xvEPA
                                 United States
                                 Environmental Protection
                                 Agency
                                 Industrial Environmental Research
                                 Laboratory
                                 Research Triangle Park NC 27711
                                 Research and Development
                                 EPA-600/S7-82-032  Oct. 1982
Project  Summary
                                Studies  of Flue  Gas
                                Desulfurization at  Louisville
                                Gas and  Electric's  Paddy's
                                Run  Station

                                0. W. Hargrove, Jr., G. P. Behrens, and W. E.  Corbett
                                  Between the Spring of 1973 and the
                                Fall of 1976,  Louisville Gas and
                                Electric's Paddy's Run lime flue gas
                                desulfurization (FGD) system logged
                                more than 4000 hours of operation
                                without any major  process or me-
                                chanical problems. Due to this oper-
                                ating success  when other similar
                                systems were encountering numerous
                                problems, EPA funded a 6-month
                                evaluation study at  Paddy's Run. A
                                program was implemented to charac-
                                terize the system in its normal mode of
                                operation and to conduct tests which
                                would simulate conditions typical of
                                other lime-based systems.
                                  The Paddy's Run FGD system
                                normally uses  carbide lime,  a by-
                                product in the production of acetylene,
                                as the alkaline additive. Contaminants
                                in the carbide lime, notably thiosulf ate,
                                are  responsible for minimizing the
                                sulfite oxidation rate which helps to
                                maintain scale-free operation of the
                                system. Substitution of commercial
                                lime for carbide lime resulted in
                                gypsum  scaling  in the scrubber.
                                Magnesium addition (—3000 ppm) with
                                commercial lime reestablished scale-
                                free operation and improved SO2
                                removal  dramatically. Addition of
                                either carbide lime or commercial lime
                                with magnesium  resulted in sulfite
                                oxidation levels well below  those
                                required to operate subsaturated with
                                respect to gypsum (less than about 16
                                percent). Under these conditions, all
                                 of the sulfate formed precipitated in a
                                 solid  solution with calcium sulfite
                                 hemihydrate.
                                  Additional tests examined the effect
                                 of chloride  addition, lime addition,
                                 point  location, and the reaction tank
                                 volume.
                                  This Project Summary was devel-
                                 oped by EPA's Industrial Environmen-
                                 tal Research Laboratory, Research
                                 Triangle Park, NC, to announce key
                                 findings of the research project that is
                                 fully documented in a separate report
                                 of the same title (see Project Report
                                 ordering information at back).

                                 Introduction
                                  Louisville  Gas and Electric (LG&E)
                                 Company's Paddy's Run No. 6 flue gas
                                 desulfurization (FGD) system was one of
                                 the first commercial-scale FGD units to
                                 be  operated successfully  in the U.S.
                                 Between its. start-up in the Spring of
                                 1973  and the Fall of 1976, the  unit
                                 logged close to 4000 hours of operation'
                                 without any major process or mechan-
                                 ical problems. Because of the demon-
                                 strated success of the Paddy's Run
                                 system, the EPA sponsored a test
                                 program to determine the factors which
                                 account for the successful operation of
                                 this FGD system.
                                  At the time that this test program was
                                 conceived, a wide range of operating
                                 problems were being encountered in
                                 many FGD units which were operating.
                                 One of the more serious process

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 problems was chemical scaling in the
 scrubber. A method being investigated
 by  many experimenters  to avoid this
 problem was to operate the FGD system
 in such a manner that the slurry liquor
 remains subsaturated with respect to
 calcium sulfate dihydrate (gypsum).
 Recognizing this fact, the EPA conceived
 a  program  whose overall objectives
 were to characterize the performance of
 the LG&E  system in  its "normal"
 operating mode, and to determine the
 features which make it possible for this
 system to operate in  a  subsaturated
 gypsum  mode. Additional tests  were
 planned to  simulate conditions  more
 typical of those encountered in  other
 lime-based systems and  to determine
 the  effects of changes  in important
 process operating parameters.
  The  intent of the program  was to
 provide useful information which could
 be  applied to other  FGD  systems.
 Ultimately, it was hoped that data from
 the successful operation at Paddy's Run
 could  be  extrapolated  to other lime/
 limestone systems.

