United States
            Environmental Protection
            Agency
             Industrial Environmental Research
             Laboratory
             Cincinnati OH 45268
EPA 600 2-80 143
June 1980
            Research and Development
oEPA
Electrolytic
Treatment of Oily
Wastewater From
Manufacturing and
Machining Plants

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                RESEARCH REPORTING SERIES

Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology. Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:

      1.  Environmental Health  Effects Research
      2.  Environmental Protection Technology
      3.  Ecological Research
      4.  Environmental Monitoring
      5.  Socioeconomic Environmental Studies
      6.  Scientific and Technical Assessment Reports (STAR)
      7.  Interagency Energy-Environment Research and Development
      8.  "Special" Reports
      9.  Miscellaneous Reports

This report has been assigned  to the  ENVIRONMENTAL PROTECTION TECH-
NOLOGY series. This series describes research performed to develop and dem-
onstrate instrumentation, equipment, and methodology to repair or prevent en-
vironmental degradation from point and non-point sources of pollution. This work
provides the new or improved technology required for the control and treatment
of pollution-sources to meet environmental quality standards.
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia  22161.

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                                          EPA-600/2-80-143
                                          June 1980
  ELECTROLYTIC TREATMENT OF OILY WASTEWATER
   FROM MANUFACTURING AND MACHINING PLANTS
                        By

                    R. L. Gealer
                    A. Golovoy
                    M. Weintraub
                Ford Motor Company
              Dearborn, Michigan 48121
                 Grant No. 580*17*
                   Project Officer

                     H. Durham
           Industrial Pollution Control Division
      Industrial Environmental Research Laboratory
                Cincinnati, Ohio *5268
INDUSTRIAL ENVIRONMENTAL RESEARCH LABORATORY
      OFFICE OF RESEARCH AND DEVELOPMENT
     U.S. ENVIRONMENTAL PROTECTION AGENCY
           •   CINCINNATI, OHIO 45268

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                                  DISCLAIMER
      This  report  has  been reviewed  by  the  Industrial  Environmental  Research
Laboratory-Cincinnati, U.S.  Environmental  Protection  Agency,  and  approved for
publication.  Approval does not signify that the contents necessarily reflect the views
and policies  of the U.S. Environmental Protection Agency, nor  does mention  of trade
names or commercial products constitute endorsement or recommendation for use.
                                       ii

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                                   FOREWORD
      When energy  and material resources  are  extracted, processed, converted, and
used, the related pollutional impacts on our environment and  even on our  health often
require that new and increasingly more efficient pollution control methods be used.  The
Industrial  Environmental  Research  Laboratory  -  Cincinnati  (lERL-Ci)  assists in
developing and demonstrating new and improved methodologies that will meet these
needs both efficiently and economically.

      This report describes a continuous electrolytic treatment process for removal of
emulsified oil from  dilute oily wastewater  streams, such as  is generated in  metal
working operations.  Results obtained from operating a pilot plant facility  demonstrate
the feasibility of the process.   The electrolytic process may offer  an alternative to
conventional chemical  treatment  for small to  medium size  machine  shops.   TKe
Industrial  Pollution Control Division is to be contacted for further information.
                                                   David G. Stephan
                                                       Director
                                       Industrial Environmental Research Laboratory
                                                      Cincinnati
                                        111

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                                   ABSTRACT
      A continuous electrolytic treatment is being developed to remove emulsified oil
from dilute oily wastewater streams, such as is generated in metal working operations.
In this process, the wastewater permeates  through  an iron  chip bed anode and steel
mesh  cathode.  A potential is applied to the electrodes, forming ferrous ions at the
anode and hydroxyl ions at the cathode.  The ferrous ions react in a complex manner
with the emulsifying agents,  destabilizing  the emulsion and  generating an oil  rich
floating sludge and essentially oil-free water.

      A pilot plant unit capable of processing about 5700  I/day (1500  gal/day) was
designed, constructed, and evaluated at an actual plant site.  Operating parameters and
process equipment were evaluated to assess the  potential and problems of the process.

      Wastewater with initial oil concentrations in  the range of 300 to 7,000 ppm of
solvent extractables has been reduced to less than 50 ppm in 90% of  the test runs, and
to less  than 25 ppm in 83%.  These test runs were done at  conditions of minimum
operating cost and minimum sludge generation.  When necessary, Freon extractables
generally are reducible to about  10 ppm or less by the addition  of more electrolytically
dissolved iron to the system at a small increase in cost.

      Preliminary economics look  favorable and overall results are quite encouraging
so that further scale-up of the process is recommended.

      This report was submitted in fulfillment of Grant No. S-804174 by Ford Motor
Company  under the sponsorship of the U.S. Environmental  Protection Agency.  The
report covers the period May 18,  1976 to August 17, 1978, and work was completed as of
August 17, 1978.
                                       IV

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                                   CONTENTS






Foreword	il1



Abstract	iv



Figures   	vl



Tables    	vii



    1.   Introduction   	  1



    2.   Conclusions and Recommendations   	  3



    3.   Experimental    	  4



             Experimental facility  	  4



             Experimental procedure	  6



    4.   Results and Discussion	   14



             Analysis of plant effluent	   14



             Operating parameters    	   19



             Effluent quality   	   29



             Durability studies    	   32



             Electrode plugging  	   *1



             Sludge flotation and sludge characteristics   	42



             An approach to automatic control     	44



             System capacity design criteria    	45



             Economic projections     	45




 References    	  ^8

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                                    FIGURES






Number



    1   A schematic diagram of the electrolytic cell	    5



    2   A flow diagram of the electrolytic process   	    7



    3   Experimental electrolytic treatment test facility	    8



    4   Flow cell, view from upstream end    	    9



    5   Sludge skimming apparatus   	    10



    6   Oily wastewater receiving and storage tank   	    11



    7   Effect of iron to oil  weight ratio on effluent oil content   	    30
                                         VI

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                                     TABLES


Number                                                                     Page

    1.  Steady-State Measurement in the Electrolytic Cell	   12

    2   Analyses of Untreated Wastewater   	   15

    3   Summary of Operating Conditions and Effluent Quality	   20

    4   Iron Dissolution Rate  	   27

    5   Results of  Treatment of Plant Wastewater With and
            Without pH Adjustment    	   28

    6   Summary of First Durability Test   	   33

    7   Summary of Second Durability Test  	   35

    8   Summary of Third Durability Test    	   36

    9   Summary of Fourth Durability Test  	   37

    10   Summary of Fifth Durability Test	   39

    11   Evaluation of the Performance of the Dissolved Air Flotation    ....   43

    12   Capital Costs of Electrolytic Treatment	   47
                                        VII

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                                   SECTION  1

                                 INTRODUCTION
     Process wastewater from metal working operations contains free or suspended oil
and emulsified oil which must be removed before the water can be discharged or reused.
These oils originate mainly from parts washer overflow and machining coolant dumping,
and the concentration typically ranges from  1,000 - 10,000 ppm as emulsified oil and
perhaps 30,000 ppm as free suspended and floating oil.  The free oil can  be removed by
gravity separation and a simple skimming operation, but the removal of the  emulsified
oil is more complicated. These oil-in-water emulsions are intimate two-phase mixtures
of oil and water with oil dispersed as microscopic droplets (0.1-100 pm diameter) in the
aqueous phase and stabilized  by the presence of surface active compounds.

     Wastewaters containing these emulsions generally are treated for discharge by pH
adjustments and the addition of salts of such metals as  iron or aluminum, to produce a
flocculant precipitate.  A common technique is to begin by treating the oily wastewater
with sulfuric acid to effect a primary emulsion break. The freed oil is collected and the
water  phase, which still may contain up to 400 ppm  of emulsified oil, is further treated
with ferric chloride and sodium hydroxide.  The ferric ion destabilizes the emulsion by
neutralizing the charge on the emulsion droplets and precipitates as ferric hydroxide —
the oil is sorbed on and into the flocculant precipitate.  These conventional methods,
while yielding water  of good quality, generally increase the dissolved solids  content of
the water and generate a voluminous sludge containing about 95% water.  For small-to-
medium  size machining  plants to  install  a  new waste treatment  facility based on
chemical treatment,  space  limitations  would  present the  greatest  problem.    The
electrolytic process  being developed by Ford Motor  Company has the potential to
overcome the limitations noted above in  that it is a continuous process which requires
less space, generates less dissolved solids, and produces less sludge  with lower  water
content.

      Earlier development work on this  process is  described in References 1-3.  The
method  is one in which the  reactive cation, iron is  introduced electrolytically as a
ferrous ion followed by in situ oxidation to the ferric state and subsequent precipitation
as ferric hydroxide.  In this method the oil-in-water emulsion is destabilized during  the
oxidation  reaction   before   extensive  coagulation and   flocculation   occur.    The
demulsification  is thought to take place  by  attack  on the  emulsifiers by hydroxyl
radicals generated during ferrous  ion oxidation, as well as by direct  reaction  of  the
emulsifiers with ferrous ion.  The demulsified oil is  then removed by adsorption  on  the
highly dispersed ferric hydroxide microfloc.

      The objective of the present work was to develop and  demonstrate on a pilot scale
the electrolytic method of removing emulsified oil from oily wastewater generated by
                                        -1-

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metal fabrication  operations, and to establish its technical and  economic feasibility.
The pilot unit was installed at the Ford Motor Company Livonia Transmission Plant and
actual plant discharge was fed to the unit for treatment.
                                         -2-

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                                    SECTION 2

                    CONCLUSIONS AND RECOMMENDATIONS
     The results of the electrolytic pilot unit study for treatment of oily wastewater
indicate  that the  process is capable of rendering the  wastewater suitable for direct
discharge to municipal sewers and possibly to surface waters.  The exact nature of the
influent, however, will strongly influence the final effluent quality from the process. In
these studies it was found that by operating the unit at minimum cost and minimum
sludge formation to just break the emulsion, the effluent contained less than 50 ppm
90% of  the  time and  less than  25 ppm 83% of the  time,  where the  influent oil
concentrations  ranged  from  300 to  7,000  ppm.  Reduction in  the effluent oil
concentration to about  10 ppm or  less generally can be accomplished, when necessary,
by an increase in  the iron concentration, since it was  observed that the ratio of iron
dissolved to oil concentration is the major parameter determining the  water  quality-
iron concentration is controlled by controlling the current in the electrolytic dissolution
of iron.

     Of  the other parameters  examined,  the  salt  type  (added  to increase ionic
conductivity and prevent electrode passivation) is the next important.  Calcium  chloride
was  found to aid in the demulsification of the oily wastewater and was ordinarily the
preferred salt.  A concentration  of  0.01N was employed in  most runs.  The use of
calcium  chloride does  cause  an inconvenience since calcium carbonate deposits may
tend to build-up on the cathode.  The pH of the as-received wastewater ranged from 8.5
to 10.5 which is typical for  machining coolants. Treatment effectiveness is the same in
this  pH  range  as it is with the pH adjusted to 6.5  to  7,  thus  pH  adjustment is
unnecessary. Flow rate through the process should be fixed to handle the plant flow and
slight variations in the flow  do not appreciably influence the effluent.

