United States
                    Environmental Protection
                    Agency
Air and Energy Engineering
Research Laboratory
Research Triangle Park NC 27711
                    Research and Development
 EPA/600/S7-85/050 Jan. 1986
4>EB\         Project  Summary
                    Thermophilic Anaerobic
                    Biodegradation  of  Phenolics
                    Frank J. Castaldi and Barbara J. Hayes
                      This report presents the results of a
                    series of anaerobic microbial acclima-
                    tion and treatment performance tests
                    conducted with synthetic phenolic sub-
                    strates. The research is a feasibility
                    level assessment of substituting anaer-
                    obic biodegradation  of phenolics for
                    solvent extraction. The tests demon-
                    strated the feasibility of biodegrading
                    phenol and p-cresol to methane under
                    thermophilic anaerobic conditions. The
                    experimental data indicate that anaero-
                    bic biodegradation of phenolics under
                    thermophilic conditions involves a dual
                    system of bioaccumulation  and
                    biodegradation. Phenolics and un-
                    known metabolites were accumulated
                    in the anaerobic floes of sludge, and
                    these compounds were apparently
                    slowly degraded over time. Despite pe-
                    riodic upsets, treatment improved  as
                    the phenolic loadings were incremen-
                    tally increased during the experiments.
                    This indicates that, although acclima-
                    tion of thermophilic anaerobic bacteria
                    to phenolics is difficult, it can be accom-
                    plished using normal microbial cultiva-
                    tion techniques. Moreover, degradation
                    intermediates identified during ther-
                    mophilic anaerobic treatment of pheno-
                    lics were similar to those found in efflu-
                    ents from anaerobic treatment systems
                    that operate at lower temperatures.
                      This Project Summary was devel-
                    oped by EPA's Air and Energy Engineer-
                    ing Research Laboratory, Research Tri-
                    angle 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
                      Fixed-bed coal  gasification waste-
                    waters are generally high in biochemi-
cal oxygen demand. The largest fraction
of the carbonaceous biochemical oxy-
gen  demand characteristic of these
wastewaters can be attributed to the
presence of phenolics. In addition to
phenols, the wastewaters contain ap-
preciable levels of cresols, xylenols, and
aromatic heterocyclic compounds with
nitrogen contained in the  ring.
  The chemistry of fixed-bed gasifier
wastewaters offers the potential for a
biological treatment  alternative to sol-
vent extraction pretreatment of high
phenolic wastewaters.  A  conventional
wastewater treatment system for fixed-
bed coal gasification quench conden-
sates consists of tar/oil separation, sol-
vent extraction (phenolics removal),
steam stripping (ammonia and acid gas
removal), aerobic biodegradation, and
assorted tertiary treatments (specific to
discharge or reuse requirements). This
system is energy intensive and presents
both health  and  safety (worker expo-
sure to solvents) and hazardous materi-
als handling (phenolic by-product) con-
siderations.
  This research is a feasibility level as-
sessment of substituting anaerobic
biodegradation of phenolics for solvent
extraction. This alternative treatment
system would consist of tar/oil separa-
tion, steam  stripping,  anaerobic bio-
degradation, aerobic biodegradation,
and assorted tertiary treatments. Anaer-
obic  biodegradation would eliminate
many of the  health and  safety concerns
posed by solvent extraction treatment
while also producing methane as a by-
product. Methane may be generated in
sufficient quantity to meet the power re-
quirements  of the entire alternative
wastewater treatment train.
  The anaerobic treatment system
would provide simultaneous storage,

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equalization, and treatment of steam-
stripped quench condensates and other
process wastewaters. Since the process
would receive wastewaters at tempera-
tures in excess of 95°C, the anaerobic
biodegradations should occur  in the
thermophilic temperature range (49 to
57°C) to minimize cooling requirements.
These temperatures are consistent with
equilibrium bioreactor temperatures es-
timated from heat balances  on the
anaerobic process.  Operation  in the
thermophilic range would thus remove
much of the cooling requirement typical
of most mesophilic microbial treatment
processes. (Traditionally, hot waste-
waters are cooled  by retention in large
aerated impoundment ponds. This
practice also permits the uncontrolled
release of volatile compounds to the at-
mosphere.) A thermophilic anaerobic
treatment process would restrict the re-
lease  of volatile compounds  Because
the emissions  are controlled during
treatment.  The major gaseous emis-
sions from the process are methane and
carbon dioxide. The thermophilic tem-
perature range should also optimize the
rate of microbial conversion.

Objectives
  The purpose of this  research was to
study the feasibility of  biodegrading
phenolics to methane  by thermophilic
anaerobic  treatment. The study was  a
feasibility  level assessment which ex-
amined techniques for culturing ther-
mophilic bacteria, acclimating these mi-
croorganisms to  phenolics, and
assessing toxicity thresholds for simple
phenol. The study was conducted with
bench-scale test reactors using syn-
thetic substrates composed of phenol,
p-cresol, organic acids, and basal salts.
Both continuous-feed and batch treat-
ment tests were conducted and treat-
ment  performance monitored. Where
possible,  degradation intermediates
were identified. These data provide the
basis for assessing the feasibility of
thermophilic anaerobic biodegradation
of phenolics.