 System Description
  The flue gas from the Paddy's Run No.
 6 boiler (65 M W) first passes through an
 ESP and then  is treated in one of two
 parallel marble-bed scrubber modules.
 The inlet flue gas typically contains
 1500-3000  ppm  of S02. During the
 EPA test program, the boiler was
 operated at half load, requiring the use
 of only one scrubber module.
  The  major features of the FGD unit
 are shown in  Figure 1. Each scrubber
 module contains  two  marble  beds in
 series, followed by two banks of chevron
                 mist eliminators. The scrubbing liquor is
                 introduced to the scrubber through
                 spray nozzles below each bed. The
                 scrubber effluent liquid streams consist
                 of the overflow  liquors from the two
                 marble beds  as  well as the scrubber
                 bottoms liquor. Approximately 7 cm (3
                 in.) of marbles are contained on each
                 bed. The downcomer weirs are of such a
                 height that the active gas/liquid contact
                 zone on each bed is about 25 cm (10 in.).
                   A unique feature of this system is the
                 mixing  well  into which the  three
                 scrubber effluent streams, the clarifier
                 overflow liquor, and  the lime  additive
                 slurry flow before they enter the main
                 reaction tank. The effective residence
                 time of the  mixing well  is about 30
                 seconds, whereas the residence times
                 of the main hold tank and surge tank are
                 about 35 and 5 minutes, respectively (all
                 of these residence times are for half-
                 load conditions). The  residence time of
                 the liquor on the beds averages 30
                 seconds, while the  normal scrubber
                 L/G is about 7.5 l/Nm3 (56 gal./103
                 scf).
                   The alkaline additive normally used at
                 Paddy's Run is carbide lime, purchased
                 from a local  acetylene manufacturer.
                 The  two basic  steps  in  producing
                 acetylene are: (1) commercial lime and
                 coke  are  heated to form calcium
                 carbide, and (2) the calcium carbide is
                 then reacted with water to form acetylene
                 and  calcium hydroxide,  commonly
                 called carbide lime.  This  regenerated
                 carbide  lime  retains some  impurities
                 from the processing which are carried
                 into the lime FGD system at  Paddy's
                 Run. The carbide lime additive is stored
                 as a 25 percent slurry in an additive tank
             Gas
             out


      Natural f
       gas   ' |
  22,500 l/min.
, L/G =7.5 l/Nm3
                                        10% solids
Flue gas -»
180,000
Nm3/hr
              Reaction tank
                770,000 I
                                                                -+40% solids
                                                                   to pond
Scrubber
bottoms
  tank
102,000 I
 Figure 1.  Simplified flow diagram - Paddy's Run No. 6 FGD system.

                                  2
and  is  fed  to  the  draft tube on  pH
demand. The pH of the reaction tank
effluent is generally 8.
  The surge tank effluent is the scrubber
feed stream. In addition, a portion of this
stream  is  routed to  the clarifier to
maintain a circulating slurry solids level
of 10  weight  percent. The clarifier
underflow (about 20 percent solids) is
sent to a set of two vacuum filters which
produce a filter cake containing 35-40
weight solids.
  System makeup water comes from:
(1)  mist eliminator wash water,  (2)
additive slurry,  (3) turning vane spray
wash water, and (4) seal  water  for
pumps and mixers. Mist eliminator and
turning vane spray washes are intermit-
tent; seal water and the lime slurry are
continuous makeup water sources.