      A preliminary economic analysis indicates  that the direct costs of the process
(power, calcium chloride, and iron  valued as scrap) can range from  about  $0.09 to
$0.17/1000 1  ($0.34 to $0.64/1000 gal) depending on the type of equipment employed in
the process.  Unanswered questions  remain with respect to extended durability of the
process,  practicability  of  a  completely  automated-continuous  process and  the best
technique for recovering oil from the generated sludge.

      To answer these  questions,  it  is recommended that the  process be scaled up to
approximately  two  to  five times the pilot  unit capacity and that  the system  be
automated to achieve unattended continuous operation.
                                         -3-

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                                   SECTION 3

                                 EXPERIMENTAL
EXPERIMENTAL FACILITY

     A schematic diagram of the electrolytic cell is shown in Figure  1.  Wastewater
enters  the cell and  permeates  through a rectangular caged bed  of iron  or steel
machining  chips which acts as anode,  and then through a  perforated sheet metal
cathode.  Sufficient voltage  is applied to dissolve the iron forming ferrous ions which
react with the emulsifying agent freeing the oil.  This oil is sorbed onto the ferric
hydroxide floe which is  formed in-situ by oxidation of the ferrous ion.  The oil-rich
ferric  hydroxide  sludge  floats  to  the surface  where it  can  be skimmed,  yielding
essentially oil-free water.

     The electrolytic cell is constructed of  1.27 cm thick plexiglas in an angle iron
frame.  The cell is  91 cm wide, 61  cm high, and 244 cm long.  Wastewater enters the
cell  through a manifold  with multiple outlets to assure uniform distribution of  flow
through the electrode.  The 7.6 cm thick anode  cage is constructed of expanded
titanium with  diamond shaped holes with approximate size of  1.5 x 0.5 cm. Since bare
titanium was found  to corrode under some circumstances because of galvanic action, it
was coated with a protective  coating of insulating varnish which alleviated the  problem.

     The front face of the anodic cage is lined with a polyethylene screen with a hole
size  of  about  0.15  on.  The screen is installed to ensure that the iron chips do not
extend  outward and  contact the cathode or, when small  enough, fall  in the space
between the electrodes.

     The anodic  cage is filled  with  low carbon steel  chips obtained from machining
operations in the plant. The optimum  size of the chips was found to be 1-2 cm long and
with diameter of 0.2-0.5 cm. Smaller diameter chips tend to fall through the screen,
and longer ones tend to form entanglements causing  difficulties  in packing the chips in
the anodic cage.  The cathode, spaced  1.27  cm from the anode, is constructed of  a
perforated steel plate. A clearance of about 4 cm is  maintained  between the bottom of
the cathode and the  bottom  of  the anodic cage to reduce the possibility of electrical
short circuiting by loose iron  chips.  The cathode height was extended up to about  1 cm
below the water level to  allow oily sludge to float over it and avoid sludge accumulation
between the electrodes.   Demulsification  reactions and sludge flotation occur in the
remaining length of the cell.

     The introduction of air for oxidation of the ferrous ion and for flotation of the
sludge is accomplished by forcing air  through a porous membrance on the cell bottom.
The  membrane has an average  pore  size of 1  ym.  In later  experiments, the use of
dissolved air flotation in  place of air bubble flotation was evaluated.


                                       -4-

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OILY EMULSION
WASTE WATER
                      DC POWER
                        SUPPLY
OIL-FERRIC HYDROXIDE SLUDGE
                                                             TREATED
                                                              WATER
  IRON CHIP BED ANODE7  AIR IN    MESH CATHODE    ^ BUBBLE
                                                  GENERATOR
                  Figure 1. A schematic diagram of the electrolytic cell

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      The cell  and ancillary  equipment (pumps,  sand  filter,  sludge skimmer, power
supplies, etc) are installed in a specially constructed enclosure within the plant. A flow
diagram for the system is shown in Figure 2, and photographs of the cell  and system are
shown in Figures  3 through 6. The 11.3 m  (3000 gal) wastewater receiving and storage
tank is outside the enclosure but inside the plant.  Nominal capacity of the  system is
about 3.8 1/min (1 gal/min).


EXPERIMENTAL PROCEDURE

      Both simulated and actual plant wastewater were processed through the cell. The
simulated  wastewater  was  processed according to  techniques developed  in  the
laboratory  to  evaluate  the overall cell performance and to compare the operational
parameters to those obtained in previous experiments with a laboratory bench  size unit.

      Simulated  wastewater  was  prepared by continuous flow  mixing of machining
coolant emulsion concentrate with water in a ratio to give the desired oil concentration.
The standard evaluations  were carried out using 2,000 ppm emulsified oil processed at
3.8 1/min (1 gal/min) using a current of 25 amp with an average potential of 15 v for 8
hr. Hydrochloric acid was added to adjust the pH to 7 and sodium chloride was added to
maintain the conductivity at  1500  ymho/cm (0.58 g/1 of sodium chloride).  Results of
these experiments indicated that steady-state conditions are reached after about 6 hr of
operation which is approximately 1.5 times the plug flow residence time. This is seen in
Table  1  which shows  turbidity reading in nephelometer  turbidity units  (NTU)  as a
function of time and position  in the cell past the cathode.

      Before October  1977,  the  plant  wastewater, which  was collected  from  the
combined plant wastewater wet well over a period oL 2 hours, was carried  in mobile
tanks to the receiving tank in batches of about 11.3 m  (3000 gal). Prior to processing,
the plant effluent was analyzed for pH, conductivity, turbidity, dissolved and  suspended
solids, and Freon extractables.  Several runs were made with each of the batches in
which the current and/or the flow rates were varied and the corresponding effluent
quality determined.  Each run lasted 6-8 hours  and used about  1.89 m   (500 gaU of
wastewater.  Before passing through the cell, sodium  chloride or  calcium chloride may
be added for conductivity and to avoid anode passivation, (which would result  in current
being expended to  generate oxygen  rather than  dissolve iron), and the  pH may  be
adjusted  with hydrochloric acid. Following the electrolytic treatment the water may be
passed through a sand filter to remove suspended solids.  Some batches, when received,
were treated  with  about. 7.6 1 of household bleach and 200  g  of cup'ric chloride to
minimize bacteria  growth and odor  development because  of  long standing in  the
receiving rank.   Laboratory  batch experiments indicated that the bleach and cupric
chloride addition  did not significantly influence the emulsion stability.

      In October  1977  a pumping system  which can continuously supply the  pilot unit
with fresh  wastewater was installed.  The inlet of the pumping system is located at a
manhole  which  receives  wastewater  from  most  of  the plant operations  via  three
streams. The composition of wastewater  delivered to the pilot  unit was  found  to be
essentially the same as that received at  the  wet well  of the wastewater  treatment
plant.

      After the installation of the pumping system the  receiving tank could be filled
daily with enough water for  one day of operation. Because it was now convenient to

                                        -6-

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                            ACID  SALT

                              \l
FREE
OIL
r
   FLOW
EQUALIZATION
   TANK
rv
              AIR
PLANT  OILY
WASTEWATER
                              PRETREATMENT
AS REQUIRED
  BY PLANT
WASTEWATER
                                           IRON CHIP
                                          CAGE ANODE
                                        DISCHARGE
                                                         OIL RICH-
                                                       IRON HYDROXIDE
                                                          SLUDGE
                                                    — 1
                                                          ELECTROLYTIC
                                                              CELL
                                                             Ttttt
                                                                           .BELT
                                                                            SKIMMER
                                                              AIR


                                                       STEEL MESH
                                                        CATHODE
                                                                   .BACKWASH
                                                                  1^" TO TANK
                                                       CLEAN
                                                       WATER
                                                        TANK
                                                      TO FILTER  BACKWASH
                 Figure 2.  A flow diagram of the electrolytic process

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I
oo
                           Figure  3.   Experimental  electrolytic  treatment test facility

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I
o
                              Figure 4.   Flow cell, view from upstream end

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Figure 5.   Sludge  skinning  apparatus

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                                                                               I

Figure 6.   Oily wastewater receiving  and  storage  tank

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TABLE 1.   STEADY-STATE MEASUREMENT IN THE ELECTROLYTIC CELL

Time, hr. Turbidity (at distance past cathode),
5 cm
0 2500
3 540
4 45
5 26
6 26
7 16
8 19
45 cm
2500
270
47
28
19
15
14
100 cm
2500
180
22
23
17
15
12
150 cm
2500
130
23
17
10
11
8
NTU
exit
2500
150
13
5
5
6
6
                           -12-

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have a  holding time  of  only  one day, the biocidal treatment with  bleach and cupric
chloride was no longer necessary.  As before, the wastewater  was analyzed  for pH,
conductivity, turbidity, Freon  extractables, solids, and anionic surfactants.  In addition,
a one  liter sample of the wastewater  was treated electrolytically  in a beaker  to
determine the proper  setting of the operating parameters for effective treatment.  This
was  done  by adding an  amount of  salt to  the wastewater to  give the  desired
conductivity, setting  the current  at 0.5 amp and observing the  time required to just
break the emulsion. The results were  used to calculate the concentration of iron which
is necessary to break the emulsion. The flow rate and current  in the pilot unit were
then set to give the same iron concentration.

     The electrolytic unit has  been operated  with a single  set of electrodes and
provided with air bubblers  for oxidation and flotation of the sludge. During a run the
current, voltage, pH, conductivity, wastewater flow rate, and turbidity are checked and,
if necessary, adjusted every hour. After  6-8 hours, when  steady  state conditions are
reached, samples of the effluent and floating sludge are collected for  analyses.

     During most  of  the  program period the floating sludge was removed by a belt
skimmer at the end  of  the unit.  In April, 1978 a  dissolved  air flotation unit was
installed to improve the  flotation of the sludge and reduce  the level of suspended solids
in the effluent.  The  unit is a Komline-Sanderson pilot flotation unit—model HR/SR-1.
(Komline-Sanderson Corp.,  Peapack, NJ).  The flotation area is 929 cm  (1 ft ).