Results and Conclusions
  The report  presents the results  of  a
series of anaerobic  microbial  acclima-
tion and  treatment  performance tests
conducted with synthetic phenolic sub-
strates. These tests  were designed to
demonstrate the feasibility of biode-
grading phenolics under  thermophilic
anaerobic conditions. Two types of ex-
periments were conducted:
  • microbial seed acclimation tests
    using mixed cultures of anaerobic
    microorganisms grown under ther-
    mophilic conditions, and
  • treatment performance tests using
    acclimated microorganisms sub-
    jected to  both continuous and
    batch biodegradation conditions.
The experimental results are discussed
relative to the feasibility of achieving
thermophilic anaerobic biodegradation
of phenolics characteristic of most
fixed-bed coal gasification wastewaters.

Microbial Seed Acclimation
Testing
  Mesophilic anaerobes from a munici-
pal sewage sludge  digester were used
to seed two test bioreactors. These
sludges were fed a mixture of phenol
and organic acids and were subjected to
mixed liquor temperatures between 52
and 55°C. These two bioreactors were
operated throughout the acclimation
period  at  different  substrate loadings.
Although the  bioreactors were loaded
similarly, they performed differently be-
cause of differences in the nature of the
microbial cultures developed  during
seed acclimation.
  The microorganisms showed  an in-
herent ability for thermophilic anaero-
bic biodegradation of  phenol  early in
the acclimation cycle.  After three  hy-
draulic residence times, a flocculent mi-
crobial mass developed that settled well
and produced an effluent that was low
in phenol. Overall chemical oxygen de-
mand (COD) reduction  lagged  phenol
removal:  optimum COD removal was
not obtained until  after  about  six  hy-
draulic residence times.  Methane was
detected in the off gas from the bioreac-
tor whenever these gases were sam-
pled during the acclimation period.
  Although the bioreactors consistently
reduced the phenol concentration in the
wastewater, the  apparent level  of
methane  produced did not keep pace
with the rate of phenol removal during
the early stages of the acclimation.
However, this was  not unexpected be-
cause methane-forming bacteria  are
usually slow to develop in most anaero-
bic treatment processes. The  bioreac-
tors also  maintained relatively low con-
centrations  of volatile  cell  mass
throughout the test, and the apparent
rate  of growth  of  new biosludge was
negligible.

Performance Testing
   Performance testing consisted of two
continuous-feed biodegradation experi-
ments with similar  populations of accli-
mated thermophilic anaerobic bacteria.
Each experiment was designed to track
the change in phenol, p-cresol, acetic
acid, and propionic acid in a test reactor.
Treatment performance data for one
test are presented in Table 1. This reac-
tor was fed phenol at 1000  mg/L,
p-cresol at 50 mg/L, and volatile organic
acid as equal quantities of  acetic and
propionic acids (i.e., 200 to  400  mg/L).
The bioreactor was operated with an hy-
draulic residence time of 20  days and a
mean cell residence time of  about
60 days. The system maintained a mass
loading of 0.04 mg  phenol/mg total
volatile suspended solids (TVSS)/day
throughout the test run.
  Test data indicate relatively uniform
treatment performance  with the re-
moval of cresol and  acetic  acid. How-
ever, variable effluent qualities for phe-
nol and propionic acid may be the result
of several system specific factors. The
mass loading of phenol to the bioreac-
tor could change the equilibrium con-
centration within the mixed liquor by no
more than 50 mg/L for each day of oper-
ation. Therefore, an apparent rise in the
mixed liquor phenol concentration of
between 78 and 230 mg/L over a single
day of bioreactor operation must be the
result of factors other than the normal
changes in biochemical reaction rate
typical of microbial processes. One
such condition is the accumulation of
phenol within the floes of sludge before
actual biodegradation occurs. This ac-
cumulation probably results from sorp-
tion of phenol to the activated sludges
because of the lipophilic  properties of
the floes.  Therefore, the biofloc may
carry much  higher concentrations of
phenol than actually are  measured in
the liquid of the  reactor. From time to
time, desorption may occur, liberating
phenol and unknown metabolites to the
reactor liquid. These compounds would
be quickly taken up by the biomass and
biodegraded  in the normal course of
process operation. However,  point-in-
time measurements will  show effluent
quality variability as reported by the test
data.  The  accumulation  and eventual
biodegradation of degradable  pollu-
tants on floes is a common  occurrence
in activated sludge treatment.  Whether
this  phenomenon presents problems
specific to thermophilic anaerobic treat-
ment of phenolics cannot be assessed
from the experimental data.

