Environ. Sci. Technol.
2009, 43, 2957–2962
Bench-Scale Studies of In-Duct
Mercury Capture Using Cupric
Chloride-Impregnated Carbons
SANG-SUP LEE,† JOO-YOUP LEE,‡ AND
T I M C . K E E N E R * ,†
Department of Civil and Environmental Engineering,
University of Cincinnati, Cincinnati, Ohio 45221, and
Department of Chemical and Materials Engineering,
University of Cincinnati, Cincinnati, Ohio 45221
Received July 14, 2008. Revised manuscript received
December 15, 2008. Accepted January 30, 2009.
A brominated activated carbon (Darco Hg-LH) and cupric
chloride-impregnated activated carbon (CuCl2-ACs) sorbent
have been tested in a bench-scale entrained-flow reactor system
which was developed for simulating in-flight mercury capture
in ducts upstream of particulate matter control devices.
The bench-scale experimental system has been operated with
the conditions of a residence time of 0.75 s and a gas
temperature of 140 °C to simulate typical conditions in the
duct of coal-fired exhaust gas. In addition, sorbent deposition
on walls which can occur in a laboratory-scale system
more than in a full-scale system was significantly reduced so
that additional mercury capture by the deposited sorbent
was minimized. In the entrained-flow system, CuCl2-ACs
demonstrated similar performance in Hg adsorption and better
performance in Hg0 oxidation than Darco Hg-LH. In addition,
the carbon content of those sorbents was found to determine
their Hg adsorption capability in the entrained-flow system.
The bench-scale entrained-flow system was able to demon-
strate the important Hg adsorption and oxidation characteristics
of the tested sorbents.
Introduction
Sorbent injection is one of the most promising control
technologies for reducing mercury emissions from coal-fired
power plants (1-3). Since the use of economical and efficient
sorbents is most important in sorbent injection, vari-
ous sorbents have been studied and developed. Among these
sorbents, activated carbons have been extensively studied
and shown their capability for mercury capture (4-6).
However, raw activated carbon has low capability in mercury
removal from flue gases with low hydrogen chloride (HCl)
concentration so that a relatively large amount of raw
activated carbon is required for mercury emissions control
from subbituminous or lignite coal-burning units producing
a low concentration of HCl in a flue gas (7-9). For
subbituminous or lignite-burning units, the use of chemically
treated activated carbons is an effective option to enhance
mercury removal efficiency and lower the amount of carbon
injection. For example, Ghorishi et al. have reported a
significant increase in Hg0 removal by impregnating HCl onto
* Corresponding author e-mail: Tim.Keener@uc.edu; tel: 1-513-
556-3676; fax: 1-513-556-2599.
†
Department of Civil and Environmental Engineering.
‡
Department of Chemical and Materials Engineering.
10.1021/es801943t CCC: $40.75  2009 American Chemical Society
Published on Web 03/12/2009
activated carbon (10). Especially, brominated activated
carbon has been tested in several full-scale systems and has
demonstrated good performance such as more than 90%
mercury removal efficiency at an injection level of less than
80 mg/m3 (5 lb/MMacf) (1, 11).
EPA’s Information Collection Request (ICR) data show
that mercury removal efficiency varies with a particulate
control system (3, 12). Full-scale test results also show
significantly higher mercury removal in a fabric filter (FF)
than an electrostatic precipitator (ESP) with a similar level
of sorbent injection (1, 11). However, while 83% of the U.S.
coal-fired boiler units operating with particulate control
devices are equipped with ESPs, only 14% are equipped with
FFs (8). In addition, full-scale test results (13) show that the
mercury capture achieved in the duct portion with a residence
time of 0.54 s reaches approximately 90% of the total mercury
capture achieved in both duct and an ESP with a residence
time of 14.04 s. These results stress the importance of using
an entrained-flow system to simulate in-duct mercury
capture upstream of an ESP rather than inside an ESP for
mercury sorbent tests. Tests reported here therefore were
designed to measure the in-duct portion of mercury capture
in order to more accurately determine the effect of kinetics
on the reaction in the duct stream.
