&EPA
United States
Environmental Protection
Agency
EPA/600/R-161/126 I September 2016
www.epa.gov/homeland-security-research
Testing Large-Volume Water Treatment
and Crude-Oil Decontamination Using
the EPA Water Security Test Bed
Office of Research and Development
Homeland Security Research Program
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EPA/600/R-161/126
September 2016
TESTING LARGE-VOLUME WATER TREATMENT AND
CRUDE-OIL DECONTAMINATION
USING THE EPA WATER SECURITY TEST BED
U.S. Environmental Protection Agency
Cincinnati, Ohio 45268
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Disclaimer
The U.S. Environmental Protection Agency (EPA), through its Office of Research and
Development's National Homeland Security Research Center (NHSRC), funded and managed
this project under Interagency Agreement (IA) DW-89-92381801 with the Department of Energy
and under contract EP-C-14-012 with CB&I Federal Services LLC, Cincinnati, Ohio 45212. This
report has been peer and administratively reviewed and has been approved for publication as an
EPA document. It does not necessarily reflect the views of the EPA. Mention of trade names or
commercial products does not constitute endorsement or recommendation for use of a specific
product.
Questions concerning this document or its application should be addressed to:
Jeff Szabo, Ph.D., P.E.
National Homeland Security Research Center
Office of Research and Development
U.S. Environmental Protection Agency
26 W. Martin Luther King Drive
Cincinnati, OH 45268
szabo. i eff@epa. gov
John Hall
National Homeland Security Research Center
Office of Research and Development
U.S. Environmental Protection Agency
26 W. Martin Luther King Drive
Cincinnati, OH 45268
hall ,i ohn@epa. gov
i
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Acknowledgements
Contributions of the following organizations to the development of this document
acknowledged:
CB&I Federal Services LLC
Idaho National Laboratory
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Table of Contents
Disclaimer i
Acknowledgements ii
1.0 Introduction 3
1.1 WSTB Description and Setup 3
2.0 Description of Experiments 9
2.1 Disinfection of Large Water Volumes 9
2.1.1 EPA AOP Trailer Testing 11
2.1.2 Solstreme™ UV System Testing 12
2.1.3 WaterStep Chlorinator Testing 13
2.1.4 Hayward Saline C™ 6.0 Chlorination System Testing 14
2.2 Crude Oil Contamination/Decontamination Tests 18
3.0 Analysis of Test Results 25
3.1 Disinfection of Large Water Volumes 25
3.1.1 EPA AOP Trailer Unit Testing 25
3.1.2 Solstreme™ UV System Testing 27
3.1.3 WaterStep Chlorinator Testing 30
3.1.4 Hayward Saline C™ 6.0 Chlorination System Testing 33
3.2 Crude Oil Contamination/Decontamination Tests 36
3.2.1 Online Sensor Data 40
4.0 Conclusions and Future Work 42
5.0 References 46
Appendix A: Quality Assurance Project Plan 47
Appendix B: Summary of Technology Specific Considerations 82
Appendix C: Technical Bulletin SURFONIC® DOS-75PG Surfactant 85
List of Figures
Figure 1. Schematic overview of Water Security Test Bed 4
Figure 2. Aerial view of the Water Security Test Bed 4
Figure 3. Water Security Test Bed system flow regulator 5
Figure 4. Water Security Test Bed discharge lagoon 5
Figure 5. Schematic layout for large volume water treatment technologies testing 6
Figure 6. Prepared crude oil subnatant for Water Security Test Bed injection 7
Figure 7. Removable 15-foot PVC coupon section 7
Figure 8. Extracted pipe coupon 8
Figure 9. Inlet bladder tank and mixing 9
Figure 10. Schematic depiction of the inlet bladder tank mixing process 10
in
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Figure 11. Advanced Oxidative Process System and influent/mixing bladder tank (black object to
the right of the system) 11
Figure 12. Solstreme™ UV System and effluent bladder tank (blue object in front of the UV
system) 12
Figure 13. WaterStep Chlorinator System bladder tanks (dark blue) 13
Figure 14. WaterStep Chlorine Generator components 14
Figure 15. Hayward Chlorine Generator 15
Figure 16. Hayward Saline C™ 6.0 Chlorination System setup on a table 16
Figure 17. Contamination of the lagoon with Bacillus globigii 16
Figure 18. Lagoon Bacillus globigii recirculation/mixing pump 17
Figure 19. Turner TD1000C Oil in Water Monitor 19
Figure 20. Effluent oil capture treatment train 20
Figure 21. Crude oil injection stock preparation 21
Figure 22. Treatment performance of the Advanced Oxidation Process trailer over the course of
5.5 hrs. Blue and orange bars represent the mean spore density in the AOP trailer influent and
effluent, respectively. The green line represents log reduction, or the amount of inactivation
occurring at each sampling point. Error bars represent the range between duplicate samples
taken at each time point 26
Figure 23. Treatment performance of the Solstreme over the course of 5.5 hrs 28
Figure 24. Spore log reduction for Solstreme UV treatment vs. UV output intensity 29
Figure 25. Free chlorine concentration (orange) and Bacillus globigii spore (blue line) density
over time in the WaterStep bladder tank 31
Figure 26. The log reduction in spores during the WaterStep experiment plotted against the Ct
value (disinfectant concentration multiplied by time) 32
Figure 27. Free chlorine concentration (orange) and Bacillus globigii spore (blue line) density
over time in lagoon water (-5,000 gal) during disinfection with the Hayward treatment unit 34
Figure 28. The log reduction in spores during the Hayward experiment plotted against the Ct
value (disinfectant concentration multiplied by time) 35
Figure 29. Benzene concentration in the Water Security Test Bed bulk water 39
Figure 30. Online total organic carbon (TOC) and hydrocarbon sensor data during the crude oil
contamination and surfactant decontamination (9/21/2015) 40
Figure 31. Online chlorine sensor data during the crude oil contamination and surfactant
decontamination (9/21/2015) 41
List of Tables
Table 1. Crude Oil Contamination/Decontamination Related Sampling Activity 22
Table 2. EPA Advanced Oxidation Process Trailer Technology-Specific Considerations and
Observations* 26
Table 3. Solstreme Technology-Specific Considerations and Observations* 29
Table 4. WaterStep Technology-Specific Considerations and Observations* 32
Table 5. Hayward Technology-Specific Considerations and Observations* 35
Table 6. Bulk Water Sampling Results 37
Table 7. Coupon Sampling Results 38
Table 8. Mobile Water Treatment Device Performance Summary 43
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Abbreviations
AOP Advanced Oxidation Process
AWWA American Water Works Association
BTEX benzene, toluene, ethylbenzene and xylene
BWS bulk water sample
CB&I CB&I Federal Services LLC
cfu colony forming units
Cb free chlorine
cm centimeter
CP Coupon
Ct Concentration of disinfectant multiplied by contact time
DPD N,N-diethyl-phenylenediamine
DRO Diesel range organics
EPA U.S. Environmental Protection Agency
ft feet
gpm gallons per minute
GRO Gasoline range organics
HPC Heterotrophic Plate Count
HSRP Homeland Security Research Program
IA Interagency Agreement
INL Idaho National Laboratory
kg kilogram
L Liter
LCD Liquid Crystal Display
m meter
MCL Maximum Contaminant Levels
Hg/L micrograms per liter
mJ/cm2 milli-Joule per square centimeter area
mL milliliter
MPN/mL most probable number per milliliter
mW-sec/cm2 milli-Watt-second per square centimeter area
NHSRC National Homeland Security Research Center
NSF Nati onal S anitati on F oundati on
NTU nephelometric turbidity units
OH hydroxyl radicals
ORO oil range organics
pH numeric scale used to measure acidity or basicity of an aqueous solution
PVC Polyvinyl Chloride
QAPP Quality Assurance Proj ect Plan
RF radio frequency
T&E Test and Evaluation
TOC Total Organic Carbon
TPH Total Petroleum Hydrocarbon
UV Ultraviolet
VOC Volatile Organic Carbon
WSTB Water Security Test Bed
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Executive Summary
The U.S. Environmental Protection Agency's (EPA's) Homeland Security Research Program
(HSRP) partnered with the Idaho National Laboratory (INL) to build the Water Security Test Bed
(WSTB) at the INL test site outside of Idaho Falls, Idaho. The WSTB was built using an 8-inch
(20 cm) diameter cement-mortar lined drinking water pipe that was previously taken out of service.
The pipe was exhumed from the INL grounds and oriented in the shape of a small drinking water
distribution system. Effluent from the pipe is captured in a lagoon. The WSTB can support
drinking water distribution system research on a variety of drinking water treatment topics
including biofilms, water quality, sensors, and homeland security related contaminants. Because
the WSTB is constructed of real drinking water distribution system pipes, research can be
conducted under conditions similar to those in a real drinking water system.
In 2014, WSTB pipe was experimentally contaminated with Bacillus globigii spores, a non-
pathogenic surrogate for the pathogenic B. anthracis, and then decontaminated using chlorine
dioxide. In 2015, the WSTB was used to perform the following experiments:
• Four mobile disinfection technologies were tested for their ability to disinfect large
volumes of biologically contaminated "dirty" water from the WSTB. B. globigii spores
acted as the biological contaminant. The four technologies evaluated included: (1)
Hayward Saline C™ 6.0 Chlorination System, (2) Advanced Oxidation Process (AOP)
Ultraviolet (UV)-Ozone System, (3) Solstreme™ UV System, and (4) WaterStep
Chlorinator.
• The WSTB pipe was contaminated with Bakken crude oil, and decontamination was
performed by flushing with clean water with addition of a surfactant.
The following is a summary of conclusions based on the testing performed at the INL WSTB:
• Results from the water treatment experiments indicate that disinfection of large volumes
of water contaminated with B. globigii spores is feasible. All treatment units achieved at
least 4-log removal of spores from the lagoon water over the course of the experiments,
with some units achieving 7-log reduction. Treated water volumes ranged from 1,250 to
5,000 gallons (4,732 to 18,927 L) with experiments ranging from 5.5 hours to 1 day. It is
likely that larger volumes of water may need to be disinfected in a real world scenario, but
all of the tested mobile treatment systems can be scaled up, or multiple units can be put
into place. Data generated from this study does demonstrate that disinfection of
contaminated water in the field is more challenging than disinfecting clean drinking water
due to the disinfectant demand present in real world wash water, the potential for low
temperature, and disinfectant dissipation due to sunlight.
• Data collected during the crude oil contamination experiment suggest that flushing the pipe
with clean water was an effective decontamination method. Benzene detected in the
WSTB pipe from the oil contamination dropped below the EPA prescribed Maximum
Contaminant Levels (MCLs) with clean water flushing, and no other benzene, toluene,
ethylbenzene and xylene (BTEX) components were detected in the water. No total
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petroleum hydrocarbons or BTEX compounds were detected on the pipe infrastructure
surface in contact with the water after flushing. Surfactant was injected because it was
assumed that oily components could persist in the water phase or on the infrastructure
surfaces. This was not the case, but online sensor data and visual observation of foaming
in the water samples indicated that surfactant may have persisted in the dead-end portions
of the WSTB pipe for weeks after the initial injection. This should be taken into
consideration if a surfactant is used during decontamination of a drinking water distribution
system.
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1.0 Introduction
The U.S. Environmental Protection Agency's (EPA's) Homeland Security Research Program
(HSRP) partnered with the Idaho National Laboratory (INL) to build the Water Security Test Bed
(WSTB) at the INL test site 50 miles (80 km) west of Idaho Falls, Idaho. The WSTB was built
using an 8-inch (20 cm) diameter cement-lined drinking water pipe that was previously taken out
of service. The pipe was exhumed from the INL grounds and oriented in the shape of a small
drinking water distribution system (see Section 1.1 for a detailed description). Effluent from the
pipe is captured in a lagoon. The WSTB can support drinking water distribution system research
on a variety of topics including biofilms, water quality, sensors, and homeland security related
contaminants. Because the WSTB is made of previously used drinking water distribution system
pipes, research can be conducted under conditions similar to those in a real drinking water system.
EPA led the experiments described in this study with technical support from CB&I Federal
Services LLC (CB&I) under contract. Testing and analyses described in this report were
conducted by CB&I in accordance with the Quality Assurance Project Plan (QAPP) (Appendix
A). EPA and CB&I personnel conducted two experiments:
• August 2015: Four mobile disinfection technologies were tested for their ability to disinfect
large volumes of biologically contaminated "dirty" water from the WSTB. Bacillus
globigii spores, a non-pathogenic surrogate for pathogenic B. anthracis, acted as the
biological contaminant. The four technologies evaluated included: (1) Hayward® Saline
C™ 6.0 Chlorination System (Elizabeth, NJ), (2) Advanced Oxidation Process (AOP)
Ultraviolet (UV)-Ozone System, (3) Solstreme™ UV System (Cincinnati, OH), and (4)
WaterStep Chlorinator (Louisville, KY).
• September 2015: The WSTB pipe was contaminated with Bakken crude oil, and
decontamination was performed using flushing with clean water and addition of a
surfactant (SURFONIC® DOS-75PG, Huntsman Corporation, The Woodlands, TX).
1.1 WS TB Description and Setup
The WSTB consists primarily of an 8-inch (20 cm) diameter drinking water pipe oriented in the
shape of a small drinking water distribution system. The WSTB contains ports for simulating
water demands from service connections and a 15-foot (5 m) removable coupon section designed
to sample the pipe interior. Figure 1 schematically depicts the main features of the WSTB.
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Legend
FM
PG
IP1
IP2
ex
H
\X
—3
s
r^j
Flow Meter
Pressure Gauge
Instrument Panel 1 (Upstream, Cellular)
Instrument Panel 2 (Downstream, Radio)
Valve, Open
Valve, Closed
Valve, Partly Open
Fire Hydrant
Flushing Hydrant
Blind Flange
Pressure Reducing Valve
Check Valve/Backflow Preventer
Service Connector (Closed)
Existing Fire Hydrant
Fire Hose
Start of WSTB
©-
Injection Port Hxl—
Not to Scale
(PGHXl—
15-ft Coupon Section
—CXh
T
-tXH
Bulk Water Sample Tap
-txa—
Drinking Water
from
INL Pumphouse
Parking
Area
Drainage
Ditch
Figure 1. Schematic overview of Water Security Test Bed.
Figure 2 shows the aerial view of the WSTB. The lower right corner shows the upstream and
system inlet; the upper left corner shows the lagoon.
Lagoon
Downstream Sensors
WSTB End
WSTB Start
Upstream Sensor and Injection
Figure 2. Aerial view of the Water Security Test Bed.
As depicted in Figure 1, drinking water was supplied to the WSTB through an existing fire hydrant.
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The drinking water was chlorinated ground water that also supplied the surrounding INL facilities.
The WSTB incorporates approximately 448 ft (137 m) of 8 inch (20 cm) diameter cement-lined
pipe. The 8 inch (20 cm) pipe system is constructed directly over the lined drainage ditch for
spill/leak containment (as shown in Figure 2). The total volume of the WSTB is estimated to be
-1,150 gallons (4,353 L). The valve near the end of WSTB along with the flow meter (shown in
Figure 3) was used to regulate and maintain flow.
Figure 3. Water Security Test Bed system flow regulator.
The water from the WSTB system is discharged to a lagoon (Figure 4) which has a water storage
capacity of 28,000 gallons (105,980 L).
North
Figure 4. Water Security Test Bed discharge lagoon.
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Water from this lagoon was used for the studies on four disinfection technologies to determine
their ability to treat large volumes of biologically contaminated water. Figure 5 shows a schematic
layout (not to scale) of the test setup for the four large volume water treatment technologies. The
four technologies used were EPA's Advanced Oxidation Process (AOP) trailer unit, the Solstreme
UV system, the WaterStep chlorinator and the Hayward chlorinator. These devices and
experimental protocols are described further in section 2.0.
WaterStep
Chlorinator &
Bladder Tank
AOP
Unit
Wort
Tent
Hayward
Chlorinator
B. globigii Mixing
Bladder Tank
Solstreme T
UV System
Solstreme Effluent
BladderTank
N
Lagoon
Top Berm
{42' * 80')
Location
#3
O
Location
#4
Location
#2
O -
Location
#1
O
o
Submersible Supply,''Mixing Pump Q
Lagoon
Influent
Figure 5. Schematic layout for large volume water treatment technologies testing.
The crude oil experiments used a positive displacement pump to inject the prepared stock
contaminant (i.e., subnatant representing the miscible portion of the crude oil) at the beginning of
the 448 ft (137 m) WSTB system. The stock was prepared in accordance to the procedure described
in the QAPP (Appendix A). Additional information is also presented later in this report. Figure 6
shows the crude oil injection setup.
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Figure 6. Prepared crude oil subnatant for Water Security Test Bed injection.
The bulk water samples (BWSs) and coupon samples were taken from the 15-foot (5 m) polyvinyl
chloride (PVC) pipe-segment designed and fabricated to contain 10 sets of duplicate removable
coupons (totaling 20 coupons) made from cement-lined pipe used to construct the rest of the
WSTB. The coupons allow for the measurement any contaminant persistence on pipe material,
and the effectiveness of decontamination. Figure 7 shows a portion of the 15-foot (5 m) PVC
coupon section.
Coupons
Figure 7. Removable 15-foot PVC coupon section.
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The pipe material for the 20 small coupons (22/32 of an inch [1.8 cm] in diameter and 0.371 square
inches [2.4 square centimeters] in area) were cut from the cement mortar-lined iron pipe obtained
from INL and set into threaded plugs that were inserted into the PVC-coupon section of the pipe.
Fi gure 8 shows a pi cture of the threaded coupon that was inserted into the pipe main. The twenty
coupons were individually numbered CP-0/CP-0D through CP-9/CP-9D in duplicate (CP =
coupon, D = duplicate).
Figure 8. Extracted pipe coupon.
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2.0 Description of Experiments
2.1 Disinfection of Large Water Volumes
This experiment was designed to assess the ability of a portable disinfection unit to treat a large
volume of water containing B. g/obigii spores. Water in the lagoon contained dirt and sediment
from the surrounding area, as well as algae. The dirt and algal growth created disinfectant demand
in the water and rendered the water "dirty." The following four treatment technologies were
evaluated for their ability to treat dirty water from the lagoon: (1) Hayward Saline C™ 6.0
Chlorination System, (2) AOP UV-Ozone System, (3) Solstreme™ UV System, and (4) WaterStep
Chlorinator. The test equipment was placed adjacent to the WSTB lagoon. A schematic layout of
the tested systems was presented previously in Figure 5.
The effectiveness of individual treatment technologies was evaluated by sampling water
containing B. globigii spores before it entered the individual treatment technology or before
treatment began, and then after disinfection to determine the treatment effectiveness. The
concentration of spores in the influent (or before treatment began) was then compared to the
concentration in the effluent (after treatment). For experiments with the AOP trailer and
Solstreme, water was pumped from the lagoon into a 2,000 gallon (7,571 L) bladder tank system
that contained a mixing pump to provide a continuous stream of B. globigii spores in contaminated
water (Figure 9).
Bacillus globigii Mixing Pump
Feed Lines to
Mix Ports
Advanced Oxidation Process and
Solstreme Feed Pump
Figure 9. Inlet bladder tank and mixing.
Figures 10 shows a schematic depiction of how the mixing pump was connected to the bladder to
perform mixing along with the inlet and outlet ports.
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Mixing
Port
Inlet Port from
Lagoon
Mixing
Port
Mixing Bladder
(10.5' x 14.5')
Outlet Port to
Mixing Pump
Mixing AOP and
Pump Solstrerne Pump
Figure 10. Schematic depiction of the inlet bladder tank mixing process.
For the AOP trailer and Solstreme unit, a target inlet concentration of greater than 106 spores/100
mL (or 104 spores/mL) was prepared using the inlet bladder tank and mixing pump shown in Figure
9. The water was then pumped through the selected treatment unit. Each unit was tested for 5.5
hours. Pre-treatment and post-treatment water samples fori?, globigii analysis were collected at
the same time.
For the WaterStep, a 1,250 gallon (4,732 L) vendor supplied bladder tank was spiked with B.
globigii spores (106 spores/100 mL or 104 spores/mL), and then filled with lagoon water. The
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bladder tank was manually agitated by pushing on its side to mix the spores. Manual agitation
took place approximately every 15 minutes throughout the experiments. Before disinfection, the
bladder tank was sampled to determine the initial spore density, and then the chlorination started.
Subsequent samples were considered as treated, or disinfected, water samples.