     Dissolved Air Flotation (DAF)  is  a liquid-solid separation process that takes
advantage of the fact that  if air is dissolved in water under pressure, and the pressure is
later  released, the dissolved air will  be released from  solution in the form  of  vast
numbers of minute bubbles.   Actual flotation occurs  when  these bubbles  become
attached to suspended solid particles, oils, or immiscible liquids, thus  increasing their
buoyancy and causing them  to rise to the surface of the liquid in  which they are
suspended.  Floated  material is  skimmed from the surface, and the clarified liquid
overflows from the rear of the unit.
                                        -13-

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                                   SECTION  4

                           RESULTS AND DISCUSSION
ANALYSIS OF PLANT EFFLUENT

     Oily wastewater from the Livonia Transmission Plant is usually white in color with
some tramp oil and scum floating on top.  Occasionally, the color of the wastewater
may be gray, the result of excess free oil and dirt. The wastewater has a mild odor of
machine oil  which sometimes turns rancid upon standing. This rancid odor is caused by
a bacterial  reaction  which releases hydrogen sulfide.  Details of the composition,
bacterial reactions  and general  comments  relating to cutting  fluids  can be found in
References 4, 5, and 6.

     The  Livonia  Transmission  Plant  represents  one of the most varied  machining
operations that would be  encountered in the industry.  The Livonia plant does drawing,
broaching,  grinding,  machining  etc.  on  various  cast  iron,    aluminum,  and steel
compositions.  As a result of this, the wastewater is one of the most complex to treat.
The major  components of  the wastewater  are emulsified ("soluble") oils, surfactants,
and tramp oils.  In addition, it sometimes contains hydraulic oils, drawing compounds,
transmission fluids, etc.  The chemical composition and physical characteristics of the
plant effluent change frequently  and unpredictably.

     Samples of the  plant effluent were analyzed for oil  by Freon extraction (Freon
extractables), turbidity, anionic  surfactants, pH, and conductivity and periodically for
dissolved and suspended  solids.   In the first  nine months of the program the batches
were collected from a wet well just before the wastewater treatment plant.  In the
following 8 months the batches were collected from a process sewer line which leads to
the wet  well.  Unless otherwise indicated,  the  tests  were performed  according to
procedures recommended by the  U.S. Environmental Protection Agency (7).  The results
of the  analyses of over 80 samples, which were subsequently used in the evaluation of
the electrolytic pilot unit, are presented in Table 2.

Freon Extractables

     Freon extractables  ranged from 313 ppm to 7164 ppm and averaged 1822 ppm with
standard deviation of 1370 ppm.  It is  comprised mostly of  soluble  oil and surfactant,
and some tramp oil.  Occasionally it may include hydraulic oils, drawing compounds,
etc.

Turbidity

     The average turbidity as  measured in Nephelometer Turbidity  Units  or  NTU's
(Model 2424 Analytical Nephelometer, Hach Chemical Company, Ames, Iowa) was 1780
NTU with standard deviation of 1280 NTU. The minimum turbidity was 300 NTU and

                                      -14-

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TABLE 2.  ANALYSES  OF UNTREATED WASTEWATER

Date
12-16-76
02-01-77
02-11-77
03-08-77
03-28-77
04-04-77
06-15-77
06-21-77
06-29-77
08-09-77
10-03-77
10-04-77
10-12-77
10-13-77
10-18-77
10-19-77
10-20-77
10-21-77
10-25-77
10-26-77
11-01-77
11-03-77
11-08-77

Freon
extractables
ppm
1300
864
3771
4973
3110
1075
7164
2004
5178
2300
1934
1326
1850
1414
3253
3058
1230
2451
848
2980
870
2472
492

Anionic
Turbidity surfactants
NTU ppm
880
1200
3300 250
3800
1600 75
1250
3250
920
2700
970 70
2700
2200
2400
1900
4300
5500
1750
3000
1100 224
3500 247
1150 121
3300 285
520 108


PH
9.4
7.3
9.1
9.1
9.6
9.0
10.2
7.8
8.0
8.1
9.5
10.1
10.0
9.6
9.4
9.8
9.3
9.6
10.1
10.0
10.1
10.6
10.3


Conductivity
;ifl~l cm~l
870
1040
1090
3000
1100
950
1080
840
700
940
1600
850
900
1500
800
870
850
480
610
500
900
1420
800
(continued)
                    -15-

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TABLE 2.  (continued)
Date

11-10-77
11-22-77
11-23-77
12-13-77
12-15-77
12-19-77
12-20-77
01-09-78
01-10-78
01-11-78
01-12-78
01-13-78
01-16-78
01-17-78
01-18-78
01-19-78
01-20-78
01-26-78
01-30-78
01-31-78
02-01-78
02-02-78
Freon
extractables
ppm

700
708
313
624
591
375
664
736
2369
1045
1450
704
825
557
586
1205
3328
3230
622
2300
1600
1250
Anionic
Turbidity surfactants
NTU ppm

800
1200
310
650
550
300
450
800
2900
1200
1700
900
900
550
560
1100
2000
4500
600
2000
1900
1500

206
150
130
180
170
120
90
170

120
90
95
160
95
70
280
-
-
-
-
-
-
Conductivity
pH yfl"1 cm"1
4
10.0 1250
9.6 620
9.9 560
10.2 780
11.4 3300
10.3 750
10.3 800
9.9 1000
10.2 1350
10.2 1400
9.6 1100
9.8 1040
10.2 1200
10.2 1340
10.1 1050
9.7 1220
9.9 1280
9.8 750
9,. 6 650
9.2 750
9.7 750
9.9 900
                                  (continued)
           -16-

-------
TABLE 2.  (continued)

Date
02-14-78
02-15-78
02-16-78
02-20-78
02-21-78
02-22-78
02-23-78
02-24-78
02-25-78
02-26-78
02-27-78
02-28-78
03-01-78
03-02-78
03-03-78
03-09-78
03-10-78
03-13-78
03-14-78
03-15-78
03-16-78
03-17-78
03-20-78

Freon
extractables
ppm
745
1004
2544
1725
1708
1331
5388
4984
3154
2050
1260
1117
1071
2538
1270
935
1296
1956
1444
3315
1342
1200
900

Anionic
Turbidity surfactants
NTU ppm
640
1300
2600
1750
2200
1750
5200
4900
5300
2400
1150
950
1200
2000
1150
1000
1200
1500
800
1900
1200
1300
750

-
100
40
60
45
130
150
90
90
40
25
30
35
45
50
60
55
35
60
45
50
-

PH
8.4
8.3
8.5
9.2
9.4
9.1
8.9
8.0
8.0
7.5
8.2
8.8
8.7
8.5
8.6
8.6
8.9
9.2
9.2
9.2
9.2
9.0
8.6

Conductivity
yfT1 cm"*
650
650
660
750
1000
950
850
850
950
750
750
1450
700
750
770
680
950
880
1000
1150
1050
780
600
(continued)
         -17-

-------
TABLE 2.  (continued)
Date
03-21-78
04-06-78
04-11-78
04-12-78
05-02-78
05-03-78
05-04-78
05-05-78
05-11-78
05-23-78
05-24-78
05-25-78
X
ff
Freon
extractables
ppm
970
826
1305
1102
968
1526
1217
2230
1186
1361
3218
3842
1822
1370
Turbidity
NTU
1100
620
1400
780
720
770
870
1600
1000
1400
2900
4200
1780
1280
Anionic
surfactants
ppm
-
50
70
40
35
40
30
45
30
45
80
90
102
70
Conductivity
pH pfl"1 cm"1
8.4
9.9
9.8
10.3
10.6
10.1
10.3
10.0
10.4
9.7
9.5
10.4
9.3
1.4
600
950
860
900
1000
1050
1080
860
850
740
800
1200
963
469
      -18-

-------
the  maximum   5500 NTU.    The turbidity  correlates  relatively well  with Freon
extractables with a correlation coefficient of 0.79.

Anionic Surfactant

     The surfactants in the wastewater are mainly petroleum sulfonates (sodium  salt)
and  carboxylates which are used to stabilize the oil-in-water emulsion and in  washing
operations.  The average concentration of  the anionic surfactants was  102 ppm with a
standard deviation of 70 ppm.  The maximum value was 285 ppm and the minimum  25
ppm.
     The pH of the plant wastewater varied between 7.3 and 11.4. The average pH was
9.3 with standard deviation of 1.4.

Conductivity

     The conductivity  of   the  wastewater varied between 480 and 3300  y mho/cm.
The average conductivity was 963  ij mho/cm.

Dissolved Solids

     The dissolved solids are comprised mainly of the inorganic salts in the wastewater.
The  dissolved solids, which contribute to the conductivity  of the effluent, ranged
between  750 and 1160 ppm and averaged 1000 ppm for the few runs analyzed.

Suspended Solids

     The suspended solids,  comprised of dirt, fine metallic  particles, scum,  paper
particles, etc., ranged between 300 and 460 ppm. The suspended solids tend to stick to
the walls of pipes, flowmeter and pumps eventually leading to reduced and inconsistent
flow rates
OPERATING PARAMETERS

     The operating  parameters  which were monitored  and  controlled during  the
experimental runs are current, flow rate, pH, and type and concentration of salt. These
parameters  were  adjusted  according to the  influent  compositions with  the major
objective of obtaining  an  effective treatment  at a  minimum cost  and with  the
generation of a sludge with as little iron content as possible. A second objective was to
assess  the influence of these variables on treatment  effectiveness.   The operating
conditions of the experimental runs conducted in the program  are presented in Table 3
along with the quality of the treated effluent.

Current

     The current  has  the  most pronounced effect on  the treatment of  the oily
wastewater.  It  is also the most convenient variable to control. For a given  influent
composition and flow rate the current determines the rate  of iron dissolution (assuming
no anodic passivation) and, thereby, the ratio of iron to oil.  Throughout this program

                                      -19-

-------
TABLE 3.  SUMMARY OF OPERATING CONDITIONS AND EFFLUENT QUALITY
Influent

Freon
Flow
extractables rate
Date ppm 1/mln
12-16-76

02-01-77
02-11-77
03-08-77

03-28-77

04-04-77

06-15-77
06-21-77

06-29-77

08-09-77
10-03-77
10-04-77
10-12-77
10-13-77
1300

864
3771
4973

3110

1075

7164
2004

5178

2300
1934
1326
1850
1414
3.8

3.8
1.9
1.9

3.8

3.8

1.9
3.8

3.8

3.8
3.8
3.8
3.8
3.8
Operating conditions
Salt


concentration Current
Normality pH amp
0.01N
NaCl
ii
»
0.02N
CaCl2
0.01N
NaCl
0.01N
CaCl2
"
0.01N
NaCl
0.01N
C«C12
"
ii
ti
n
»
8.1

7.0
7.3
8.3

7.8

7.3

6.9
7.5

6.9-

7.0
7.0
6.8
7.0
9.0
35

20
35
35

35

25

35
35

25

25
30
30
30
30

Conduc-
Voltage tivity
volt ufl"1 cm"1
18

8
13
12

10

11.5

12
11

11

16
6
8
8
8
1750

2200
2200
1650

2200

1900

2100
2200

1600

2000
2800
2000
2000
2000
Freon
extrac-
tables
PPn
22

-
230
16

8

5

71
18

11

10
281
5
-
_
Effluent quality

Tr.rbidity
NTU
5

330
170
2

115

1

110
8

12

7
570
3
650
440
Dissolved
Surfactant solids
ppm ppm


-
-


20 1480

— mm

-


— _

1
-
1200
-
_
                                                                       (continued)