In this study, a bench-scale entrained-flow system was
constructed and operated for simulating in-duct mercury
capture using a mixture of air and elemental mercury vapor.
In addition, cupric chloride-impregnated carbons, which
demonstrated excellent performance in our previous studies
(7, 14), were tested and their results were compared with
those of a representative brominated activated carbon.
Although a few test results were obtained in air with sulfur
dioxide (SO2), most entrained-flow tests were conducted in
air to obtain the Hg0 oxidation capability of cupric chloride
and Hg adsorption capability under the minimum influence
of other flue gas components. Therefore, the performance
results obtained from the bench-scale entrained-flow system
may not be directly used for the projection of full-scale
performance.
Experimental Section
Sorbent Preparations. Three concentrations of cupric
chloride were impregnated onto Darco-Hg which is raw
activated carbon (Norit Americas Inc., Marshall, TX). Portions
of 0.24, 0.5, and 1.125 g of copper chloride dihydrates
(CuCl2 · 2H2O, Aldrich Chemical. Co., Milwaukee, WI) were
added to 100 mL of isopropyl alcohol (99.8%, Pharmco
Products Inc., Brookfield, CT), respectively, under vigorous
stirring until its complete dissolution. Darco-Hg activated
carbon (4.5 g) was then added in each cupric chloride
solution, and the mixtures were kept at room temperature
for about 3 h with continuous stirring. Each solution was
then filtered, and each resulting solid was dried at 100 °C for
about 2 h to create cupric chloride-impregnated activated
carbon sorbents.
To find the concentrations of cupric chloride in the
sorbents, the filtered solutions were analyzed for the residual
concentrations of copper and chloride in the solutions using
atomic absorption spectrophotometry (AAnalyst 300, Perkin-
Elmer, Waltham, MA) and ion chromatography (DX-600,
Dionex, Sunnyvale, CA), respectively. Then, the concentra-
tions of cupric chloride impregnated onto each sorbent were
determined from the difference before and after the im-
pregnation process. The results showed that 3.8%, 6.5%, and
10% (w) cupric chlorides (as CuCl2) were impregnated onto
each Darco-Hg activated carbon, respectively. These sorbents
VOL. 43, NO. 8, 2009 / ENVIRONMENTAL SCIENCE & TECHNOLOGY 9 2957
FIGURE 1. Schematic of an entrained-flow reactor system simulating in-duct mercury capture.
TABLE 1. Surface Areas and Mean Particle Sizes of the Sorbents Tested in This Study
sorbent description
Darco-Hg lignite coal-based activated carbon
3.8% CuCl2-AC 3.8% (w) CuCl2-impregnated activated carbon
6.5% CuCl2-AC 6.5% (w) CuCl2-impregnated activated carbon
10% CuCl2-AC 10% (w) CuCl2-impregnated activated carbon
Darco Hg-LH brominated, lignite coal-based activated carbon
were found to have similar surface areas and mean particle
diameters as those of Darco-Hg from the analysis using a
single point BET technique (Monosorb Surface Area Analyzer,
model MS-12, Quantachrome Instruments, Boynton Beach,
FL) and laser particle counting system (PC-2000, Spectrex
Corporation, Redwood city, CA) as shown in Table 1. In
addition, brominated activated carbon known commercially
as Darco Hg-LH (Norit Americas Inc., Marshall, TX) served
as a benchmark sorbent in this study.
Experimental Conditions. An entrained-flow reactor was
designed and constructed to simulate mercury capture in
the ductwork. The 8 m long 2.5 cm diameter reactor was
made of borosilicate glass which is inert to mercury vapor.
Sections were connected using glass spherical joints and
spring clamps (35/25 size, Ace Glass, Inc. Vineland, NJ).
