4/6/2016

Universidad ORT Uruguay, Montevideo, April 4-8, 2016

Management and remediation of

sites for extractive industries
Subhasis Ghoshal
Department of Civil Engineering
McGill University, Canada

Organizer: Prof. Lorena Betancour, Universidad ORT Uruguay

Pump-and-Treat Remediation

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Pump and Treat Remediation

Wide use since 1980s
75% of Superfund sites

1990s: ability to achieve complete aquifer restoration?

Slow decrease in contaminant concentrations, tailing
and rebound

Technology Objectives
Objective of technology
Hydraulic containment using pumping wells (& to a lesser
extent: subsurface drains, trenches and barrier walls
Treatment of contaminated water

Prerequisites
thorough site characterization
Contaminant types and distribution
Hydrogeology

Source removal (excavation, pumping of NAPL)?

Treatment objectives realistic goals needed

For high degree of clean-up: homogeneous and permeable
strata in aquifers, no NAPL contamination, non-sorbing
contaminants

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The Clean-up Challenge: Tailing and Rebound

Tailing: progressively slower rate of decline in
contaminant concentrations

Rebound: rapid increase in contaminant

concentrations after pumping has stopped

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Tailing and Rebound

Effect of Tailing and Rebound on Remediation
Longer treatment times
Residual concentration in excess of cleanup
standard
Contributing factors
Slow release of solutes from NAPLs
Slow contaminant desorption
Slow precipitate dissolution (for heavy metals)
Slow diffusion of compounds from clay layers
and lenses

Factors contributing to tailing:

Effect of mass transfer from source (sorbed phase,
NAPL or diffusion limited zone)

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Factors contributing to tailing:

Effect of clay layer thickness and

Factors contributing to tailing:

Effect of geological stratification

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Capture Zones
Hydraulic containment: to prevent further
spreading of plume
Extraction wells create capture zones

Groundwater
Flow Lines

Equipotential Lines

PW = pumping well

Capture Zones

Groundwater flow

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Placement of well with respect to

plume size

Optimizing Design and Operation

Pulsed pumping

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Variations and Alternatives

Horizontal and inclined wells

Intercepting Fractures

Accessing Beneath Structures

Enhancements to Pump and Treat

Surfactants (SURFace ACTive agents)
Micelle

Water
CMC

NAPL
Monomer

Critical Micellar Concentration (CMC)

Surfactant concentration

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Enhancements to Pump and Treat

Surfactants (SURFace ACTive agents)
Aqueous Phase

Surfactant Micelle

Solubilization
related to Kow

NAPL Phase

Enhancements to Pump and Treat

Ci, total

Solute Concentration (moles/L)

Surfactants (SURFace ACTive agents)

Ci, micellar

Ci, aqueous
CMC
Surfactant Concentration, Csurf (moles/L)

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Enhancements to Pump and Treat

Soil Flushing

k g h
Nc =

l

Iron-Nanoparticles for
groundwater remediaion

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Groundwater Contamination by
Chlorinated Solvents
Solvent
Release

Pollutant
Plume
Solvent

Water
Well

Trichloroethylene,
perchloroethylene
Carcinogenic, neurotoxic
Restoration of groundwater
to meet drinking water
standards have not been
successful
~1 million Kg of chlorinated
solvents improperly
discharged into ground in
U.S & Canada

Why Nano Fe(0)?

Fe203

Heavy metals

Chlorinated
organics

Theron et al., 2008

Core-shell structure of nanoscale

zero valent iron (NZVI) particles

Very High Reactivity

Niche applications for
reducible pollutants
(chlorinated organics, heavy
metals, nitrates, radioactive
waste, PCBs)
Rapid in situ treatment of
groundwater contamination
Low cost and commercially
available
Toxicity?