As in the case of the WaterStep unit, the Hayward Saline C™ 6.0 Chlorination System also did
not use the inlet/outlet bladder tank system for operation. It is an in-situ type of treatment
technology where the salt used for generating the chlorine comes from the same contaminated
"pool" or source of water. The testing protocol for this treatment device took place in the lagoon
and is described in Section 2.1.4.
2.1.1 EPA AOP Trailer Testing
On August 17, 2015, the first large volume disinfection study using the EPA AOP system was
performed. The system setup is depicted in Figure 11, where it has been removed from its transport
trailer.
Ozone generator
(controller)
UV generator
(controller)
Speece Cone for
Ozone Diffusion
UV lamp and
Ozone generator
behind the
manifold
Figure 11. Advanced Oxidative Process System and influent/mixing bladder tank (black
object to the right of the system).
The AOP system was custom-built at the EPA Test and Evaluation (T&E) Facility in Cincinnati,
Ohio. The AOP system consists of four major components: the Power Prep 66 (air preparation
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unit), CD2000 (ozone production unit), Trojan UVMax (UV generation unit), and the Aquionics
UV (UV generation unit). During this study, the AOP system was operated with the CD2000
ozone generator and the Aquionics UV system operated in series. The Trojan UVMax unit was
not used during this study. UV light and ozone act individually as disinfectants, but photolysis of
ozone by UV light can lead to the formation of highly reactive hydroxyl radicals (*OH) through
multiple mechanisms. The *OH is a short lived but potentially potent disinfectant.
The bulk water samples (BWSs) for B. globigii concentrations (BWS-0 through BWS-6) were
collected from the inlet and outlet of the system simultaneously using the grab sampling technique
in 100-mL sterile sample bottles with a 10 mg sodium thiosulfate tablet. The BWS sampling ports
at both inlet and outlet of the system were opened and the water was drained for 15 seconds prior
to collection of the sample. The AOP system was powered by a portable generator that had to be
shut down for refueling twice during the 6 hour sampling period.
2.1.2 So/streme ™ UV System Testing
On August 18, 2015, the large volume disinfection study using both Solstreme™ UV system, was
performed. The Solstreme™ UV system setup is depicted in Figure 12.
Electrodeless Lamp/Flowcell
Water Inlet
Water Outlet
Figure 12. Solstreme™ UV System and effluent bladder tank (blue object in front of the
UV system).
The Solstreme™ UV system uses a patented microwave-actuated electrodeless lamp technology
to provide UV disinfection. The microwave is generated using a focused magnetron which
activates UV energy inside the patented-electrodeless lamp. A typical UV lamp uses an electrical
current passing through electrodes to excite the lamp to produce UV light; the Solstreme UV lamp
uses radio frequency (RF) energy to induce the lamp to produce UV light through a quartz glass
envelope. The electrodeless lamps can be run at higher power levels allowing it to produce greater
12
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amounts of UV light than its counterpart electrode-based lamps. The National Sanitation
Foundation (NSF) Standard 55 "Class A" Rated UV systems are required to operate at a minimum
UV light dosage of 40 mJ/cm2 (or 40 mW-sec/cm2) (USEPA, 2003). The Solstreme system in
comparison is expected to generate a higher level of UV dose compared to an equi valent electrode-
based UV lamp. The manufacturer expects the Solstreme system operating under optimal
conditions can deliver an equivalent total dosage of up to 1,700 mW-sec/cm2 (NeCamp, 2008).
However, the design of the instrument made it impossible to verify the dosage.
Similar to the AOP System, the BWS for B. globigii concentrations (BWS-0 through BWS-6) were
collected from the inlet and outlet of the system simultaneously using the grab sampling technique
in 100-mL sterile sample bottles with a 10 mg sodium thiosulfate tablet. The BWS sampling ports
at both inlet and outlet of the system were opened, and the water was drained for 15 seconds prior
to collection of the sample.
2.1.3 WaterStep Chlorinator Testing
On August 18, 2015, concurrent with the Solstreme™ UV System the WaterStep Chlorinator was
tested. The system setup is depicted in Figure 13.
Battery
WaterStep
Chlorinator
Water Inlet
Bacillus globigii
injection inlet/outlet port
Figure 13. WaterStep Chlorinator System bladder tanks (dark blue).
The WaterStep (WaterStep, 2013) system uses electricity and sodium chloride (table salt) to
generate chlorine to disinfect water. This occurs by applying a potential to a cell that contains
electrolytic plates (an anode and cathode). Chlorine gas is formed at the anode, which forms free
chlorine when dissolved in water ("free chlorine" is a mixture of hypochlorous acid and
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hypochlorite ion, depending on pH). This free chlorine migrates into a 1,250 gallon (4,732 L)
bladder tank where it can disinfect the contained water. The system was operated using a 12 volt
DC battery on a cart (as shown in the middle of Figure 13). The battery was placed on a trickle
charger to maintain full charge for operational stability during the testing. The WaterStep Chlorine
generator setup is depicted on Figure 14.
| Chlorine gas (Venturi)
Salt water addition
Chlorine generator
Chlorinated water outlet
UHAt*
Water inlet
Figure 14. WaterStep Chlorine Generator components.
Note: image is from a previous experiment. It is presented here for illustration purposes
only.
BWSs for B. globigii concentrations (BWS-0 through BWS-5) were collected from the same
sampling port that served as both inlet/outlet of the system using the grab sampling technique in
100-mL sterile sample bottles with a 10 mg sodium thiosulfate tablet. The BWS sampling port
was opened and the water was drained for 15 seconds prior to collection of the sample.
2.1.4 Hay ward Saline C™ 6.0 Chlorination System Testing
The Hay ward Saline C™ 6.0 Chlorination System is an in-situ type of treatment technology, and
it was operated using the lagoon as the "pool" or source of water. The Hay ward unit generates free
chlorine using the same principle as the WaterStep, with free chlorine being generated from
dissolved salt in water. A potential is applied to a cell that contains electrolytic plates (an anode
and cathode). Chlorine gas is formed at the anode, which forms free chlorine when dissolved in
water (a mixture of hypochlorous acid and hypochlorite ion, depending on pH). Flow moves
through the chlorine generating cell, and dissolved free chlorine leaves the cell in the effluent
(Hayward, 2013). The Hayward system as configured during the testing is shown in Figure 15.
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Output Selector/Display
Electrolytic Cell
Hayward Effluent
•C MTMT10K MiagH
FAILUUTOWUflM^B
INAilY Oi i*AJ* ¦
. WBA* FTf «•
.00 Norms*" **23
.VESSBMAVI^*^*
.sjnrrowAU.P'UJjJB
,WArTowmKiTi»M
WK« #1*1*1*^00
. . •.¦¦¦' H
sss^B
Hayward Influent/Flow Sensor
Figure 15. Hayward Chlorine Generator,
The manufacturer recommends 3,500 mg/L to 5,000 mg/L salt to be added to the pool for
operations. On August 18, 2015 (the day before this system was tested), the lagoon was mostly
drained and approximately 126 lbs (57 kg) of salt was added to the lagoon near the water inlet
from the WSTB pipe. The water from the WSTB was then run at 5 gpm (19 L/min) for
approximately 16 hours (releasing 4,800 gallons [18,170 L]) to mix the undrained water with and
dissolve the salt in the lagoon. In total, it is estimated that approximately 5,000 gallons (18,927
L) of water was in the lagoon after filling. The overall Hayward system setup is depicted in Figure
16.
15
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Figure 16. Havward Saline C™ 6.0 Chlorination System setup on a table.
On August 19, 2015, the large volume disinfection study using the Hayward system was initiated.
At 9:10 AM, 17 L of B. globigii stock solution were added to the lagoon to reach a target
concentration of greater than 106 spores/100 mL (or 104 spores/mL) in the lagoon. Figure 17 shows
the addition of B. globigii to the lagoon simultaneously at multiple locations.
Recirculation Pump
Lagoon Inlet
Figure 17. Contamination of the lagoon with Bacillus globigii
A sump pump with a distribution manifold was used to recirculate the lagoon water and to provide
mixing for the B. globigii stock in the lagoon (shown in Figure 18).
16
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Hayward Chlorinator
B. globigii addition to Lagoon
Recirculation
Pump
Figure 18. Lagoon Bacillus globigii recirculation/mixing pump.
At 10:00 AM, the initial, pre-disinfection B. globigii samples were collected from the four corner
locations around the lagoon where water was pooled. Thereafter, the Hayward system was started.
The amount of chlorine generated (i.e., output) of the system varies depending upon available salt
in the water flowing through the system. The output is adjustable from 0 to 100% of the systems
rated capacity and is displayed as % output on the display.
During chlorination of pool water under typical usage of the system, the amount of chlorine
generated is automatically controlled based on the salt levels and automated measurement of
chlorine levels in the water using a chemical controller feedback system. The tested field system
was not equipped with a chemical feedback controller and was instead operated in manual mode.
In manual mode, when the available salt falls below the level required for the set output level in
%, the system stops generating chlorine and the LCD display flashes "LG SALT" (Hayward,
2013). A low salt alarm indicator came on as soon as the system was started at 100%. An additional
bag of salt was added to bring the total salt added to -154 lbs (70 kg) of salt. However, the low
salt alarm remained. In accordance with the vendor manual (Hayward, 2013), the system was reset,
and the output selector was lowered to 50% and stepped up in increments of to a final setting of
60% setting which was found to be stable for operation. This setting was used to run the system
for the remainder of the test.
The system was operated at the manufacturer recommended rate of 40 gpm (18 L/min)) flow
through the electrolytic cell that produced chlorine, and the chlorinated water was pumped back to
the lagoon. Chlorine levels coming out of the Hayward chlorinator and the lagoon were monitored
throughout the day. The free chlorine coming out of the Hayward chlorination cell was measured
to be in the range of 4.3 mg/L. The chlorine level in the lagoon crept up slowly starting at 0.2 mg/L
at noon, 0.61 at 1:00 PM, 1.07 at 3:00 PM and 1.19 at 3:30 PM. Based on the rate at which the
17
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chlorine level was increasing, it was decided that the unit would be left to run unattended overnight.
The BWSs for B. globigii effluent concentrations (BWS-0 through BWS-5) were collected from
the lagoon periodically throughout the day using the grab sampling technique in 100 mL sterile
sample bottles with a 10 mg sodium thiosulfate tablet. The following day on August 20, 2015, at
8:30 AM, the final BWS sample was collected and the chlorine from the lagoon was measured to
be 12.2 mg/L. At time of arrival at the site, it was noted that while the Hayward pump was still
operating at 40 gpm (151.4 L/min), the low salt alarm was active. It is unknown when the salt
activation would have stopped. However, the measured value of 12.2 mg/L of chlorine was
sufficient to achieve inactivation B. globigii spores in the lagoon.
2.2 Crude Oil Contamination/Decontamination Tests
These experiments involved contamination of the WSTB using crude oil and the subsequent
decontamination of WSTB using flushing at 15 gpm (56.8 L/min) followed by an injection of a
surfactant. The contamination/decontamination experiment consisted of the following main steps:
• Step 1 - Pipe conditioning (cultivation of biofilm)
• Step 2 - Instrumentation panel setup, effluent oil capture treatment train, and background
sampling
• Step 3 - Preparation of contaminant stock (subnatant, miscible portion of Crude Oil) and
injection into the WSTB
• Step 4 - Preparation of decontaminant and decontamination using flushing along with a
surfactant for crude oil removal,
• Step 5 - Post-decontamination flushing, reconditioning, and monitoring
Step 1 - Pipe conditioning (cultivation of biofilm)
Biofilm cultivation and pipe conditioning occurred by passing INL tap water through the WSTB
continuously starting May 2015 until the late-September/early October 2015 contamination and
decontamination testing. After initial flush to remove any debris at startup in May 2015, the flow
rate was set at 2.5 gpm (9.5 L/min) during the conditioning period with a total discharge of 25,200
gallons (95,392 L) per week to the lagoon. This flow rate allowed for weekly trucking and disposal
of the accumulated discharge.
Step 2 - Instrumentation panel setup, effluent oil capture treatment train, and background
sampling
Instrument Panel Setup - The initial upstream/downstream instrument panel setup was completed
in May 2015. In August 2015, a Turner Designs Hydrocarbon device (Model TD1000C), which
measures oil in water was installed at the downstream sensor location (shown in Figure 19). The
TD1000C is an online "hydrocarbon in water" monitor that detects aromatic hydrocarbons in water
using fluorometry principles in combination with a proprietary flow cell (Turner, 2009).
The WSTB upstream/downstream instrumentation panels are also equipped with online sensors
that continuously measure two basic water quality parameters: free chlorine and total organic
carbon (TOC). Each of the instrumentation panels contains one Hach® CL-17 chlorine analyzer
(Loveland, CO) and one RealTech M4000 TOC analyzer. The Hach CL-17 chlorine analyzer uses
colorimetric N,N-diethyl-phenylenediamine (DPD) chemistry to monitor water continuously for
18
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free chlorine (Hach, 2014). The RealTech M4000 uses the UV 254 nanometer wavelength (i.e.,
UV254) absorption measurement for determining the TOC content (RealTech, undated). UV254
instruments are often used as an inexpensive indicator of TOC in water. UV254 measurements are
known to have some bias towards aromatic organics; however, they are relatively inexpensive to
maintain and operate when compared to the traditional UV-persulfate based TOC analyzers.
CZ3WIEGMANN
Figure 19. Turner TD1000C Oil in Water Monitor.
Effluent Oil Capture Treatment Train - A carbon-based effluent oil capture treatment train was
designed and implemented at the downstream location of the WSTB. The dual-drum treatment
train capture (adsorbent) media contained a media mix of 30% TIGG oil removal media and 70%
of TIGG 5DC 1240 NFS coconut-based activated carbon. Only one 55 gallon (208 L) drum of
carbon was required to reduce the volatile organic compounds (VOC) of concern (benzene) to a
concentration to below the targeted drinking water MCL values. Additional drums were added to
the treatment train to accommodate operating flow rates, operating pressure, and increase the
empty-bed contact time. In total, the effluent oil capture treatment train was comprised of four
drums. Two drums were connected in series and the flow split evenly between each set of two-
drums. During the surfactant decontamination step, the first drum in each set of drums was taken
offline. This was done to prevent the potential release of the captured oil in the first drum. Figure
20 shows the overall oil capture treatment train with cam-lock connects to put individual drums in
series and/or to take them offline as needed.
19
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Figure 20. Effluent oil capture treatment train.
Background Sampling - Prior to initializing the contamination Step (Step 3), on September 21,
2015 at 8:30 AM, bulk water samples (BWS-0) and Coupon Samples (CP-0 and CP-OD) were
collected to establish background levels. The BWS-0 sample was analyzed for background crude
oil components such as VOCs, benzene, toluene, ethylbenzene, and xylene (BTEX), gasoline range
organics (GRO), diesel range organics (DRO), and oil range organics (ORO). The coupon sample
(CP-OD) was analyzed for biofilm density using heterotrophic plate count (HPC). And the CP-0
was analyzed for crude oil components along with the BWS-0 sample. Free chlorine (CL-F-#) was
also measured periodically during the testing. All sampling activities related to crude oil testing
are summarized in Table 1 and analytical methods are described in the QAPP (Appendix A).
Step 3 - Preparation of contaminant stock (miscible portion of Crude Oil) and injection into
the WSTB
Preparation of Crude Oil Contaminant Stock - The crude oil for this study was obtained from
Marathon Petroleum Corporation. The oil procured was from the Bakken shale in North Dakota.
On September 20, 2015 at 16:05 PM, a measured amount of crude oil (2.5 liters) and Snake River
water (22.5 liters) was mixed in a 25 liter carboy (shown in Figure 21). The detailed preparation
methodology is documented in the QAPP (Appendix A).
20
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Figure 21. Crude oil injection stock preparation.
On September 21, 2015, at 8:40 AM, 20 liters of the mixed water was drawn from the bottom of
the carboy spigot into a 5 gallon (19 L) bucket for injection.
Prior to the contamination step, the Effluent Oil Capture Treatment Train was connected to the
WSTB, and the flowrate was increased to 15 gpm (56.8 L/min). However, the increase in flow
resulted in an increase in line pressure into the carbon drums above the levels recommended by
the manufacturer. Therefore, the WSTB system flowrate was reduced to 13 gpm (49.2 L/min)
during the contamination/decontamination step and evenly split between the two 2-drum effluent
oil capture treatment trains.
Contamination Test Protocol - On September 21, 2015, at 9:03 AM, the crude oil suspension was
introduced into the WSTB using a positive displacement pump. As indicated previously in Step
2, the oil capture system was designed to contain any crude oil component from entering the
lagoon. Once flushing and decontamination activities were completed, the unit was disconnected.
During the injection, initially the WSTB was operated at 15 gpm (56.8 L/min) (adjusted to 13 gpm
[49.2 L/min] as mentioned previously) for approximately 1 hour. In accordance with the QAPP
(Appendix A), the injection duration was one hour so that there was a contact of one hour after
the bolus of crude oil suspension reached the coupon section of the pipe. All sampling activities
related to crude oil testing are summarized in Table 1.
Step 4 - Preparation of decontaininant and decontamination using flushing along with a
21
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surfactant for crude oil removal
Preparation of Decontaminant Asent Stock - The surfactant Sulfonic TDA-6 was identified as
the decontaminant of choice based on pilot-scale decontamination experiments at EPA's Test and
Evaluation (T&E) Facility (U.S. EPA, 2008). However, CB&I's technical discussions with the
sales/technical representatives of the Huntsman Chemical Corporation (conducted over several
weeks) led to the identification of SURFONIC® DOS-75PG as a better choice. Specifically,
because this surfactant is derived from a naturally occurring material and is non-toxic to the marine
environment when released. Additionally, SURFONIC® DOS-75PG surfactant has been shown
to undergo 90% to 98% biodegradation in 11 to 17 days (Appendix C - Technical Bulletin
SURFONIC® DOS-75PG Surfactant).
The previous flushing tests using the Sulfonic TDA-6 were performed using a 5% Surfonic TDA-
6 solution (U.S. EPA, 2008). The technical bulletin (Appendix C) property specifications also
suggest using the product as a 5% solution. At the time of testing, Huntsman was only able to ship
3 gallons (11.3 L) of the surfactant. For the one-hour flushing event, a flow rate of 15 gpm (56.8
L/min) would generate 900 gallons (3,407 L) of water. If the entire available stock of the surfactant
was used, it would only result in a 0.3% (3 gallon/900 gallons [11.3 L/3,407 L]) solution for
cleansing. Therefore, for the purposes of the decontamination step, the surfactant was pumped
through the pipes at the rate of 0.05 gpm (0.19 L/min) without dilution for one hour, which used
up the available surfactant stock.
Decontamination Test Protocol - Once the crude oil injection was stopped, the WSTB was
flushed for 2 hours at 13 gpm (49.2 L/min) between 10:00 AM and 12:00 PM. This flushing
without surfactant was conducted to generate data on whether flushing alone removes crude oil
subnatant from the water and pipe surfaces. Following the 2 hour flush at 12:00 PM, an attempt
was made to pump the undiluted surfactant at the aforementioned rate of 0.05 gpm (0.19 L/min)
using a positive displacement gear pump. This was not successful due to the high viscosity of the
surfactant.
An alternate method of surfactant introduction was devised by isolating the valves close to the
injection area and temporarily depressurizing the injection pipe section to manually introduce the
surfactant in individual pulses every 15 minutes (three times). This pulsed introduction of
surfactant was performed between 1:00 PM and 1:45 PM. The surfactant had to be diluted in 50
liters of water to allow for pouring through a funnel into the depressurized pipe section with the 2
inch connection. A total of 2 gallons (7.6 L) of the surfactant was introduced during this process.
The plan to hold the surfactant stagnant in the pipe overnight was abandoned because of the pulsed
injection. The water flow out of the WSTB was reduced to 5.0 gpm (19 L/min) at 4:15 PM to
reduce the volume of water going to the lagoon overnight. All sampling activities related to crude
oil testing are summarized in Table 1.
Step 5 - Post-decontamination flushing, reconditioning, and monitoring
Additional BWSs and CPs were collected. The sampling activities are described in Table 1.
Table 1. Crude Oil Contamination/Decontamination Related Sampling Activity
22
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Sample ID
Sample Description
Estimated Timeline &
System Flow
Step 2 - Background
BWS-0
(Control)
• Collected sample at 8:30 AM prior to
injection of crude oil.