Program Objectives
  The  overall  objective of the test
program was to determine quantitatively
the reasons for the operating success of
the Paddy's Run System. This unit had
not  experienced problems such as
chemical  scaling or mist eliminator
pluggage which have been associated
with many other lime and  limestone
SOa  scrubbing systems. One  important
aspect of this trouble-free operation is
the system's ability to operate subsat-
urated with respect to  gypsum. This
permits  the system to operate without
gypsum scaling problems.
  It has been established that subsatur-
ated conditions  are related  to sulfate
coprecipitation  with calcium  sulfite.
Laboratory studies have verified the
formation of calcium  sulfite-sulfate
hemihydrate solid solution1. These
studies  indicate that sulfate  can be
incorporated  into the calcium  sulfite
lattice to a  maximum sulfate  to total
sulfur ratio of about 0.16. In addition,
the  sulfate/total sulfur ratio in the
solids is directly related to the gypsum
relative saturation in the liquor. As long
as the sulfate production rate does not
exceed the rate at which sulfate can be
incorporated into the sulfite lattice, the
liquor from which the solids precipitate
will  remain subsaturated with  respect
to gypsum.  Gypsum scaling is not a
problem in a liquor which is subsaturated
with respect to  gypsum.
  There were several areas of interest
regarding operation in the subsaturated
mode. The primary area is the sulfite
oxidation rate. System parameters
which may impact the oxidation rate or
otherwise influence the subsaturated
mode of operation include additive type

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(carbide lime  vs. other additives),
reaction tank configuration, and soluble
ion concentrations. It was anticipated
that studies involving  these parameters
would yield insight into the question of
why subsaturated gypsum operation is
possible at Paddy's Run.
  To fulfill the overall program objectives,
four test phases  were originally out-
lined:
  Phase I—Carbide Lime Testing.
  Phase II—Commercial Lime Testing.
  Phase  III—Hold Tank  Modification
  Testing.
  Phase IV—Chloride/MgO Testing.
The objectives of each test phase are
discussed below.

Phase I—Carbide Lime
Testing
  The initial phase of testing involved
characterizing the LG & E Paddy's Run
No. 6 FGD system in  normal operation;
i.e., using carbide sludge as the lime
additive. The results of this test phase
served as the "base case" for compar-
ison with subsequent test results.

Phase II—Commercial Lime
Jesting
  The second phase of testing was per-
formed using commercial lime as the
alkaline additive  rather  than carbide
lime. The major goal of this phase was to
identify differences in operation which
might be caused by the change in the
lime additive. Particular attention was
given to monitoring oxidation rate
effects because oxidation was known to
be  a  key variable in  operating sub-
saturated with respect to  gypsum.
  All subsequent tests were conducted
using commercial lime as the additive.

Phase III—Hold Tank
Modification Testing
  Lime systems have the  advantage of
a very rapid additive dissolution rate.
Taking only  this factor into account,
high lime utilization efficiencies should
be attainable even for very short reac-
tion tank residence times. In one portion
of this test phase, the reaction tank resi-
de nee time was reduced to study the im-
pact of this change on the performance
of the system.
  A mechanical  feature of  LG&E's
Paddy's Run FGD unit, which is unique
to that particular system,  is the mixing
well. It has been suggested that a key to
the success of the LG&E system is as-
sociated with the operation of this mix-
ing well. This hypothesis was tested in a
second reaction tank modification test
which eliminated the effect of the mixing
well. This was accomplished by changing
the lime addition point from the mixing
well to the reaction tank.

Phase IV—Chloride/MgO
Testing
  The final phase involved testing the
effects  of chloride and magnesium
levels on subsaturated gypsum opera-
tion. It had been reported that increased
chloride ion concentrations may
decrease the amount of sulfate which
can  be  purged from the system  as a
solid solution  with calcium sulfite.
Indications that increasing magnesium
concentrations enhance the coprecip-
itation of calcium sulfate with calcium
sulfite  had also been reported. Sup-
porting evidence for these claims was
not found in recent laboratory studies
by Jones'3;  however, measurements
of these effects in an  actual operating
system  were desired  during this test
phase.