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Nanoscale Zero Valent Iron

23

Bioremediation vs remediation with Fe0

Biodegradation

Reactions with Fe0

Roberts et al., 1996

Arnold et al., 2005

Reactions with Fe0

Stable reaction products are
acetylene, ethene, ethane

Biodegradation Reactions
Only Dehalococcoides - Capable of
complete dechlorination to ethene

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nZVI-based
in situ remediation
Source
Injection of nZVI-slurry

Water table

Groundwater flow direction

nZVI and pollutant
reaction

Iron oxides and

hydroxydes

Contaminated Plume
Decontaminated Zone
R

Direct introduction of nZVI into the environment

Cl

Fe

+ H+

R H
+ Cl-

nZVI-based in situ remediation

Contaminant Source
Injection of nZVI-slurry

Water table

Groundwater flow direction

Contaminated Plume
Decontaminated Zone

Limited transport of bare nZVI

Polymer
-nZVI

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Iron Nanoparticle Aggregation &

Effects of Polyelectrolyte Coating
Electostatic repulsion force

Magnetic attraction forces

Electostatic + steric repulsion force

Polymer
Coating:
Carboxymethyl
Cellulose (CMC)
Magnetic attraction forces

Bare-nano Iron
accumulation
In a sand packed
column

Polymer
stabilized
nano-iron
distribution in
a sand packed
column

Mobility enhancement:
polymer coated nZVI
Causes for enhanced mobility:
Reduced aggregation of nZVI due to charge and steric
stabilization
dispersed particles
reduced deposition and filtration of nZVI in porous
media

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Polymer-Coated NZVI
H2O

FeSO4 + NaBH4 + stabilizer

Fe

+ sulfate and boronic salts

Carboxymethyl cellulose: very efficient in colloidally stabilizing particles

Synthesized particle size different for the different polymers
All polyelectrolytes showed binding to the Fe(0)/FeOOH surface.
Cirtiu, Raychoudhury, Ghoshal, Moores.
Colloids and Surfaces A: Physicochem. Eng. Aspects 390 (2011) 95 104

Bottom-up synthesis of CMC-NZVI

H2O

FeSO4 + NaBH4 + stabilizer

Fe

+ sulfate and boronic salts

5 g/L CMC, 1 g/L Fe 5 nm avg dia.

FTIR spectrum of CMC-ZVI
5 g/L CMC, 2 g/L Fe 75 nm avg dia.

Transmittance (%)

CMC-ZVI
CMC

Carboxymethyl cellulose (CMC)

stabilizer

R
C

Fe

Fe

Bidentate bridging
interaction

asymCOO
-

symCOO

600 900 1200 1500 1800 2100 2400 2700 3000 3300 3600 3900
-1

Wavenumber (cm )

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NZVI Transport Fundamentals

Column Transport experiments

Inlet; Co= 70 mg/L-725 mg/L
Sand size (dc)= 450m
(F3050)
Particle size (dp)=5.5nm-75nm
Syringe
pump

L=9 cm; D=1 cm

Flow = 0.45 cm/min
IS=0.1mM-10mM

sampler
Outlet; C

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CMC-nZVI Transport in Packed Columns

0

L=column
length

C/C0

Inlet concentration = Co
(constant at all time t)

1.0

1.0

0.8

0.8

0.6

0.6

0.4

Tracer KNO3

0.2
0.0

0.4

C0=0.725 gL-1

0.2

Simulated C/C0
(without aggregation)

0.0

Pore volume (PV)

Pore volume =V*t/(L*n)

n=porosity , V=velocity

Outlet concentration = C
(changes with time t)

CLASSICAL COLLOID DEPOSITION MECHANISMS IN

POROUS MEDIA
2C
C
C
= D 2 vx
kC
t
x
x
Dispersion
coefficient

Pore water
velocity

k=

3(1 n)v
o
2d c

Deposition rate Attachment

efficiency
constant

Single collector
efficiency

k=deposition rate coefficient, n=porosity,

v=interstitial velocity, dc=average sand size

(i) Diffusion
(ii) Interception
(iii) Sedimentation

Particle diameter
dependent

Attachment efficiency: Probability of

sticking on sand surface after collision
(i) Solution chemistry
(ii) Surface charge

Interception
Flow direction

Single collector efficiency: Probability

of collision between particle-sand

Colloid

Sedimentation
Diffusion
Collector

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Single collector contact efficiency (0)

Single-Collector Contact Efficiency

0.06
0.05

Single collector efficiency (0)

with different particle size (dp)