September 21, 2015
Flow at 2.5 gpm (9.5 L/min)
CP-0 and CP-
OD
• Collect at the same time as BWS-0
• After sampling the flow was increased. At
9:05 AM the flow was found to be at 11
gpm (4.16 L/min). The pressure drop
across the Carbon Treatment system was
too high. The pressure regulators in line
with the Carbon system were adjusted and
a flow upwards between 13 (49.2 L/min)
and 15 gpm (56.9 L/min) was achieved.
September 21, 2015
Initial Flow at 2.5 gpm (9.5
L/min) then raised for
injection scenario.
Step 3 - Injection (Start 9:03 AM - Stop 10:00 AM - Travel Time ~ 1 hour)
BWS-1,
BWS-1D, CP-
1 and CP-ID
• Collected the post 15-minute sample later
to accommodate for lower flow at 10:25
AM to ensure that the crude oil reached the
coupon section.
September 21, 2015
Flow at 15 gpm (56.9
L/min)
BWS-2 and
CP-2, CP-2D
• Collected the 45-minute at 10:55 AM.
September 21, 2015
Flow at 15 gpm (56.9
L/min)
Step 4 - Flushing (10:00 AM - 12:00 PM) / Surfactant Decontamination initial pumped
injection attempt at 12:00 PM and then manual introduction between 1:00 and 1:45 PM
BWS-3, CP-3
and CP-3D
• Collected within 15 minutes of the
introduction of surfactant (i.e., 12:15 PM).
• Allow surfactant to reach the end of the
pipe after the manual introduction was
completed - estimate 60 minutes.
September 21, 2015
Flow at 15 gpm (56.9
L/min)
BWS-4, CP-4
and CP-4D
• Collected the 1-hour sample after the
surfactant injection was completed at 2:45
PM.
September 21, 2015
Flow at 15 gpm (56.9
L/min)
BWS-5,
BWS-5D, CP-
5, and CP-5D
• Collected at the 2-hour BWS sample at
3:30 PM and CP samples at 3:45 PM. The
3-hour sample had to be pushed to the next
day because of FedEx® overnight shipping
deadline. At 4:15 PM the flow was turned
down to 5 gpm (19 L/min) to prevent
lagoon overflow at night time.
September 21, 2015
Flow at 15 gpm (56.9
L/min) at the end of the day
set to 5 gpm (19 L/min)
Step 5 - Post Decontamination Flushing and Monitoring
BWS-6, CP-6
and CP-6D
• Collected sample at 9:00 AM.
September 22, 2015
Flow at 5 gpm (19 L/min)
BWS-7
• Collected sample at 12:00 PM.
September 22, 2015
Flow at 5 gpm (19 L/min)
BWS-8
• Collected sample at 3:00 PM.
September 22, 2015
23
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Sample ID
Sample Description
Estimated Timeline &
System Flow
Flow at 5 gpm (19 L/min)
BWS-9, CP-7,
and CP-7D
• Collected sample at 9:45 AM.
September 23, 2015
Flow 5 gpm (19 L/min)
BWS-10, CP-
8, CP-8D
• Collected sample at 9:45 AM.
September 24, 2015
Flow at 5 gpm (19 L/min)
BWS-11, CP-
9, CP-9D
• Collected sample at 9:45 AM.
September 25, 2015
Flow at 5 gpm (19 L/min)
BWS-12
• INL collected sample at 9:45 AM (7 days
after the start of reconditioning).
September 30, 2015
Flow at 5 gpm (19 L/min)
BWS-13
• INL collected sample at 9:45 AM (14 days
after the start of reconditioning).
October 7, 2015
Flow at 5 gpm (19 L/min)
BWS, bulk water sample; CP, coupon; D, duplicate; 1, 2, 3, etc., sequential sample number; gpm, gallons per minute;
L/min, liters per minute; INL, Idaho National Laboratory
After completion, the WSTB blank coupons were left in place for shutdown and winter storage.
24
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3.0 Analysis of Test Results
3.1 Disinfection of Large Water Volumes
The four mobile disinfection units were tested for their ability to disinfection B. globigii spores in
water from the WSTB lagoon. Data analyses and results from the disinfection experiments are
presented in the following sections. Summary descriptions of the disinfection units and
experimental design are included for clarity and context.
3.1.1 EPA AOP Trailer Unit Testing
Water flowing through the EPA AOP trailer unit was subjected to treatment with UV light and
ozone. Both UV light and ozone are disinfectants, but irradiation of ozone with UV light can lead
to the formation of *OH (hydroxyl) radicals, which are short lived but potentially potent biocides.
Before the treatment experiments began, two thousand gallons of water from the WSTB lagoon
containing naturally occurring dirt and algae was pumped into the influent bladder tank. B. globigii
spores were mixed into this volume and were kept well dispersed in the influent bladder tank using
a recirculation pump (see section 2.1 for more detail). This served as the influent feed for the AOP
trailer. Treated effluent from the AOP trailer was stored in another 2,000 gallon (7,571 L) bladder
tank until experiments concluded. The trailer was operated for 5.5 hours at a flowrate of 5 gpm
(19 L/min), with samples being taken every hour, except for the last sample.
Figure 22 shows the AOP trailer influent spore density (blue bars) and the density of spores in the
treated effluent (orange bars). Influent and effluent samples were taken simultaneously, so the
difference between the bars at each time point represents the amount of spore inactivation taking
place, or log reduction (green line) at that point in time. The influent B. globigii density is stable
throughout the treatment periods at approximately 2.3xlO5 colony forming units (cfu)/ml. This
indicates that the recirculating pump attached to the 2,000 gallon (7,571 L) influent bladder tank
kept the spores well mixed throughout the course of the experiment.
Effluent spore densities in the treated water varied over the course of the treatment experiment.
On average, a 4-log reduction was observed between the AOP trailer influent and effluent.
However, individual log reduction values fluctuated from a high of 5 at 120 and 240 minutes of
operation, to a low of 1.5 at 300 minutes. This inconsistent disinfection may be related to a number
of factors such as: 1) Changing lagoon temperature (from 15°C to 25°C) affecting ozone diffusion
into the water and ozone generator output; 2) changing turbidity of the influent water with
temperature and mixing in the tank; 3) inconsistent UV lamp output with temperature; 4) hours of
operation; 5) unknown factors related to other site specific conditions and the unit being removed
from the trailer. Also, the AOP system was powered by a portable generator that had to be shut
down for refueling after the 240 minute sampling point, which may have negatively impacted the
performance. However, a 5-log reduction in spores does appear possible. The factors mentioned
above that could have influenced disinfection performance were not explored in-depth, and their
impact requires further investigation.
25
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BBH
0 60 120 180 240 300 330
Time (min)
Mean Influent Spore Density (CFU/mL) Mean Effluent Spore Density (CFU/mL)
Log Reduction
Figure 22. Treatment performance of the Advanced Oxidation Process trailer over the
course of 5.5 hrs. Blue and orange bars represent the mean spore density in the AOP
trailer influent and effluent, respectively. The green line represents log reduction, or the
amount of inactivation occurring at each sampling point. Error bars represent the range
between duplicate samples taken at each time point.
Table 2 contains a summary of AOP technology-specific equipment observations recorded during
the treatment experiments and considerations for similar field deployments. The terms Low,
Medium and High are the opinions of the authors of this study, and are based on their experience
operating the equipment in the field. The text in the table is meant to support these opinions, and
they are specific to this piece of equipment. Other equipment operators may come to different
conclusions under different conditions.
Table 2. EPA Advanced Oxidation Process Trailer Technology-Specific Considerations
and Observations*
Technology
Considerations
Rating and Comments
Market Availability
Low. Originally custom designed by EPA for a remediation project to
provide advanced oxidation with UV and Ozone. A trailer-mounted
system that was re-purposed and tested for disinfection. One ozonation
process component (Speece Cone diffuser) not commercially available.
Other UV and ozonation process components commercially available.
Capital Cost
High (estimated > $40,000). Custom design, process components,
plumbing, trailer, etc.
Shipment to Site
Medium. Requires a tow vehicle to pull the trailer to site. Trailer may
require State inspection and driver that meets the training requirements
for towing the vehicle.
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Technology
Considerations
Rating and Comments
Setup
Considerations
Medium. Requires 110 and 220 Volt AC electric or generator, the
plumbing connections to the process units need to be reassembled on
site. The Ozonator cone setup requires 2-3 persons onsite to assemble.
Operational
Considerations
Medium. Requires operation of valves to remove air from the process
units, valve adjustment to meet pressure and flow requirements. Some
of the vented air may contain contaminated droplets of water that need
to be contained or recirculated back through the system. There is excess
ozone emissions from process unit that needs to be destroyed or vented.
The catalytic destruction unit was un-operable the unit had to be vented.
Flow rate needs to be less than 5 gpm (19 L/min).
Maintenance and
Consumables
Low. UV lamp replacement, pump repair when needed. Dual voltage
electric supply (see setup consideration).
Result Summary
Under the tested conditions, an average of 4-log removal of B. globigii
was observed in this flow through type operation (removal varied from
1.5 to 5 log). Improved understanding of the EPA AOP system
performance may improve the consistency of disinfection.
* Mention of trade names or commercial products does not constitute endorsement or recommendation for use of a specific product.
3.1.2 So/streme ™ U V System Testing
The Solstreme unit disinfects water through UV light only. Disinfection experiments were
performed in the same manner as for the EPA AOP trailer discussed in Section 3.1.1. Figure 18
shows the Solstreme influent spore density (blue bars) and the density of spores in the treated
effluent (orange bars). Influent and effluent samples were taken simultaneously, so the difference
between the bars at each time point represents the amount of spore inactivation taking place, or
log reduction (green line) at that point in time. Like the AOP trailer experiments, influent spore
density was over the course of the experiment at approximately 1.6xl05 cfu/ml. This was a
positive finding since a consistent influent concentration was desired over the course of the
experiment.
The effluent spore densities from the Solstreme consistently decrease as the experiment
progressed. A corresponding increase in spore log reduction over the course of the experiment
was also observed. After discussing this finding with the Solstreme manufacturer, a possible
reason for this increase in disinfection performance emerged. The Solstreme UV output is higher
at higher temperature. Over the course of the experimental period (from early morning to mid-
afternoon), the air and lagoon water temperature at the test site increased from 12° to 28°C and
15° to 25°C, respectively. It should be noted that no free chlorine residual was detected in the
water.
Figure 23 shows the log reduction data from Figure 24 plotted against the output intensity from
the Solstreme device over the course of the experiment. The Solstreme output intensity is a
proprietary, unitless measure of the UV output. Typically, for an electrode-based UV bulb, the
intensity is measured in milli-watts per square centimeter (mW/cm2). However, the electrodeless
design of the Solstreme unit does not allow for direct conventional radiometer based UV intensity
measurements. Figure 24 provides an indirect measure of the UV intensity based on achievement
27
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of 3.5 to 4-1 og inactivation of B. globigii spores in lagoon water with —11 to 13 NTU turbidity (pH
of approximately 7.5). The increase in output intensity of the Solstreme in Figure 24 is perhaps
due to the increase in water temperature over the course of the experiment. In the future, it may
be beneficial to add a heating element to the Solstreme influent water line to bring water to a
temperature between 25° to 30°C. Increased disinfection may be due to hydroxyl radical formation
due to photolysis of the water with higher temperature. The influence of air and water temperature
on disinfection performance merit further investigation.
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Figure 24. Spore log reduction for Solstreme UV treatment vs. UV output intensity.
Solstreme output intensity is a proprietary, unitless measure of UV intensity. Both linear
and logarithmic best fit lines are shown.
Table 3 contains a summary of Solstreme technology-specific equipment observations recorded
during the treatment experiments and considerations for similar field deployments. The terms Low,
Medium and High are the opinions of the authors of this study, and are based on their experience
operating the equipment in the field. The text in the table is meant to support these opinions, and
they are specific to this piece of equipment. Other equipment operators may come to different
conclusions under different conditions.
Table 3. Solst
treme Technology-Specific Considerations and Observations*
Technology
Considerations
Rating and Comments
Market Availability
Medium. New startup company developed an innovative electrodeless
UV lamp design. Made upon order (http://www.solstreme.com/)
Capital Cost
Medium (estimate $15,000).
Shipment to Site
Low. Requires a custom-box (wooden crate or cardboard box with
contoured foam) and can be shipped via third party shipper to site. No
chemicals or hazardous materials to ship. Can be carried in a truck or a
personal vehicle to site.
Setup
Considerations
Low. Plug and play, needs 110 Volt AC electric. If water is turbid, a pre-
filter is recommended for optimal use. Temperature of the water (i.e.,
cold < 55°F) impacts operations. Comes with cam lock type connectors.
One person can set it up in the field.
Operational
Considerations
Low. High turbidity and cold water adversely affect the disinfection
process. It gets better results with water in the 70°F to 90°F temperature
range and low turbidity. If high disinfection is desired, a heat exchanger
may also be needed to regulate water temperature but this requires
further investigation. The cost of this heat exchanger would depend on
its size.
Maintenance and
Consumables
Low. If the processed water is turbid or contains certain dissolved
materials that stick to the quartz sleeve, the system (inside quartz sleeve)
will need to be cleaned frequently. Other than regular commercially
available cleaning agents, no other consumables are required. The UV
lamp is electrodeless microwave technology, expected by the
manufacturer to last more than 10 years. The quartz sleeve although
robust needs to be handled carefully while cleaning. A plunger type
device for cleaning the interior of the sleeve is recommended and gloves
should be used to prevent smudging of the outside surface.
Result Summary
Under the tested conditions, a 3.5-to 4-log removal of B. globigii was
observed in a flow through type operation during the experiment.
* Mention of trade names or commercial products does not constitute endorsement or recommendation for use of a specific product.
29
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3.1.3 Water Step Chlorinator Testing
The WaterStep chlorination system disinfects through generation and application of free chlorine.
Free chlorine was generated by electrolysis of sodium chloride (table salt). The WaterStep system
operates by applying a potential to a cell that contains electrolytic plates (an anode and cathode).
Chlorine gas is formed at the anode, which is channeled through a venturi tube to mix with process
water forming free chlorine when dissolved in water (a mixture of hypochlorous acid and
hypochlorite ion, depending on pH). This free chlorine migrates into a 1,250 gallon (4,732 L)
bladder tank where it can disinfect the contained water. Disinfection experiments with the
WaterStep were conducted by spiking the 1,250 gallon (4,732 L) tank with B. globigii spores,
filling with lagoon water, and then chlorinating. These experiments differ from those conducted
with the AOP trailer and Solstreme in that there is no continuous influent and effluent flow. There
is one contained volume of contaminated water that is exposed to free chlorine, which can disinfect
the B. globigii spores over time.
Figure 25 shows the increase in free chlorine concentration inside the WaterStep bladder tank over
the course of the experiments, and the subsequent decrease in B. globigii spores. No free chlorine
was detected in the water at the time the experiment began. During the first 60 minutes after the
chlorinator was turned on, the free chlorine concentration in the bladder tank increased slowly due
to the organic demand in the water (turbidity was measured as 11 to 13 NTU). However, after the
first hour, the demand was overcome and free chlorin in the bladder tank increased at a faster rate.
Free chlorine peaked at 210 minutes, at which time the chlorinator was turned off. The subsequent
free chlorine samples reflect the decay due to demand and temperature in the bladder tank.
At the start of the experiment, B. globigii spores were mixed in the bladder tank volume by pushing
on the outside of the tank to move the water around and promote mixing. The first three samples
taken from the bladder tank show that the volume was well mixed. B. globigii spore density
averaged 2.4><107 cfu/100 ml (2.4><105 cfu/ml) over the first three samples. Figure 21 shows that
even as the free chlorine concentration rose from 0.14 to 3.30 mg/L from 60 to 120 minutes, spore
density remained the same. This is due to a well-known phenomenon in the field of disinfection
knowns as a "lag phase" or "shoulder". Bacillus spores are well known to be resistant to
inactivation via oxidative disinfectants, and their concentration will remain stable for a period time
in the presence of disinfectants before decreasing (AWW A, 1999; Rice et al., 2005). Once free
chlorine did inactivate the B. globigii spores, approximately 7-log reduction was achieved after
300 minutes of contact time.
30
-------
Mean Spore Density
(CFU/lOOmL)
Free Chlorine
Concentration (mg/L)
l.E+08
¦g l.E+07
0
,3 l.E+06
D
S, l.E+05
g l.E+04
01
a, l.E+03
O
a-
w l.E+02
|j l.E+01
1.E+00
100 150 200
Time (min)
Figure 25. Free chlorine concentration (orange) and Bacillus globigii spore (blue line)
density over time in the WaterStep bladder tank.
Figure 26 displays the log reduction of B. globigii spores plotted against disinfectant (free chlorine)
concentration multiplied by the contact time with the disinfectant (Ct). The Ct concept is often
used in the disinfection field to determine the combination of disinfectant concentration and
contact time needed to achieve a log reduction for a microorganism at fixed pH and temperature
conditions. If the disinfection kinetics are linear, different combinations of disinfectant
concentration and contact time can yield the same Ct (AWWA, 1999). Often, disinfection kinetic
curves for Bacillus spores developed using empirical data are not linear due to the "lag phase" or
shouldering phenomenon mentioned earlier in this section. The disinfection kinetics displayed in
Figure 25 and 26 are not linear, and this non-linearity is exacerbated by the presence of disinfectant
demand in the lagoon water as well as varying temperature over the course of the experiment.
8
7
6
5
4
3
2
1
0
0 500 1000 1500 2000
Ct (mg-min/L)
31
-------
Figure 26. The log reduction in spores during the WaterStep experiment plotted against the
Ct value (disinfectant concentration multiplied by time).
Ct values have been compiled in the literature for disinfection of pathogenic and non-pathogenic
Bacillus spores. These Ct values were often collected in experiments focused on disinfection of
drinking water, which generally has less disinfectant demand than the lagoon water used in these
experiments. For example, a Ct of 106 mg-min/L was needed for a 3-log reduction of B. anthracis
Ames at pH 7 and 25° C in the presence of 1 mg/L free chlorine. The 3-log reduction Ct value for
B. globigii spores at similar conditions was 136 mg-min/L (US EPA, 2012). In the WaterStep
experiments with lagoon water, the 3-log reduction Ct was 707 mg-min/L at pH 7 and temperature
ranging from 20 to 25°C.
Some of the increase in the Ct values found in lagoon water comes from the fact that temperature
started lower than in the drinking water Ct experiments (15°C to 25°C), where temperature was
constant (25°C). Disinfectant concentration is generally fixed in lab Ct studies, where it had to
increase from zero once the chlorinator was started. Furthermore, disinfectant demand is much
less of a factor in lab studies, unlike the WaterStep field studies where disinfectant concentration
had to build over time in the presence of an organic load. These factors resulted in a Ct value that
is approximately 5 to 6 times higher than those found for the same or similar spores observed under
drinking water treatment conditions.
Table 4 contains a summary of WaterStep technology-specific equipment observations recorded
during the treatment experiments and considerations for similar field deployments. The terms Low,
Medium and High are the opinions of the authors of this study, and are based on their experience
operating the equipment in the field. The text in the table is meant to support these opinions, and
they are specific to this piece of equipment. Other equipment operators may come to different
conclusions under different conditions.
Table 4. WaterStep Technology-Specific Considerations and Observations*
Technology
Considerations
Rating and Comments
Market Availability
High. Commercially available off-the-shelf product from a non-profit
organization for producing drinking water in communities in developing
countries. Self-contained kit, could be used in disaster zone to purify
water if there was no power available from the electrical grid. Available
from http://waterstep.org/
Capital Cost
Medium (estimate $8,000). Includes storage bladders, pump, battery,
charger, solar cell, mounting/transportation rack, and salt based chlorine
generator (Chlorinator).
Shipment to Site
Medium. Needs to go on a truck or commercial transportation. Could be
transported in a smaller vehicle, if mounting and transportation rack are
not used.
Setup
Considerations
Medium. Need flat surface to spread out the bladder tanks. Need to
recirculate chlorinated water to provide contact time for disinfection.
Not a flow through system. Test kit (strips or colorimetric) required to
32
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periodically check chlorine generation. After disinfection, if chlorine is
not consumed, the excess chlorine may need to be neutralized before
discharging to the environment.
Operational
Considerations
Low. Simple to operate on a short-term basis. If extended contact period
is required greater than 3 hours, the salt solution needs to be replenished,
electrolytic cell has to be drained, and if not on 110 volt AC power, the
battery needs to be charged.