Conclusions
  The following conclusions result from
the study of thermophilic  anaerobic

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Table 1

Test
Day
1
4
5
6
7
8
W
11
12
13
14
15
16
17
18
19
20
22
25
27
Thermophilic Performance Test
Influent

Phenol
(mg/L)
_b
—
1030
-
-
7070
-
570
—
-
-
-
-
-
7000
-
7000
-
7020
-

Cresol
(mg/U
50
-
31
-
-
38
-
48
-
-
_
-
-
_
47
-
48
14
31
<5
Acetic
Add
(mg/L)
300
370
-
-
-
350
-
230
320
310
770
97
-
-
250
-
200
<5
-
-
Propionic
Acid
(mg/L)
280
310
-
-
-
440
-
230
490
240
760
775
-
-
300
-
590
<5
95
-

COD
(mg/L)
3040
3100
2970
3120
-
-
-
2440
-
3140
-
2890
-
-
2570
-
2960
2680

2810

Phenol
(mg/L)
<5
-
<5
79
<5
-
230
<5
55
70
6.2
<5
<5
75
790
720
<5
76
<5
733

Cresol
(mg/L)
<5
-
<5
<5
<5
-
<5
<5
<5
<5
<5
<5
<5
<5
-
<5
<5
<5
<5
<5
Effluent3
Acetic
Acid
(mg/L)
<5
<5
<5
<5
<5
<5
<5
<5
<5
<5
-
<5
<5
36
-
84
6
<5
<5
-

Propionic
Acid
(mg/U
97
-
96
-
94
-
703
770
86
770
-
88
70S
95
-
76
90
700
80
-


COD
(mg/U
170
-
237
234
724
_
570
790
775
750
726
734
753
282
-
350
270
204
702
224
"Reactor total volatile suspended solids (TVSS) equals 1400 mg/L during test.
bBlank (-) means parameter not analyzed.
degradation of synthetic phenolic sub-
strates:
  • Experimental results indicate that
    phenol and p-cresol can be metabo-
    lized to  methane  under ther-
    mophilic anaerobic conditions. This
    microbial treatment process was
    sustained for a  period of 6 months
    with  continued improvement in
    treatment performance. A phenolic
    toxicity  threshold for the microbial
    process was not evident when the
    degradations were performed with
    acclimated microorganisms. Rela-
    tively short  acclimation  periods
    were  required to achieve consistent
    treatment performance (i.e., greater
    than 90 percent removal of phenol)
    at low  substrate concentrations.
    However, extended periods of accli-
    mation  (i.e.,  greater than six hy-
    draulic  residence times) were re-
    quired to achieve acceptable
    treatment at higher substrate (phe-
    nolic) loadings.  Generally, accept-
    able treatment occurred coincident
    with the development of a floccu-
    lated  biomass.  However, the pres-
    ence  of dispersed microorganisms
    signalled  poor  treatability. These
    observations indicate that stable
    treatment performance could be
    maintained with conventional  mi-
    crobial acclimation techniques.

 •  The experimental data indicate that
    thermophilic anaerobic biodegrada-
  tion of  phenolics involves a dual
  system of bioaccumulation and
  biodegradation. Phenolics and un-
  known  metabolites  are  accumu-
  lated in the anaerobic floes, and
  these compounds are released to
  the liquid at various times during
  treatment.  Process control would
  specify  a condition that optimizes
  the degradation of toxics in the liq-
  uid phase  while maintaining an
  equivalent level of treatment for the
  sludges. Operating under this con-
  dition would minimize the produc-
  tion of new cell mass.
• Although the test bioreactors expe-
  rienced upset conditions in the early
  stages of the acclimation study,
  phenolic wastes were continuously
  fed to the systems throughout the
  upset periods. Despite these peri-
  odic upsets, system  performance
  improved as the waste  loadings
  were incrementally increased dur-
  ing the experiments. This indicates
  that, although  acclimation of ther-
  mophilic anaerobic bacteria to phe-
  nolics is difficult, it can be accom-
  plished using normal microbial
  cultivation techniques.
• The experimental observations indi-
  cate that proportional increases in
  reactor biomass relative to pollutant
  loading  will not guarantee that the
  individual phenolic compounds and
  intermediates will be  uniformly de-
graded. This would imply that sys-
tem kinetics may not fit a conven-
tional microbial substrate utilization
model.
The experimental data indicate that
degradation intermediates  identi-
fied during thermophilic anaerobic
treatment of phenolics were similar
to those found  in effluents from
anaerobic treatment  systems that
operate at lower  temperatures.

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    F. J. Castaldi andB. J. Hayes are with Radian Corp., Austin, TX 78766.
    William J. Rhodes is the EPA Project Officer (see below).
    The complete  report, entitled "Thermophilic  Anaerobic  Biodegradation of
       Phenolics," (Order No. PB 86-122 603/AS; Cost: $11.95. subject to change)
       will be available only from:
            National Technical Information Service
            5285 Port Royal Road
            Springfield, VA 22161
            Telephone: 703-487-4650
    The EPA Project Officer can be contacted at:
            Air and Energy Engineering Research Laboratory
            U.S. Environmental Protection Agency
            Research Triangle Park, NC 27711
United States
Environmental Protection
Agency
Center for Environmental Research
Information
Cincinnati OH 45268
Official Business
Penalty for Private Use $300

EPA/600/S7-85/050
           0000339   PS

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