0.04
0.03
0.02
0.01

100

200

300

400

500

600

700

Particle size (nm)

CMC-nZVI deposition in granular porous media

Influent

Particle-collector
attachment
Effluent

t=t0

Particle size
(dp)

Influent PSD

Influent

Collector

Concentration

t=tend

sedimentation

Concentration

Flow path 2

Particle-particle
attachment

t=t0
t=tend
Particle size
(dp)

Effluent PSD

Effluent
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CMC-nZVI Transport:
Effect of Particle Concentration
1.0

Adhesive torque
(Tadhesive) due to DLVO
interaction energy
Tapplied /Tadhesive>1 suggests
possibility of detachment

0.8

C/C0

Sand
grain

Torque (Tapplied) due to

hydrodynamic drag

0.8

0.6

0.6
C0=0.07gL-1
-1
C0=0.2gL

0.4

C0=0.725gL
Fitted Curve

0.2
0.0

1.0

0.4

-1

0.2

0.0

Pore volume (PV)

Accounting for detachment of deposited particles
provides reasonable fits

k det S dep
C
C n
C
= D 2 v
k dep ,i Ci (t ) +
x i =1
t
x

NZVI Reactivity

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Remediation of Metal Contaminants

Chromium removal:
Cr6+ precipitates on iron surface and can also get transformed to Cr3+
FeOH + Cr2O72- Fe-Cr2O7- + OHReduction of Cr6+ to Cr3+:
3Fe(0) + Cr2O2- + 7H2O 3Fe2+ + 2Cr(OH)3 + 8OHCr(III) readily precipitates as Cr(OH)3 or as the solid solution (Fex,Cr1-x)(OH)3
Fe(0) +2H2O Fe2+ + H2 +2OHFe2++CrO2- + 4H2O (Fex,Cr1-x)(OH)3 + 5OHR.W. Puls et al. (1999), OCarroll et al. (2013)

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Chemical Transformation Organic contaminants

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NZVI Reactivity to TCE

Reactions under Iron Excess Conditions
Liu et al., 2005. Environ.Sci. Technol.

The Problem:
Surface passivation

Oxide passivation
layer
Fe0

NZVI reacts with water and

oxygen, forms oxide layer:
Fe3O4/FeOOH

Solutions:
Surface functionalization

Doping with
metal (Pd)

Carbon support

Fe0

S2-

Fe(0) + 2H2O Fe(OH)2 + H2

Thick oxide layers hinders

electron transport

Addition of
inorganic ions
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NZVI reactivity
Bimetallic
nanoparticles

Yan et al. 2012

Aged, passivated nZVI

Many folds
increase
in reactivity with
Pd,
but..Pd
contributes
to toxicity

Oxide passivation
layer

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Yan et al (2010)

TCE degradation kinetics

1.0

C/C0

0.8
No NZVI
NZVI only
NZVI-Pd

0.6
0.4
0.2
0.0
0

10

12

14

16

Time (hr)
Initial TCE Concentration

30 mg/L

NZVI concentration

2.0 g/L

NZVI-Pd

0.1 g/L (0.5% wt/wt of Pd)

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Sulfidation of NZVI
33 % less loss of
electrons to water:
Sulfidated-NZVI
thus more longlasting
120

bare NZVI
Sulfidated NZVI

Hydrogen (mM)

100

80

60

40

20

0
0

10

15

20

25

30

Time (days)

Rajajayavel and Ghoshal, Water Research, 2015, In press

TCE degradation kinetics with sulfide functionalized NZVI

Rajajayavel and Ghoshal, Water Research, 2015, 78:144-153
1.0
No NZVI
NZVI only
0.7 mM Sulfide
1.0 mM Sulfide
1.6 mM Sulfide
2.4 mM Sulfide
3.1 mM Sulfide
NZVI-Pd

C/C0

0.8
0.6
0.4

kobs (h-1) for sulfide

amended NZVI > kobs for
bare NZVI by up to ~40
times.
TCE is primarily degraded to
ethene and acetylene.