Maintenance and
Consumables
Low. Table salt is the only consumable. For optimal chlorine generation,
the electrolytic cell needs to be cleaned periodically. Pumps, hoses and
O-rings need to be checked periodically for wear and cracking.
Result Summary
Under the tested conditions, a 7-log removal of B. globigii was observed
in a batch type operation with 300-minutes of contact time.
* Mention of trade names or commercial products does not constitute endorsement or recommendation for use of a specific product.
3.1.4 Hayward Saline C™ 6.0 Chlorination System Testing
The Hayward saline chlorinator was operated in a manner similar to WaterStep, except that
disinfection took place in the lagoon instead of a bladder tank. The Hayward unit generates free
chlorine using the same principle as the WaterStep, with free chlorine being generated from
dissolved salt in water. A potential is applied to a cell that contains electrolytic plates (an anode
and cathode). Chlorine gas is formed at the anode, which forms free chlorine when dissolved in
water ("free chlorine" is a mixture of hypochlorous acid and hypochlorite ion, depending on pH).
Flow moves through the chlorine generating cell, and dissolved free chlorine leaves the cell in the
effluent.
The Hayward chlorination cell was set up on a table next to the lagoon. The night before the
experiment, the lagoon was drained and 126 lbs (57 kg) of salt was poured into the lagoon. Flow
into the lagoon was then set so that 5,000 gallons (18,927 L) would be in the lagoon at the start of
the Hayward disinfection experiment. The morning of the experiment, B. globigii spores were
poured into approximately 5,000 gallons (18,927 L) and mixed via a sump pump positioned in the
lagoon. Pre-disinfection spore samples collected from the four corners of the lagoon (see section
2.1.4) resulted in a mean spore concentration of 1.7><107 cfu/100 ml with a standard deviation of
2.4><106 cfu/100 ml (14% relative standard deviation). This result suggested that the spores and
salt, which was dissolved, were well mixed in the lagoon. The sump pump was operated
continuously to ensure the salt and spores were well mixed in the lagoon. Flow with dissolved salt
and spores was then pumped from the lagoon, though the Hayward chlorination cell and back into
the lagoon.
Figure 27 shows the increase in free chlorine in the -5,000 gallons (18,927 L) in the lagoon over
the course of 22.5 hours (pH 7.5). Most samples were taken over the course of 5.5 hours on the
first day of experimentation, with the final sample being taken the following morning. The data
shows that free chlorine increased in the lagoon more slowly than in the WaterStep bladder tank
(Section 3.1.3). For comparison, at 210 minutes after the start of the experiment, free chlorine was
12.2 mg/L in the WaterStep bladder tank, but only 0.65 mg/L in the lagoon. This could be due to
more organic demand since there was sediment and algae on the bottom of the lagoon.
Furthermore, sunlight could have contributed to degradation of the free chlorine in the lagoon
during the day, and some of the free chlorine residual likely dissipated into the air from the surface
33
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of the lagoon. After 22.5 hours, the free chlorine concentration in the lagoon had reached 12 mg/L.
No sunlight and decreased temperature during the night could contribute to a rise in free chlorine
levels.
Mean Spore Density (CFU/100 mL)
Free Chlorine Concentration (mg/L)
200 400 600 800 1000 1200 1400 1600
Time (min)
Figure 27. Free chlorine concentration (orange) and Bacillus globigii spore (blue line)
density over time in lagoon water (-5,000 gal) during disinfection with the Hayward
treatment unit.
Spore decrease within the first 5.5 hours was 0.5 log in the presence of 1.2 mg/L free chlorine, but
this had increased to 4.3-log in the presence of 12 mg/L at 22.5 hours. For comparison, the
WaterStep unit had achieved a 6-log reduction when 12 mg/L free chlorine was achieved. It is
important to note that if the Hayward unit had continued to operate past 22.5 hours, a 6 to 7 log
reduction might have occurred. If the log reduction continued as illustrated in the graph, then an
estimated 7 log reduction would be achieved in the next 10 to 12 hours.
Figure 28 shows log reduction plotted against Ct. In the lagoon, the Hayward unit achieved 4.3
log reduction at a Ct of almost 7,000 mg-min/L (pH 7.5). For comparison, 4-log reduction Ct for
B. cmthracis Sterne at pH 7 and 2 mg/L free chlorine was 280 and 90 mg-min/L at 5° and 25° C,
respectively (Rice et al., 2005). Interpolating between these values for 15°C, which was close to
the lagoon temperature, yields a Ct value of 185 mg-min/L for drinking water disinfection. The
Ct for 4-log removal using the Hayward unit was approximately 6,400 mg-min/L, or 35 times more
than the Ct for drinking water.
These results highlight the challenges associated with disinfecting biological agents in a real world
environment. The volume of water in the lagoon was larger and more spread out in the lagoon
compared to the WaterStep bladder (Section 3.1.3). This kept the temperature in the 15° to 20° C
range. Disinfection is slower at lower temperature. In addition, the aforementioned organic
demand and free chlorine dissipation factors in the lagoon likely slowed disinfection. Despite these
challenges, the results show that disinfection of a chlorine resistant microorganisms like Bacillus
spores in real world dirty water is possible given time, planning, and the appropriate equipment.
34
-------
0 1000 2000 3000 4000 5000 6000 7000 8000
CT (mg-min/L)
Figure 28. The log reduction in spores during the Hayward experiment plotted against the
Ct value (disinfectant concentration multiplied by time).
Table 5 contains a summary of Hayward technology-specific equipment observations recorded
during the treatment experiments and considerations for similar field deployments. The terms Low,
Medium and High are the opinions of the authors of this study, and are based on their experience
operating the equipment in the field. The text in the table is meant to support these opinions, and
they are specific to this piece of equipment. Other equipment operators may come to different
conclusions under different conditions.
Table 5. Hayward Technology-Specific Considerations and Observations*
Technology
Considerations
Rating and Comments
Market Availability
High. Commercially available in-situ chlorine generator, off-the-shelf
product from a pool product manufacturer. Commonly used for
disinfecting swimmins pools. Available from http://www.havward-
Dool.com/
Capital Cost
Low. $4,000
Shipment to Site
Low. Small package easy to ship or carry in a car.
Setup
Considerations
Medium. Can be setup on a table. Requires a 40 gpm (151.4 L/min)
pump to run salted water through the system. Salt needs to be added to
the source water in sufficient quantities (3,000 to 5,000 mg/L). Chlorine
generation can be varied as needed. Need to recirculate chlorinated water
to provide contact time for disinfection. Not a flow through system. Strip
kit required to periodically check chlorine generation.
Operational
Considerations
Low. Requires 110 volt AC power, high capacity (40 gpm [151.4
L/min]) pump. Initial setup requires the chlorine production of the
system to be slowly ramped up by starting at -50% production rate and
increased incrementally. Salt may need to be added depending upon
usage. It could be operated using bladder tanks, but also suited for open
pools.
35
-------
Technology
Considerations
Rating and Comments
Maintenance and
Consumables
Low. Table salt (NaCl -98%). Pump and hoses need to be checked as
needed.
Result Summary
Under the tested conditions, the unit achieved a 4.3 log reduction of B.
globigii in 300 minutes at a Ct of almost 7,000 mg-min/L.
Ct, concentration of disinfectant multiplied by the contact time
* Mention of trade names or commercial products does not constitute endorsement or recommendation for use of a specific product.
3.2 Crude Oil Contamination/Decontamination Tests
As described in detail in section 2.2, Bakken crude oil was mixed with water from the Snake River
and allowed to mix overnight in a carboy. Before injection, the bottom oil layer containing
dissolved or emulsified oil components was removed from the carboy. This subnatant water layer
was injected into the flow in the WSTB pipe, and the slug of contaminated water contacted the
inner surfaces of the WSTB pipe.
Tables 6 and 7 show the results for the suite of oil components analyzed for in the water samples
and on the removable coupon surfaces, respectively. In the water phase (Table 6), the subnatant
injection resulted in a spike in total petroleum hydrocarbons, gasoline-range organics and benzene.
Total petroleum hydrocarbon is the summation which includes gasoline-, diesel-, and oil-range
organics. Only gasoline range organics were detected. Other BTEX components and longer chain
oil components such, diesel-, and oil-range organics were not detected.
Interestingly, some constituent in the background showed up or interfered with the gasoline-range
organic/total petroleum hydrocarbon test. However, there was a spike in both parameters during
injection of the subnatant and water mixture. Gasoline range organics and total petroleum
hydrocarbons were 0.17 mg/L before injection, spiked up to 0.24 and 0.34 mg/L during injection
(a 40 and 100% increase over baseline, respectively), and then settled back to 0.16 mg/L during
flushing after the contaminant slug had passed. It should be noted that all personnel on site could
detect an oil or gasoline smell in the water samples removed from the WSTB pipe when the oil
slug was present.
The measured gasoline range organics and total petroleum hydrocarbons spiked again when
surfactant was introduced. This is likely due to the methods for both parameters also detecting the
surfactants in water, but this was not confirmed. The measured gasoline range organics and total
petroleum hydrocarbons decreased once the main surfactant pulse had cleared the pipe, but
background levels remained elevated above the initial baseline up to 16 days after the surfactant
addition. This data suggest that some of the surfactant still persisted in the WSTB pipe for more
than two weeks after its introduction. Upon shaking a water sample, it was noticed that some
foaming did occur in the water samples that would suggest the presence of surfactant, or
solubilized materials from the pipe walls.
Throughout the test, no components from the Bakken oil were detected on the pipe coupon
surfaces. At two and three days after injection of the oil, ethylbenzene and toluene were detected
on the coupons. It is possible that Bakken oil components were trapped some place in the
36
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Table 6. Bulk Water Sampling Results
Date
Experimental Phase
Time
Elapsed
Time
hr
GRO
(C6-
C12)
mg/L
DRO
(C10-
C20)
mg/L
ORO
(C20-
C34)
mg/L
TPH
mg/L
Benzene
ug/L
Ethylbe
nzene
ug/L
m,p-
Xylene
ug/L
o-
Xylene
ug/L
Toluene
ug/L
Total
Xylenes
ug/L
Method Detection Limit, ug/L
(1)
(2)
(2)
0.63
0.68
1.0
1.1
0.72
1.1
MCL, ug/L
NA
NA
NA
NA
5
700
10,000
10,000
1,000
10,000
9/21/2015
Background
8:30
0.0
0.17
0.0
0.0
0.17
0.0
0.0
0.0
0.0
0.0
0.0
Crude Oil Inject, Start
Flush
10:25
1.9
0.24
0.0
0.0
0.24
21.5
0.0
0.0
0.0
0.0
0.0
10:55
2.4
0.34
0.0
0.0
0.34
32.0
0.0
0.0
0.0
0.0
0.0
Flush End, Inject
Surfactant
12:15
3.8
0.16
0.0
0.0
0.16
1.9
0.0
0.0
0.0
0.0
0.0
Surfactant Injection
Pulses
14:45
6.3
8.0
0.0
0.0
8.0
0.0
0.0
0.0
0.0
0.0
0.0
15:30
7.0
6.9
0.0
0.0
6.9
0.0
0.0
0.0
0.0
0.0
0.0
9/22/2015
Residual Surfactant,
Flowing Water
9:00
24.5
0.31
0.0
0.0
0.31
0.0
0.0
0.0
0.0
0.0
0.0
12:00
27.5
0.31
0.0
0.0
0.31
0.0
0.0
0.0
0.0
0.0
0.0
15:00
30.5
0.45
0.0
0.0
0.45
0.0
0.0
0.0
0.0
0.0
0.0
9/23/2015
9:45
49.3
0.28
0.0
0.0
0.28
0.0
0.0
0.0
0.0
0.0
0.0
9/24/2015
9:45
73.3
0.26
0.0
0.0
0.26
0.0
0.0
0.0
0.0
0.0
0.0
9/25/2015
9:45
97.3
0.29
0.0
0.0
0.29
0.0
0.0
0.0
0.0
0.0
0.0
9/30/2015
9:45
217.3
0.29
0.0
0.0
0.29
0.0
0.0
0.0
0.0
0.0
0.0
10/7/2015
9:45
385.3
0.31
0.0
0.0
0.31
0.0
0.0
0.0
0.0
0.0
0.0
DRO, diesel range organics; GRO, gasoline range organics; MCL, maximum contaminant levels; ORO, oil range organics; TPH, total petroleum hydrocarbon; NA, No
applicable/no sample; MCL, maximum contaminant level.
37
-------
Table 7. Coupon Sampling Results
Date
Experimental Phase
Time
Elapsed
Time
hr
Benzene
ug/kg
Ethylbenzene
ug/kg
m,p-Xylene
ug/kg
o-Xylene
ug/kg
Toluene
ug/kg
Total Xylenes
ug/kg
Method Detection Limit, ug/kg
3.0
3.0
5.8
3.8
6.2
5.8
9/21/2015
Background
8:30
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Crude Oil Inject, Start Flush
10:25
1.9
0.0
0.0
0.0
0.0
0.0
0.0
10:55
2.4
0.0
0.0
0.0
0.0
0.0
0.0
Flush End, Inject Surfactant
12:15
3.8
0.0
0.0
0.0
0.0
0.0
0.0
Surfactant Injection Pulses
14:45
6.3
0.0
0.0
0.0
0.0
0.0
0.0
15:30
7.0
0.0
0.0
0.0
0.0
0.0
0.0
9/22/2015
Residual Surfactant,
Flowing Water
9:00
24.5
0.0
0.0
0.0
0.0
0.0
0.0
9/23/2015
9:45
49.3
0.0
12.0
0.0
0.0
11.0
0.0
9/24/2015
9:45
73.3
0.0
8.4
0.0
0.0
7.4
0.0
9/25/2015
9:45
97.3
0.0
0.0
0.0
0.0
0.0
0.0
MCL, maximum contaminant level.
-------
WSTB and detached broke loose days after the contamination event and adhered to the coupons.
However, no corresponding increase in toluene or ethylbenzene was detected in the bulk water
samples. It is possible that some toluene and/or ethylbenzene were present on the coupons below
the method limit of detection, and these coupons had higher amounts. It is also possible that the
spike in toluene and ethylbenzene on the coupons on Sept. 23 and 24 was external contamination
or some other unknown occurrence.
Figure 29 shows a more detailed picture of the spike in benzene that occurred during injection of
the Bakken oil subnatant phase from the carboy. The figure shows the phase before injection of
the Bakken crude oil-water mixture (Background), while the oil slug was travelling down the
pipe (Crude Oil Subnatant Injection), during clean water flushing (flushing @15 gpm [56.8
L/min]), surfactant addition (Surfactant Injection-three pulses) and then during clean water flow
(Flow@15 gpm [56.8 L/min] with residual surfactant). No benzene was detected in the
background water sample before injection of the Bakken oil-water mixture. A spike in benzene
was detected when the oil components were travelling down the pipe. However, after the oil
slug exited the pipe and clean water was flushed through, the benzene level dropped
precipitously. It appears that simple water flushing cleared the pipe of benzene. No benzene
was detected during the addition of surfactant or thereafter.
35
30
25
g 20
01
c
QJ 15
N 1J
cu
CO
10
B
3
C
k
Crude Oil
Injection
Flushing @
15 gpm
Surfac-
tant
inject
(three
pulses)
Flow @ 15 gpm with
residual surfactant
g
r
o
u
n
d
Benzene MCL (5 pg/L)
»
Benzene Method Detection Limit =
0.63 ng/L
w ¦' • 1 11 1 "
0
8
1 2 3 4 5 6 7
Time (Hrs)
Figure 29. Benzene concentration in the Water Security Test Bed bulk water.
The results of the Bakken crude oil injection show that the oil components such as total petroleum
hydrocarbons and BTEX do not persist in the bulk water phase. The inner pipe surface represented
by the coupon samples in Table 7 show some presence of ethylbenzene and toluene on Days 3 and
4 (post injection on Day 1) at detectable concentrations. However, these results are outliers
compared with the other coupon samples, and no corresponding spikes in ethylbenzene and toluene
were observed in the bulk phase. Flushing clean tap water through the WSTB pipe after the oil
39
-------
slug had exited was enough to drop the levels of benzene below the MCL in bulk water, and to
undetectable levels thereafter both in bulk water and coupon samples. Surfactant was added to the
pipe because it was anticipated that some oily components would persist in the water or on the
infrastructure. However, it appears that flushing alone may have been sufficient to clear the pipe
of Bakken oil subnatant, and surfactant addition may not have been necessary. Because no
constituents from the Bakken oil were detected on the coupons prior to surfactant addition,
additional experiments are merited to better understand the potential role of surfactants when
contaminants are detectable.
3.2.1 Online Sensor Data
Figure 30 presents data from the downstream online M4000 TOC sensor from RealTech
(RealTech, undated) and Turner oil in water monitor during the day the
contaminant/decontaminant tests were conducted. It was expected that these sensors would have
the best chance at detecting the Bakken oil subnatant components.
30
25
txo
— 20
C
O
-Q
(0
u
o
T3
>
X
(0
-------
compared to the crude oil on a mass basis. The UV-based TOC sensor does see a brief spike in
TOC value after the surfactant addition (between 4:00 and 5:00 pm) at the beginning of the phase
when the corresponding hydrocarbon response is very high. The pulsed method of the surfactant
injection is also reflected in the spiky nature of the online hydrocarbon instrument response. The
sharp spikes in both sensors observed throughout the experiment are likely due to some
undissolved globules of oil passing through the instruments.
Figure 31 shows data from the online Hach colorimetric chlorine sensors during the day the
contaminant/decontaminant injection test was conducted. From Figure 31, it appears that the
chlorine sensor does not respond to the Bakken oil subnatant components that comprised most of
the crude oil injection, but they do respond to the surfactant injection. It is unknown if the chlorine
sensor response to the surfactant was due to the interference in the colorimetric analysis or due to
actual reduction in the chlorine values. Furthermore, spikes in the data similar to those observed
in the TOC and hydrocarbon sensors are seen at the same points in time. Like the TOC and
hydrocarbon sensors, these spikes are attributed to globules of oil interfering with the colorimetric
analysis in the chlorine sensor. It should be noted that the discussions of the data from Figures 30
and 31 are preliminary.
l.o
0.9
0.8
0.7
|o.e
-------
4.0 Conclusions and Future Work
Experiments performed at the EPA WSTB in 2015 generated useful data on the ability of mobile
water treatment devices to disinfect Bacillus spores in "dirty" water, or water with disinfectant
demand resulting from naturally-occurring particles. Experiments also focused on contamination
of the WSTB pipe with oil and effectiveness of decontamination with flushing and surfactants.
The following bullets are a summary of conclusions drawn from the testing performed at the
WSTB with mobile water treatment devices:
• The experimental setup was able to provide a consistent source of Bacillus spores in lagoon
water for treatment experiments. This was true whether the spores were added to a bladder
tank or the lagoon.
• The EPA AOP (UV/ozone) trailer achieved an average of 4-log removal of Bacillus spores
in the flow through the disinfection system. Log removal varied between 1.5 and 5.0 over
the course of the 5.5 hour experiment and two thousand gallons of water were treated.
Disinfection performance may be improved if temperature were constant, which can
influence ozone diffusion into the water as well as UV lamp output. Equipment with less
wear and usage may perform more consistently. Finally, shutting down and restarting the
disinfection unit may have negatively impacted performance.
• The Solstreme UV disinfection unit achieved an average spore log reduction of 3.7, with
log removal increasing from 3.0 to 4.0 over the course of the 5.5 hr experiment. This could
have been due to the increase in temperature experienced during the daylight hours
elevating the UV output/efficiency and leading to greater disinfection. Adding an inline
heat exchanger could potentially help enhance the disinfection performance of the
Solstreme since it would help provide a consistent influent temperature. Two thousand
gallons of water were treated during the experimental run.
• The WaterStep unit achieved 6.8 log removal in a 1,250 gallon (4,732 L) bladder tank
within 5 hours of the start of the experiment while achieving 12.2 mg/L free chlorine.
However, this was the smallest volume disinfected during the overall testing period.
• The Hayward salt water chlorination unit achieved 4.3-log reduction of Bacillus spores
after 22.5 hours of operation and achieved 12 mg/L free chlorine. Assuming the results
can be extrapolated, it was estimated that an additional 10-12 hours of disinfection would
have achieved 7-log removal. Treatment conditions were the most difficult in this
experiment since disinfection occurred in 5,000 gallons (18,927 L) of water contained
within the open lagoon. More sediments were present on the bottom of the lagoon, which
were not present at those high levels in the other experiments. Furthermore, temperature
was lower and exposure to sunlight likely degraded the free chlorine generated in the
lagoon.