Heating tapes (Fisher Scientific, Inc. Pittsburgh, PA) with
separate controllers (Omega Engineering, Inc., Stamford, CT)
were used for every 2-m section of the reactor, and type K
thermocouples were placed in leak tight fittings at 2-m
intervals for monitoring the duct temperature. The tips of
the thermocouples were placed so as to not interfere in the
gas flow. Fiberglass pipe insulation (McMaster-Carr, Aurora,
OH) was used to insulate the entire length of the reactor. The
inlet air flow was preheated in a furnace at a temperature of
700 °C (Lindberg, Watertown, WI) before entering the reactor.
Sorbent particles were injected through a venturi-type
Bernoulli feeder. The feeder operates by allowing particles
to be entrained off of a rotating variable speed circular top
which has a precise groove cut that contains the particles.
An aspirator (shown in Figure 1) is mounted above and close
to the groove and picks up the particles by means of suction
and then they are conveyed to the reactor where they are
injected. The sorbent injection rate is controlled by the speed
of the rotating top.
Operating conditions consisted of a total air flow rate of
139.5 L/min at a reactor temperature of 140 °C and have a
flow velocity of 6.7 m/sec approaching that (∼15 m/sec) of
full-scale ductwork. With this air flow rate, a residence time
2958 9 ENVIRONMENTAL SCIENCE & TECHNOLOGY / VOL. 43, NO. 8, 2009
surface area (m2/g)
mean particle
from Norit’s datasheet from measurements diameter (µm)
600 450 ((30) 23
400 ((50) 23
420 ((30) 23
400 ((70) 23
550 350 ((60) 22
of 0.75 s was also obtained, and this residence time is within
the range of that in the full-scale ductwork upstream of an
ESP.
To minimize additional mercury capture by sorbents
deposited on the reactor wall, Hg0-laden gas was injected
after the first 3 m of the reactor where most of sorbent
depositions were found. In addition, the reactor was con-
tinuously vibrated by using vibrating pens (McMaster-Carr,
Aurora, OH) located at 2-m intervals as shown in Figure 1.
This technique was found to be extremely successful in
minimizing the amount of sorbent that deposited on the
walls. These experimental conditions are also summarized
in Figure 1.
Experimental Procedure and Data Analysis. During the
sorbent injection, a portion of the effluent gas was sampled
at a flow rate of 1.5 L/min to measure the outlet mercury
concentrations. The outlet mercury speciation was conducted
by using the Ontario Hydro Method (15). The sampled gas
passed through a 1 M KCl impinger solution and a 4% (w/v)
KMnO4/10% (v/v) H2SO4 impinger solution to capture
oxidized mercury and elemental mercury in the sampled
gas, respectively. Oxidized mercury (Hg2+out) and elemental
mercury (Hg0out) concentrations in the effluent gas were
determined by analyzing those solutions using a cold vapor
atomic absorption spectrophotometer (CVAAS, model 400A,
Buck Scientific Inc., East Norwalk, CT).
At the beginning of each test, the reactor was heated to
an operating temperature of 140 °C by injecting a sorbent-
free, filtered, dehumidified, and purified air flow supplied by
an air compressor (Balston compressed air filters, model
A912A, Parker Hannifin Corp., Cleveland, OH). An Hg0-laden
air flow generated from elemental mercury permeation tubes
(VICI Metronics, Inc., Poulsbo, WA) in a permeation tube
oven (Dynacalibrator model 500, VICI Metronics, Inc.,
Poulsbo, WA) was also injected. Blank Hg0 concentrations
were measured at several locations such as the outlet of the
mercury permeation oven, 1 m after Hg0 injection, and the
outlet of the reactor system in the absence of sorbent, and
similar blank Hg0 concentrations were obtained from all
measurements. Throughout the blank tests, it was confirmed
that neither Hg0 oxidation nor removal took place inside the
reactor without sorbent injection, and injected Hg0 was
quickly mixed with air flow. The average inlet Hg0 concen-
tration was determined to be 6.5 ppbv from the blank
measurements, and its variation was confirmed within 0.5
ppbv.
