.'*'
                    United States
                    Environmental Protection
                    Agency
Industrial Environmental Research
Laboratory
Research Triangle Park NC 27711
'W
                    Research and Development
EPA-60O/S2-84-137  Sept. 1984
SERA         Project Summary
                    Toxicity Treatability  of  Iron  and
                    Steel  Plant  Wastewaters:
                    A  Resource  Document
                    B. H. Carpenter, M. R. Branscome, C. W. Westbrook, W. F. Gutknecht, and
                    A. Gaskill
                      The full report documents an assess-
                    ment of the biotoxicity reduction and
                    concurrent pollutant reduction achieved
                    by 24 wastewater treatment systems
                    serving 8 iron and steelmaking process
                    subcategories. Sampling programs, de-
                    signed to provide measurements before
                    and  after successive unit  treatment
                    processes, were conducted at seven
                    plants.  Chemical analyses  were  per-
                    formed for conventional, priority, and
                    regulated pollutants. Additional tests
                    were made to identify other potentially
                    harmful metals and organics. Bioassays
                    were performed  using  both minnows
                    and daphnia. The results of chemical
                    analyses were compared with toxic
                    concentration limits in relating biotoxic-
                    ity to pollutant concentrations.
                      Cokemaking wastewater treatment
                    systems tested that employed single-
                    stage bioreaction yielded more highly
                    toxic effluents than did the physical/
                    chemical treatment. Ironmaking waters
                    treated  to below 2,000  fjg/L total
                    metals were nontoxic to  minnows.
                    Steelmaking waters after flocculation
                    and clarification retained toxic levels of
                    lead and zinc. Hot forming wastewaters
                    showed low biotoxicity where metal
                    concentrations were reduced sufficient-
                    ly. Cold forming  wastewaters showed
                    varying biotoxicities associated with the
                    levels of oil and grease, organics, and
                    metals remaining after treatment. Treat-
                    ment studies for  hot coating and pick-
                    ling wastewaters showed good reduc-
                    tion of biotoxicity.
                      This Project Summary was developed
                    by EPA's Industrial Environmental He-
search Laboratory, Research Triangle
Park, NC, to announce key findings of
the research project that is fully docu-
mented in a separate report of the same
title (see Project Report ordering infor-
mation at back).

Introduction
  Raw wastewaters from iron and steel-
making processes have been shown to
contain potentially  biotoxic pollutants.
Outfall compliance data identify toxicities
that persist after currently applied treat-
ments. Treatments have been assessed
for removal of identified and regulated
pollutants, but not for concurrent reduc-
tion of biotoxicity. As part of EPA's
industry-specifictoxicity information pro-
gram, this study develops data on waste-
water  toxicity, its  treatability, and its
variability from eight iron and steelmaking
process subcategories.
  With the cooperation of the plants,
wastewater treatment systems were se-
lected  to include eight iron and steel-
making process categories: cokemaking,
ironmaking, steelmaking, continuous cast-
ing, hot forming, pickling, cold forming,
and hot coating. Many technologies in-
cluded in  the treatment systems were
representative, to some extent, of BPT,
BAT, or NSPS. Several systems were
chosen to identify possible limitations in
biotoxicity removal. Each study was car-
ried out while the production facility was
operating at rates reasonably represent-
ative of normal production.
  Wastewater treatment systems in steel
plants  are somewhat unique. While those
studies use many of the unit processes

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inherent in BPT and BAT models,  a
complete match, process by process,
seldom exists. Selected systems included
processes  that  have been  shown to
decrease pollutant loadings.
  Samples  were taken  upstream  and
downstream of treatment system  unit
processes. Composite samples were ob-
tained using automatic samplers except
where work areas were designated haz-
ardous.  Composites in such areas were
made from  a sequence of grab samples.
Grab samples were also taken to prevent
loss of cyanide, volatile organics, and oil
and grease through  degradation  that
might occur during composite sampling.
  Containers were packed  in  ice for
immediate delivery to testing laboratories,
and were  analyzed within  prescribed
holding periods.
  Ten percent of the composite samples
taken were split for chemical analyses by
the two laboratories involved, for quality
control purposes. All sampling and  ana-
lyzing were done according to a compre-
hensive quality assurance plan prepared
for the study.

Summary and Conclusions
  Analytical results  indicated that the
wastewaters sampled were  generally
representative of their respective process
subcategones. While some raw vyaste-
waters  were  markedly  different  from
median values developed previously, the
overall  characterizations  show  typical
subcategory trends.
  Toxicity and pollutant reductions affect-
ed  by treatments were determined, and
are presented in detail in the full report.
Where  treated wastewaters  remained
toxic, pollutants with remaining concen-
trations greater than toxic limits previous-
ly determined in other studies are given
here. These are  identified as probable
causes. Using this method, little evidence
of synergistic effects was found. That is,
where several toxic pollutants remained
just below  their toxic limits, their com-
bined presence did not appear to induce
higher biotoxicity.