• Results from the four mobile water treatment units indicate that disinfection of large
volumes of water contaminated with biological agents is possible. It is likely that larger
42
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volumes of water may need to be disinfected in a real world scenario, but all of these
systems can be scaled up, or multiple units can be put into place. Data generated from this
study does demonstrate that disinfection of dirty water in the field is more challenging than
disinfecting clean drinking water due to the disinfectant demand present in real world wash
water, the impact of low temperature, pH and turbidity on disinfection, and disinfectant
dissipation due to exposure to sunlight.
• Table 8 provides a combined performance summary of the mobile water treatment devices
evaluated at the WSTB in August 2015. A more detailed summary table including
technology specific considerations is included as Appendix B.
Table 8. Mobile Water Treatment Device Performance Summary
Water
Treatment
Technology
Tested
Capital
Cost
Average Log
Reduction
Volume
Treated
(gal)
Flow
(gpm)
Performance Summary
EPA AOP
Trailer (UV
and Ozone)
$40,000
4.0
2,000
5
Immediate disinfection,
log reduction was unstable
during this study due to
experimental challenges
Solstreme
(UV)
$15,000
3.5 to 4.0
2,000
5
Stable, immediate
disinfection, easy to
transport and set up.
Water Step
(Chlorinator)
$8,000
7.0
1,250
N/A
64og reduction in 300
min, lowest total treated
volume.
Hayward
(Chlorinator)
$4,000
4.3
5,000
40
44og reduction in 1,350
min, under most difficult
disinfection conditions.
The following bullets are a summary of conclusions based on the testing performed at the INL
WSTB with crude oil:
• Bakken oil contaminated water (subnatant) was successfully injected into the WSTB pipe.
This was confirmed by the increase in benzene and total petroleum hydrocarbons observed
in the water when the contaminant was in the pipe. A detectable smell of oil or
hydrocarbons was present in the sampled water.
• Data from water samples collected during the experiment suggest that flushing the pipe
with clean water was an effective decontamination method. Benzene dropped below the
MCL during flushing and no other BTEX components were detected in the water. No total
petroleum hydrocarbons or BTEX compounds were detected on the pipe infrastructure
coupons during or shortly after the crude oil injection. Toluene and ethylbenzene were
detected at low levels on the coupons days after injection and decontamination, but it is
unclear if these were outlier samples or if interference played a role. No Bakken oil
components were detected on subsequent coupon samples.
43
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• Surfactant was injected because it was assumed that oily components would persist in the
water phase or on the infrastructure/pipe surfaces. This was not the case, but visual
observation of foaming in the water samples might suggest that surfactant persisted in the
WSTB pipe for days after the initial injection. Therefore, caution should be used when
introducing a surfactant into a water system for the purposes of decontamination as it may
not be easy to completely remove it in a timely manner.
Specific research needs that emerged during this study and should be addressed in the future are
as follows:
• In water treatment experiments using the AOP trailer, disinfection performance could have
been impacted by the following issues: 1) changing lagoon temperature (from 15°C to
25°C) affecting ozone diffusion into the water and ozone generator output; 2) changing
turbidity of the influent water with temperature and mixing in the tank; 3) inconsistent UV
lamp output with temperature; 4) hours of operation; 5) unknown factors related to other
site specific conditions and the unit being removed from the trailer. All of these issues
should be explored in-depth.
• The increase in output intensity of the Solstreme in Figure 24 is perhaps due to the increase
in water temperature over the course of the experiment. In the future, it may be beneficial
to add a heating element to the Solstreme influent water line to bring water to a temperature
between 25° to 30°C. Increased disinfection performance may be due to hydroxyl radical
formation due to photolysis of the water with higher temperature. The influence of air and
water temperature on disinfection performance merit further investigation.
• The sharp spikes in on-line sensors signals observed throughout the experiment are likely
due to some undissolved globules of oil passing through the instruments. However, this
was not confirmed.
• The measured gasoline range organics and total petroleum hydrocarbons spiked when
surfactant was introduced. This is likely due to the methods for both parameters also
detecting the surfactants in water, but this was not confirmed.
Future research using the WSTB will focus on addressing other outstanding EPA National
Homeland Security Research Center needs.
• Bacillus spores can be persistent on drinking water infrastructure, and decontamination of
persistent spores is a challenge. Future work will examine physical removal of adhered
Bacillus spores using pigging or ice pigging. Pigging involves insertion of a grinding
mechanism into the pipe which physical scours the internal pipe wall. The principle behind
ice pigging is similar, except that a slurry of ice is used to scour the pipe wall.
• If an oil spill occurs, the potential for a fire resulting from ignition of the spilled oil is
increased. Fires from oil spills often burn at elevated temperatures, and polyfluoroalkyl
firefighting foams are often used to control the flames. If the spill occurs near a water body
44
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with a drinking water intake, it is possible that the foams could make their way into a water
distribution system. Therefore, future work will focus on the persistence of polyfluoroalkyl
firefighting foams on drinking water infrastructure and decontamination.
• Previous decontamination research has focused on drinking water distribution system
materials. There is a need to examine the persistence of chemical and biological
contaminants in home plumbing materials and in appliances. To further that goal, copper
plumbing lines will be connected between the WSTB pipe and an adjacent vacant building.
This plumbing system will have removable sections of copper, PVC and polyethylene with
cross-links (PEX) piping so that pre-and post-decontamination contaminant persistence
can be examined. Appliances such as refrigerators, washing machines, dishwashers and
hot water heaters will also be installed. These appliances will be contaminated with
chemical or biological agents, and the effort necessary to decontaminate them will be
tested.
45
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5.0 References
American Water Works Association (AWW A). 1999. Water Quality and Treatment: A Handbook
of Community Water Supplies, 5th ed. McGraw-Hill, New York.
Hach. 2014. CL17 Chlorine Analyzer - User Manual, Edition 9, Hach Company, Loveland, CO,
USA.
Hayward. 2013. Saline C™ 6.0 Commercial Salt Chlorine Generator Owner's Manual - Version
ISHCSC60 RevE. Hayward Commercial Pool Products 10101 Molecular Drive, Suite 200,
Rockville, MD, USA.
NeCamp, D.R. 2008. X-3-5 Ultraviolet Water Purification system. 'A discussion of X-3-5
ultraviolet technology and its benefits.' X-3-5 LLC, Solstreme, Cincinnati, Ohio, USA. February
2008.
United States Environmental Protection Agency (US EPA). 2003. Ultraviolet Disinfection
Guidance Manual. EPA/815/D-03/007.
RealTech. Undated. Owner's Manual Version 1.1 for the REALTECH M4000 UV254 Monitor,
edition and date are not indicated on the manual. RealTech Inc., Ontario, Canada.
Rice, E.W., Adcock, N.J., Sivaganeson, M. and Rose, L.J. 2005. Inactivation of spores of Bacillus
anthracis Sterne, Bacillus cereus, and Bacillus thuringiensis subsp. israelensis by chlorination.
Applied and Environmental Microbiology, 71(9):5587-5589.
Turner Designs Hydrocarbon Instruments (Turner). 2009. Operation Manual for TD1000C™ Oil
in Water Monitor. March 30, 2009, P/N 101687, Rev. E, Turner Designs Hydrocarbon
Instruments, 2023 Gateway Blvd. Suite 101, Fresno, CA, USA.
United States Environmental Protection Agency (US EPA). 2008. Pilot-Scale Tests and Systems
Evaluation for the Containment, Treatment, and Decontamination of Selected Materials from
T&E Building Pipe Loop Equipment. US EPA, Cincinnati, OH, USA. EPA/600/R-08/016.
United States Environmental Protection Agency (US EPA). 2012. Technical Brief: Inactivation of
Bacterial Bioterrorism Agents in Water: Summary of Seven Studies. US EPA, Washington, DC.
EPA/600/R-12/521.
United States Environmental Protection Agency (US EPA). 2015. Water Security Test Bed
Experiments at the Idaho National Laboratory. EPA/600/R-15/146.
WaterStep 2013. Instruction Manual for the M-100 Chlorine Generator. WaterStep, 625 Myrtle
St., Louisville, KY, USA (www.waterstep.org. accessed April 7. 2016).
46
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Appendix A: Quality Assurance Project Plan
47
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QUALITY ASSURANCE PROJECT PLAN
EPA QA ID No. - 61_2014_QAPP
EXPERIMENTS IN THE WATER SECURITY TEST BED AT
IDAHO NATIONAL LABORATORY
EPA Contract No. EP-C-14-012
Work Assignment No. 1-08
CB&I DN: 500438-QA-PL-000145
Prepared for:
U.S. ENVIRONMENTAL PROTECTION AGENCY
National Homeland Security Research Center (NHSRC)
26 West Martin Luther King Drive
Cincinnati, Ohio 45268
Prepared by:
CBI
CB&I Federal Services LLC
5050 Section Avenue
Cincinnati, Ohio 45212
Ruth Corn, Contract-level Contracting Officer Representative
Jeff Szabo, Ph.D., P.E., Work Assignment Contracting Officer Representative
John Hall, Alternate Work Assignment Contracting Officer Representative
Revision No. 2
September 10, 2015
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Summary of Work Assignment 1-08 Quality Assurance Project Plan
Revision No. 1
The Quality Assurance Project Plan (QAPP) for Work Assignment (WA) 0-08, Revision 0, dated
September 3, 2014 (EPA QA ID No. - 612014QAPP), is being revised to include the
following elements:
• Updated Work Assignment and CB&I Document Numbers.
• Replaced Mr. Steve Jones as CB&I QA Manager with Mr. Don Schupp.
• Added Ms. Jill Webster as a Project Chemist.
• Added evaluation of technologies to determine the ability to decontaminate large
volumes of water to be conducted in mid-August, 2015.
• Added crude oil contamination/decontamination experiment to be conducted in mid-
September 2015.
• Extended the project schedule through May 2016, with another B. globigii
contamination/decontamination experiment.
Revision No. 2
The QAPP for WA 1-08, Revision 1, dated July 2, 2015 (EPA QA ID No. - 612014 QAPP), is
being revised to address the observations from the EPA technical systems audit (TSA) conducted
in August 2015.
• Page headers were revised on all pages to reflect the newer revision number to avoid
potential confusion.
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Revision No. 2
Page 1 of 2
Approval/Distribution
CB&I Federal Services LLC Concurrences:
1. E. Radha Krishnan, P.E.
Program Manager
Signature Date
2. Paul C. Kefauver
Project Leader
Signature Date
3. Donald A. Schupp, P.E.
Quality Assurance Manager
Signature Date
U.S. Environmental Protection Agency Endorsement for Implementation:
4. Jeff Szabo, Ph.D., P.E.
Work Assignment Contracting Officer Representative
Signature Date
5. John Hall
Alternate Work Assignment Contracting Officer Representative
Signature Date
6. Ramona Sherman
NHSRC Quality Assurance Manager
Signature Date
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Date: September 2015
Revision No. 2
Page 2 of 2
Approval/Distribution
Quality Assurance Project Plan Distribution List
U.S. Environmental Protection Agency:
Jeff Szabo, Ph.D., P.E. Work Assignment Contracting Officer Representative
John Hall Alternate Work Assignment Contracting Officer Representative
Ramona Sherman NHSRC Quality Assurance Manager
CB&I Federal Services LLC:
E. Radha Krishnan, P.E.
Paul C. Kefauver
Donald Schupp, P.E.
Greg Meiners
Srinivas Panguluri, P.E.
Tim Kling
Lee Heckman
Jill Webster
Sue Witt
Program Manager
Project Leader
Quality Assurance Manager
Lead Project Scientist
Data acquisition and electronic communications networking
specialist
T&E Chief of Operations
Project Microbiologist
Project Chemist
Project Scientist
ALS Environmental
Mr. Rob Nieman
Analytical Project Manager
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Revision No. 2
Page 1 of 2
TOC
Table of Contents
No. of
Pages Addendum Date
1.0 PROJECT DESCRIPTION AND OBJECTIVES 1 2 09/2015
1.1 Background and Project Description
1.2 Project Objectives
2.0 PROJECT ORGANIZATION AND RESPONSIBILITIES 3 2 09/2015
2.1 Proj ect Organization
2.2 Project Schedule
3.0 SCIENTIFIC APPROACH 13 2 09/2015
3.1 Technologies
3.2 Experimental Design and Test Conditions
3.3 Measurements and Analytes
4.0 SAMPLING PROCEDURES 5 2 09/2015
4.1 Site-Specific Factors
4.2 Sampling Procedures
4.3 Sampling Containers and Quantities
4.4 Sample Preservation and Holding Times
4.5 Sample Labeling
4.6 Sample Packing and Shipping
5.0 MEASUREMENT PROCEDURES
5.1 Analytical Methods
5.2 Calibration Procedures
09/2015
6.0 QUALITY METRICS (QA/QC CHECKS)
6.1 QC Checks
6.2 QA Objectives
09/2015
7.0
DATA ANALYSIS, INTERPRETATION, AND MANAGEMENT
7.1 Data Reporting Requirements
7.2 Data Validation Procedures
7.3 Data Summary
7.4 Data Storage
09/2015
5.0 REPORTING
8.1 Deliverables
8.2 Final Report
09/2015
9.0
REFERENCES
09/2015
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TOC
Appendices
A CB&I T&E SOP 304: Heterotrophic Plate Count (HPC) Analysis Using IDEXX SimPlate Method
B
Hach Method 10102 for Measuring Free Chlorine in Water
c
CB&I T&E SOP 309: Preparation and Enumeration of B. globigii Endospores
D
Preparation of the G02 4,000 ppm Solution
E
EPA Sample Chain of Custody Form
F
EPA Water Concentrator SOP
G
Characterization of gasolines, diesel fuels & their water soluble fractions
H
Bakken Crude Oil
List of Tables
Revision
Date
2-1
Project Roles and Responsibilities
2
09/2015
3-1
Crude Oil Contamination/Decontamination Related Sampling Activity 2
09/2015
3-2
B. globigii Contamination/Decontamination Related Sampling Activity 2
09/2015
4-1
Summary of Experimental Sampling Strategy
2
09/2015
4-2
Grab Sampling and Analytical Procedures
2
09/2015
6-1
QA/QC Checks for Grab Samples
2
09/2015
6-2
QA/QC Checks for Online Equipment
2
09/2015
7-1
Reporting Unit Measurements
2
09/2015
List of Fisures
Revision
Date
2-1
Project Organization
2
09/2015
3-1
Schematic Overview of WSTB
2
09/2015
3-2
Large Volume Testing Schematic
2
09/2015
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Section 1
1.0 PROJECT DESCRIPTION AND OBJECTIVES
1.1 Background and Project Description
EPA's National Homeland Security Research Center (NHSRC) has partnered with Idaho National
Laboratory (INL) to build the Water Security Test Bed (WSTB) at INL in Idaho Falls, Idaho. The
centerpiece of the WSTB is an 8-inch diameter drinking water pipe that was taken out of service.
The pipe was exhumed from the INL grounds and oriented in the shape of a small drinking water
distribution system. The WSTB has service connections to simulate water demands, fire hydrants,
and removable coupons to collect samples from the pipe interiors. Experiments focused on
contamination (Crude Oil), decontamination (Dispersant or Surfactant) and triggered flushing
events will take place in the WSTB. Additional experiments will focus on treatment of large
volumes of biologically contaminated water with mobile disinfection technologies; however, the
WSTB pipe will not be used for these experiments. Instead the lagoon water will be pumped
through a set of tanks and selected treatment systems.
Under contract to EPA (Contract No. EP-C-14-012), CB&I Federal Services LLC (CB&I) has
been providing technical support in developing new technologies and evaluation of existing
technologies at the EPA Test & Evaluation (T&E) Facility in Cincinnati, Ohio. CB&I will provide
technical support for on-site setup and testing to EPA on an as-needed basis. This Quality
Assurance Project Plan (QAPP) outlines the tests that will be performed in the WSTB. This QAPP
follows the guidance for a Category B measurement project.
1.2 Project Objectives
The planned studies have the following goals:
1. Conduct decontamination tests on the WSTB with selected decontaminants (Dispersant
orSurfactant) following intentional contamination (Crude Oil) of the WSTB, and evaluate
the effectiveness of the selected decontaminants for removing contaminants from the
WSTB.
2. Evaluate select online instrumentation installed on the WSTB to determine their efficacy
in detecting anomalous contamination events in the WSTB and trigger flushing of the
WSTB through the flushing hydrant.
3. Perform studies on disinfection technologies to determine their ability to treat large
volumes of biologically contaminated water.
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Page 1 of 3
Section 2
2.0 PROJECT ORGANIZA TION AND RESPONSIBILITIES
2.1 Project Organization
The overall project management and distribution of responsibilities among the project personnel
are described in this section. Figure 2-1 presents the organization chart for the project. Table 2-1
presents contact information for project personnel. Ms. Ruth E. Corn serves as the EPA T&E
Contract-level Contracting Officer Representative (CLCOR). Dr. Jeff Szabo, the EPA Work
Assignment Contracting Officer Representative (WACOR) for this study, is responsible for overall
technical direction and adhering to the guidelines of the QAPP. Mr. John Hall is the EPA Alternate
WACOR and will assist Dr. Szabo. Ms. Ramona Sherman, the EPA NHSRC Quality Assurance
(QA) Manager, is responsible for approval of QA documents and QA project assessments.
Mr. Radha Krishnan, P.E., serves as the CB&I Program Manager for the EPA T&E Contract. The
CB&I Program Manager will be responsible for the overall project management, program
coordination, and management review of deliverables. Mr. Paul Kefauver, CB&I Project Leader,
will be responsible for project planning, coordination of activities, and peer review of deliverables.
Mr. Donald Schupp, P.E., is the CB&I QA Manager. Mr. Schupp will be responsible for the
oversight of CB&I T&E quality program implementation, including QA review of documents and
deliverables, and project assessments.
Mr. Greg Meiners, Mr. Srinivas Panguluri, Mr. Dave Elstun, and Mr. Gary Lubbers with CB&I
will provide on-site support for setup and operation of the WSTB. Mr. Greg Meiners will serve
as the Lead Project Scientist. Mr. Meiners will be responsible for experimental start-up, collection
and analysis of the samples, interpretation of the data, and completion of the final report. Mr.
Srinivas Panguluri, P.E. will serve as the data acquisition and electronic communications
networking specialist. Mr. Dave Elstun and Mr. Gary Lubbers will assist with the on-site
equipment setup and testing as needed (including injection pump(s), instrumentation, and data
acquisition). Mr. Lee Heckman, CB&I Project Microbiologist, will provide sample analysis
support. Mr. Timothy Kling, Ms. Sue Witt, and Ms. Jill Webster with CB&I will provide as needed
remote support to Mr. Meiners on an as-needed basis.
Mr. Rob Nieman of ALS Environmental (ALS) will oversee chemical analyses performed at that
laboratory.
2.2 Project Schedule
This revision presents anticipated activities expected to be performed between May 2015 and
May 2016. A detailed timeline is presented later in the "Experimental Design and Test
Conditions" (Section 3.2).