  All major tests outlined for each test
phase were  conducted during the test
program. However, due  to differences
encountered between commercial and
carbide  lime operation, the order of the
tests had to be changed. As discussed in
the  Results section, operation  with
commercial  lime led to  scaling in the
scrubber. Therefore, magnesium addi-
tion was employed to eliminate the scal-
ing conditions prior to the hold  tank
modifications test phase. Consequently,
the test phases were renumbered to:
  Phase I—Carbide Lime Testing.
  Phase II—Commercial Lime Testing.
  Phase III—MgO Addition Testing.
  Phase IV—Hold Tank Modification
  Testing.
  Phase V—Chloride Addition Testing.
Magnesium addition was  necessary
throughout the last three test phases to
maintain system operability.

Results

Phase I—Carbide Lime
Testing
  Phase I was conducted over a 6-week
period beginning mid-November 1981.
The FGD system operated according to
LG&E's  standard operating procedures
during this period. (The only change was
that the relatively high magnesium-
content  liquor  normally  used to slurry
the carbide lime was not used, so that
carbide  and commercial  lime could be
compared with low dissolved magnesium
concentrations in the scrubbing liquor.)
The scrubber feed pH set point was 8.0
which  resulted in scrubber  effluent
liquor pHs of  4.5-5.0. The L/G during
this operating period (and through most
of the program) was about 7.5 l/Nm3 (56
gal./103 scf).
  The  S02 removal efficiency ranged
from 75 to 83 percent according to the
DuPont on-line analyzer. The  DuPont
analyzer measured inlet SC>2 concentra-
tions between 1800 and 2000 ppm. Wet
test methods showed inlet SC>2 concen-
trations of 2000 to 2500 ppm. The SO2
removal efficiency calculated from wet
test results was about 5 percent lower
than  that measured  from  DuPont
analyzer results  because of higher
manually determined outlet concentra-
tions.
  The  concentrations  of important
dissolved ions which were measured in
the system during Phase I are plotted in
Figure 2.  Note that the calcium level
increased by about 50  to 70  percent
across the scrubber due to the dissolution
of solids in the low pH scrubber liquor.
Also,  note that the dissolved sulfate
level also increased across the scrubber,
but only by about  20 to 40 percent.
  The calcium solids dissolution which
occurred in the Paddy's  Run system at
base case conditions  is a significant
operating characteristic. Roughly 30 to
50 percent  of  the total alkalinity
required  for SO2 removal  was being
derived from calcium sulfite dissolution
in the scrubber. A significant portion of
the sulfate ion increase was also due to
solids  dissolution since some sulfate
exists  in  a  solid solution with the
calcium sulfite. The large amount  of
solid phase alkalinity required was due
to the relatively  low L/G employed
which  limited the total available liquid
phase  alkalinity.  The relatively long
slurry  residence time on the marble
beds (20-30 seconds) provided the time
required  for the  relatively slow solid
dissolution reactions to occur. Thus, the
mechanical design of the Paddy's Run
marble bed scrubbers resulted in the
large  percentage  increase  in calcium
ion concentration  which was observed
across the scrubber.
  If the concentrations of both Ca" and
SOJ increase across the scrubber, the
gypsum relative saturation will also
increase. This effect is shown in Figure
3. Since the  system  oxidation  level
remained below  15 percent during
Phase I,  the scrubber feed liquor
remained subsaturated with respect to
gypsum. The  lower bed downcomer