-------
TABLE 3.  (continued)

Influent

Freon
extractables
Date ppm
10-18-77

10-19-77
10-20-77
i 10-21-77
(X)
*•" 10-25-77

10-26-77

11-01-77
11-03-77
11-08-77
.11-10-77
11-22-77

11-23-77
12-13-77
12-15-77


3253

3058
1230
2451

848

2980

870
2472
492
700
708

313
624
591


Flow
Operating conditions
Salt



rate concentration Current Voltage
1/min Normality pH amp volt
3.8

1.9
3.8
3.8

1.9

3.8

3.8
1.9
3.8
3.8
3.8

3.8
7.6
1.9


0.01N
CaClo
it
11
.01N
NaCl
.01N
NaCl
.01N
CaCln
11 *
11
it
ii
0.01N
CaCl2
"
ii
0.02N
CaClo

6.8

6.2
6.8
6.8

6.7

7.5

9.8
9.6
10.1
9.7
9.4

9.6
9.9
11.3


35

35
30
35

35

35

20
30
30
25
20

20
30
35


14

16
16
16

14

18

12
12
14
14
12

14
13
11


Conduc-
tivity
pfl""1 cm~l
1700

1750
1430
1450

1900

1580

1450
1690
1400
1400
1500

1250
1350
3400


Freon
extrac-
tables
ppn,
_

15
16
286

35

9

61
13
13
8
11

6
190
145


Effluent quality

Dissolved
Turbidity Surfactant solids
NTU ppm ppm
390

9
9
440

40

8

110
14
2
2
1

1
90
140


_ -

1180
1610
_ _

1000

1260

930
980
990
880
1070

1220
1080
90 2020

(continued)

-------
                                                         TABLE 3.   (continued)
I
Is)

Influent


Freon
extractables
Date ppm
12-19-77
12-20-77
01-09-78
01-10-78
01-11-78
01-12-78
01-13-78
01-16-78
01-17-78
01-18-78
01-19-78
01-20-78
01-26-78
01-30-78
375
664
736
2369
1045
1450
704
825
557
586
1205
3328
3230
622

Flow
rate
1/min
3.8
3.8
3.8
3.8
3.8
3.8
1.9
3.8
3.8
3.8
3.8
3.8
3.8
Operating conditions




Salt
concentration Current Voltage
Normality pH amp volt
0.01N
CaCl2
,'•
ti
ii
ii
it
ii
0.005N
CaCl2
0.01N
CaCl2
ii
0.01N
CaCl2
10.1
9.7
9.3
9.6
9.8
9.6
9.3
9.8
9.9
9.6
9.4
Pump Failure
9.0
8.7
30
25
25
35
35
30
12
20
10
10
20
30
15
14
14
13
14
14
12
13
9
6
5
9
17
6

Conduc-
tivity
1300
1220
1400
1700
1850
1600
1650
1650
1400
1780
1500
1350
1400
Freon
extrac-
tables
ppn
7
7
14
122
31
8
14
12
32
9
27
-
10
Effluent quality

Dissolved
Turbidity Surfactant solids
NTU ppm ppm
1 20 920
6 12 780
4 — —
215
4 - -
10
3
4
13
4
8 - -
110 -
5
                                                                                                              (continued)

-------
Influent

Freon
extractables
Date ppm
01-31-78

02-01-78
02-02-78
02-14-78
M 02-15-78
i
02-16-78
02-20-78

02-21-78

02-22-78
02-23-78
02-24-78

02-25-78
02-26-78

02-27-78
2300

1600
1250
745
1004

2544
1725

1708

1331
5308
4984

3154
2050

1260
Flow
rate
1/min
3.8

3.8
3.8
3.8
3.8

3.8
3.8

3.8

3.8
1.9
1.9



3.8

3.8
Operating conditions
Salt

concentration
Normality pH
0.01N
CaCl2
"
ii
"
»

ii
0.01N
Nad
0.01N
CaCl2
"
ii
0 . 02N
CaCl2


0.01N
CaCl2
It
8.4

8.6
9.2
8.2
8.1

8.2
9.3

9.3

9.1
8.0
7.2

*Pn*im

6.7

8.0

Current
amp
30

30
25
20
30

35
35

35

35
30
30


r allure — —
25

25

Conduc-
Voltage tivity
volt ufl'1 cm~l
16

12
15
9
13.5

17
J.1

12

12
9
11



19

22
2000

1400
1400
1450
1200

1300
1850

1950

1900
1600
2500



1720

1550
Effluent quality
Freon
extrac-
Dissolved
tables Turbidity Surfactant solids
ppm NTU ppm ppn
10

18
8
4
8

15
_

36

37
20
5



7

8
7 1

5
5
4
3

3
140

150

90
13
8

___«._M__Pttmn 1?d~f 1 tit*
__.«._«»«j-mjj^ ^ OAJUJH.
5

8
_

-
-
-
-

850
_

-

1810
-
1760



-

-
(continued)

-------
                                                          TABLE 3.  (continued)
 i
N)
Influent
Freon Flow
extractables rate
Date ppm 1/min
02-28-78
03-01-78
03-02-78
03-03-78
03-09-78
03-10-78
03-13-78
03-14-78
03-15-78
03-16-78
03-17-78
03-20-78
03-21-78
04-06-78
1117
1071
2538
1270
935
1296
1956
1444
3315
1342
1200
900
970
826
3.8
3.8
3.8
3.8
3.8
1.9
3.8
3.8
3.8
1.9
3.8
3.8
3.8
Operating conditions
Salt
concentration Current Voltage
Normality pH amp volt
0.01N 8.6
CaCl?
" 8.5
8.1
8.2
" 7.8
8.0
8.5
8.5
11 8.0
" 8.2
—————Pump Failure — —
0.01N 8.2
CaCl2
8.0
" 9.2
25
25
25
35
15
12.5
20
10
25
10
20
20
20
25
39
27
27
7
6
8
5
10
5
12
13
10
Conduc-
tivity
ufl""l c«~l
1800
1470
1800
1670
1560
1680
1520
1760
1850
1650
1650
1400
1650
Freon
extrac-
tables
ppm
11
4
10
17
10
15
7
14
15
8
18
-
12
Effluent quality
Dissolved
Turbidity Surfactant solids
NTU ppm ppm
4
2
7
12
4
43
6
5
37
5 _
12
60
7
1520
1860
1420
1640
-
910
1290
1390
1250
890
.
-
-
                                                                                                              (continued)

-------
                                                            TABLE 3.  (continued)
i
N>
Influent Operating conditions
Freon Flow Salt
extractables rate concentration Current
Date ppm 1/min Normality pH amp
04-11-78
04-12-78
05-02-78
05-03-78
05-04-78
05-05-78
05-11-78
05-12-78
05-23-78
05-24-78
05-25-78
X total
X CaCl2
1305 3.8 0.01N
CaCl2
1102 3.8 "
968 3.8 "
1526 3.8 "
1217 3.8 "
2230 3.8 "
1186 3,8 "
Batch of
05-11-78 3.8 "
1361 3.8 "
3218 3.8 "
3842 3.8 "

8.8
8.5
8.4
8.3
8.4
8.5
9.0
9.0
8.7
8.7
9.1

20
20
20
20
35
35
35
35
70
35
35

Freon
Conduc- extrac-
Voltage tiyity tables
volt yfl~* co~l ppm
11 1450
11 1400 13
13 1350 17
13 - 104
19 1450 22
17 - 32
20 1500
22 - 12
20 - 69
11 1600 25
12 1500 28
35
27
Effluent quality
Turbidity
NTU
9
68
30
340
120
120
6
14
65
8
30
70
60
Dissolved
Surfactant solids
ppm ppm
890
-
-
-
-
-
-
-
-
1257

-------
current adjustment was primarily relied upon to obtain effective treatment.  Only with
difficult-to-treat batches, where maximum  operating current was not sufficient at the
usual flow  rate  of 3.8 1/min, were other parameters such  as flow  rate or salt
concentration adjusted. Maximum operating current is limited by the onset of excessive
oxygen evolution at the^inode at the expense of iron dissolution.  This occurs at current
density  of  10 mA/cm  _  of projected electrode which for the exposed  electrode
dimensions used (3820 cm ) corresponds to 38 A.

     In this program the current ranged between 10 and 35 A. The current used in each
case was the  minimum required  to break the emulsion  as  determined  by  visual
observation  of the change in  turbidity. Usually the flow rate was at the design value of
3.8 1/min, however, in several cases  the flow rate was reduced to  1.9 1/min resulting in
an equivalent current of twice that for standard conditions.

     The average current required for effective treatment  was 31.5 A (adjusted to 3.8
1/min) with standard deviation of 15.6 A.  Generally, the required current was found to
increase with the influent  oil concentration.  But  as mentioned previously the proper
setting of the current for effective treatment was determined by a beaker test.

     The beaker test  was found  to be  useful because  our  experience at the Livonia
Transmission Plant has shown that knowledge of the concentration of oil and surfactants
in the wastewater may not always be sufficient to  establish the proper operating
conditions, since other  unidentified components in the plant  wastewater may effect the
performance of the electrolytic  cell.  Therefore, simple correlations, which  would
predict  the  setting of the  operating parameters with certainty  based on  influent
properties, could not  be established.  While this situation may be true at the Livonia
Transmission Plant where wastewater is received from  a large number of diversified
operations,  it is  likely that  in other plants, where  the composition of  wastewaters
remains fairly  constant, simple correlations could be established.    In  any event, a
feedback control  based on effluent quality may be feasible.  This is discussed  in a later
section.

Operating Voltage

     The voltage  across the  electrode was  found to  depend  on  the current, the
conductivity of the wastewater, and the  extent  of anodic fouling.  Generally, the
voltage varied  between 5 and 30  volts and averaged 13  volts.  In some  instances the
operating voltage increased to 4-0 volts or more due primarily to anode fouling. In these
cases the tests were stopped  and corrective measures were taken to reduce the voltage
to  normal levels.  A  detailed discussion of  voltage increase  is   presented later in
conjunction  with the durability studies.

     Based  on the data  of  current and voltage,  the  average  electrical  energy
consumption fpr the electrolytic dissolution of  iron was calculated to be 5.76 M3/m
(1.6 kW-hr/m ; 6  kW-hr/1000 gal) of wastewater  for the range  of oil concentrations
encountered.  The calculation was based on  the use of 0.01N CaCl and flow rate of  3.8
1/min.

pH Effects

     To study the influence  of pH on the performance of the electrolytic cell two sets
of experiments were conducted.  One set of experiments was conducted to determine

                                      -26-

-------
the  influence  of pH on  the rate  of iron dissolution, the  other  to compare  the
performance of the electrolytic cell with and without pH adjustment of the influent.