Each sorbent (0.025-0.3 g) was premixed with 2 g of
montmorillonite K 10 clay (Aldrich Chemical Co. Milwaukee,
WI) and then injected through a venturi-type Bernoulli feeder
at a constant feeding rate for 10 min. The sorbent particles
were separated from the flue gas stream at the end of the
reactor by a cyclone made of borosilicate material. After each
test run during 10 min, sorbent particles collected in a cyclone
and deposited on the reactor wall were obtained by washing
those with acetone (99.5%, Reagent grade ACS/USP, Pharmco
Products Inc., Brookfield, CT). Then, a sorbent mass balance
was taken to determine an actual sorbent injection rate into
the reaction zone. All the collected spent sorbent particles
were analyzed for the amount of mercury adsorption (Hgads)
by following the digestion procedure described in the Ontario
Hydro Method.
Results and Discussion
Performance of the Entrained-Flow System. The flow
conditions in the full-scale ductwork such as a residence
time of less than 1 s and a gas temperature of around 140
°C can be obtained in the entrained-flow system by providing
it with flow and heating as explained in the previous
experimental section. However, compared to the full-scale
ductwork, the entrained-flow system has a significantly higher
ratio of inside surface area to the volume of the system (S/V
ratio ) 2/R; where R is a radius of the ductwork). Assuming
that a Reynolds number of 500,000 and a flue gas velocity of
15.24 m/sec (50 ft/sec) are applied to the full-scale ductwork,
the full-scale system has an S/V ratio of 4.37 (m2/m3) while
the entrained-flow system has an S/V ratio as high as 160
(m2/m3). This significantly higher S/V ratio of the entrained-
flow system can cause a significant amount of sorbent
deposition on reactor walls so that mercury vapor can be
additionally captured by the deposited sorbent.
To minimize the sorbent deposition in our tests, the
entrained-flow system was provided with the highest flow
rate eligible to the current system configurations. In addition,
Hg0 vapor was injected after the first 3 m of the reactor which
was found to have relatively higher sorbent deposition.
Vibrating pens were also applied to prevent sorbent deposi-
tion, and montmorillonite clay was injected together with
each sorbent because coinjection of montmorillonite clay
was found to decrease the amount of sorbent deposition
and make the sorbent particles more easily detached from
the reactor walls by vibration. In addition, montmorillonite
clay was found to be inert toward Hg0 vapor from our blank
tests.
After each test, individual sorbent and mercury mass
balances were taken with respect to fractions escaping from
the reactor, collected in the cyclone, and deposited on the
reactor wall. As a result, approximately 10% of the injected
sorbent was found to be deposited on the reactor wall, and
only 10-15% of the total mercury adsorption was achieved
by the deposited sorbent for all of the tests conducted in this
study. Therefore, additional mercury capture by deposited
sorbent was also minimized in the entrained-flow system.
From the entrained-flow tests, Hg adsorption efficiency
was determined from the amount of mercury adsorbed (Hgads)
onto each sorbent. The amount of effluent oxidized mercury
(Hg2+out) was measured in the outlet of the reactor system,
and effluent oxidized mercury percentage was determined.
In addition, the sum of these amounts was defined as Hg0-
FIGURE 2. Mercury speciation results of replicate tests with
6.5% CuCl2-AC at 20 mg/m3 based on inlet Hg0.
removal total because elemental mercury was removed in
the form of oxidized mercury, which can be captured by fly
ash and wet scrubbers in full-scale systems. Three replicate
tests were conducted with 6.5% CuCl2-AC at 20 mg/m3 to
examine reproducibility of entrained-flow test results. Figure
2 shows mercury speciation results obtained based on the
inlet Hg0. As shown in the figure, mass balance closures of
three replicate tests are in the range of the inlet Hg0
concentration (6.5 ( 0.5 ppbv), and Hgads, Hg2+out, and Hgads
+ Hg2+out generally increase in proportion to the mercury
mass balance closure. These results indicate that the varia-
tions in Hgads, Hg2+out, and Hgads + Hg2+out are ascribed to the
variation in the inlet Hg0 concentration rather than the errors
from the measurements of Hgads, Hg2+out, and Hg0out. There-
fore, the efficiency values reported here were determined
based on the sum of the amount of mercury adsorbed (Hgads),
the amount of effluent oxidized mercury (Hg2+out), and the
amount of effluent elemental mercury (Hg0out). In addition,
the mercury mass balance closures of all tests were in a
reasonably acceptable range (87-110%).
