higher than 110 beats per min ute after one minute of rest in the next rest period, the following work cycle will be shortened by another 33 percent. This shortening of the work period must continue until the worker's HR is no greater than 110 beats per minute.

6.7

First aid procedures in response to chemical exposures will be conducted in accordance with the appropriate material safety data sheet ( MSDS ) for the chemical involved. If an incident occurs and MSDSs are not available for a particular hazardous chemical (e.g., wastewater), the following general first aid procedures will be performed: First Aid

**•** Skin Contact

– Rinse t he affected area thoroughly and copiously with clean water. Seek medical attention if irritation is experienced after cleaning.

**•** Eye Contact

– Flush t he eyes thoroughly at the nearest eyewash station for 15 minutes. Follow up with medical attention.

**•** Ingestion

– Notify t he hospital and carry out any procedures recommended.

The first aid kit will be maintained on each site in the equipment sta ging area. The

contents of the first aid kit will include at a minimum:

**•** Adhesive bandages;

**•** Antiseptic wipes;

**•** A compress;

**•** An eyewash solution;

**•** Gauze pads;

**•** A cold pack; and

**•** A triangular bandage.

The injuries most likely to be encountered at Belews Creek are cuts and bruises; the first aid kit will be maintained and stocked accordingly.

6.8

Water samples to be analyzed for various contaminants may be preserved with sulfuric acid (H 2 SO 4 ), hy drochloric acid (HCl), sodium hydroxide (NaOH), an ammonium sulfate buffer solution (NH 4 SO 4 )

, and/or sodium arsenite ( NaAsO 2 ) before shipment to the analytical laboratory. Nitrile gloves and splash goggles must be worn when handling these corrosive

chemica ls to prevent chemical burns. Sample preservation must be performed in a well

ventilated area (preferably an operational lab hood) to avoid potential accumulation and inhalation of any toxic vapors. When pouring samples, skin protection must also be worn ( long

Sample Preservation and Safety Considerations6

- 8 sleeved cotton coveralls or uncoated Tyvek®, safety glasses with side shields or splash goggles, and nitrile gloves). Sodium arsenite is a known carcinogen and is toxic so extra care should be taken when handling any solutions containing sodium arseni te.

In some instances, the use of these preservation chemicals could create a chemical reaction (i.e., generation of heat or release of toxic vapors). For instance, if acids are added to a wastewater sample containing cyanide or sulfides, dangerous and t oxic vapors will be emitted. If the sample reacts violently, notify the crew chief and stop preserving the sample immediately.

In the case of a chemical spill, the following procedures must be followed:

**•** Don protective clothing (nitrile gloves as a minim um).

**•** Ventilate area (open doors, windows, or turn on ventilation).

**•** Use spill control pillows or prepared neutralizers to contain/clean up spill. Do not

add water to acid.

**•** Place spilled material in a heavy plastic container, label the container, and cont act site for disposal information.

**•** Notify the crew chief of the spill and the procedures used.

At any time, if personnel do not feel comfortable about cleaning up the spilled material or if a large quantity has been spilled, notify site personnel. The s ite may have an emergency response team who will respond to the chemical spill.

In the case of fire, notify the site contact. If the fire can be easily extinguished using a portable fire extinguisher, and personnel have received fire extinguisher traini ng, extinguish the fire using the portable extinguisher.

6.9

All ERG sampling crew personnel have participated in ERG's annual eight

- hour health and safety training program as specified by ER G's Corporate Health and Safety Policy. Training and Medical Monitoring Requirements

This training includes:

**•** Toxicology;

**•** Exposure limits;

**•** Chemical, biological, and physical hazards;

**•** Heat and cold stress;

**•** Confined spaces;

**•** PPE;

**•** Decontamination; and

**•** Emergency plans and procedures.

All ERG personnel i nvolved with sample collection and preservation are active participants in the Medical Monitoring Program. Field sampling personnel have received a

baseline medical information review

.6

- 9 6.10

This sub section provides g uidance for field personnel project schedules and field work, particularly overtime. It is important to remember extended work schedules will contribute to poor production and motivation. All field teams will rotate to ensure that sampling team

members rec eive sufficient rest to avoid injuries resulting from fatigue or inattention. Shift Work Protocol

It is common practice to perform 12

- hour work days under project management direction. If this work schedule is exceeded the following guidelines will be recognized:

1. A 15

- hour maximum work day will be 15 hours , provided that it does not occur on consecutive days, or more than three times in ANY SEVEN

- DAY PERIOD.

2. Each shift will be followed by nine hours off per 24

- hour period, excluding driving time to and from the hotel.

3. No more than seven consecutive days of work will be allowed without a

minimum of 24 hours off.

4. Each work day will be reviewed as a 24

- hour cycle to assure all field workers receive adequate time off.6

- 10 Table 6

- 1. Sample

- Point

- Specific PPE and Potential Hazards

Sampling

Point Number Sampling Point Description PPE Required a Potential Physical Hazards b

SP

- 1 Influent to FGD Wastewater Treatment System Steel

- toed boots, hard hats, gloves

, and safety glasses Splash hazard: Potential for splashing from the sample tap. Sample tap will be below waist

level.

SP

- 2 /SP

- 4 Influent to Bioreactor System Steel

- toed boots, hard h ats, gloves, and safety glasses Splash hazard: Potential for splashing from the sample tap. Sample tap will be below waist

level.

SP

- 3/SP

- 5 Efflue nt from Bioreactor System Steel

- toed boots, hard h ats, gloves, and safety glasses Splash hazard: Potential for splashing from the sample tap. Sample tap will be below waist

level.

a

– Splash protection (face shield) required if sampling port is waist high or above. Hearing protection (ear plugs)

will be worn if needed.

b

– Additional physical hazards, if any, will be identified during the formal on

- site health and safety briefing. Updates to this table will be made as needed.7

- 1 7. R EFERENCES

1. Eastern Resea rch Group, Inc. 2009. Generic Sampling and Analysis Plan for Coal

- Fired

Steam Electric Power Plants

. (February)

.

2. U.S. EPA. 200 9

. Steam Electric Power Generating Point Source Category: Final Detailed Study Report . EPA 821

- R

- 0 9

- 0 08 . Washington, DC. ( Octob er ). Available online

at: http://www.epa.gov/guide/steam/finalreport.pdf. DCN SE00003

.