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Revision No. 2
Page 2 of 3
Section 2
Al S l-n\ iionmenUil
Rob Sicilian
Ruth Corn
CIJ&I Chief of Operaiions
MISIU" OA \hinnuer
Riinionii Sherman
¦|\\ Alternate
WACOR
John 11 all
CIJ&I Program Mummer
C"IicK; I OA Mummer
Donald Sclmpp. /'/:
¦:i»A WACOR
CIJ&I Project Personnel
(ireu Mfillers
(iary Lubbers
David Hstun
Lee I lech man
Sue Witt
Jill W ebster
Figure 2-1: Project Organization
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Revision No. 2
Page 3 of 3
Section 2
Table 2-1: Project Participant Contact Information
Name of
Person/Affiliation
Project Role
Phone Number, email
Ruth Corn/EPA
T&E Contract CLCOR
513-569-7610,
Corn. Ruth® eDa. gov
Jeff Szabo/EPA
WACOR
513-487-2823
Szabo. Jeff(a), eoa.gov
John Hall/EPA
Alternate WACOR
513-487-2814,
Hall. John®,eoa.gov
Ramona Sherman/EPA
NHSRC QA Manager
513-569-7640,
Sherman. Ramona® epa. gov
Radha Krishnan/CB&I
Program Manager
513-782-4730,
Radha.Krishnan® cbifederalservices.com
Paul Kefauver/CB&I
Project Leader
513-569-7057,
Paul. Kefauver® cbifederal services.com
Donald Schupp/CB&I
Q A Manager
513-782-4974,
Don. SchuDD® cbifederal services.com
Timothy Kling/CB&I
Chief of Operations
513-487-2819
Tim oth v .Klin g® cbi federal servi ces. com
Greg Meiners/CB&I
Lead Project Scientist
513-487-2821,
Greg. M ei ners® cbi federal servi ces. com
Srinivas Panguluri/
CB&I
Data acquisition and
electronic communications
networking specialist
513-782-4893,
Sri ni vas. Pangul uri ® cbi federal servi ces. com
Gary Lubbers/CB&I
Craftsman
513-569-7076,
Garv. Lubbers® cbifederal services.com
David Elstun/CB&I
Craftsman
513-569-7051,
Davi d. El stun® cbi federal servi ces. com
Lee Heckman/CB&I
Project Microbiologist
513-569-7065,
J ohn. Heckman® cbi federal servi ces. com
Sue Witt/CB&I
Project Scientist
513-782-4726,
Sue. Witt® cbi federal servi ces. com
Jill Webster/CB&I
Project Chemist
513-487-2822,
Jill .Web ster®,cbifederal services.com
Rob Nieman/ALS
Analytical Project Manager
513-733-5336
Rob .Ni eman® ALSG1 ob al. com
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Section 3
3.0 SCIENTIFIC APPROACH
3.1 System/Technology Overview
The WSTB system and the decontamination treatment systems are described in this section.
3.1.1 WS TB Description
The WSTB at INL is constructed from 8-inch diameter drinking water pipe that has been taken out
of service. The pipe was exhumed from the INL grounds (by INL personnel) and oriented in the
shape of a small drinking water distribution system. The WSTB has service connections to
simulate water demands and removable coupons to sample pipe interiors. Experiments focused
on contamination and decontamination will take place in the WSTB. Figure 3-1 depicts the main
features of the WSTB.
End o(
Flow Meter
Pressure Gauge
Instrument Panel 1 (Upstream, Cellular)
Instrument Panel 2 (Downstream, Radio)
Valve, Open
Valve. Closed
Valve, Partly Open
Fire Hydrant
Flushing Hydrant
Blind Flange
Pressure Reducing Valve
Check Valve'BdcWIuw Preventer
Service Connector (Closed)
Existing fire Hydrant
Drinking Water
from
INL Pufflphouse"
Fire Hose £
Not to Scale
15-ft Coupon Section
1 00-
TIT™
Bulk Water Sample Tap
Start of WSTB |—|—J
Injection Port -1x3
Parking
Area
Drainage
Ditch
Figure 3-1: Schematic Overview of WSTB
As depicted in Figure 3-1, the source water at INL is connected to the WSTB through an existing
fire hydrant. The WSTB consists of 400-feet of 8-inch diameter cement-lined iron pipe. The total
volume of the WSTB is estimated to be 1,044 gallons. During infrastructure decontamination
experiments, a positive displacement pump will be used to inject the target contaminant at the
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Section 3
beginning of the 400-foot pipe length (as shown in Figure 3-1). A 15-foot PVC pipe-segment is
installed that contains 10 sets of duplicate removable coupons of specified pipe material to measure
biofilm growth, contamination, and effectiveness of decontamination (a.k.a. coupon section in
Figure 3-1). The pipe material for the 20 small coupons (7/10 of an inch in diameter) has been cut
from cement mortar-lined iron pipe from INL and set into threaded plugs that will be inserted into
the coupon section of the pipe. The twenty coupons are individually numbered CP-0/CP-0D
through CP-9/CP-9D (D represents duplicate since duplicate coupons are removed during
sampling).
The lagoon has a water storage capacity of 28,000 gallons. The water, contaminant, and
decontaminant used during the pipe conditioning and experimental phases (described later in
Section 3.2) will be conveyed via the drainage ditch and discharged to the lagoon. The discharged
water will be trucked out for disposal on a weekly basis. During the conditioning phase, the system
will be operated at 2.5 gallons per minute (gpm), resulting in a total of 25,200 gallons discharged
per week (gpw). The partially closed valve near the end of WSTB (shown in Figure 3-1), along
with the flow meter, will be used to regulate and maintain flow. During the
contaminant/decontaminant injections, the system will be operated at a higher flow rate (-15 gpm)
to reduce travel time and manage sampling activities. The higher system flow rate operations (-15
gpm) will be for short durations (1 to 2 hours at a time). Overall, even if the system was run at
this high flow rate for a full day, the total discharge is 21,600 gallons, which is within the lagoon
capacity. Suitable arrangements will be made by INL to empty the lagoon on a more frequent
basis, as necessary, during the experimental phase.
As shown in Figure 3-1, the WSTB will be equipped with sensors in the instrumentation panels
(IP1 and IP2) that continuously measure two basic water quality parameters: free chlorine and
Total Organic Carbon (TOC). One Hach CL-17 chlorine analyzer and one RealTech M4000 TOC
analyzer will be included in each of the instrumentation panels. The Hach CL-17 chlorine analyzer
uses colorimetric DPD chemistry to monitor water continuously for free chlorine. The RealTech
M4000 uses the ultraviolet (UV) 254 nanometer wavelength (i.e., UV254) for determining the
TOC content. UV254 instruments are often used as an inexpensive indicator of TOC in water.
UV254 measurements are known to have some bias towards aromatic organics; however, they are
relatively inexpensive to maintain and operate when compared to the traditional UV-persulfate
based TOC analyzers. The 8-inch pipe system is constructed directly over the lined drainage ditch
for spill/ leak containment. Figure 3-1 depicts the drainage ditch offset in order to present the
equipment more clearly.
Two fire hydrants will be installed in the pipe and one of the units (downstream location) is a
flushing hydrant that will be used to automatically flush the pipe when anomalous water quality
events are detected in the WSTB for the dechlorination/flushing test described in Section 3.2.2.
3.1.2 Treating Large Volumes of Contaminated Water
As mentioned previously, up to four large volume water treatment technologies are expected to be
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Section 3
tested to determine their ability to disinfect large volumes of biologically contaminated water.
Figure 3.2 depicts a schematic layout of the proposed testing.
Treatment
Technologies to be
Tested
To Disposal
(Truck)
Lagoon
B. globigii
Thiosulfate to
de-chlorinate
Inlet
Bladder
Tank(s)
Outlet
Tank/
Trough
Figure 3-2: Large Water Volume Testing Schematic
The following four technologies will be studied to determine their effectiveness in
decontaminating large volumes of water contaminated with B. globigii'. 1) Hayward Saline C 6.0
Chlorination System, 2) Advanced Oxidation Process (AOP) Ultraviolet (UV)-Ozone System, 3)
Solstreme UV System, and 4) WaterStep Chlorinator.
1. Hayward Saline C 6.0 Chlorination System - This is a commercial pool chlorination
system that operates by electrolyzing sodium chloride (NaCl), salt that has been added to
the pool to form free chlorine for disinfection. To operate the system salt is added directly
to the pool at least 24 hours before the system is started. Roughly 28 pounds of salt is
recommended for every 1,000 gallons of pool water to reach 3500 ppm.
2. AOP UV-Ozone System - The AOP system in a trailer was custom-built at the EPA T&E
Facility in Cincinnati, Ohio. The AOP system is comprised of four major components -
the Power Prep 66 (air preparation unit), CD2000 (ozone production unit), Trojan UVMax
(UV generation unit), and the Aquionics UV (UV generation unit). This AOP system was
designed for the treatment and destruction of organic compounds and microbes in water.
The AOP trailer will be operated with both the CD2000 ozone generator and the Aquionics
UV system operating in series.
3. The Solstreme™ UV System - Uses an electrode-less lamp technology to provide UV
disinfection. The system is expected to provide much higher level of UV dose compared
to an equivalent electrode based UV lamp.
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4. WaterStep Mobile Water System (MWS) - The MWS uses sodium chloride (salt) to
generate chlorine to disinfect water. The system operates on either 120V electricity, 12
volt DC battery, or available hand pumps and solar panels.
3.2 Experimental Design and Test Conditions
Overall, three different types of experiments or tests will be performed using the WSTB. They are
presented in the order of the projected timeline for current contract year (June 1, 2015 through
May 31, 2016). The disinfection of large volumes of water, not using the WSTB is summarized in
Section 3.2.1 (August 2015), and the contamination/decontamination tests are summarized in
Section 3.2.2 (September 2015). Dechlorination/flushing tests are described in Section 3.2.3
(previously completed and optional for the current year). The detailed projected timeline is
summarized below for completing the equipment setup and performing the experiments:
• May 14, 2015 - The WSTB was drained and shut down over the winter (2014 to 2015).
Return the WSTB to baseline activity in accordance to the previous version of this QAPP
(Revision 0). Fill pipe and collect large volume samples to determined, globigii residual
from previous testing in October 2014. Set up and turn on upstream and downstream
instrument panels.
• May 19, 2015 - Decontaminate pipe with C102 in accordance to the previous QAPP
(Revision 0). Collect samples ford, globigii, CIO2, and free and total chlorine.
• May 20, 2015 - Flush pipe with fresh water and begin conditioning in accordance to the
previous QAPP (Revision 0). Purge flow is 2.5 gpm.
• August 12, 2015 through 21, 2015 - Personnel onsite to prepare and conduct testing
using the following four large water volume decontamination technologies: 1) Hayward
Saline C 6.0 Chlorination System, 2) Advanced Oxidation Process (AOP) Ultraviolet
(UV)-Ozone System, 3) Solstreme UV System, and 4) WaterStep Chlorinator.
• September 14 - 18 or 21 - 25, 2015 - Conduct crude oil contamination/decontamination
testing (in the WSTB)
• September 25, 2015 - October 30, 2015 - Collect large volume samples by INL, and
analyze by CB&I.
• October 31, 2015 - Drain and winterize pipe by INL. Place instrument panels in storage.
• April/May, 2016 - Fill pipe and set the instrument panels in place. Begin conditioning of
the pipe.
3.2.1 Disinfection of Large Water Volumes
This experiment will assess the ability of a portable disinfection unit to disinfect a large volume
of water containing Bacillus spores. The following four treatment technologies will be evaluated
to decontaminate the water from the lagoon: 1) Hayward Saline C 6.0 Chlorination System, 2)
Advanced Oxidation Process (AOP) Ultraviolet (UV)-Ozone System, 3) Solstreme UV System,
and 4) WaterStep Chlorinator. The effectiveness of individual treatment technology will simply
be evaluated based on a mass balance approach where the water containing B. globigii spores
drawn from the lagoon will be sampled before it enters the individual treatment technology and
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then after to determine its effectiveness.
Water will be pumped from the lagoon into an inlet bladder tank system that contains a mixing
pump to provide a continuous stream of B. globigii spores contaminated water as shown in Figure
3-2. A target inlet concentration of greater than 106 spores/100 mL (or 104 spores/mL) will be
prepared using the inlet tanks and mixers. The water will then be pumped through one or more of
the treatment units to be tested. Each unit will be tested for a minimum of 1 hour, up to a maximum
of 6 hours. Pre-treatment and post-treatment water samples for B. globigii analysis will be
collected at the same time. Two pre-treatment and two post-treatment samples will be collected
for each system per hour. Each treatment system is expected to be operated at nominal rate of 5
gpm. If disinfectant such as free chlorine is used in the treatment unit, this will be measured once
per hour.
The Hayward Saline C 6.0 Chlorination System is an in-situ type of treatment technology,
therefore it will be operated using the lagoon as the "pool" or source of water. The day before this
system is tested, the lagoon will be drained and approximately 126 lbs of salt will be added to the
lagoon where the water flows in from the WSTB. The water from the WSTB will then be run at 5
gpm for approximately 15 hours (releasing -4,500 gallons) and allowed to mix with the salt in the
lagoon. Required amount of B. globigii will be added to reach a concentration of greater than 106
spores/100 mL (or 104 spores/mL) in the lagoon. For the purpose of evaluation, influent samples
from four locations in the lagoon will be collected, then the system will be started and operated at
the manufacturer recommended rate of 40 gpm for greater than 6 hours and periodic
treated/effluent samples will be collected.
3.2.2 Contamination/Decontamination Tests
These experiments involve contamination of the WSTB using crude oil (September 2015), and the
subsequent decontamination of WSTB using a flushing event at 15 gpm for 1 hour followed by an
injection of Dispersant and/or Surfactant (for crude oil decontamination). Each
contamination/decontamination experiment consists of the following main steps:
Step 1 - Pipe conditioning (cultivation of biofilm)
Step 2 - Instrumentation panel, injection equipment setup and background sampling
Step 3 - Preparation of contaminant stock and contaminant injection (addition of crude
oil to the WSTB)
Step 4 - Preparation of decontaminant and decontamination using flushing along with a
dispersant and/or surfactant for crude oil removal,
Step 5 - Post-decontamination flushing, reconditioning, and monitoring
The actual experiment/testing dates may vary depending upon CB&I/EPA/INL personnel
availability and prevailing weather conditions or other unforeseen events. The dates presented in
the subsequent section are dependent on the starting time-line presented earlier. Any changes in
start date may shift the actual dates and times mentioned in this document.
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Step 1 - Pipe conditioning (cultivation of biofilm)
To effectively study the adsorption of contaminants on pipe walls, it is essential to ensure that
there is a viable biofilm. The biofilm could influence adsorption of the contaminant on the pipe
wall in addition to metabolism, biodegradation, or detoxification of the contaminant.
Previously under EPA Contract EP-C-09-041, CB&I performed a literature review of biofilm
cultivation and identified four primary techniques that could potentially be used for cultivating
biofilm within the WSTB.
1) Sequential batch fermentation and introduction into the WSTB;
2) Using the WSTB as a reactor by passing water with low concentrations of carbon, nitrogen,
and salts;
3) Use of an external annular reactor;
4) Natural biofilm cultivation by passing water through the WSTB.
The fourth option, natural cultivation of biofilm, has been chosen as the cultivation procedure for
testing of the WSTB. This will be accomplished by passing INL tap water through the WSTB
continuously over a period of time (estimated to be a minimum of 4 months - starting mid-May
2015 for the late-September 2015 Contamination/Decontamination testing). After initial flushing
to remove any debris, the flow rate will be set at 2.5 gpm with a total discharge of 25,200 gallons
per week to the lagoon, which allows for weekly trucking and disposal of the accumulated
discharge.
Step 2 - Instrumentation panel, injection equipment setup and background sampling
In late-September 2014, a simple dye tracer study (using non-toxic biodegradable dye, such as
Bright Dyes - www.brightdves.com) was performed to visually confirm the theoretical
calculations of travel times and system flows. This dye tracer study is not planned to be repeated
during future tests.
Mid-September 2015 - Crude Oil Testing
Prior to the contamination Step (Step 3), bulk water samples (BWS-X) and Coupon Samples (CP-
X) will be collected to establish background levels. The BWS samples will be analyzed for crude
oil components such as volatile organic compounds (VOCs), benzene, toluene, ethylbenzene, and
xylene (BTEX), gasoline range organics (GRO), diesel range organics (DRO), and oil range
organics (ORO). Coupon samples will be analyzed for biofilm density using heterotrophic plate
count (HPC), as well as crude oil components. It is expected that crude oil components will be
non-detectable in the baseline samples. Free chlorine (CL-F-#) will also be measured periodically.
All sampling activities related to crude oil testing are summarized in Table 3-1 and analytical
methods are described in Table 4-2.
Step 3 - Preparation of contaminant stock and contaminant injection (addition of crude oil
to the WSTB)
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Mid-September 2015 - Crude Oil Testing
Preparation of Crude Oil (Contaminant Stock) - The crude oil for this study will be obtained from
Marathon Petroleum Corporation. The oil procured will be from the Bakken shale in North Dakota.
In general, the Bakken crude oil presents the same physical properties as gasoline or other fuels.
It will float on water, as its specific gravity is less than 1, and it is considered moderately volatile.
It is also known as "North Dakota Sweet," or "North Dakota Light" crude oil, due to its low sulfur
content. In this respect, it is similar to traditional crude oil from West Texas, known as West Texas
intermediate crude. This type of crude oil is very desirable, and out of each barrel produced,
approximately 95% of it is refined into gasoline, diesel fuel, or jet fuel. (Appendix H - RR10,
2015).
A review of literature indicates that the maximum dissolution of gasoline/diesel (water soluble
fraction) is achieved to 95% completion in 17.5 hours. In this referenced methodology (Guard,
H.E. et al., 1983 - Appendix G), 210 mL of gasoline/diesel is added to 1,890 mL of water (a mix
ratio of 1:9). The mixture is stirred slowly so the meniscus remains intact. The sample is drained
from the bottom of the flask (Guard, H.E. et al., 1983). Since Bakken Crude is considered mostly
gasoline, this methodology will be tested with tap water in Cincinnati. At Idaho this process will
be repeated using water from the Snake River. One 25 liter Nalgene carboy with bottom spigot
will be setup on a stir plate with gentle mixing. The carboy will contain 22.5 liters of water and
2.5 liters of crude. After a minimum of 17.5 hours of mixing, 20 liters of mixed water will be
drawn from the bottom for injection. The drawing from the bottom of the carboy simulates a
miscible crude drawn into the intake of a water treatment plant during a spill event. The 17.5 hour
mixing process represents some weatherization that may occur during a spill event. Preliminary
testing will be performed at the T&E Facility to determine confirm the crude mix ratio.
Contamination Test Protocol - The crude oil suspension as prepared above, will be introduced
into the WSTB using a positive displacement pump. Prior to the introduction of the crude oil (and
in conjunction with the INL) a commercially available appropriately-sized granular activated
carbon (GAC) system will be connected to the outlet of the WSTB. The purpose of this system is
simply to contain any crude oil component from exiting to the lagoon. Once flushing and
decontamination activities are completed the unit will be disconnected. The WSTB will be
operated at 15 gpm under this condition with a minimum contact time of approximately 1 hour (to
accommodate for travel time). Injection duration is also estimated to be 1 hour so that there is a
contact of 1-hour after the bolus of crude oil suspension reaches the coupon section of the pipe.
All sampling activities related to crude oil testing are summarized in Table 3-1 at the end of main
step descriptions.
Step 4 - Preparation of decontaminant and decontamination using flushing along with a
dispersant and/or surfactant for crude oil removal
Mid-September 2015 - Crude Oil Testing
Preparation of Decontaminant Agent Stock - The surfactant, Surfonic TDA-6, was identified
based on EPA pilot testing at the T&E Facility (EPA, 2008). The EPA study indicated that Surfonic
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TDA-6 was effective in removing diesel from the drinking water pipe surfaces. Therefore, Surfonic
TDA-6 (or equivalent decontaminant) will be applied during the current pilot-scale
decontamination of crude oil from the WSTB pipe surface. Twenty five liters of Surfonic TDA-6
flushing mix will be prepared with water for injection.
Decontamination Test Protocol - Once the injected crude oil slug has cleared the pipe, the WSTB
will be flushed for 2 hrs at 15 gpm. This will provide data on whether flushing along removes
crude oil from the water and pipe surfaces. Following the 2 hr flush, the prepared Surfonic stock
solution will be injected into the WSTB (see Table 3-1). Injection of the Surfonic stock solution
will continue until it has reached the end of the pipe (estimated to be approximately 1 hour and 5
minutes based on theoretical calculations and the dye tracer travel time confirmation). Injection
will be stopped, online instrumentation will be stopped, and water flow out of the WSTB will be
stopped for 18-24 hours so that the water containing the surfactant will be stagnant in the pipe to
perform crude oil removal. All sampling activities related to crude oil testing are summarized in
Table 3-1 at the end of main step descriptions.
Step 5 - Post-decontamination flushing, reconditioning, and monitoring
Late-September 2015 - Crude Oil Testing
Following collection of the samples for Step 4 (shown in Table 3-1), the WSTB will be flushed
with fresh water for approximately 1 hour at 15 gpm to clear the surfactant. The flow will then be
reduced to 5 gpm. BWS and CP will be collected following the procedures described in Section
4.2. All sampling activities related to crude oil testing are summarized in Table 3-1.
Table 3-1. Crude Oil Contamination/Decontamination Related Sampling Activity
Sample ID
Sample Description
Estimated Timeline &
System Flow
Step 2 - Background
BWS-0
(Control)
• Collect a sample prior to injection of crude
oil
September 21, 2015
Flow at 2.5 gpm
CP-0, CP-0D
and C12-F-1
• Collect at the same time as BWS-0
• After sampling, turn up flow to 15 gpm
September 21, 2015
Flow at 2.5 gpm
Step 3 - Injection (Start 9:00 AM - Stop 10:00 AM - Travel Time ~ 1 hour)
BWS-1,
BWS-1D, CP-
1 and CP-ID
• Collect after 15 minutes of the injection of
crude oil reaches the coupon section (i.e.,
10:15 AM).