      To study the effect of pH on the  rate of  electrolytic dissolution of iron the cell
was  filled with clean tap water and the pH  adjusted to a desired value.  The electric
power was turned on at a specified current and  the water  recirculated in the cell. The
concentration of iron in the water was determined hourly over a period of 5 hours. The
data  were used  to  calculate  the rate of  iron dissolution in ppm/hr.  The  results
presented in Table *, show that pH does not affect the rate of electrolytic dissolution of
iron.  It should be noted that  this is  true only as long as the cell  operates  below  the
limiting current density.


                  TABLE    4.     IRON   DISSOLUTION  RATE
                                             Iron dissolution rate
                     pH                             ppm/hr

6
10
25 amp
15
15
35 amp
21
19

      To evaluate the influence of pH on the performance of the electrolytic cell, large
batches of wastewater  were collected in the storage tank.  Each batch was treated in
the electrolytic cell with and without pH adjustment, while maintaining other operating
parameters constant. A direct comparison of the Freon extractables is shown in Table 5
along with detailed operating conditions. These runs indicate that pH adjustment may
not  be necessary for   effective treatment  of  the plant wastewater.    Subsequent
experimental runs have, in fact, shown that the electrolytic cell performs well without
adjusting the pH of the  influent, which simplifies and reduces the cost  of the process.

Salt Effects

      The main purpose of salt addition is to avoid passivation of the iron chips  and
increase the conductivity of the wastewater, thereby reducing power consumption.  In
addition,  the   type  and  concentration of salt  influences the effectiveness of  the
electrolytic treatment.  It is known, for example,  that bi-  and  tri- valent salts, because
of their high  ionic strengths,  are much more active in destabilizing and  breaking
emulsions  than mono-valent salts  (8).  An increase  in concentration  also affects
emulsion breaking.

      In this program two  salts  were evaluated:  sodium chloride and calcium  chloride.
Sodium chloride  is preferable economically,  however,  calcium chloride is preferable
with respect  to treatment  effectiveness.  This feature is particularly noticeable with
batches of wastewater which are difficult to treat electrolytically.

      Most of  the runs  listed in Table  3 were done with CaCl-.  In a few  cases, NaCl
permitted fairly adequate treatment.  In cases where it did  not, the full  run  was not
made with NaCl,  but with CaCl-.


                                       -27-

-------
Freon Arilgnle surfactant
extractables Salt
before concentration % of
treatment Freon
PPm N ppm extractables pH
2980 CaCl2, 0.01 N 247 8.3 7.5
10
870 CaCl2, 0.01 N 121 13.9 7.1
10
i
iv» 	 	 • 	
00
' 2472 CaCl2, 0.01 N 285 11.5 Z.I
9.6
492 CaCl2, 0.01 N 108 22.0 10
700 CaCl2, 0.01 N 206 29.4 7.2
9.7
664 CaCl2, 0.01 N 90 13.5 10.3
7.0


Flow
rate
1/mln
3.8
3.8
3.8
3.8
1.9
1.9
3.8
3.8
3.8
3.8
3.8


Current
amp
35
35
35
20
30
30
30
25
25
25
25


Voltage
volt
18
20
21
12
15
12
14
19
14
14
13


Turbidity
NTU
8
5
135
110
10
14
4
11
6
6
3


Freon
extractables
ppm
9
18
210
61
13
13
14
10
8
7
9

-------
     Electrolytic treament of plant wastewater in a 1-liter  beaker has also shown the
superiority of CaCl2.  For example, a batch of 2-21-78 could not be broken after 18.5
minutes  at  0.5  A  using  0.01N  NaCl but with 0.01N CaCl2 an effective treatment
resulted within 16 min.  In another beaker study (2-23-78) it took W minutes  at 0.5 A to
break the emulsion using 0.01N NaCl, but with 0.0IN CaCl2 it took only 24 minutes.

     Laboratory tests have shown that CaCU, FeS
-------

|l50
CO
Ul
ffi
?
o
g; 100
X
UJ
1
U.
K- 5O
UJ
ID
•
_J
U.
U.
Ul
n
A
—


INFLUENT OIL CONCENTRATION
_ O 	 700 ppm
A A 	 4770 ppm


o
A 0
A 0
A ° 0
1 1 I
                  0.05          0.1           0.15
                  DISSOLVED  IRON/ INFLUENT OIL
0.2
Figure 7.  Effect of iron to oil weight ration on  effluent oil content
                             -30-

-------
transmission  fluid additives may tend to enhance the emulsion stability or selectively
adhere to or react with the iron rendering it less active.

     The presence of small amounts of bacteria does not significantly influence the
operation of the electrolytic cell; however, if the wastewater is allowed to stand, it will
turn rancid with the formation of hydrogen sulfide and the generation of a biological
growth.  This resulting wastewater is more difficult  to treat than the original  since
hydrogen sulfide presumably precipitates some of the iron as iron sulfide.  Also, the
Freon extractable value may be in error as to the  concentration  of  oil  because the
Freon-water  interface is virtually non-existant.

Turbidity

     The turbidity of the electrolytically treated and sand filtered wastewater ranged
between 1 and 650 NTU and averaged 60 NTU  (excluding  NaCl runs and the 7.6  1/min
run).  The turbidity results  from remaining emulsified oil  and fine suspended particles
(mostly iron  hydroxide).  The turbidity  was found to have a positive correlation with
Freon extractables with a correlation coefficient of 0.88.  As will be discussed later on
this feature may be used for automatic feed back control.

Surfactants

     The concentration of  anionic surfactants in the treated water ranged between  1
and 90 ppm.  When the treatment was effective the concentration of surfactants was 20
ppm or  less.  Higher concentrations, accompanied by foaming in the cell, were observed
when the treatment  was only partially effective.

BOD

     A few tests of biological oxygen demand (BOD) indicated that 5 day BOD value of
the treated wastewater is about 90 ppm.

Dissolved Solids

     The effluent dissolved solids varied between 780 and 2020 ppm.  The average was
1257 ppm with standard deviation of 346. The  process adds a maximum of 550 ppm to
what is present in the influent.  By comparison, conventional methods with chemicals
generally add about  2,000-3,000 ppm of dissolved solids.

Suspended Solids

     Prior to the use of the dissolved  air flotation unit  or  sand filter the suspended
solids, comprised  mainly of iron hydroxide, ranged between 600 and 2240 ppm.  It was
observed that the concentration of suspended solids depends on the floating ability of
the iron hydroxide-air sludge.  In  most cases the oily sludge,  generated when treating
actual plant wastewater, did not float well without forced flotation.

     When the dissolved air flotation unit was  used to force flotation of the sludge the
concentration of suspended solids in the processed wastewater ranged between 25 and
135 ppm.  Sand filtered wastwater had a negligible amount  of suspended solids.  This
will be discussed in more detail later in the report.
                                       -31-

-------
DURABILITY STUDIES

      The objectives of the durability studies were to evaluate the performance of the
cell under uninterrupted-continuous operation, to identify any operational problems, and
to alleviate any potential problem areas.

      The durability tests  were conducted as follows:   About 5.6 m  (1500 gal) of
wastewater were pumped into the storage tank  and analyzed for pH, conductivity,
turbidity, Freon extractables, and  anionic surfactants.  In addition, a  1 liter sample of
the wastewater was treated  electrolytically  at an iron  chip  anode in a  beaker to
determine the initial setting of the operating conditions.  The procedure for the beaker
test is described in the Experimental section.

      During  the  durability   test  the  treated  wastewater  was analyzed for  pH,
conductivity,  turbidity, and  Freon extractables,  and the  operating  conditions  were
adjusted for minimum  iron and minimum sludge formation. Minor maintenance work,
which did not  disrupt the test, such as the addition of iron  chips and brushing between
the electrodes, was also performed. 3V hen the supply of wastewater in the storage tank
was low, a new batch of about 5.6 m  was pumped to the storage tank. In this manner,
the electrolytic cell operated 24 hours a day without interruption.

      During the program period five durability tests have  been conducted.  Each test
started with new iron chips and clean electrodes. The results of the five durability tests
are presented in Tables 6 thru 10.  These results show that, when the electrodes are
kept clean, the electrolytic cell provides efficient treatment.  Also encouraging is the
fact that the rise in the operating voltage is not as rapid as was  experienced in the first
part of the program with interrupted runs.

      The major operational problem  is  the accumulation of oily  sludge in the anodic
chip cage and in the space between the anode and cathode which  restricts the flow of
wastewater through the electrodes.   Eventually,  the  electrodes  become  completely
blocked, the influent  flows  over  the  iron chips, and the performance  of the  cell
decreases substantially.

      It was found that brushing and purging with air between the electrodes to remove
the accumulated sludge alleviates this problem  temporarily.  To date we were able to
operate the cell continuously up to 14 days.

First  Durability Test

      The first durability  test is summarized  in Table  6.   The  test lasted 11 days and
used about 60 m   (16,000 gal) of wastewater.  Throughout the  test the space between
the electrodes  was  brushed  several  times  a day to  reduce  the  rate  of  sludge
accumulation.   After 11  days  the  test  was  discontinued  because  of  excessive
accumulation of sludge which  blocked the flow of wastewater through the anode.

Second Durability Test

      The test, summarized in Table 7, continued for 8 days and consumed about 27 m
(7200 gal) of wastewater.  As  in the first test frequent brushing between the electrodes
was necessary to avoid rapid sludge  accumulation in the electrodes, and the test was
stopped for similar reasons.

                                       -32-

-------
                                                  TABLE 6,  SUMMARY OP FIRST DURABILITY TEST
V
Influent CaCl_
oil con- concen-
centration tration
Date
1-09-78
1-10-78





1-11-78








1-12-78




1-13-78

Time ppm
1
8


10

2
8



10


2

8

9

3
10
2
:00pm 736
: 00am "


:00am 2369

: 30pm "
: 00am "



:00am 1045


:40pm

: 00am "

:00am 1450

: 00pm "
:00am
:00pm 704
0
0


0

0
0



0


0

0

0

0
0
0
N
.01
.01


.01

.01
.01



.01


.01

.01

.01

.01
.01
.01
Flow
rate
pH 1/min
9.
9.


9.

9.
9.



9.


9.

9.

9.