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liquor was also subsaturated during
most of this test phase,  except for a
short period when the system oxidation
level approached  15 percent and the
inlet relative saturation approached 1.0.
However, the increased gypsum relative
saturation across the scrubber, which
was caused primarily by calcium solids
dissolution, was not sufficient to create
scaling problems during Phase I.
       30
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-------
 between 0.9 and 1.0. Since the increases
 in Ca++ and SOI across the lower bed
 were  approximately equal during the
 two phases, the increase in  gypsum
 relative saturation was about 30 percent
 in  both Phase I and Phase II. The
 resulting lower  bed effluent  gypsum
 relative saturation was between 1.1 and
 1.3 during Phase II.
   Gypsum relative saturations less than
 1.3 are below what is generally consid-
 ered  to be the  critical  scaling limit.
 However, the lower bed effluent stream
 is a composite of the liquor leaving the
 entire lower bed. Regions on the bed
 which were burdened with higher than
 average S02  loadings would have
 experienced higher than average gypsum
 relative  saturations. In this situation,
 localized scaling might be expected.
 This  is exactly  what was observed
 throughout Phase II, even when the
 scrubber liquid  rate was raised to  its
 maximum value.
   The  results  from Phases  I and  II
 support  the  data gathered during
 coprecipitation laboratory studies which
 were performed by Radian for EPA2. In
 both  phases,  the gypsum  relative
 saturation of the scrubber feed liquor
 •B   fs
     1.0
 I
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 a
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   0.05
             Scrubber
             effluent
            	*
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            Phase I
            Results
Phase II
Results
               approached equilibrium as the solid
               sulfate/total sulfur ratio approached
               0.16. This  is  about the maximum
               amount of sulfate which can be incor-
               porated into the calcium sulfite hemi-
               hydrate crystal  lattice.  Infrared scans
               run on solid samples from both phases
               indicate that all of the sulfate in the solid
               phase present  was calcium sulfite-
               sulfate  solid solution. If  any of  the
               gypsum solids formed in the scrubber
               during Phase II were  carried to  the
               reaction  tank, they were  redissolved
               because  the reaction tank liquor was
               subsaturated with respect to gypsum.
                 Additionally, further work sponsored
               by the EPA has  identified  several
               reduced sulfur compounds as well as
               polynuclear  aromatics  in the  carbide
               lime2. Thiosulfate is one of these com-
               pounds which is a known inhibitor of the
               oxidation reaction of sulfite to sulfate. It
               is very likely that the successful opera-
               tion of the Paddy's Run system with car-
               bide lime is a result of  these contami-
               nants minimizing the sulfite oxidation
               rate. When commercial lime was used
               without inhibitors, the sulfite oxidation
               increased  to the  point where  the
               increase in gypsum relative saturation
               across the scrubber resulted in chemical
               scaling.


               Phase HI—MgO
               Addition  Testing

                 Once it was recognized that scaling
               under base  case  conditions was un-
               avoidable, a decision to  begin magnes-
               ium  addition was  made. Addition  of
               magnesium should increase liquid
               phase alkalinity and decrease the re-
               quirement for solids dissolution across
               the scrubber. It  was hoped that lower
               solids dissolution rates would alleviate
               the scaling.
                 The most dramatic effect of magne-
               sium addition was its impact on the liquid
               phase most alkalinity and the resulting
               SO2  removal efficiency. Table 1 sum-
               marizes this effect. Magnesium concen-
               trations of 170 mmole/liter (—4000 ppm)
               resulted in  removal efficiencies above
Table 1.     Effect of Magnesium Concentration On SOz Removal Efficiency

