N 1
                     United States
                     Environmental  Protection
                     Agency
Municipal Environmental Research
Laboratory
Cincinnati OH 45268
                    Research and Development
EPA-600/S2-83-074 Nov. 1983
&ERA         Project  Summary
                     Land  Treatability  of  Refinery and
                     Petrochemical  Sludges

                     K. W. Brown, L. E. Deuel, Jr., and J. C. Thomas
                     The land disposal of API separator
                     sludges was investigated with regard
                     to  decomposition  rates of  organic
                     constituents and the possible impact
                     of these materials on plants and sur-
                     face water or groundwater  quality.
                     Two oily  sludges  (one  from a pe-
                     troleum refinery and one from a pet-
                     rochemical plant) were studied  as to
                     their phytotoxicity, biodegradability
                     in soils, water-soluble constituents,
                     and field mobility.
                      Concentrations of refinery sludge of
                     5% v/v and above depressed ryegrass
                     emergence  and  yield.  The  pet-
                     rochemical sludge suppressed emer-
                     gence and yield proportional to the
                     amount of sludge applied,  and the
                     suppression lasted longer than that
                     of the refinery sludge.
                     Biodegradation rates were greatest
                     when  small applications of sludge
                     were made at frequent intervals. Op-
                     timum  application  rates  for  both
                     wastes was 5% to 10% (wt/wt).
                     The water-soluble  compounds  in
                     both sludges were low in degradabil-
                     ity, potentially toxic, and extremely
                     mobile in high concentrations. These
                     results  indicate  a need for careful
                     management of land  treatment sites
                     to avoid groundwater contamination.
                     Gas-liquid  chromatography   (GLC)
                     combined with column chromatogra-
                     phy is recommended  for effective
                     monitoring of oily wastes applied to
                     soils.
                     This Project Summary was devel-
                     oped by EPA's  Municipal  Environ-
                     mental Research Laboratory, Cincin-
                     nati, OH,  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
 Soil disposal may prove to be the most
economical and environmentally sound
means  of  disposing  of many  of  our
complex industrial  wastes. Such  dis-
posal  can  be effective provided  that
application rates and scheduling do not
result in conditions that allow undesir-
able  components  or  degradation  pro-
ducts to run off or leach through the  soil,
and provided no materials accumulate to
toxic levels in the soil.
 Soil disposal of many wastes is effec-
tive because the soil  has large  surface
areas in which to absorb and inactivate
waste components. And if the soil is
properly managed, it  also  presents an
ideal medium for microbial decomposi-
tion because of the presence of oxygen,
water, and the nutrients needed for de-
gradation of organic constituents.
 Oily wastes are often separated from
reusable constituents or more easily  dis-
posed of  materials by the use  of  API
separators at petrochemical plants  and
depots. Certain fractions of the materials
accumulate as sludge in these pits  and
must be periodically dredged or pumped
out. These wastes have classically been
disposed of by deep-sea dumping, deep-
well  injection, incineration, landfilling,
and back-lot dumping.  But all of these
techniques have either economical or
environmental drawbacks that limit their
utility.
 This report  investigates the soil  dis-
posal of API separator sludges with re-
gard to decomposition rates or  organic
constituents and the possible impact of
these materials on plants  and  surface

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water or groundwater quality.  Because
of the complexity of the study, it  was
divided into four sections: phytotoxicity,
biodegradation,    water-soluble   con-
stituents, and field mobility of contam-
inants.