0.2
0.0
0

10

12

14

Time (hr)
Initial TCE Concentration

30 mg/L

NZVI concentration

2.0 g/L

NZVI-Pd

0.1 g/L (0.5% wt/wt of Pd)

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Coating NZVI with

carboxymethyl cellulose
(polyelectrolyte) results in
identical reactivity as bare
NZVI with sulfide
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Case Studies

Emulsified NZVI
NZVI particles emplaced within a
surfactant-stabilized, biodegradable, waterin-oil emulsion.
Oil membrane is hydrophobic and miscible
with DNAPL.
Biodegradation enhanced by vegetable oil
and surfactant components of EZVI.

Brooks, 2000

Geosyntec consultants, NASA

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Case study Emulsified NZVI

Demonstration of In Situ Dehalogenation of DNAPL through Injection of
Emulsified Zero-Valent Iron at Launch Complex 34 in Cape Canaveral
Air Force Station, Florida.
Launch Complex 34 was used as a launch site for Saturn
rockets from 1960 to 1968.
Rocket parts were cleaned on racks.
Solvents ran off to the surface or discharged into drainage
pits.
Approx 20,600 kg to 40,000 kg of solvent likely present

(Eddy-Dilek et al., 1998) (Battelle, 1999a)

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Case study Emulsified NZVI

EZVI injected in 8 injection wells using pressure pulse technology
Monitored changes in CVOCs in:
Groundwater
5 depth intervals, 2 up gradient and 2 down gradient wells; and
Soil cores
8 depth intervals, 6 locations

(Quinn et al., 2005)

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TCE Contaminated Site

- NASA Rocket Launching Pad

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Case study Emulsified NZVI

Pre-Demonstration (March 2002)

Post-Demonstration (Nov 2002)

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EZVI treatment: TCE Degradation Products

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Theoretical Cost of Treatment using NZVI

For
Acetylene, n=4
Ethene, n=6
Ethane, n=8

Minimum: 4e- or 2Fe0 / TCE

or: 0.85:1 (by mass)
Assuming $50/Kg Fe0:
$44/Kg TCE (acetylene)
$66/Kg TCE (Ethene)
$88/Kg TCE (Ethane)

Fe0 delivery to all TCE molecules?

Permeable Reactive Barriers

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Permeable Reactive Fe(0) Barrier

Permeable Reactive Barrier Walls

In-situ remediation for chlorinated
hydrocarbons & heavy metals
Usually contain iron or other zero-valent
metals
Hydraulic retention time is key

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Reactive Barrier Walls

1) funnel and gate

2) continuous trench

Case Study
Elizabeth City, NC
Contamination of groundwater with Cr(VI) and TCE
(overlapping plumes)
TCE (20 000 ug/L), cDCE and VC: degreasing operations
Cr (10 mg/L in groundwater, 14,500 mg/Kg in soil):
electroplating operations

Permeable reactive barrier

Continuous wall configuration: 46 mX 7.3m X 0.6m
granular iron: reactive medium

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Cr(VI) reduction by Fe0

From Gould (1982)

A = surface area of zero-valent Fe (cm2/L)
k = 5.45X10-5 L/cm2.min

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TCE transformation

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PRB Case Study

Cost Comparison with Pump and Treat
Reactive Wall

Pump and Treat

Installation

$500 000

$500 000

Monitoring

$32 000/yr

$32 000/yr

Maintenance

$0

$200 000/yr

Equipment

$0

$500 000/20 yrs

Savings = $ 4.5 million/20 yrs

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Bioremediation

Bioremediation
Bioremediation: Engineered or natural process in
which biological reactions break up or transform
pollutant compounds, thereby remedying or
eliminating environmental contamination
Mineralization: Conversion of an organic molecule
into its inorganic constituents (e.g., CO2, NO3-, SO42-,
PO43-)
Biodegradation: A subset of biotransformation
which causes simplification of an organic compounds
structure by breaking intermolecular bonds

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Why do microbes degrade organic

compounds?
To obtain energy for growth and maintenance
Electron transfer (redox) reactions provide energy
and result in biodegradation
Microbially-mediated redox reactions involve
electron donor (usually: organic matter /organic
pollutant)
electron acceptor (usually: oxygen, nitrate,
sulfate, CO2)
As a source of C for building cell materials

Fundamentals of Bioremediation

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Biodegradation of Common Pollutants

BTEX, PAHs aerobic & anaerobic biodegradation

Chlorinated hydrocarbons
Aerobic biodegradation (pollutant acts as electron
donor and O2 acts as electron acceptor) DCE
reductive dehalogenation (pollutant acts as
electron acceptor, occurs under sulfate reducing
and methanogenic conditions) PCE,TCE, DCE,
TCA
Cometabolic biodegradation (e.g., toluene:
primary substrate, TCE cometabolic substrate)

Where do electron acceptors come from?