                                         Dissolved Magnesium S02 Removal
                                             Content (ppm)     Efficiency (%)
                                        99 percent.  At magnesium concen-
                                        trations of about 90-95 mmole/liter
                                        (—2000 ppm), removals between 90and
                                        95 percent were  obtained which were
                                        still significantly higher than the 75 per-
                                        cent achieved with either commercial or
                                        carbide lime alone.
                                          In  addition to  the increased SO2
                                        removal efficiency, the higher magnes-
                                        ium levels had a major impact on system
                                        operability. This is shown in Figure 6.
                                        When the magnesium concentration
                                        was  maintained at 170 mmole/liter
                                        (4000  ppm),  essentially no calcium
                                        dissolution occurred in the scrubber.
                                        Under these conditions, the sulfate/total
                                        sulfur ratio in the solid phase was about
                                        0.05 and the gypsum relative saturation
                                        was below 0.2 throughout the scrubbing
                                        loop. However, when the magnesium
                                        concentration  was  dropped  to 90
                                        mmole/liter (—2000 ppm), the scrubber
                                        effluent pHs dropped,  and calcium
                                        dissolution was noted in the scrubber.
                                        During  the same period the solid  phase
                                        sulfate/total  sulfur ratio rose to 0.13,
                                        and gypsum  scaling was observed  on
                                        scrubber internals. The gypsum scale
                                        thus formed was dissolved as the
                                        magnesium level was again increased.
                                          It was noted, however, that operation
                                        with magnesium addition is not without
                                        its drawbacks. High magnesium  levels
                                        appear  to lead to solids settling and
                                        dewatering problems. During Phase III,
                                        operation with  magnesium concen-
                                        trations above 180 mmole/liter (—4400
                                        ppm) led to clarifier operating problems.
                                        The  increased magnesium levels  in-
                                        creased the soluble sulfite and sulfate
                                        levels and created conditions which
                                        were conducive to excessive nucleation.
                                        This  created  small solid crystals which
                                        would not settle very efficiently. Clarifier
                                        settling problems were observed for
                                        almost  a week  following  2  days  of
                                        operation at  4400 ppm  magnesium. A
                                        reduction in the magnesium  level
                                        reestablished the formation of rosette
                                        crystal  structures which settled  much
                                        more efficiently. Figure 7 is an electron
                                        micrograph of scrubber solids when the
                                        dewatering  system was  performing
                                        satisfactorily.
Figure 5.  Comparison of oxidation
          rate and gypsum relative
          saturation values - Phase I
          vs. Phase II.
Note: Inlet flue gas contained
—2000 ppm SO2 and the dissolved
chloride concentration in the
scrubber liquor was <500 ppm.
200 (baseline}
2000
4000

75
90-95
99+


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Dissoved Mg
Concentration 750
(mmole/liter)
100
Dissolved Ca++ 20
Concentration JQ
(mmole/liter)
rt
CO 0 0 ° °0
0 o °° o '
00 ° °
Lower bed
**? Exit liquor
/ I Feed liquor
	 AA— -f< X_> f^-Affr-*-*! 	 A^ •» « « - -,
    Gypsum
     relative
    saturation
/.o
7.0
0.5
n
.Tj'Z.oive/'Aet/
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75 20 25 30 ' "5 ' ' 70 75 ' 20
Jt//?e 7S77 ^u/y 7377


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Figure 6.  Impact of magnesium level on oxidation and gypsum scaling potential
          (Phase III).
                                       Phase IV—Hold Tank
                                       Modification  Jesting
                                         Two reaction tank modifications were
                                       tested during Phase IV operation. First,
                                       the mixing well effect was eliminated by
                                       relocating the lime additive point from
                                       the mixing well  to the main  reaction
                                       tank.  In a second test, the residence
                                       time of the reaction tank system was
                                       reduced from about 35 minutes to about
                                       5  minutes  by bypassing the mam
                                       reaction tank. Both tests were conducted
                                       with Mg(OH)2 addition.
                                         Operation in  both  configurations
                                       proved to  be successful. As expected,
                                       the  effects of  magnesium  on SOa
                                       removal for each  configuration were
                                       quite similar to those shown in Phase III
                                       However, there were some differences
                                       in the gypsum relative saturations and
                                       the sulfite oxidation fraction for the two
                                       configurations. These differences  are
                                       shown  in  Figure 8.  Oxidation was
                                       somewhat higher during operation in
                                       the reduced residence time configuration.
                                       Mixing Well Elimination Test
                                         Basically, the effects of magnesium
                                       on  total  system  operation in this
                                       configuration were  similar to  those
                                       experienced in Phase III. With the lime
                                       additive point change, the system
                                       remained operable at magnesium levels
                                       above 100 mmole/liter (2400  ppm).