Cokemaking
  Three treatment systems were studied:
two using  single-stage  bioreaction (no
nitrification), and  one using physical/
chemical treatment.
  Plant C's bioreactor feed is first cooled
and diluted with river water. The two
parallel biobasins  used 136 aerators.
Retention time was 62  hours. Effluent
was clarified after polymer addition.
Toxicity (LCso) to minnows was reduced
from 0.61 to 3.8; daphnia ECso was not
reduced significantly (<1 to 1.5). Am-
monia, cyanide, and benzo(a)pyrene were
reduced39,6, andO percent, respectively,
and all were above toxic concentrations
in the treated waters.
  Plant D's bioreactor feed was diluted
also. Less aeration was used, and reten-
tion time  was  32 hours. Bioreactor ef-
fluent passed through a thickener before
discharge. Upsets in operation permitted
carryover  of solids, and initial toxicities
were  higher than those from  later re-
samples. Toxicity to  minnows  was re-
duced from 0.17 to 32.3;  for  daphnia,
from 0.16 to 31. Remaining biotoxicity
coincides with  concentrations of ammo-
nia, phenol, benzo(a)pyrene, cyanide, and
zinc that exceed toxic limits.
  Plant G's treatments include equaliza-
tion, clarification, filtration, carbon ad-
sorption, and alkaline chlorination. Equal-
izer holding time was 24 hours; clarifier
overflow, 0.0037 mVmin; filter flow-
through, 0.045 mVm2 x min;  adsorber
flowthrough, 0.09  m3/m2 x min;  and
chlorinator detention time, 2.8 hours.
  M innow LC50 was reduced from 0.85 to
71.5; daphnia ECso was not reduced, and
remained at 5.3. Residual chlorine, cya-
nides, and copper (extraneously in-
troduced) all exceeded-toxic  concentra-
tions in the final effluent.

Ironmaking
  Plant A's recycle system uses thicken-
ers (holding time 3.6 hours) with polymer
addition  and sludge recycle.  Overflow
passes to a cooling tower  and  makeup.
Slowdown is clarified  and chlorinated,
then used for coke quench. No reduction
in biotoxicity to either minnows (21.6) or
daphnia (6.8) was shown.  Chlorine and
zinc remained above toxic limits, although
the latter was 98.8 percent removed.
  Plant D's treatments included floccula-
tion and thickening, with an overflow rate
of 0.03 mVm2 x min at a flow rate of 56.8
mVmin. Raw  and  treated waters were
nontoxic to minnows; EC5o's were 42 for
daphnia.  Ammonia, lead,  and  zinc ex-
ceeded criteria or toxic limits.

Steelmaking
  Two treatment systems were studied at
Plant A.
  That  for a  suppressed combustion
process used hydroclones, settlers, poly-
mer addition, and thickening (5-hour
holding time). Minnow LCso's were 71 on
treated waters; daphnia EC5o's, 58.6.
Phenol, lead, and zinc were 0, 99, and
99.4 percent removed, respectively, but
still exceeded toxic concentrations. Am-
monia (60 percent removed) at 0.4 mg/L
may have contributed to toxicity.
  The system for wet open combustion
used  thickening  after polymer addition,
and pH adjustment.  Slowdown passed
through  a second  thickener.  Minnows
survived in a 65 percent dilution; daphnia
EC50 was >32. Ammonia, lead, and zinc
were  65, 93, and 98  percent removed,
respectively, but remained above toxic
concentrations.

Continuous Casting
  Plant B's treatments were: scale pits,
deep  bed filters (walnut shells), cooling
towers, and recycle.  Raw and treated
water were nontoxic to minnows. Daphnia
were  killed  in  a  60 percent sample.
Ammonia, zinc, and copper were removed
0, 30 and 10 percent, respectively, and
remained slightly above toxic limits.
  Plant E's treatment included: scale pits,
deep  sand filters,  cooling towers, and
recycle. Minnow LCso's were unchanged
at 2.4-2.75;  daphnia ECso's remained at
6.2-6.6.  Nickel, zinc,  and  copper were
removed 7, 17,  and 13 percent, respec-
tively, but remained above  toxic concen-
tration limits.

Hot Strip and Cold Rolling Mills
  Plant A treated combined hot and cold
rolling wastewaters using  scale pits, oil
skimming, flocculation with alum  and
polymer, and  clarification (1.6 hours
retention). Then a central treatment was
applied to these and waters  from the
slabbing mill. This included scalping with
chlorination and settling basins. Minnows
survived in 64 percent raw and treated,
hot-forming wastewaters;  daphnia
showed an EC5oof >32. Residual chlorine
may have contributed to the toxicity.
  The cold rolling raw wastewater showed
a minnow LCso of 0.45 and a daphnia ECso
of 8.3. Further increases in toxicity were
shown after sump waters were  added.
Tetrachloroethylene,  lead, nickel, and
zinc were reduced 0, 65, 26,  and 13
percent, respectively, from their above
toxic levels by treatment  and dilution (31
times) with hot-forming wastewaters. After
central treatment, the biotoxicities were
essentially the same as those of the raw
hot-forming  wastewaters.
  Plant D combined slabber and scarfer
wastewaters with those from hot-form-
ing, and applied oil skimming  and filtra-
tion  using  sand and anthracite coal.
Minnow LC50 was 35 on filtered waters;
daphnia, >32. Ammonia, nickel, and zinc
were  removed 41,51, and >75 percent.