Near ground surface, O2 available in abundance
If BOD of contaminant zone >> dissolved O2, then
only anaerobic biodegradation feasible
Deep in subsurface, no O2 but naturally abundant
nitrate, sulfate to sustain anaerobic biodegradation

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Aerobic Unsaturated Zone

Volatilization
Oxygen Exchange

Dissolution
Aerobic
uncontaminated
groundwater

Anaerobic core

Mixing, Dilution

Advection

Aerobic Processes

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Anaerobic degradation of chlorinated

organics by Dehalococcoides

.,

These are the only group of microbes that are capable of

complete dechlorination of chlorinated solvents.
Dhc., are not ubiquitous and often are present in low
numbers. (Hendrickson et al., 2002)
Strict anaerobes that require anoxia and reducing
conditions for growth.
Difficult to grow as pure culture.
Enriched with mixed culture consortia of bacteria

Dehalococcoides sp.,
http://www.beem.utoronto.ca/research/67

(Methanogens, Acteogens, Sporumosa...)

86

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Dehalococcoides work in consortium with other

bacteria

Growth Factors

Carbon source
Electron donor
pH
Temperature
nutrient availability

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SIREM KB-1 A Case study

KB-1 is the commercial name for mixed culture
dechlorinating bacteria.
It is the most widely used bio-augmentation
culture in the world.

Site history
Portland, Oregon
TCE released during 1980s
TCE and cDCE ~ 592 mg/L and 92 mg/L
50 to 110 feet below ground surface

Ref: http://www.siremlab.com/products/kb-1

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KB-1 A Case study

The full scale implementation consisted of a 150 foot
long bio-barrier amended with an electron donor
and KB-1.
Approximately 200 injection points were used to
inject 270,000 kilograms of electron donor and 2,000
liters (L) of KB-1.
The site was continuously monitored for it
performance.
TCE dechlorination products (cDCE and VC) were generated initially,
followed by a rapid decline with observed increases in ethene.

TCE concentrations were below federal MCLs (5 g/L) in 6 months

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http://www.sirem-lab.com/images/PDF/case-study-maulfoster.pdf

Bioremediation Requirements
Other than electron acceptors, N, P, what other
conditions are required?
pH: 6-8, adequate buffering capacity
Temperature: subsurface ground temperature
usually ideal but if less than 5oC, usually low
biodegradation rates
Moisture > 40%
Absence of toxic agents, e.g., high conc. of heavy
metals

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Bacterial Metabolic Genes

GENE

PLASMID/
CHROMOSOME
ENCODED

POLLUTANT

STRAIN

alk

Plasmid (OCT)

alkanes
(C6-C10)

Pseudomonas putida

bph

Chromosome

PCBs

Alcaligenes
eutrophus H850

nah

Plasmid (pKA1)

naphthalene,
anthracene,
phenanthrene

Pseudomonas
fluorescens 5R

phl

Chromosome

phenol

Alcaligenes
eutrophus JMP134

xyl

Plasmid (TOL)

xylene,
toluene

Pseudomonas putida
mt-2

Biodegradation Kinetics
Cell growth rate:

Monods Kinetics:

dX
= X
dt

mC

Ks + C

Substrate degradation kinetics:

dC
CX
= m
dt
Y (K s + C )

X = cell concentration (mg cells/L)

= specific growth rate (day-1)

Ks = half saturation constant (mg/L)

m = maximum specific growth rate (day-1)

C = substrate concentration (mg/L)

Y = yield coefficient (mg cells/mg substrate)

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In-Situ Bioremediation
Permeable Biobarriers