                                                         Reduced reaction

Dissolved
(mmole/liter)

Dissolved
Ca ^Concentration
(mmole/liter)


Gypsum
relative
saturation

^SO"
Total S


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                                                           25
                                                10
Figure 7.  Typical rosette formed in
          lime system (July 5,1977).
Figure 8.
                                            15       20
              July 1977                 August  1977

Impact of magnesium on system operation during Phase IV.
                                                                                                              24

-------
Slurry  streams  subsaturated  with
respect to gypsum were present through-
out the system, and  the  solid phase
sulfate/total  sulfur  ratio remained
about 0.05 to 0.07. When the magnesium
level was reduced and  maintained
below  100 mmole/liter, however,
significant calcium dissolution occurred
in the  scrubber,  and the  oxidation
fraction and gypsum relative saturations
approached inoperable levels.
  The  main effect expected from the
lime additive  point  change was an
alteration in the product crystal structure.
When  the lime  additive enters the
mixing  well,  lime particles  dissolve
directly into the scrubber effluent liquor,
which is relatively high in soluble sulfite
and has a relatively low pH. Locally high
relative saturations thus occur in the
region of  the  dissolving solid  Ca(OH)a
particles which promotes nucleation. In
the configuration where lime enters the
mam reaction  tank, the dissolving lime
particles encounter reaction tank liquor
which  has a  higher  pH and lower
soluble sulfite  concentration. Since the
localized relative saturations generated
in this situation would not be expected
to be  as  high,  more orderly crystal
growth  should be promoted by the "no
mixing well" configuration.
  The  results from  the draft tube
elimination test  support  this theory.
Shortly after the lime additive point was
moved  from the mix well, the crystal
morphology began changing from the
rosettes which were produced during
Phase III to structures which were more
platelet-like.  During  this transition,
solids settling  problems were encount-
ered. However, continued operation in
the "no mixing well" configuration and a
reduction  m magnesium concentration
resulted in calcium sulfite platelets
similar to those  produced in many
limestone FGD systems. The  large
platelets  formed during the latter
portion of this  test  settled well and
clarifier and  filter efficiencies  were
restored.  Figure 9  is  an electron
micrograph of  the platelet  solids.
Reduced  Reaction Tank
Volume

  The objective of the reduced reaction
volume test was to assess  system
operability with the main reaction tank
eliminated from the scrubbing loop. The
system did  remain operable with the
major difference being increased oxida-
tion in the reduced volume configuration
(Figure 8). This increased oxidation was
thought to have been caused by liquid
level control  problems in the  mixing
well. At times, the upper agitator blade
in the mixing well was exposed to the
air causing a frothing effect which could
have  increased  02  transfer into the
slurry  relative to normal  operation.
Other than this effect, operation with a
small reaction tank  volume was  very
similar to that with the normal reaction
tank configuration.


Phase V—Chloride Addition
Testing

  The final test phase was devoted to
determining  the effect of  increased
chloride levels on  system chemistry.
CaCb  was  added  to the  system to
increase the chloride level from 10
mmole/liter (350 ppm) to 80 mmole/liter
(2800 ppm). Since operating time was
limited during this phase, the magnesium
level was increased simultaneously to
maintain system operability. A ratio of 1
mole of magnesium added for each 2
moles of chloride was found to maintain
the scrubbing solution's liquid phase
alkalinity. The results of Phase V testing
are shown m Figure 10.
   Since the magnesium concentration
was increased in conjunction with the
increase in  chloride, extensive  data
concerning the  independent effect of
chloride are not available.  However,
data gathered early in this phase, before
the system was at steady state, indicate
the chloride  effect. An initial spike in
chloride concentration of 270 mmole/liter
(9600  ppm)  occurred.  The  results of
Figure 9.  Calcium sulfite hemihydrate
          platelets formed during "no
          mixing well" test.
operating at this high chloride concen-
tration were as expected. The calcium
concentrations were higher than  nor-
mal; an initial spike was noted in the oxi-
dation rate; significant dissolution  of
solid phase calcium in the scrubber was
evident; and scaling conditions  were
observed  on the lower  bed.  As the
chloride  concentration  in scrubbing
slurry and the clarifier liquor equalized
at about SOmmole/liter (2800 ppm), the
solid oxidation fraction  dropped  to
below 0.1 and subsaturated conditions
were again measured in lower bed ef-
fluent liquor. The  need for  calcium
solids dissolution was eliminated as the
magnesium/chloride ratio increased m
the scrubber feed liquor.
  As mentioned previously, the magne-
sium  concentration  was  increased  to
offset the addition of chloride.  Since a
magnesium level of 125  mmole/liter
(3000 ppm)  had maintained  system
operability at the conclusion of Phase IV
and since 1 mole of  magnesium electri-
cally balances 2 moles of chloride, the
magnesium concentration was increased
to about  160 mmole/liter to offset the
70 mmole/liter increase  in chloride.
Since the  magnesium  sulfite  and
carbonate salts are soluble, the liquid
phase alkalinity was essentially the
same in Phase V (after the initial spike in
chloride)  as during  Phase IV. The low
calcium dissolution rates in the scrubber
measured between  August 25 and  30
reflect this.