Phytotoxicity
 In  the  phytotoxicity  study,  measure-
ments were made of the impact of two
oil-water separator sludges on the emer-
gence and yield  of ryegrass (Loluim
multiflorum Lem.) grown on four diverse
soils in  the  greenhouse. One sludge
was from a petroleum refinery, and the
other was  from a  petrochemical plant.
Each was  applied at rates of 0%,  596,
1096, and  2096  v/v to each of the  four
soils to determine  the  influence  of ap-
plication  rates. After growth periods of
approximately 6 weeks, the grass  was
harvested,  and the  soil-sludge mixture
was air-dried, cultivated,  and  reseeded.
Eight harvests were made in sequence.
Soil wettability was measured  twice to
evaluate  physical problems.
 Concentrations of  refinery sludge  of
596 v/v  and above  depressed ryegrass
emergence and yield through two mech-
anisms:  phytotoxic  constituents  and
impaired water relations. The phytotoxic
constituents initially acted to retard plant
growth.  Several months  were required
for the sludge to degrade sufficiently to
allow normal  plant growth.  Subsequent
yield reductions  resulted from the  im-
paired water  relations  associated  with
residual hydrophobic hydrocarbons.  This
impairment was evidenced  by the in-
creased  water adsorption times  of the
sludge-treated soils.
 The petrochemical sludge had  higher
concentrations of both  organic carbon
and aromatics, and it suppressed emer-
gence and  yield  proportional  to   the
amount of sludge applied. The suppres-
sion lasted longer  than  that caused  by
the refinery sludge. Seedling emergence
from soils  treated  with 2096  refinery
sludge did not  differ from that  in  the
unamended control by the second plant-
ing;  but the  corresponding treatments
with the petrochemical  sludge resulted
in  depressed emergence for  the  first
five  replantings. Grass  yield  from  the
2096 refinery sludge treatment required
 1 3  months to reach control levels. The
corresponding petrochemical  treatment
yield reaches only  47% of the control
levels 17 months after application.

Biodegradation
 The biodegradation rates  of the  two
sludges  were studied  using  a soil re-
spirometer as  a  model for field studies.
Biodegradation rates were measured by
C02 evolution and residual hydrocarbon
analysis.  The  microbial  population was
determined  after 6  months  of  incuba-
tion of the waste-soil mixture. Parame-
ters  studied included soil  texture,  soil
moisture,  mineral nutrient amendments,
application rates, application  frequency,
and temperature. Maximum degradation
rates were achieved with Norwood sandy
clay at a temperature of 30C. The great-
est rate  of  biodegradation per  unit of
waste applied  occurred  when small ap-
plications  were made at frequent inter-
vals. Addition of mineral nutrients effec-
tively increased the  biodegradation rates
of both the refinery and the petrochemi-
cal sludges. The soil microcosm was
stimulated  by  small  applications  of
waste, but reduced numbers of microor-
ganisms were found when the applica-
tion  rates exceeded  5 g/100 g of soil
for either  sludge. Thus a comparison of
degradation  rate and the microbial pop-
ulation indicates that the optimum appli-
cation  rate  for both  wastes  is 596 to
1096 (wt/wt).

Water-Soluble Constituents
  A study of the water-soluble constitu-
ents of the refinery sludge was performed
using Bastrop sandy loam, Nacogdoches
clay loam, and Norwood loam. The sludge
was extracted with water, and the water-
soluble fraction (WSF) was  partitioned
into benzene. Concentrated extracts were
applied to soil thin-layer chromatographic
(soil TLC) plates and eluted with deionized
water. Soil column leaching studies sup-
plemented the soil TLC, and the analyses
of column leachates and soil TLC were
performed using gas-liquid chromatog-
raphy.
  Analysis of  the  WSF  yielded  largely
mono-  and  diaromatic  hydrocarbons
such as phenols and naphthalenes. Most
of  the  WSF  was  highly  mobile as  a
group on soil  TLC plates where the sol-
utes moved with the wetting front. Since
the  waste  constituents were  concen-
trated to achieve resolution, the mobility
may have been  a  result of concentra-
tions in excess of the adsorption capacity
of the soil. No significant mobility dif-
ferences occurred among the three soils
because of the  extreme mobility of the
WSF. Compounds  of increased polarity
and molecular  weight exhibited de-
creased  movement in all  soils.  Soil
column  results were inconclusive  be-
cause of confounding by soluble soil
organic matter.
  The low degradability and the potential
toxicity  of the  soluble compounds  in
conjunction with their extreme mobility
when applied at high concentration sug-
gests that careful  management  of land
treatment sites will be needed to assure
that groundwater   contamination  does
not occur.