Performance of Mercury Sorbents. Cupric chloride-
impregnated sorbents showed remarkable performance in
Hg0 removal in the previous fixed-bed tests (7) conducted
under typical simulated flue gases of subbituminous/lignite
coals. In this study, raw activated carbons were chemically
promoted with three different concentrations of cupric
chloride and tested in the entrained-flow system. One (6.5%
CuCl2-AC) of the cupric chloride-impregnated carbons was
compared for its test results with raw (Darco Hg) and
brominated (Darco Hg-LH) activated carbons in Figures 3,
4, and 5. As shown in Figure 3, raw activated carbon did not
demonstrate good performance in Hg adsorption efficiency
under air flow in the entrained-flow system. The Darco Hg-
LH showed Hg adsorption performance comparable to that
of 6.5% CuCl2-AC. On the basis of these results and surface
areas of both sorbents shown in Table 1, the relationship
between the Hg adsorption efficiency and the total surface
area of the sorbent injected during each test is presented in
Figure 4. The relative standard deviation of 7% in Hg
adsorption efficiency determined based on the sum of Hgads,
Hg2+out, and Hg0out from the previous replicate tests shown
VOL. 43, NO. 8, 2009 / ENVIRONMENTAL SCIENCE & TECHNOLOGY 9 2959
FIGURE 3. Hg adsorption efficiencies of Darco Hg-LH, 6.5%
CuCl2-AC, and Darco Hg.
FIGURE 4. Relationship between Hg adsorption efficiency and
total surface area of injected sorbent.
in Figure 2 was applied to all data points for error bars shown
in the figure. The Darco Hg-LH showed unnoticeable Hg
adsorption performance compared with 6.5% CuCl2-AC with
respect to surface area. The Hg adsorption efficiencies of
both sorbents increased with an increase in their total surface
areas available in the entrained-flow system, suggesting that
the Hg adsorption is limited by the readsorption of the
resultant oxidized mercury generated from the reaction
between Hg(0) and CuCl2. In Figure 5, the effluent oxidized
mercury results obtained with Darco Hg-LH and 6.5% CuCl2-
AC showed that 6.5% CuCl2-AC had slightly higher effluent
oxidized mercury. Therefore, except for slightly higher Hg0
oxidation, the 6.5% CuCl2-AC sorbent demonstrated very
similar performance in mercury control to Darco Hg-LH. In
addition, significant amounts of Hg0 were found to be
oxidized by the sorbents, but the resultant oxidized mercury
was not adsorbed onto both sorbents. These results indicate
again that Hg removal capability of both sorbents is limited
by the readsorption of the resultant oxidized mercury.
2960 9 ENVIRONMENTAL SCIENCE & TECHNOLOGY / VOL. 43, NO. 8, 2009
FIGURE 5. Percentages of effluent oxidized mercury determined
from entrained-flow tests with Darco Hg-LH and 6.5% CuCl2-AC.
FIGURE 6. Hg adsorption efficiencies of cupric chloride-
impregnated activated carbons with different cupric chloride
loadings obtained from digestion of their spent sorbents.
Hg adsorption efficiencies of CuCl2-AC sorbents obtained
from the digestion analysis of their spent sorbents after each
test are also shown in Figure 6. Similar to the test results of
Darco Hg-LH and 6.5% CuCl2-AC, Hg adsorption efficiency
increased almost in proportion to the sorbent injection rate
for all CuCl2-AC sorbents, and very slightly increased with an
increase in CuCl2 loading in each sorbent. This suggests that
mercury adsorption onto CuCl2-AC sorbents is limited by
external mass transfer resistance due to the low mercury
concentration rather than limited by the CuCl2 loading in
the sorbent. Meanwhile, effluent oxidized mercury was
slightly dependent on CuCl2 loading, but was not strongly
dependent on sorbent injection rate as shown in Figure 7.