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 respectively, but remained above toxic
 concentration limits.
   Plant F applied scale pits, settling, oil
 skimming, and deep-bed filtration to hot-
 forming  wastewaters.  Neither the raw
 nor the treated  wastewaters were bio-
 toxic. Ammonia, nickel, and zinc were
 removed 0,  73, and 89 percent, respec-
 tively, but their remaining concentrations
 slightly exceeded some toxicity limits.

 Slabbing  Mills
   Plant A's slabbing mill wastewaters
 were combined with hot-strip mill waters
 for treatment. Raw wastewaters from the
 slabbing mill were only slightly toxic to
 minnows; the EC5o for daphnia could not
 be calculated due to inappropriate choice
 of dilutions for the test, but was reduced
 by treatment. Ammonia was not reduced
 and exceeded toxic limits.
   Plant B applied scale pits, polymer
 addition, and settling basin with  oil
 skimming. Raw and treated waters were
 nontoxic to  minnows and daphnia. Lead
 and nickel  were reduced 67 and 36
 percent, respectively, but remained very
 slightly above toxic limits.

 Section Mills
   Plant A applied scale pits, oil skimming,
 clarification, dilution, and cooling.  Raw
 and treated waters were nontoxic to
 minnows; toxicity to daphnia was  not
 defined. Metals were reduced 97 percent.
 Ammonia remained at <0.4 mg/L.
   Plant E applied oil skimming, cooling,
 and  recycle, with blowdown to central
 treatment with combined wastewaters.
 The waters  were not toxic to minnows
 and only slightly toxic to daphnia before
 and after oil skimming.

 Pickling
   Plant F (combination  acids) applied
 neutralization, polymer addition,  clarifi-
 cation, and dilution to raw wastewaters.
 Treated waters  were nontoxic to min-
 nows, and  75 percent  of the daphnia
 survived in 100 percent sample. Ammonia
 and  nickel  were reduced  0 and 99.6
 percent, respectively, but remained above
 toxic limits.
   Plant B (hydrochloric acid) combined
 these wastewaters with cold-rolling wa-
 ters and applied oil skimming, air oxida-
 tion, neutralization with lime, and clar-
 ification after polymer addition. Minnow
 LC5o was reduced from 8.8 to nontoxic;
 daphnia, from 90 percent killed  in a 6
 percent sample to 100 percent killed in a
,95 percent sample. The pH was low after
 treatment. Final toxicity may  have been
due to additives that were not determined
in the analyses.

Cold  Forming
  Plant A applied oil skimming, followed
by a central treatment of combined waste-
waters. Raw waters were  nontoxic to
minnows, as were treated waters. Daph-
nia ECso was reduced only to 4.2 by
treatment. High oil and grease and other
organics are suspected causes of remain-
ing toxicity.
  Plant B's cold-rolling  system was dis-
cussed under Pickling, above.

Hot Coating
  Plant C  applied equalization, neutral-
ization with lime, and clarification with
polymer. The effluent was  nontoxic to
minnows and daphnia, although zinc (98
percent removed) remained above toxicity
limits.

Central Treatment
  Plant E's combined waters for central
treatment  showed a minnow LDSO of 2.4
and an ECso for daphnia of 0.1. Central
treatment  applied chrome pretreatment,
cyanide pretreatment, equalization, neu-
tralization  with caustic and acid, floc-
culation with polymer,  clarification and
surface skimming. Minnows survived 65
percent in a 100 percent sample; daphnia
ECso was  38. Ammonia, chlorine,  and
nickel  were  reduced 0, 0,  and 99.5
percent, respectively, but remained above
toxic concentration limits.

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      B. H. Carpenter et at. are with Research Triangle Institute, Research Triangle Park,
      NC 27709.
      David C. Sanchez is the EPA Project Officer (see below).
      The complete report, entitled "Toxicity  Treatability of Iron and Steel Plant
        Wastewaters:  A Resource  Document," (Order No. PB 84-232 495; Cost:
        $13.00, 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:
              Industrial Environmental Research Laboratory
              U.S. Environmental Protection Agency
              Research Triangle Park, NC 27711
   •6 U S GOVERNMENT PRINTING OFFICE. 1984 — 759-015/7814
United States
Environmental Protection
Agency
                                     Center for Environmental Research
                                     Information
                                     Cincinnati OH 45268
Official Business
Penalty for Private Use $300

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