Bioavailability
Contaminated soil matrix
water

NAPL

solid

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Bioremediation
Can contaminants sorbed on to soil or present in
NAPLs be biodegraded?
Conventional theory: only dissolved
contaminants are degraded by bacteria ----bioavailability
Once dissolved phase contaminants are depleted
by biodegradation, sorbed or NAPL contaminants
will desorb/dissolve in response to the decrease in
aqueous phase concentration and thereafter
biodegrade

Limited Bioavailability
Low aqueous solubility of HOCs
Entrapment in micropores
Strong binding (sequestration) to soil organic matter
with aging
conventional analytical techniques inadequate for
predicting bioavailability

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Limited Bioavailability
Desorption/dissolution rates may influence
biodegradation rates
Overall biodegradation rates can be influenced by
rates of desorption/dissolution or intrinsic rate of
microbial uptake
Desorption/dissolution is often found to be the rate
controlling phenomena

Mass Transfer and Biodegradation Processes at the

Particle Scale

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Identifying Rate Controlling Phenomena

Bulk phase dissolution

and Intrapore diffusion
Bi >1

Bi <1

Intrapore diffusion
and biodegradation
>1

<1

Diffusion control

Bulk phase dissolution

and biodegradation
Da<1

Biokinetic control

* After Ramaswami et al. 1997

Da>1

Dissolution control

The Biot number, Bi.

Thiele modulus, .

Damkohler number, Da.

In-Situ Bioremediation
Enhanced Pump and Treat

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In-Situ Bioremediation
Enhanced Pump and Treat

In-Situ Bioremediation
Bioventing

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In-Situ Bioremediation
Air Sparging

In-Situ Bioremediation
Intrinsic Bioremediation and Natural Attenuation

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How do you prove that bioremediation is

occurring in-situ?
How to distinguish between biotic and abiotic
processes?
Difficulty of performing mass balances in the field

How do you prove that bioremediation is

occurring in-situ?
Direct measurements
Increase in number of bacteria (especially pollutant
degrading bacteria)
Compare bacterial adaptation before and during
bioremediation
Decrease in electron acceptor concentrations
Formation of by-products
Ratio of biodegradable to non-biodegradable
components

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How do you prove that bioremediation is

occurring in-situ?
Experiments in the field
Stimulating bacteria within subsites to test for
increased contaminant losses
Monitoring conservative tracers to assess abiotic
losses
Radio-labelling contaminants to determine the fate
of carbon

How do you prove that bioremediation is

occurring in-situ?
Modelling experiments
To represent abiotic loss mechanisms
To estimate biodegradation rate
Compared to actual losses in the field
Need more than one piece of evidence needed to
prove biodegradation in the field

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Ex-situ Bioremediation
When to use ex-situ technologies?
High degree of heterogeneity
Low-permeability
Rapid treatment time required

Ex-situ Bioremediation
Slurry phase treatment (Bioreactors)

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Ex-situ Bioremediation
Slurry phase treatment (Bioreactors)
Rate-limiting step?
Rate of desorption/dissolution process
Rate of microbial uptake (biodegradation
kinetics)
water

NAPL

dC
A
= K t ( Ceq C )
dt
V

solid

Ex-situ Bioremediation
Landfarming
Aeration and mixing
Microbial seed

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Ex-situ Bioremediation
Biopiles
above-ground, engineered composting systems
used for the treatment of contaminated soils

monitoring
devices

nutrient and
water addition
water knockout tank

protective
membrane

contaminated
soil

berm

blower

berm

impermeable base

leachate
collection
pipe

Biopiles
Soil preparation includes
screening, crushing, mixing, adding bulking agents
pH adjustment
enhancement of indigenous microbes
Design elements
Protective membrane
Impermeable base
Aeration + air filtration
Moisture + nutrient addition
Leachate collection system
Temperature
Monitoring

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Biopiles under Construction

Impermeable Liner

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Biopiles
Applicability
Mainly for petroleum products
Lighter, volatile hydrocarbons removed through
aeration
Medium to heavy hydrocarbons biodegraded
Less effective for chlorinated hydrocarbons that
are degraded anaerobically

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