Field Mobility  Study
 The field mobility study was conducted
to evaluate the fate of two  land-treated
oily wastes under  conditions that dupli-
cated field conditions as nearly  as pos-
sible. Controlled applications were made
of the  refinery sludge and  the petro-
chemical  sludge to  large  undisturbed
soil  monoliths  under field  conditions.
Soil samples were taken  periodically to
determine degradation and  residual  or-
ganics,  and leachate was collected and
monitored for potential groundwatpr con-
taminants. The same four  soils  were
used as in the  phytotoxicity study.
 Degradation  rates for neither sludge
were measurably influenced  by  soil  pH
or cationic distribution.
 Soil texture   profoundly affected  the
depth of migration. Depth of penetration
was inversely related to the degradation
rates observed when  fertility was  not a
limiting factor.  The deeper  the migra-
tion, the slower the decomposition. With-
holding nitrogen fertilizer reversed  the
trend and retarded decomposition in  the
zone of incorporation. This observation
is an  anomaly attributed to nutrients
leached from the surface  profile and to
the attendant  nutritive requirements re-
lated to the  material  balance within a
given depth interval. Hydrocarbon levels
within surface  horizons were materially
greater than subsurface horizons requir-
ing a greater nutritive level.
 Climatic  factors were  normalized over
soils because of the juxtaposition of  the
field-installed   lysimeters.   Degradation
rates were diminished for both  refinery
and petrochemical  sludges over the win-
ter months corresponding to the  lowered
soil temperatures.
 Gas-liquid chromatogrphy (GLC) analy-
sis together with  column chromatogra-
phy was an effective  means of monitor-
ing the fate of complex waste hydrocar-
bons applied to soils.
 Significant amounts  of  water  moved
through all the soil profiles during  the
study period, buy hydrocarbons were not
found in detectable  concentrations in
leachate  from  any of the  lysimeters.
Leachate  collected as long  as  2 years
after waste application remained free of
hydrocarbons.

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Conclusions and Recommen-
dations
 Though oily  sludges applied  to  land
may initially be phytotoxic and  reduce
the yield of the vegetation that manages
to emerge, the toxicity diminishes with
time. Thus soils used for land treatment
of oily sludges can eventually be reveg-
etated.
 A comparison of degradation  rate with
the microbial  population indicates that
the optimum  application rate  for  both
the refinery  and petrochemical sludges
is 5% to 10% (wt/wt).
 The water-soluble compounds in  both
sludges are  potentially toxic, low in de-
gradability,  and extremely mobile when
applied at   high  concentrations.  Thus
careful  management of land treatment
sites   is  recommended   to   prevent
groundwater contamination.
 The  mobility  of waste organics and
their degradation products  in soil  are
not well understood.  GLC analysis com-
bined with column chromatography can
be  effectively  used  to monitor  these
wastes  in soils. Additional  information
should  be  developed on  the  fate and
mobility of organic wastes in the soil  so
that land treatment facilities can  be de-
signed  and  managed to  protect our
groundwater resources.
 The full report was  submitted in fulfill-
ment of Grant No. R805474013 by the
Texas  Agricultural Experiment Station
under the sponsorship of the U.S. Envi-
ronmental Protection  Agency.
K. W. Brown, L E.  Deuel, Jr., and J. C.  Thomas are with Texas Agricultural
Experiment Station,  College Station, TX 7784O.
Robert E. Landreth  is the EPA Project Officer (see below).
The complete report, entitled "Land Treatability of Refinery and Petrochemical
  Sludges," (Order No. PB 83-247 148; Cost: $19.00. 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:
        Municipal Environmental Research Laboratory
        U.S. Environmental Protection Agency
        Cincinnati, OH 45268
                                          •frUS GOVERNMENT PRINTING OFFICE 1983-659-017/7216

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