September 21, 2015
Flow at 15 gpm
BWS-2, CP-2,
CP-2D and
C12-F-2
• Collect after 45 minutes of the injection of
crude oil reaches the coupon section (i.e.,
10:45 AM)
September 21, 2015
Flow at 15 gpm
Step 4 - Flushing (10:00 AM - 12:00 PM) / Surfactant Decon. (12:00 PM - 1:00 PM)
BWS-3, CP-3
and CP-3D
• Collect within 5 minutes of the
introduction of surfactant (i.e., 12:05 PM).
September 21, 2015
Flow at 15 gpm
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Sample ID
Sample Description
Estimated Timeline &
System Flow
• Allow surfactant to reach the end of the
pipe - estimate 60 minutes. Stop flow.
BWS-4
• Collect after 1 hour of the surfactant
reaches end of the pipe (i.e., 2:00 PM)
September 21, 2015
Flow at 0 gpm
BWS-5,
BWS-5D and
C12-F-3
• Collect after 2 hours (i.e., 3:00 PM)
September 21, 2015
Flow at 0 gpm
BWS-6, CP-4
and CP-4D
• Collect after 3 hours (i.e., 4:00 PM)
September 21, 2015
Flow at 0 gpm
BWS-7, CP-5,
CP-5D and
C12-F-4
• Collect after 1,200 - 1,440 minutes
(20 - 24 hrs.) i.e., 9:00 AM. Restart flow
flush (5 gpm)
September 22, 2015
Flow at 0 gpm/5gpm
Step 5 - Post Decon. Flushing and Monitoring
BWS-8, CP-6,
CP-6D and
C12-F-5
• Collect after at 3 hours from the start of
flow flush (12:00 PM)
September 22, 2015
Flow at 5 gpm
BWS-9, CP-7,
CP-7D and
C12-F-6
• Collect after at 1,200 - 1,440 minutes (20 -
24 hrs.) from the start of flow flushing and
turn down flow to 2.5 gpm.
September 23, 2015
Flow reset at 2.5 gpm
BWS-10, CP-
8, CP-8D
• Collect after 1,440 minutes of the start of
reconditioning
September 24, 2015
Flow at 2.5 gpm
BWS-11, CP-
9, CP-9D
• Collect after 1,440 minutes of the start of
reconditioning
September 25, 2015
Flow at 2.5 gpm
BWS-12
• INL will collect 7 days after the start of
reconditioning
September 30, 2015
Flow at 2.5 gpm
BWS-13
• INL will collect 14 days after the start of
reconditioning
October 7, 2015
Flow at 2.5 gpm
After completion, leave the WSTB blank coupons in place for shutdown and winter storage.
3.2.3 Dechlorination/Flushing Experiments
The purpose of these experiments are to demonstrate the feasibility of using online water sensors
in concert with flushing hydrants to intelligently divert and remove contaminants from water
distribution systems. For these experiments, the Hach CL-17 and the Real Tech instruments will
be used to signal a flushing hydrant to open and flush the injected contaminant from the WSTB.
For this purpose, a test will be performed using sodium thiosulfate as the "injected contaminant"
to de-chlorinate the system for approximately 30 minutes. A set point or trigger value of measured
chlorine level (e.g., 0.05 mg/L or lower) using the Hach CL-17 at the upstream location will be
used for opening the flushing hydrant valve. After the chlorine value at the upstream recovers
(e.g., > 0.5 mg/L) to the background value, the valve will be automatically triggered to close. Grab
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samples will be collected and analyzed for free chlorine residuals at a downstream location from
the flushing hydrant. The purpose of this grab sample will be to determine if dechlorinated water
is able to "jump" across the "tee" to the flushing hydrant and proceed downstream. Free chlorine
levels for these grab samples will be measured using the Hach DR/890 Pocket Colorimeter. The
triggered flushing experiment will be independent of the contamination/ decontamination
experiment and will occur after the contamination/decontamination experiment if time and weather
permits. These tests were completed in 2014 and may be repeated in 2015 or 2016.
For the second objective, the Hach CL-17 will be used to trigger a flushing event based on chlorine
concentrations, as described above. The RealTech M4000 TOC instrument's ability to trigger
events based on organic concentrations will be evaluated at a later date and the QAPP will be
amended accordingly.
3.3 Measurements and Analytes
The samples generated during the studies described in Section 3.2, will be analyzed for the
following parameters:
• B. globigii (BWS-B (background) and all BWS numbered samples)
• HPC (only sampled prior to start of test - CP-0/CP-0D, BWS-0)
• Free Chlorine (via Hach CL-17 - online upstream/downstream)
• TOC (via RealTech UV254 - online upstream/downstream)
• Free chlorine residuals (downstream grab samples - field measurement)
• Crude Oil components (VOC's, BTEX, GRO, DRO and ORO) BWS and CP numbered
samples
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4.0 SAMPLING PROCEDURES
4.1 Site-Specific Factors
Contamination/decontamination and flushing experiments will be conducted at INL. Samples will
be shipped to the EPA T&E Facility for microbial analysis including HPC and B. globigii and to
ALS Environmental in Cincinnati, Ohio for chemical analysis including VOC, BTEX, GRO, DRO,
and ORO. A summary of the experimental sampling strategy (including the number of samples)
is presented in Table 4-1.
Table 4-1. Summary of Experimental Sampling Strategy
Sample/
Sampling
Location
Matrix
Measurement
Measurement
Location
Sampling Frequency
Total No.
of
Samples
Contamination -
Decontamination
Tests/
WSTB
Biofilm
HPC
T&E Facility
1 sample in duplicate
2
Biofilm/
Coupon
VOC/BTEX
ALS
Laboratory
9 samples in duplicate
18
Water
B. globigii
T&E Facility
38 100 mL samples (all in
duplicate)
76 (100 ml)
Water
VOC/BTEX
ALS
Laboratory
10 samples in duplicate
20
Water
GRO
ALS
Laboratory
10 samples in duplicate
20
Water
ORO+DRO
ALS
Laboratory
10 samples in duplicate
20
Water
Free Chlorine
Field Site
6 samples
6
4.2 Sampling Procedures
Extraction of Biofilm and Spores from Coupon Surface for HPC analyses
The coupons will be collected from the WSTB carefully without touching the surface that was
exposed to WSTB water. The biofilm and spores will be scraped from the surface using a
disposable sterile surgical scalpel. The extracted material will be collected in a sterile sample
bottle with a sodium thiosulfate tablet and 100 mL of pre-filled carbon-filtered water. The
extracted sample will be transferred to a cooler at 4°±2°C. The samples will be shipped overnight
to the EPA T&E Facility and analyzed upon receipt.
Samples for HPC Concentration Measurement
The BWS for HPC concentrations (BWS-0) will be collected using the grab sampling technique
in 100-mL sterile sample bottles with a sodium thiosulfate tablet. The BWS sampling port will be
opened and the water will be drained for 15 seconds prior to collection of 100 ml of water from
the WSTB. The extraction of biofilm from the coupon surface (CP-0/CP-0D) will be conducted
as described in the previous paragraph. The samples will be transferred to a cooler at 4°±2°C. The
samples will be shipped overnight to the EPA T&E Facility and analyzed upon receipt.
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B. alobiaii spores during water treatment experiments
The samples for B. globigii concentrations will be collected using the grab sampling technique in
100-mL sterile sample bottles with a sodium thiosulfate tablet. The sampling port will be opened
and the water will be drained for 15 seconds prior to collection of 100 ml of water from the WSTB.
If needed, 20 L will be collected in 1-gallon flexible plastic bladders (cubitainers) with sodium
thiosulfate tablets (0.01% w/v). A sample of water will be removed from the cubitainers to ensure
that no free chlorine residual is present. The samples will be transferred to a cooler at 4°±2°C. The
samples will be shipped overnight to the EPA T&E Facility and analyzed upon receipt.
To estimate the BWS background (BWS-B), a sample bottle containing sterile buffer solution will
be exposed to background air while the actual BWS is being collected to serve as the background
control.
Samples for Free Chlorine - Field Measurement
During the dechlorination/flushing experiments, grab samples will be collected from a downstream
location of the flushing hydrant using the grab sampling technique and a laboratory beaker and
analyzed for free chlorine. The sample will be immediately processed for measurement using the
Hach Method 10102 (pocket Colorimeter) in the field.
Water Sample Concentrator (if needed)
Once received at the EPA T&E Facility, the 20 L water samples (labeled WSC) will be subjected
to concentration using the water sample concentrator. Vince Gallardo will operate the water
sample concentrator according to EPA NHSRC's Water Sample Concentrator Standard Operating
Procedure (SOP) 030 (Automated Concentrator Ultrafiltration Protocol - Appendix F). The
resulting concentrated sample will be placed into sterile 100 mL sample bottles and analyzed in
the same manner as all other 5. globigii BWS.
Hayward Saline C 6.0 Chlorination System The BWS for B. globigii concentrations from the
influent (i.e., the lagoon water mixed with B. globigii) prior to operating the system will be
collected. After the system is started, periodic effluent/treated samples (BWS-0 through BWS-6)
will be collected from the lagoon. Both influent and effluent samples will be collected using the
grab sampling technique in 100-mL sterile sample bottles with a sodium thiosulfate tablet.
Advance Oxidation Process (AOP) Trailer
The BWS for B. globigii concentrations (BWS-0 through BWS-6) will be collected from the inlet
and outlet of the system using the grab sampling technique in 100-mL sterile sample bottles with
a sodium thiosulfate tablet. The BWS sampling ports at both inlet and outlet of the system will be
opened and the water will be drained for 15 seconds prior to collection of 100 ml of water.
Solstreme, Water Treatment System
The BWS for B. globigii concentrations (BWS-0 through BWS-6) will be collected from the inlet
and outlet of the system using the grab sampling technique in 100-mL sterile sample bottles with
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a sodium thiosulfate tablet. The BWS sampling ports at both inlet and outlet of the system will be
opened and the water will be drained for 15 seconds prior to collection of 100 ml of water.
WaterStep Mobile Water System
The BWS for B. globigii concentrations (BWS-0 through BWS-5) will be collected from the inlet
to the WaterStep MWS sampling port using the grab sampling technique in 100-mL sterile sample
bottles with a sodium thiosulfate tablet. The influent sample wil be collected from the sample port
after the MWS system bladder tank is filled and prior to system operation). Because it is a closed
system (where the chlorine generated is continuously mixed with the contents in the MWS system
bladder tank), periodic effluent samples from the bladder tank will be collected to represent the
various stages of treatment. The BWS sample port of the system will be opened and the water will
be drained for 15 seconds prior to collection of 100 ml of water.
Extraction of Crude Oil from Coupon Surface for VOC/BTEX analyses
The coupons will be collected from the WSTB carefully without touching the surface that was
exposed to WSTB contaminated/decontaminated water. The coupon surface will be scraped using
a disposable sterile surgical scalpel. The extracted material will be collected in the sample bottle
provided by ALS for this analysis. The extracted sample will be transferred to a cooler at 4°±2°C
and shipped to ALS Environmental (so that it arrives before the 48 hour hold-time) to be analyzed
upon receipt.
BWSs for VOC/BTEX/GRO/DRO/ORO
The BWS for VOC and BTEX combined, DRO and ORO combined, and GRO will be collected
using the grab sampling technique in the 40 mL Volatile Organic Analyte (VOA) vial 100-mL
with preservative (hydrochloric acid) provided by ALS Environmental. The BWS sampling port
will be opened and the water will be drained for 15 seconds prior to collection of the sample from
the WSTB. The samples will be transferred to a cooler at 4°±2°C. The samples will be shipped
overnight to ALS Environmental for analysis.
4.3 Sampling Containers and Quantities
Sample containers and quantities are shown in Table 4-2.
4.4 Sample Preservation and Holding Times
Sample preservation and holding times are shown in Table 4-2.
4.5 Sample Labeling
Sample identification is discussed in Section 3 and summarized below.
Samples collected for analysis will be identified by type (BWS, CP, or Grab), collection interval
(-0, -1, -2, etc.), analysis (B. globigii, HPC, free chlorine CL2-F, BTEX/VOC, GRO, ORO/DRO),
and date collected. Duplicate coupons will be identified using a "D" after the collection interval.
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Section 4
Table 4-2: Grab Sampling and Analytical Procedures
Measurement
Sampling Method
Analysis Method
Sample Container/
Quantity of
Sample
Preservation/
storage
Holding
times
Free Chlorine
As specified in
Section 4.2
Appendix B
Hach Method 10102
Glass beaker (~50
mL)
None
Immediate
B. globigii spore
As specified in
Section 4.2
Appendix C
CB&I T&E SOP
309
100 mL sterile
sample bottles
20 L cubitainers1
The bottles
contains sodium
thiosulfate tablet.
Cool 4 ± 2°C
Analyze
upon receipt
at the EPA
T&E
Facility.
HPC
As specified in
Section 4.2
Appendix A
CB&I T&E SOP
304
100 mL sterile
sample bottles
The bottles
contain sodium
thiosulfate
tablets. Cool 4 ±
2°C
48 hours
VOC/BTEX
(Bulk Water)
As specified in
Section 4.2
EPA Method
SW8260B
40 mL VOA vial
The bottles
contain
hydrochloric acid.
Cool 4 ± 2°C
14 days
GRO (Bulk
Water)
As specified in
Section 4.2
EPA Method
SW8015A
40 mL VOA vial
The bottles
contain
hydrochloric acid.
Cool 4 ± 2°C
14 days
ORO/DRO (Bulk
Water)
As specified in
Section 4.2
EPA Method
SW8015B
1 L amber bottle
minimum 200 mL
Cool 4 ± 2°C
7 days
VOC/BTEX
(Biofilm
Coupons)
As specified in
Section 4.2
EPA Method
SW8260B/5035
sampling kit2
40 mL tared VOA
vial with a stir bar
Cool 4 ± 2°C
48 hours
1 The 20 L cubitainer samples will be concentrated via the water sample concentrator and placed into the 100 mL
sterile sample bottles for analysis.
2Method 5035 - Closed-System Purge-and-Trap and Extraction for Volatile Organics in Soil and Waste Samples
4.6 Sample Packaging and Shipping
The biofilm samples, BWSs, and WSC samples will be preserved in coolers with ice and shipped
to the EPA T&E Facility overnight. Chain-of-custody forms will be completed and shipped with
the samples. The Chain-of-Custody form is presented as Appendix E.
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Section 5
5.0 MEASUREMENT PROCEDURES
5.1 ANALYTICAL METHODS
The analysis methods are shown in Table 4-2. The microbiological methods are further discussed
below for the B. globigii contamination/decontamination testing.
HPC determinations will follow T&E SOP 304, Heterotrophic Plate Count (HPC) Analysis Using
IDEXX SimPlate Method. This method is based on multiple enzyme technology which detects
viable bacteria in water by testing for the presence of key enzymes known to be present in these
organisms. It uses multiple enzyme substrates that produce a blue fluorescence when metabolized
by bacteria. The sample and media are added to a SimPlate plate, incubated, and then examined
for fluorescent wells. The number of fluorescing wells corresponds to a Most Probable Number
(MPN) of total bacteria in the original sample. This method is included as Appendix A in this
document.
Preparation and analysis of B. globigii will follow T&E SOP 309, Preparation and Enumeration
ofB. globigii Endospores. B. globigii is an aerobic spore-forming bacteria used as a surrogate for
evaluating the performance of water treatment systems for removal of bacterial endospores. In
analyzing spores, the indigenous vegetative cells are inactivated by heat treatment. The surviving
bacterial spores in the sample are analyzed by culturing that permits the spores to germinate and
produce bacterial cells. Tryptic soy agar will be used for culturing B. globigii. This method is
included as Appendix B in this document.
The samples are diluted, as necessary, depending on the expected concentration of cells/spores in
the sample. For example, the expected initial concentration of spores in this study is 106
spores/mL. The initial samples will be diluted up to 105 fold. Duplicate plates using 0.1 mL of
the 104 and 105 fold diluted samples will be analyzed using the spread plate method. If the number
of colonies is too many to count in more than one plate, the sample will be diluted and re-analyzed.
If the number of colonies is too many to count for one measurement, the remaining plates will be
considered for enumeration of spore concentration for the sample.
For the crude oil injection test, Standard EPA Methods will be used for analyzing the chemical
constituents. Specifically, EPA Method SW8260B will be used for VOC/BTEX in bulk water,
EPA Method SW8015A will be used for GRO in bulk water and EPA Method SW8015B will be
used for ORO/DRO in bulk water. Due to the limited coupon sample quantity, only VOC/BTEX
contents of the coupon will be analyzed. Specifically, EPA Method SW8260B will be used for the
coupon sample analysis and extraction will be performed using the EPA Method 5035 sampling
kit.
5.2 CALIBRATION PROCEDURES
The calibration procedures, linearity checks, and continuing calibration checks are included in the
T&E SOPs or the instrument manuals for the analysis methods referenced in Table 4-2.
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Section 6
6.0 QUALITY METRICS (QA/QC CHECKS)
6.1 QC Checks
Instalments/equipment will be maintained in accordance with the EPA ORD Policies and
Procedures Manual, Section 13.4 Minimum Quality Assurance (QA)/Quality Control (QC)
Practices for ORD Laboratories Conducting Research and in accordance with the SOPs and
analysis methods listed in Table 4-2, and for field instruments, in accordance with the
manufacturer's instructions. Table 6-1 presents the QA/QC checks to be implemented for the
measurement of the specific parameters.
6.2 QA Objectives
The objectives of this study are described in Section 1.2. These objectives will be addressed by
collecting data on contaminant reduction. Table 6-1 lists the QA/QC checks that will be used to
verify the validity of the analyses conducted on grab samples conducted during this study. Table
6-2 summarizes the QA/QC requirements for the optical devices used in this study.
The RPD is calculated for duplicate analyses based on the following:
(C1-C2)
RPD = — — x 100%
0.5(Ci + C2)
where:
RPD = Relative Percent Difference
CI = Larger of two values
C2 = Smaller of two values
If calculated from three or more replicates, the relative standard deviation (RSD) will be used
according to the following equation:
RSD = 100% —
y ave
where:
RSD = relative standard deviation (%)
5 = standard deviation
yaVe = mean of the replicate analyses
Standard deviation is defined as follows:
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Section 6
f^(y* ~ yave)1
where:
5 = standard deviation
yt = measured value of the ith replicate
yaVe = mean of the replicate measurements
n = number of replicates
Table 6-1: QA/QC Checks for Grab Samples
Measurement
QA/QC Check
Frequency
Acceptance
Criteria
Corrective Action
B. globigii
Positive control
using stock
Once per
experiment
±10 fold of the
spiking suspension
Investigate laboratory
technique. Change
stock organisms and
use new set of media
plates. Re-analyze the
spiking suspension and
change it if necessary.
B. globigii
Negative Control
using sterile buffer
Once per
experiment
0 CFUVplate
Investigate laboratory
technique. Use a new
lot. Re-analyze.
B. globigii
Negative control
for heat shock
Once per
experiment
0 CFU of
vegetative
cell/plate
Investigate the hot
water bath. Heat
samples for longer
period.
B. globigii
Duplicate
Once per
experiment
<20% variation
Consider other
dilutions. Reanalyze.
B. globigii
Field blank (an
open bottle of
sterile water in the
vicinity of the
BWS location)
Every 5 BWS
0 CFU/plate
Determine if
background values
impact results.
HPC
Negative Control
Before every set
of measurements
No fluorescent
wells
Re-analyze sterile
buffer and change it if
necessary.
HPC
Positive Control
Once per
experiment
Fluorescent wells
Investigate laboratory
technique. Re-analyze.
HPC
Duplicate
Once per
experiment
Duplicate plates
much agree within
5%
Investigate laboratory
technique. Re-analyze.
Free Chlorine
Manufacturer DPD
color standards kit
Once per
experiment
As specified by the
color standards kit
Clean the colorimeter
measuring cell. Clean
the DPD standards vials
and recheck.