9.
9.
9.
9
6


6

6
8



8


8

8

6

6
6
3
3
3


3

3
3



3


3

3

3

3
3
1
.8
.8


.8

.8
.8



.8


.8

.8

.8

.8
.8
.9
Current
amp
25
25


35

35
35



35


35

35

30

30
30
12
Freon
extract-
Voltage Turbidity ables
volt NTU
25
14 4


14.5

13 10
14 215



14


14 16

14 5

12

13 8
12 10
13 3
ppm Comments
Beginning of test.
14 Water level 1.3 cm higher upstream
of electrodes. No sludge
floating.
- Operating conditions adjusted for
new batch.
-
122 Water level 1.9 cm higher upstream of
electrodes and overflowing chips.
% cell covered with floating
sludge.
New batch of wastewater. Space
between electrodes cleaned with
brush to stop flow over chips.
Water level equal on both sides
of electrodes.
31 Water level 2.2 cm higher upstream
Electrodes cleaned with brush.
- Operating conditions adjusted for
new batch.
7
8
Operating conditions adjusted for
                                                                                                     running unit unattended through
                                                                                                     the weekend.
                                                                                                                   (continued)

-------
                                                             TABLE 6.   (continued)
I
f
Influent
oil con-
CaCl2
c oncen-
centration tratlon
Date
1-16-78






1-17-78

1-18-78


1-19-78

Time
8: 00am



10: 30am
3: 00pm
3: 20pm
8: 00am
3: 00pm
8: 30am

3: 00pm
8: 30am
3: 00pm
ppm
704



825
it
it
11
557
it

586
M
1205

0



0
0
0
0
0
0

0
0
0
_N 	
.01



.01
.01
.01
.01
.005
.005

.01
.01
.01
£tL
9.3



9.8
9.8
9.8
9.8
9.9
9.9

9.6
9.6
9.4
Flow

rate Current
1/mln
1.9



3.8
3.8
3.8
0.8
3.8
3.8

3.8
3.8
3.8
amp
12



20
20
15
15
10
10

10
10
20

Voltage
volt
13



10
9
6.5
8
6
5

5
5
9

Turbidity
NTU
9



-
4
4
-
13
33

•38
4
8
Freon
extract-
ables
ppm
14



-
12
—
_
32
38

28
9
27


Comments
Water level 3.2 cm higher upstream
Brushed between electrodes.
Washed chips and added some
fresh chips
Conditions adjusted for new batch.
iQ
Reduced current due to excess FeTJ.
Pump slowed up during night.

Water level 1.9 cm higher upstream
White foam on water surface.
No floating sludge.

Electrodes were brushed.

         1-20-78   l:00pm    3328
0.01    9.9   1.9
                                                              15
Operating conditions adjusted for
  unattended run through weekend.
         1-23-78   Pump failed during weekend.  Test stopped.

-------
TABLE 7.  SUMMARY OF SECOND DURABILITY TEST

Influent
oil con-
CaCl2
concen-

centration tration
Date
1-26-78

1-27-78


1-30-78



1-31-78


2-01-78



2-02-78



2-03-78



Time
10: 00am
2 i 00pm
9: 00am
2: 30pm

8: 00am


3: 00pm
9:00»m

4 : 00pm
8: 20am


3: 30pm
8: 30am


3 : 30pm
8: 30am

1 : 00pm
2: 00pm
ppm
3230
It
II
ft

It


622
II

2300
ft


1600
ii


1250
ti

H
N
0.01
0.01
0.01
0.01




0.01
0.01

0.01
0.01


0.01
0.01


0 -01
0 .01

0 .01
Experiment stopped
£H_
9.0
9.0
9.0
9.0




8.7
8.7

8.4
8.4


8.6
8.6


9.2
9.2

9.2
to
Flow



rate Current Voltage Turbidity
1/min
3.8
3.8
3.8
1.9




3.8
3.8

3.8
3.8


3.8
3.8


3.8
3.8

3.8
improve
amp
30
30
30
15




15
15

30
30


30
30


25
25

25
electrodes
volt
10
10
17
6




6
6

13
17


12
12


16
18

15
design.
NTU
_
12
110
90




18
5

10
7


4
5


60
180

5

Freon
axtract-
ables
ppm Comments
Beginning of test.
Floating sludge over 80% of cell.
Electrodes cleaned with brush.
Operating conditions adjusted for
run through weekend.
Flow of wastewater to cell stopped
during the weekend because of
pump instability.
Test continued with a new batch.
10 Water level higher upstream of
anode. Electrodes brushed.
8
10 Water level higher upstream.
Brushed electrodes. Added some
iron chips
30 Electrodes brushed every 3 hours.
18 Water level 1.9 cm higher upstream of
electrode. Brushed between
electrodes.
- Electrodes brushed hourly.
Wastewater flows over iron chips.
Brushed between electrodes.
8 Electrodes brushed hourly.


-------
TABLE 8.  SUMMARY OF THIRD DURABILITY TEST
Influent
oil con-
CaCl2
concen-
centration tration
Date
2-14-78

2-15-78

2-16-78


2-17-78
Time
10: 15am
3 : 00pm
8: 30am
11: 30am
8: 00am
10: 30am
3: 00pm
8: 00am
ppm
745
ii
»
1004
it
2544
it
ii

0
0
0
0
0
0
0
0
N
.01
.01
.01
.01
.01
.01
.01
.01
pH
8.0
8.2
8.5
8.1
8.1
8.4
8.2
8.2
Flow

rate Current
1/min
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8
amp
15
20
20
25
30
25
35
35

Voltage
volt
8
9
11
14
14
11.5
17
17

Freon
extract-

Turbidity ables
NTU
_
4
3
—
3
-
3
3
Ppm
_
4
5
"•
8
-
14
15.4
Comments
Beginning of test.


A new batch

A new batch

Test stopped because of excessive
                                                   deposits on cathode.

-------
TABLE 9.  SUMMARY OF FOURTH DURABILITY TEST
Influent
oil con-
CaCl2
concen-

centration tration
Date
2-23-78

2-24-78

2-25-78

2-26-78

2-27-78



2-28-78


3-01-78


3-02-78




Time
l:00pm
3: 15pm
8: 15am
11 : 30am
9 : 30am
11 : 30am
8: 00am
2: 00pm
8: 00am

12 : 30pm
3 : 30pm
10: 30am
12 : 30pm
3: 30pm
8: 30am
1 : 00pm
3: 30pm
10: 00am


l:20pm
3: 15pm
ppm
5388
11
ii
4984
If
3154
ti
2050
„

1260
II
II
1117
11
1117
1071
11
„


2538
tl
N
0.01
0.01
0.001
0.02
0-02
0.02
_
0.01
0.01

0-01
0.01
0.01
0.01
0.01
0.01
0.01
0.01
o.oi


0.01
0.01
pH
8.3
8.0
8.2
8.0
7.2
8.0
^
7.5
6.7

8.1
6.7
6.4
8.6
8.6
8.6
8.5
8.6
6.8


7.8
8.1
Flow
Freon
extract-
rate Current
1/min
1.9
1.9
1.9
1.9
1.9
1.9
_
3.8
3.8

3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8


3.8
3.8
amp
35
30
30
30
30
30
«.
25
25

20
25
25
25
25
25
25
25
16


25
25
Voltage
volt
11
9
17
20
11
12
mm
12
19

14
18
22
23
25
25
30
39
44


17
17
Turbidity
NTU
_
13
560
—
8
-
1
—
5

-
13
8
14
5
4
-
2
7


10
2
ables
ppm
_
20
-
—
5
—
-
•~
7

-
16
8
-
13
11
-
4
13


-
5

Comments
Beginning of test.

CaCl2 flow rate decreased overnight
A new batch
Electrodes brushed
New batch
Flow rate slowed to 0.4 1/min
A new batch
Electrodes purged with air and
brushed.
New batch

Electrodes purged with air
New batch

Electrodes purged with air
New batch
Electrodes purged with air
Overvoltage. Electrodes brushed and
purged with air. Iron chips worked
Kith tap water. Added more chips.
New batch
(continued)

-------
OO
 1
         3-04-78
                                                             TABLE  9.   (continued)




Date Tiflw^
3-03-78 8: 15am
l:00om
3
:15pm
Influent
oil con-
centration
ppm
2538
1270
ii
Ca
Cl->


concen-
tration
N
0
0
0
.01
.01
.01
pH
7.0
8.2
8
.0

Flow
rate
JL/JBin
3.8
3.8
3.8



Freon
extract
Current
amp
25
25
35
Voltage
volt
27
27
27
Turbidity
NTU
7
7
12
ables
ppm Comments
10.3 Electrodes purged with air
New batch
17
                    9:00am
0.01
8.0   3.8
                                                              22
                                                                       44
Water overflowing electrodes.
Overvoltage.  Test stopped.

-------
                                          TABLE  10.   SUMMARY  OF FIFTH DURABILITY TEST
Influent
oil con-
CaCl2
c oncen-

centration tration
Date
3-09-78

3-10-78

3-11-78
3-12-78
3-13-78


3-14-78


3-15-78

3-16-78


3-17-78

Time
l:00pm
3: 30pm
11: 00am
3: 15pm
9: 00am
10 : 30am
8 : 20am
12: 50pm
3 : 00pm
8: 00am
12: 20pm
3: 00pm
11: 00am
1 : 40pm
8: 00am

2 : 30pm
10: 00am
3: 45pm
ppm
935
ii
ii
1296
II
II
II
1956
"
M
1444
II
It
3315
11

1342
II
1200
N
0.01
0.01
0.01
0.01
0.01
0.01
0.01
0.01
0.01
0.01
0.01
0.01
0.01
o.oi
0.01

0.01
_
0.01
£«
7.8
7.8
7.0
8.4
8.0
7.2
6.9
8.7
8.5
7.7
8.5
8.2
7.3
8.3
8.0

8.2
8.2
8.5
Flow
rate
1/min
3.8
3.8
3.8
1.9
1.9
1.9
1.9
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8

1.9
—
1.9

Current
amp
20
15
15
7.5
8
12.5
15
20
20
20
10
10
10
20
25

10
10
10

Voltage
volt
10
6
7
4
3.5
6
6
7
8
7
4
4.5
4.5
9.5
9.5

5.5
5.5
4

Freon
extract-

Turbidity ables
NTU
_
1
4
12
27
43
14
18
8
6
15
5
6
6
37

28
5
-
ppm

-
9.5
-
29
15
10.3
-
3.4
7
-
14
8.6
—
15

—
8
-
Comments
Beginning of test.

Electrodes purged with air.
New batch.
Electrodes purged with air.

Electrodes purged with air.
New batch.

Electrodes purged with air.
New batch.

Electrodes purged with air.
New batch.
Wastewater supply pump failed.
Cell shut down temporarily.
New batch.
Flow rate slowed to 0.8 1/min over
New batch. Cell set to run ni*i&£
3-20-78
9:00am
                            8.2
                                                      10
unattended during weekend

Pumps failed.  No flow to cell.
Electrodes brushed and purged with
air.