This indicates that only the raw carbon surfaces may be
responsible for the readsorption of the resultant oxidized
mercury and Hg(0) oxidation may be independent of surface
area above a certain critical value. Figure 8 illustrates Hg0-
removal totals (the sum of Hg adsorption and effluent
FIGURE 7. Percentages of effluent oxidized mercury determined
from entrained-flow tests with cupric chloride-impregnated
activated carbons.
FIGURE 8. Hg0-removal totals of brominated (Darco Hg-LH) and
cupric chloride impregnated (CuCl2-ACs) activated carbons.
oxidized mercury) obtained with brominated and cupric
chloride-impregnated sorbents in the entrained-flow system.
It clearly shows that the Hg0-removal total increases with an
increase in CuCl2 loading in sorbent due to the Hg0 oxidation
capability of CuCl2. In addition, the entrained-flow results
of Darco Hg-LH show a similar trend as full-scale test results
obtained from the literature (1).
Additional entrained-flow tests were conducted in air with
1500 ppmv SO2 to find the effects of other flue gas
components on the performance of Darco Hg-LH and CuCl2-
AC sorbents. These tests also examine possible biases by the
presence of Cl2 in the KCl solution used for measuring effluent
oxidized mercury as reported by Cauch, et al. (16). Figure 9
compares entrained-flow results obtained in air to those in
air only with SO2 for Darco Hg-LH and 6.5% CuCl2-AC. The
efficiency values were determined from two replicate tests
FIGURE 9. Entrained-flow test results of (a) 6.5% CuCl2-AC and
(b) Darco Hg-LH at an injection rate of approximately 30 mg/m3
in air without and with 1500 ppmv SO2.
for each sorbent. As shown in the figure, only very slight
performance decrease by SO2 injection was found for both
sorbents, although SO2 is known as the most applicable
inhibitor of Hg0 oxidation and adsorption for carbon-based
sorbents (8, 17). Therefore, while flue gas components may
have relatively minimal effects on the performance of Darco
Hg-LH and CuCl2-AC sorbents, significant amounts of effluent
oxidized mercury found from the tests of both sorbents
suggest further investigation into the capability of fly ash to
adsorb the resultant oxidized mercury using the entrained-
flow system. In addition, similar amounts of effluent oxidized
mercury found from both tests without and with SO2 confirm
that biases by the presence of Cl2 in the KCl solution are
negligible in these entrained-flow tests. As shown in the figure,
6.5% CuCl2-AC still shows slightly higher effluent oxidized
mercury and Hg0-removal total than Darco Hg-LH in the
tests with 1500 ppmv SO2. Considering that bromine loading
in Darco Hg-LH is approximately 15% (18), CuCl2-AC sorbents
have better Hg0 oxidation capability than Darco Hg-LH. In
addition, CuCl2-AC sorbents will benefit from the utilization
of a waste stream from the printed circuit board (PCB)
industry, and would thus be environmentally beneficial to
both of the utility and electronic industries.
This study evaluated Hg0 oxidation and adsorption
capabilities of Darco Hg-LH and CuCl2-AC sorbents in an
entrained-flow system. As a result, CuCl2-AC sorbents
demonstrated better performance in Hg0 oxidation than
Darco Hg-LH while similar Hg adsorption performance was
shown between these sorbents. In addition, both sorbents
showed minimal effects of SO2 on their Hg0 oxidation and
adsorption capabilities. Further studies using a fixed-bed
system and X-ray absorption fine-structure spectroscopy are
expected to be able to determine the reaction mechanism
between CuCl2 and Hg0 and to identify the species responsible
for Hg0 oxidation of CuCl2-AC sorbents.
VOL. 43, NO. 8, 2009 / ENVIRONMENTAL SCIENCE & TECHNOLOGY 9 2961
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ES801943T