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Section 6
Measurement
QA/QC Check
Frequency
Acceptance
Criteria
Corrective Action
VOC/BTEX
(Bulk Water)
Initial calibration
check
Once per batch of
20 samples
Pass
If fails repeat
calibration
VOC/BTEX
(Bulk Water)
laboratory control
sample, matrix
spike, and matrix
spike duplicate
Once per batch of
20 samples
Method Criteria
If any of the QA/QC
checks fail utilize the
duplicate sample.
Report with appropriate
qualifier if necessary.
GRO (Bulk
Water)
Initial calibration
check
Once per batch of
20 samples
Pass
If fails repeat
calibration
GRO (Bulk
Water)
laboratory control
sample, matrix
spike, and matrix
spike duplicate
Once per batch of
20 samples
Method Criteria
If any of the QA/QC
checks fail utilize the
duplicate sample.
Report with appropriate
qualifier if necessary.
ORO/DRO (Bulk
Water)
Initial calibration
check
Once per batch of
20 samples
Pass
If fails repeat
calibration
ORO/DRO (Bulk
Water)
laboratory control
sample, matrix
spike, and matrix
spike duplicate
Once per batch of
20 samples
Method Criteria
If any of the QA/QC
checks fail utilize the
duplicate sample.
Report with appropriate
qualifier if necessary.
VOC/BTEX
(Biofilm
Coupons)
Initial calibration
check
Once per batch of
20 samples
Pass
If fails repeat
calibration
VOC/BTEX
(Biofilm
Coupons)
laboratory control
sample, matrix
spike, and matrix
spike duplicate
Once per batch of
20 samples
Method Criteria
Report with appropriate
qualifier if necessary.
a - Colony Forming Unit
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Section 6
Table 6-2. QA/QC Checks for Online Equipment
Instrument/
Measurement
Calibration/QC
Alternative
Frequency
Acceptance
Criteria
Corrective Action
RealTech UV254/
TOC
Custom Zero using
deionized water
One time per quarter
according to
instrument O/M
manual
N/A
Clean the quartz
windows using 5%
bleach solution.
Hach CL-17/
Free Chlorine
Factory calibration
- do not change.
Perform a one-point
check against a
DPD colorimetric
method calibration
based on DPD
method
Quarterly
±10%
Clean colorimeter
and check the
instrument flow.
Modern
Water/Multisensor
1200
Factory calibration
and setup
performed by the
vendor onsite
Leased equipment
for the crude oil test.
Setup/calibration
performed upon
initiation by vendor
NA
NA
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Section 7
7.0 DATA ANAL YS/S, INTERPRET A TION, AND MAN A GEMENT
7.1 Data Reporting Requirements
All data generated during the study will be presented in tabular/spreadsheet format. Table 7-1
identifies the reporting units for the various parameters.
Table 7-1. Reporting Units for Measurements
Measurement
Units
B. globigii
CFU/ mL
HPC
MPN/mL
Free Chlorine
mg/L
TOC
mg/L
VOC/BTEX (Bulk Water/Biofilm
Coupons)
Mg/L
GRO (Bulk Water)
Mg/L
ORO/DRO (Bulk Water)
Mg/L
7.2 Data Validation Procedures
Calculations will be carried out on a computer and will be checked initially by the analyst for gross
error and miscalculation. The calculations and data entered into computer spreadsheets will be
checked by a peer reviewer for accuracy, and checking the calculation by hand or checking entries
of data from the original. Detected errors will be corrected and other data in the same set
investigated before it is released to the EPA WACOR.
7.3 Data Summary
All sample data will be presented by CB&I in tabular/spreadsheet format and submitted to the EPA
WACOR for evaluation. Tabular data summaries will be included in the main discussion of the
reports and raw data will be included as appendices.
7.4 Data Storage
Laboratory records will be maintained in accordance with Section 13.2, Paper Laboratory
Records, of the Office of Research and Development (ORD) Policies and Procedures Manual.
Controlled access facilities that provide a suitable environment to minimize deterioration,
tampering, damage, and loss will be used for the storage of records. Whenever possible, electronic
records will be maintained on a secure network server that is backed up on a routine basis.
Electronic records that are not maintained on a secure network server will be periodically backed
up to a secure second source storage media, transferred to an archive media (e.g., compact discs,
optical discs, magnetic tape, or equivalent), or printed. Electronic records that are to be transferred
for retention will be transferred to an archive media or printed, as directed by EPA.
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Section 8
8.0 REPORTING
8.1 Deliverables
Monthly progress reports will be prepared by the Project Leader and sent to the Program Manager,
and submitted to EPA every month. CB&I will prepare data packages for each analysis to be
placed into CB&I's project central file.
8.2 Final Report
CB&I will be responsible for preparing a data report that will include a description of the WSTB,
how contaminant injections were performed, how decontamination was performed, analyses of
data collected from experiments in the WSTB (including the degree of attachment crude oil), and
the effectiveness of flushing and decontamination. Infrastructure samples (Ci) taken during crude
oil injection will serve as the baseline or initial level of crude oil in the water or on the coupons.
Samples taken during flushing and surfactant addition (Cd) will be compared to the samples taken
during contamination as follows to determine percent decontamination (%D):
Ci — Cd
Coupons will be sampled in duplicate, and Ci and Cd will be the mean of these duplicates. The
duplicate values and well as the range between these duplicate values will be reported in the
tabulated data.
The effectiveness (%E) of individual large volume treatment technologies will be evaluated based
on a mass balance approach where the water containing B. globigii spores will be sampled before
it enters the individual treatment technology (Ci) and then after (Ce) to determine its effectiveness.
Ci — Ce
%E = ——
Ci
%E will be calculated for each time point sampled, but an overall mean %E will be calculated that
using the mean Ci and mean Ce that includes all of the data collected over the course of the
experiment. In this case, the variance of Ci and Ce (Sci and Sce, respectively) will be calculated
and standard error (SE) will be calculated for the mean %E as follows (n is the number of samples).
V n n
The analytical data will be presented in tabular form unless otherwise noted. Tabular data
summaries will be included in the main discussion of the reports, and raw data will be included as
appendices.
The report will include all data tabulated in Microsoft® Excel and Word formats, and will be
provided in print and electronic formats. It will include narratives of the methods and results.
Interpretive graphs will also be provided.
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Revision No. 2
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Section 9
9.0 REFERENCES
CB&I Federal Services LLC (2011). T&E Administrative SOP 101: Central Files. EPA T&E
Facility, Cincinnati, Ohio.
CB&I Federal Services LLC (2012). T&E Technical SOP 304: Heterotrophic Plate Count (HPC)
Analysis Using IDEXX SimPlate Method. EPA T&E Facility, Cincinnati, Ohio.
CB&I Federal Services LLC (2012). T&E Technical SOP 309: Preparation and Enumeration of
B. globigii Endorspores. EPA T&E Facility, Cincinnati, Ohio.
EPA 1994. Method 8020A - Aromatic Volatile Organics by Gas Chromatography, Revision 1,
September 1994.
EPA 1996. Method 8260B - Volatile Organic Compounds by Gas Chromatography/Mass
Spectrometry (GC/MS). Revision 2 1996.
EPA 2007. Method 8015C - Non-halogenated Organics by Gas Chromatography (FID). Revision
3, 2007.
EPA 2008. Pilot-Scale Tests and Systems Evaluation for the Containment, Treatment, and
Decontamination of Selected Materials From T&E Building Pipe Loop Equipment. EPA
Document ID: EPA/600/R-08/016, January 2008.
Guard, H.E., Ng, J., and Laughlin, R.B. (1983). Characterization of Gasolines, Diesel Fuels and
their water soluble fractions. Naval Biosciences Laboratory, Oakland, CA. September 1983.
Hach (2001b). CL-17 Chlorine Analyzer Instrument Manual, Catalog Number 54400-18 10/01
3ed Edition 03, 2001.
Nicholson, W. I., and Setlow, P. (1990). Sporulation, germination and outgrowth. In Molecular
Biology Methods for Bacillus, Edited by Harwood and Cutting, John Wiley and Sons, New York.
RealTech Owner's Manual Version 1.1 for the REAL UV254 M4000 UV254 Monitor, edition and
data are not indicated on the manual.
Rice, E. W., Fox, K. R., Miltner, R. J., Lytle, D. R. and Johnson, C. H. (1994). A microbiological
surrogate for evaluating treatment efficiency. In Proc. of AWWA/WQTC, San Francisco.
RR10. (2015). Bakken Crude Oil. Distributed by the NW Area Committee www.rrtl0nwac.com.
80
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Appendix
Appendix A_304
Heterotrophic Plate C
Appendix A
CB&I T&E SOP 304 - Heterotrophic Plate Count
(HPC) Analysis Using IDEXX SimPlate Method
Appendix B_DR 4000
Chlorine-Free Methoc
Appendix B
Hach Method 10102 for Measuring Free Chlorine in
Water
E
Appendix C_309 for
Preparation of B. glot
Appendix C
CB&I T&E SOP 309: Preparation and Enumeration of
B. globigii Endospores
E
Appendix D
Preparation of the G02 4,000 ppm Solution
¦_ 1
Appendix
D-G02_International.
ESI
^ I
Appendix E
EPA Sample Chain of Custody Form
Appendix
E_EPA_COC_Form. pc
pi
Appendix F
EPA Water Concentrator SOP
mL-1
Appendix F_Water
Concentrator SOP.pd
Gasoline In Water
a270016.pdf
Appendix G
Characterization of gasolines, diesel fuels & their
water soluble fractions
BakkenCrude Info 1
50213064220.pdf
Appendix H
Bakken Crude Oil
81
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Appendix B: Summary of Technology Specific Considerations
82
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Technology
Considerations
EPA AOP trailer*
Solstreme*
Water Step*
Hay ward*
Market
Availability
Low. Originally custom
designed by EPA for a
remediation project to provide
advanced oxidation with UV
and Ozone. A trailer-mounted
system that was re-purposed
and tested for disinfection.
One ozonation process
component (Speece Cone
diffuser) not commercially
available. Other UV and
ozonation process components
commercially available.
Medium. New startup company developed
an innovative electrodeless UV lamp
design. Made upon order
fhttD://www. solstreme. com/)
High. Commercially available off-
the-shelf product from a non-profit
organization for producing drinking
water in communities in developing
countries. Self-contained kit, could
be used in disaster zone to purify
water even if there was no power.
Available from httD://watersteD.ora/
High. Commercially available in-
situ chlorine generator, off-the-
shelf product from a pool product
manufacturer. Commonly used for
disinfecting swimming pools.
Available from
httD://www.havward-Dool.com/
Capital Cost
High (estimated > $40,000).
Custom design, process
components, plumbing,
trailer, etc.
Medium (est. $15,000).
Medium (est. $8,000). Includes
storage bladders, pump, battery,
charger, solar cell,
mounting/transportation rack, and
salt based chlorine generator
(Chlorinator).
Low. $4,000
Shipment to
Site
Medium. Requires a tow
vehicle to pull the trailer to
site. Trailer may require State
inspection and driver that
meets the training
requirements for towing the
vehicle.
Low. Requires a custom-box (wooden crate
or cardboard box with contoured foam) and
can be shipped via third party shipper to
site. No chemicals or hazardous materials
to ship. Can be carried in a truck or a
personal car to site.
Medium. Needs to go on a truck or
commercial transportation. Could
be transported in a car, if mounting
and transportation rack are not used.
Low. Small package easy to ship or
carry in a car.
Setup
Considerations
Medium. Requires 110 and
220 Volt AC electric or
generator, the plumbing
connections to the process
units need to be reassembled
on site. The Ozonator cone
setup requires 2-3 persons
onsite to assemble.
Low. Plug and play needs 110 Volt AC
electric. If water is turbid, a pre-filter is
recommended for optimal use. Temperature
of the water (i.e., cold < 55°F) impacts
operations. Comes with cam lock type
connectors. One person can set it up in the
field.
Medium. Need flat surface to spread
out the bladder tanks. Need to
recirculate chlorinated water to
provide contact time for
disinfection. Not a flow through
system. Strip kit required to
periodically check chlorine
generation. After disinfection, if
chlorine is not consumed, the excess
chlorine needs to be neutralized
before discharging to the
environment.
Medium. Can be setup on a table.
Requires a 40 gpm (151.4 L/min)
pump to run salted water through
the system. Salt needs to be added
to the source water in sufficient
quantities (3,000 to 5,000 ppm).
Chlorine generation can be varied
as needed. Need to recirculate
chlorinated water to provide contact
time for disinfection. Not a flow
through system. Strip kit required
to periodically check chlorine
generation.
83
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Technology
Considerations
EPA AOP trailer*
Solstreme*
Water Step*
Hay ward*
Operational
Considerations
Medium. Requires operation
of valves to remove air from
the process units, valve
adjustment to meet pressure
and flow requirements. Some
of the vented air may contain
contaminated droplets of
water that need to be
contained or recirculated back
through the system. There are
excess ozone emissions from
process unit that need to be
destroyed or vented. The
catalytic destruction unit was
un-operable, the unit had to be
vented. Flow rate needs to be
less than 5 gpm (18.9 L/min).
Low. High turbidity and cold water
adversely affect the disinfection process. It
gets better results with water in the 70°F to
90°F temperature range and low turbidity.
If high disinfection is desired a heat
exchanger may also be needed to regulate
water temperature. The cost of the heat
exchanger will depend on the size of the
unit.
Low. Simple to operate on a short-
term basis. If extended contact
period is required greater than 3
hours, the salt solution needs to be
replenished, electrolytic cell has to
be drained, and if not on 110 volt
AC power, the battery needs to be
charged.
Low. Requires 110 volt AC power,
high capacity (40 gpm (151.4
L/min)) pump. Initial setup requires
the chlorine production of the
system to be slowly ramped up by
starting at -50% production rate
and increased incrementally. Salt
may need to be added depending
upon usage. While it could be
operated using bladder tanks, but
suited for open pools.
Maintenance
and
Consumables
Low. UV lamp replacement,
pump repair when needed.
Dual voltage electric supply
(see setup consideration).
Low. If the processed water is turbid, the
system (inside quartz sleeve) will need to
be cleaned frequently. Other than regular
commercially available cleaning agents, no
other consumables are required. The UV
lamp is electrodeless microwave
technology, expected to last more than 10
years. The quartz sleeve although robust
needs to be handled carefully while
cleaning. A plunger type device for
cleaning the interior of the sleeve is
recommended and gloves should be used to
prevent smudging of the outside surface.
Low. Table salt is the only
consumable. For optimal chlorine
generation, the electrolytic cell
needs to be cleaned periodically.
Pumps, hoses and O-rings need to
be checked as needed.
Low. High purity salt (NaCl
-98%). Pump and hoses need to be
checked as needed.
Result
Summary
Under Tested
Conditions
Under the tested conditions,
an average of 4-log removal
of B. globigii was observed in
this flow through type
operation (removal varied
from 1.5 to 5 log). Improved
understanding of the EPA
AOP system performance
may improve the consistency
of disinfection.
A 3.5-to 4-log removal of B. globigii was
observed in a flow through type operation.
A 7-log removal of B. globigii was
observed in a batch type operation
with 300-minutes of contact time.
The unit achieved a 4.3 log
reduction of B. at a Ct of almost
7,000 mg-min/L.
* Mention of trade names or commercial products does not constitute endorsement or recommendation for use of a specific product.
84
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Appendix C: Technical Bulletin SURFON/C® DOS-75PG Surfactant
85
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HHLI
Enriching lives through innovation
Technical Bulletin
SURFONIC® DOS-75PG Surfactant
GENERAL NAME Dioctyl sodium sulfosuccinate
PRODUCT DESCRIPTION
SURFONIC® DOS-75PG surfactant is an anionic sulfosuccinate surface-active agent
with excellent wetting and surface tension reducing properties. The solvent system is
a mixture of propylene glycol and water. SURFONIC® DOS-75PG surfactant is
compatible with other anionic surfactants and with nonionic surfactants.
APPLICATIONS • wetting agents • detergents
• solubilizing agents • dispersants
• emulsifiers
SALES SPECIFICATIONS
Property
Appearance, 25°C
Anionic Active, wt%
Color, Pt-Co
pH, 5% in distilled water
'Methods of Test are available from Huntsman Corporation upon request.
TYPICAL PROPERTIES
Specifications Test Method*
Clear liquid ST-30.1
69-71 ST-31.145
60 max. ST-30.12
5.0-7.0 ST-31.36, C
Chemical Properties
Molecular Weight (theoretical) 444
Water Solubility Soluble
Regulatory Information
DOT/TDG Classification Not Regulated
HMIS Code 1-1-0
CAS Number 577-11-7
TSCA Inventory Yes
WHMIS Classification D2B
Canadian DSL Yes
Physical Properties
Flash point, PMCC, °F 248
Flash point, PMCC, °C 120
Freeze point, °F -4
Freeze point, °C -20
Density, g/ml at 25°C (77°F) 1.120
Weight, lbs/US gal at 25°C (77°F) 9.33
Viscosity, Brookfield
cps at 20°C (68°F) 700
86
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HUMTSBFI^IjPIlM
Enriching lives through innovation
TOXICITY AND SAFETY
For information on the toxicity and safe handling of this product, please read the Material Safety Data Sheet
prior to use of the product.
HANDLING AND STORAGE
SURFONIC® DOS-75PG surfactant may be satisfactorily stored in stainless steel tanks using stainless steel
pipes and pumps. Carbon steel tanks are not recommended; storage in carbon steel for extended periods of
time may cause discoloration of the product due to rusting. For this reason, lined, stainless steel or fiberglass
tanks are recommended. An inert atmosphere such as nitrogen should be maintained in larger storage
vessels.
Solid sediment may form upon standing. There should be circulation in the storage vessel to keep solids
suspended.
Low pressure steam coils in storage tanks and steam tracing of transfer lines should be provided in cases
where low environmental temperatures may make pumping of the product difficult.
SHIPPING DATA
Product is available in tank cars, tank trucks and drums of 485 pounds (220 kilograms) net weight. Small
samples are available by contacting our sample department at 1-800-662-0924.
BIODEGRADABILITY AND ENVIRONMENTAL SAFETY
SURFONIC® DOS-75PG surfactant and related products have been shown to undergo 90% to 98%
biodegradation in 11 to 17 days.
General References
Swisher, R. D., Surfactant Biodegradation, Marcel Dekker, 1987.
Huntsman Corporation
Business Offices
10003 Woodloch Forest Dr.
The Woodlands, TX 77380
(281)719-6000
Huntsman Advanced Technology
Center
Technical Service
8600 Gosling Rd.
The Woodlands, TX 77381
(281)719-7780
Samples 1-800-662-0924
www.huntsman.com
Copyright © 2007 Huntsman Corporation or an affiliate thereof. All rights reserved.
SURFONIC® is a registered trademark of Huntsman Corporation or an affiliate thereof in one or more, but not all countries.
Huntsman Petrochemical Corporation warrants only that its products meet the specifications stated in the sales contract. Typical properties,
where stated, are to be considered as representative of current production and should not be treated as specifications. While all the
information presented in this document is believed to be reliable and to represent the best available data on these products, NO
GUARANTEE, WARRANTY, OR REPRESENTATION IS MADE, INTENDED, OR IMPLIED AS TO THE CORRECTNESS OR
SUFFICIENCY OF ANY INFORMATION, OR AS TO THE MERCHANTABILITY OR SUITABILITY OR FITNESS OF ANY CHEMICAL
COMPOUNDS FOR ANY PARTICULAR USE OR PURPOSE, OR THAT ANY CHEMICAL COMPOUNDS OR USE THEREOF ARE NOT
SUBJECT TO A CLAIM BY A THIRD PARTY FOR INFRINGEMENT OF ANY PATENT OR OTHER INTELLECTUAL PROPERTY RIGHT.
EACH USER SHOULD CONDUCT A SUFFICIENT INVESTIGATION TO ESTABLISH THE SUITABILITY OF ANY PRODUCT FOR ITS
INTENDED USE. Liability of Huntsman Petrochemical Corporation and its affiliates for all claims is limited to the purchase price of the
material. Products may be toxic and require special precautions in handling. For all products listed, user should obtain detailed information
on toxicity, together with proper shipping, handling and storage procedures, and comply with all applicable safety and environmental
standards.
87
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vvEPA
United States
Environmental Protection
Agency
PRESORTED STANDARD
POSTAGE & FEES PAID
EPA
PERMIT NO. G-35
Office of Research and Development (8101R)
Washington, DC 20460
Official Business
Penalty for Private Use
$300
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