    (continued)

-------
TABLE 10.  (continued)

3-20-78
3-21-78

3-22-78
3-23-78
Influent
oil con-
centration
Time ppm
3: 00pm 900*
8: 30am "
2: 00pm "
4: 00pm 970
8: 30am "
3: 00pm 2050
8: 30am "
CaCl2
concen-
tration
N
0.01
-
0.01
0.01
0.01
0.01
0.01
pH
8.2
8.1
8.2
8.0
6.4
8.6
8.4
Flow
rate Current
1 /ruin amp
3.8
-
3.8
3.8
3.8
3.8
3.8
20
20
20
20
20
35
35
Freon
extract-
Voltage Turbidity ables
volt NTU ppm
13
11
12
12.5
13
23
32
-
1
12
3
60
90
2
-
5
18
9
-
5
New batch.
Flow rate
overnight.
Electrodes
New batch.
Electrodes
New batch.
Flow rate
Comments

slowed to 1.9
purged with
purged with
slowed to 2.3


1/min
air.
air.
1/min
                                                  .
                                         Test  stopped — long weekend.

-------
     The first two durability tests demonstrated that the accumulation of oily sludge in
the anodic chip cage  and in the space between  the  two electrodes  can  be a major
operational problem.  To reduce the rate of sludge accumulation in the space between
the anode and cathode, the electrodes were redesigned. The cathode, which in the past
extended above the water level, was shortened to about one centimeter below the water
level to allow the oily sludge to float over it. In addition, pressurized air is bubbled in
the space between the electrodes  to provide turbulence  and washing action,  thereby
minimizing the accumulation of sludge.

Third Durability Test

     The test started with the new electrode design.  To avoid accumulation of oily
sludge  air was bubbled continuously between the electrodes. The test was stopped after
three days because of severe build up  of  insoluble calcium  carbonate deposits on the
cathode.  Apparently, the continuous bubbling of air between the electrodes  and the
relatively high concentration  of calcium  ion resulted in a rapid build-up of CaCO-j
deposits.  Results are given in Table 8.

Fourth Durability Test

     To avoid the deposits of  CaCO,, it was decided to replace the CaCU partially or
completely with NaCl.  This action, however, resulted in less  effective  treatment and it
was necessary to return to CaCl. at a concentration of 0.01N.

     The fourth durability test (Table 9) continued for nine  days and used  about 38 m
(10,000 gal)  of  wastewater.  During the  test the space between the electrodes  was
purged with  air twice a  day for 5 minutes and sometimes brushed.   Accumulation of
sludge  between the electrodes was  not  observed.  Also the CaCO, deposits on the
cathode were light and did not interfere with the operation of the cell. Oily sludge did
accumulate in the anodic cage leading, eventually, to elevated voltage  and  physical
plugging of flow.  In-situ washing of the iron chips with cold tap water for 10 minutes
alleviated this condition temporarily.

Fifth Durability Test

      The fifth  durability test (Table 10)  lasted  14 days and used about 57 m  (15,000
gal) of wastewater.  During the test the space between the electrodes was purged with
air twice a day and occasionally brushed.  In addition the water upstream  of the anode
was continuously and vigorously agitated to maintain the influent well mixed and avoid
separation of free oil droplets.  This  action appears to have also slowed the rate of
plugging of  the anode.   Except  for  some pump failures the cell performed  well
throughout the test.


 ELECTRODE PLUGGING

      An increase in the operating voltage upon  aging of the iron chips,  was  observed
 early  in the program.  During that time the  cell  was operating approximately 8  hours
 through the day and shut down for the  night.  After several days  of operation  the
 voltage usually exceeded the limit of the power supply,  the chips had to  be replaced,
 and the electrodes were steam cleaned.

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      An increase in the operating voltage was also observed during the durability tests,
 but at a slower  rate.  To determine what contributes to the rise in the voltage,  the
 following experiments were conducted at the end of the fourth durability test when  the
 operating voltage had increased to 44 volts.

      In the first  experiment  the iron chips were replaced with new ones. The cell  was
 filled  with wastewater and the conductivity  was adjusted to 1700  y mho/cm, as at
 the end of the fourth  durability  test.  When  the power was  turned on to 25 A  the
 operating voltage was 25 volts.  Thus replacing the iron chips reduced the operating
 voltage by 19 volts.  In the next experiment the cathode was cleaned to remove oily  and
 calcium deposits. This action had no effect on the operating voltage.  Next, the anodic
 cage was cleaned with steam to remove oily deposits from the front face of the anode.
 This action brought the operating voltage down to 14 volts.

     Thus, it appears,  that the increase in the operating voltage is due primarily to
 accumulation of oily sludge in the anode cage.

     As mentioned  in the  Experimental section, the front face  of the anode is
 constructed of two layers:  expanded titanium sheet and polyethylene screen. This type
 of construction appears  to trap and accumulate oily sludge.  By replacing the two-layer
 construction with a single titanium sheet with  proper hole size, it may be  possible to
 reduce the rate of sludge accumulation and extend  the service life of the anode.


 SLUDGE FLOTATION AND SLUDGE CHARACTERISTICS

     The  sludge  generated by the electrolytic process is a mixture of water,  oil,  and
 iron hydroxide.   Sludge flotation  appears to depend on the ratio' of  iron  to  oil,  the
 wastewater composition, and the type of assisted flotation equipment.  During most of
 the program period,  sludge flotation was effected by the use of  porous membrane air
 bubblers which were located at the bottom of the cell. These bubblers were  found to be
 somewhat deficient.  Flotation requires the generation of fine air bubbles which adhere
 to the oily floe.  If the bubbles are too large mixing instead of flotation may occur. In
 these experiments, the membrane properties  changed with  time and the bubble size
 changed from fine to larger bubbles.  It should  be  noted  that in laboratory experiments
 with simulated wastewater no  difficulties were encountered in forcing the sludge to
 float with similar  flotation equipment, and  at  about the  same  iron  to oil ratio.
 Therefore, it seems  that some components of the plant  wastewater render the sludge
 more difficult to  flocculate and to float.  Indeed, the wastewater processed occasionally
contained organic solvents, drawing compounds, grinding wheel resins, etc.  Therefore,
air bubbler flotation may be more effective with other wastewaters  which may have
simpler compositions.

     In order to  obtain a more effective sludge flotation, a dissolved air flotation  unit
 (Komline-Sanderson  model HR/SR-1)  was  installed.    The  treated  wastewater  was
pumped at a rate of 3.8 1/min to the dissolved air flotation unit (D.A.F.) yielding a
thick, easy to handle, floating sludge.

     The  performance of the D.A.F. is presented in Table 11. The unit removed from
 86 to 98%  of the  suspended solids, and reduced iron concentration by as much as 97%.
 The average removal of suspended  solids was 93%.  Thus it  appears that the sludge
 generated  by the electrolytic  process can  be  forced to float and  that dissolved  air

                                      -42-

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       TABLE  11,  EVALUATION OF THE PERFORMANCE OF THE DISSOLVED AIR FLOTATION


Date
5-02-78


5-03-78


5-04-78


5-05-78


5-11-78


5-12-78


5-23-78


5-24-78


5-25-78



Sampling
location*
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3

Turbidity
NTU
800
150
30
1200
355
340
650
150
120
1200
260
120
690
57
6
2400
50
14
850
120
65
760
70
8
700
80
30
Freon
extrac tables
ppm

85
17
_
202
104
_
77
22
_
97
32
_
74
-
_
31
12
_
113
69
_
89
25
_-." :
56
28
Suspended
solids
ppm
679
80
nil
1595
135
'
840
57
•
1122
84
-
1643
25
-
2240
40
-
680
33
-
949
131
-
779
57
—
Iron
concentration
ppm
110
22
nil
110
21
'
95
8.5
-
140
22
-
105
7
-
250
7.5
-
100
5
• -
105
6.5
-
65
3
-

1 - Before dissolved air flotation.
2 - After  dissolved air flotation,
3 - After sand filtration
                                       -43-

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 flotation is very effective for that purpose.  If final polishing of the effluent through a
 sand filter is required to remove the last  traces of suspended solids, the use of D.A.F.
 would substantially reduce the loading on the  filter.  In addition, the  D.A.F. would
 occupy far less floor space than an air bubbler flotation system.

      The  sludge collected by the D.A.F. unit was analyzed to determine oil and water
 content.  The sludge as  received from the D.A.F. contained 6 to 12%  oil,  86% water,
 and the balance insoluble solids. The total volume of generated sludge averages about 1
 to 2% of the volume of wastewater treated. This volume is immediately decreased by a
 factor of  two since about one-half of the water  drains from the sludge within  30
 minutes upon standing. If the sludge is permitted to stand overnight, then agitated, the
 water is not  as readily drained from the sludge.  This presumably is a result of entrained
 air being lost from the  oil-iron floe and hydration of the iron hydroxide.  Thus, the
 sludge should be removed and drained within a relatively short time frame.

      A few  exploratory experiments have  been  carried out to upgrade  the sludge
 quality and to recover the oil.  For example, by  adjusting the pH of the sludge to about
 one with HC1, phase separation takes place.  Separation by centrifuging was found  to
 yield an oily sludge phase of about 60% oil. Additional work is  necessary in  this area  to
 determine the best technique for oil recovery.


 AN APPROACH TO AUTOMATIC CONTROL

      To develop any type of automated system, it first is  necessary  to establish the
 parameters to be  monitored and controlled.   For the  electrolytic  oily  wastewater
 treatment  process, the response to be measured is the effluent oil concentration.  Even
 though the treatment effectiveness is not  always predictable  based strictly on influent
 oil content, the degree of treatment, or effluent water quality, as shown in  this study is
 dependent  on the ratio  of the  amount of iron  dissolved to the amount of oil in the
 influent.  Thus, the effluent oil content will be determined by the iron dissolution rate
 which in turn is determined  by the  electrode current. Consequently,  the  effluent oil
 concentration may be controlled by using it as a response to control the current. Other
 parameters such as flow  rate and salt concentration would be kept constant.

      The effluent oil concentration  that can be discharged from the electrolytic cell is
 governed by  imposed environmental  regulations.   The standard  method employed  to
 determine  oil concentration directly is  based upon a solvent extraction technique (7)
 which is time consuming and for that reason cannot be  used for feedback control.

      Analytical instruments to measure directly the oil  concentration  are available,
such  as infrared  and ultraviolet spectrophotometers.  These instruments  were not
evaluated in  depth in the present program; however, they are expensive  and  may require
skilled operators.

      As  was shown in  this study, light scattering  or  turbidity of  the  wastewater
correlates  with effluent oil content with a correlation  coefficient of 0.88.   Since
turbidity is a simple measurement  with a rapid response, it  may be used to monitor
effluent water quality and the signal used to set  the current.  By using feedback control,
the required  water quality with minimum  iron addition and minimum sludge generation
can be obtained from the process.