Solid Solution Chemistry

  A major objective of this program was
to'determine the basis for the operation
of the Paddy's Run  system in  a mode
which was subsaturated with respectto
gypsum.  During the course  of  this
program,  the solid phase sulfate/total
sulfur ratio was found to have  a major
impact on the gypsum saturation level
in the system's reaction tank liquor. This
same  result  was  also  found  in a
laboratory study previously conducted
by Radian1. In Figure 11, the field  data
from  the  LG&E test program  are
compared with the correlation  of solid
phase sulfate/total sulfur versus gypsum
relative saturation  derived  from the
laboratory experiments. While there is
scatter due to (1) unsteady-state opera-
tion, and (2) uncertainties in the gypsum
relative  saturations and analytical
results in Phase I, the results from the
field testing show that the reaction tank
liquor remained subsaturated when the
solid  phase sulfate/total  sulfur   level
remained below about 0.16.

-------
                     250
    Dissolved
  Mg^andCL
ion concentration
  (mrnole/liter)
  Qissolved Ca++
ion concentration
  (mmole/'liter)
   Gypsum
   relative
   saturation
    Sutfate
    Total S
    In solids
 1.5

 1.0


 0.5

 O


0.15

0.10


0.5
r                                   Lower bed
                                   Exit liquor
                             -\
                                   O
O    O
O
                            24   25    26   27    28   29   30   31
                                           August 1977
Figure 10.  Phase V system chemistry parameters.
                      Conclusions

                        • Carbide lime  contains  oxidation
                          inhibitors which allow the Paddy's
                          Run system to operate in a scale-
                          free mode. Without these oxidation
                          inhibitors, testing with commercial
                          lime resulted in gypsum  scaling in
                          the scrubber.
                        • Magnesium addition markedly
                          improved SC>2 removal efficiency by
                          increasing the liquid phase alkalinity
                          (98 percent removal at —3000 ppm
                          Mg++ with low chloride levels).
                        • Addition of magnesium (—3000
                          ppm) enabled  the Paddy's Run
                          commercial  lime system to operate
                          without scaling by (1) reducing  the
                          sulfite oxidation fraction,  and  (2]
                          reducing the  amount of calcium
                          sulfite dissolution which occurred m
                          the scrubber.
                        • Extremely high sulfate magnesium
                          concentrations (—4000 ppm Mg1"*
                          with low chloride levels) resulted in
                          the formation of solid crystals with
                          poor settling/dewatering character-
                          istics.
                        • An increase in chloride  tended to
                          increase sulfite oxidation and  the
                          tendency to scale.  Magnesium
                          addition can offset this effect.
                        • Lime systems can function with  low
                          reaction tank residence times due
                          to the rapid dissolution of lime. The
                          size of the  reaction tank and  the
                          lime addition point  location can
                          affect the crystal structure.
References

 1. Jones, Benjamin F., Philip S. Lowell,
   and Frank B. Meserole. Experimental
   and  Theoretical Studies  of Solid
   Solution Formation in Lime and
   Limestone SO2 Scrubbers, Volumes
   I  and II,  EPA-600/2-76-273a,b
   (NTIS PB264953 and 264954)
   October 1976.
 2. Holcombe,  L. J. and K. W Luke.
   Characterization of Carbide Lime to
   Identify Sulfite Oxidation Inhibitors,
   EPA-600/7-78-176 (NTIS PB286646).
   September 1978.

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