-------
     With an arbitrary  initial current setting, it is  envisioned that a water sample
would be acquired downstream of the cathode, sandfiltered to remove iron/oil floe, and
its  turbidity  measured.   The millivolt  response from the  instrument  would  be
programmed into a microprocessor and compared to a preset value which corresponds to
the desired water quality. A current change would then be  made, either increased or
decreased depending on  whether turbidity is  above  or  below the set  point.   The
magnitude of the current change would be related to the magnitude of  the  difference
between the signal and the set point. The time interval between resetting and the next
sampling will depend upon the flow time between the electrode and the sampling point.
The  system  would continue  to search for minimum current  by examining changes in
turbidity.  The uppec, bound  on the  current  would be  the passivation current (current
density of 10 mA/cm ).

     To avoid large and rapid excursions in influent oil concentration, an equalization
tank, capable of  containing  a few hours  of  the plant flow should be employed.  This
would allow designing the electrode size for a time averaged oil content  (rather than
peak) and  reduce the requirement for rapidity of response of the control system.

     Maintenance requirements, such as the means to assure clear instrument windows,
remain to be established.
SYSTEM CAPACITY DESIGN CRITERIA

     To design a treatment cell, the main feature that needs to be established is the
size of  the electrode.  This will determine, at the passivation  current density, the
amount  of iron  which  can be dissolved  to produce a desired effluent quality.   The
required total  current is  proportional to  the  influent  oil  flux,  which  is  in  turn
proportional  to  the  flow  rate  and oil  concentration (1).   For  the  Livonia Plant
wastewater, examination of the data, along with previous experience (1), indicates that
in most  instances, a current of 0.007 amperes per liter per minute of flow per (ppm) of
influent oil concentration is adequate to provide an effluent with less than 25 ppm of
Freon extractables.  Since current density is limited by passivation to about 100 A/m ,
the electrode area  required can  be  estimated at about 7x10"  square meters per liter
per minute per (ppm).  For example,  to  treal 38 1/min  (10  gal/min) of wastewater
containing 2000 ppm of  oil  would require 5.3 m of electrode area.

     In designing a system for a particular plant site, it  is recommended that simple
beaker or small bench scale studies be carried out to establish the electrode area design
constant for that wastewater to obtain the desired water quality.


ECONOMIC PROJECTIONS

     To establish  the  overall economics  of the electrolytic process accurately is
difficult at this time. It will be necessary to have a scaled-up process handling a major
portion  of  a  manufacturing plant effluent  to determine electrode durability, mainte-
nance, manpower  requirements, etc. These have not been fully addressed in this study.
Nevertheless, some preliminary economic estimates of  operating and capital costs can
be made from the  current studies.  Economics projections for  a  few scenarios are
presented below.

-------
 Scheme 1. A process scheme with air bubblers and without automation.

      This situation represents the approach used during the first phase of the program.
 The  system would represent  the  least  expensive approach  both from  a  capital
 investment and direct operating cost standpoint.   However, as previously noted, there
 may  be a deficiency of effectiveness of the air bubblers after some time of operation.
 This would lead to rapid loading of the sand filter.

      Assuming a  plant  size   of about  76  m  /day  (20,000  gal/day)  the  capital
 requirements would be about $50,000 including flow meters, pumps, power supplies, etc.
 The capital costs are itemized in Table 12.  Direct operating costs based on the present
 study  include  $0.04/nT  ($0.15/1000  gal)  electrical   (at ,$0.025/kW-hr),  $0.04/m3
 ($0.15/1000 gal) calcium chloride (at $0.07/kgX and  $0.01/nrT  ($0.04/1000 gal) for iron
 based on iron scrap value. This equals $0.09/m  ($0.34/1000 gal) of wastewater treated.
 This cost would be the same for all of the schemes  described in this section since the
 major costs are electrical, salt, and iron.  Added to this would be the operating costs
 associated with flotation air, pumps,  motors,-etc.  For comparison, direct, chemical
 costs for common batch systems generally range from around  $0.22-$0.29/m  ($0.85 to
 $1.10/1000 gals).  Credit for the waste oil is not included.

 Scheme 2.  A process scheme with dissolved air flotation and without automation.

      The major advantages of  this scheme are that flotation and skimming would be
 much more efficient and would occupy much less  space than  Scheme 1.  Both capital
 and operating costs would be increased.  Capital  would be increased by $30,000 for a
 dissolved air  unit capable of handling from 19 to 114 m  /day (5,000 to 30,000 gal/day).
 Operating  costs for this  unit,  based on information furnished  by the  manufacturer,
 average about $0.08/m ($0.30/1000 gal).  This includes cost of pumping, skimming, etc.
 With automatic skimming, manpower costs would decrease and the quality of the sludge
 may be improved. Other costs  would be similar to Scheme 1 with only minor saving of
 manpower.

 Scheme 3.  A process with dissolved air flotation and  automated control.

      This scheme would be the  most efficient from a manpower standpoint and would
 result in optimum  operation. The automatic feedback control technique remains to be
 evaluated.  The feedback system envisioned would control the current by sensing the oil
 content in  the  effluent from the cell.   Systems to monitor the oil range from  $800 to
 $8,000 depending on the plant wastewater to be treated.  For Livonia Plant wastewater,
 a system to monitor turbidity, which was shown to correlate with oil content, may be
 employed.   In  this case, a  total feedback system  would  be around $5,000 with no
increase in direct operating cost.  Manpower would be decreased since adjustment  and
settings of the  process would be automated. Maintenance cost of  the feedback system
is not known.
                                      -46-

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        TABLE 12.   CAPITAL COSTS  OF ELECTROLYTIC  TREATMENT
1.  Process with air bubblers-without automation

        Flow equalization tank    -   $10,000
        Pumps                     -      2,500
        Mixing tank               -      1,500
        Electrolytic cell-shell   -      3,000
        Power supplies            -      8,000
        Belt skimmer              -      3,500
        Sludge collector          -      3,000
        Flow meters               -      1,500
        Electrode                 -      2,500
        Air bubblers              -      2,000
        Air compressor            -      2,000
        Sand filter               -      1,500
        Installation              -'      9,000
                                      $50,000
2.  Process with dissolved air flotation-without automation

        Scheme 1 costs            -    $50,000
        Dissolved air flotation   -     30,000
                                       $80,000
3.  Process with dissolved air flotation-with automation

        Scheme 2 costs            -    $80,000
        Automation (turbidity     -      5,000
                     system)           $85,000
                              -47-

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                                 REFERENCES
1.   Weintraub, M. H.,  and R.  L. Gealer, Development  of Electrolytic Treatment of
     Oily Wastewater, American Institute of Chemical Engineers, 70th Annual Meeting,
     New York, NY, Nov. 13-17, 1977, paper No. 151.

2.   Dzieciuch, M. A., M. H. Weintraub, and R. L. Gealer, Electrolytic Treatment of
     Oily Wastewater—Laboratory Investigation, 149th Meeting of The Electrochemical
     Society, Washington, D.C., May 2-7,  1976, Abstract No. 260.

3.   Weintraub, M. H.,  M.  A. Dzieciuch, and R. L. Gealer, Electrolytic Treatment of
     Oily Wastewater—Engineering  Development, 149th Meeting of  Electrochemical
     Society, Washington, D.C., May 2-7,  1976, Abstract No. 261.

4.   Cutting Fluid Technology, Tribology International, Vol. 1,  No.  1, February 1977.

5.   Rossmore, H. W., Microbiological Causes of Cutting Fluid Deterioration, Society
     of Manufacturing Engineers, Dearborn, MI, 1974, paper No. MR74-19.

6.   Tomko, 3.,  Cutting  Fluid Maintenance, Society  of  Manufacturing Engineers,
     Dearborn, MI, 1971, paper No. MR 71-804.

7.   Methods   for  Chemical  Analysis  of Water  and  Wastes,   U.S. Environmental
     Protection Agency,  Environmental  Monitoring and  Support Laboratory,  1974.
     Cincinnati, OH.

8.   Becher, P.,  Emulsions:   Theory and Practice,  Reinhold Publishing Corp.,  New
     York, NY, 1965. p. 183.
                                      -48-

-------
                                  TECHNICAL REPORT DATA
                           (Please read Instructions on the reverse before completing)
 REPORT NO.
 :PA-6UO/Z-80-14o
                                                          3. RECIPIENT'S ACCESSION NO.
 TITLE AND SUBTITLE

 ELECTROLYTIC TREATMENT OF  OILY  WASTEWATER FROM
 MANUFACTURING  AND MACHINING PLANTS
                                                          5. REPORT DATE
                                                           JUNE  1980
                                                          6. PERFORMING ORGANIZATION CODE
 AUTHOR(S)

R.L.  GEALER,  A. GOLOVOY and M.H. WEINTRAUB
                                                          8. PERFORMING ORGANIZATION REPORT NO.
 PERFORMING ORGANIZATION NAME AND ADDRESS

FORD MOTOR COMPANY
ENGINEERING  and RESEARCH STAFF
DEARBORN, MICHIGAN 48121
                                                          10. PROGRAM ELEMENT NO.

                                                             1BB610
                                                          11. CONTRACT/GRANT NO.

                                                             GRANT  NO.  S804174
2. SPONSORING AGENCY NAME AND ADDRESS
INDUSTRIAL ENVIRONMENTAL  RESEARCH  LAB-Ci
OFFICE OF RESEARCH AND DEVELOPMENT
U.S.  ENVIRONMENTAL PROTECTION  AGENCY
CINCINNATI, OHIO  45268
                                                           13. TYPE OF REPORT AND PERIOD COVERED
                                                             FINAL
                                                           14. SPONSORING AGENCY CODE

                                                             EPA/600/12
5. SUPPLEMENTARY NOTES
 6. ABSTRACT
     A  continuous electrolytic treament is being developed to remove emulsified oil from dilute
oily wastewater streams, such as is generated in metal working operations.  In this process, the
wastewater permeates through  an iron chip bed anode and steel mesh cathode.  A  potential  is
applied to  the electrodes, forming ferrous ions at the anode and hydroxyl ions at the cathode.  The
 :errous ions react in a complex manner with the emulsifying agents, destabilizing the emulsion and
 generating an oil rich floating sludge and essentially oil-free water.
     A  pilot plant unit  capable of  processing about 5700 I/day (1500 gal/day) was designed,
constructed, and evaluated at an actual plant site.  Operating parameters and process equipment
were evaluated to assess the potential and problems of the process.
     Wastewater with initial  oil concentrations in the range  of 300 to  7,000 ppm of solvent
extractables has been  reduced to less than 50 ppm in 90%  of the test runs, and to less than 25 ppm
 in 83%.  These test runs were done at conditions of minimum operating cost and minimum sludge
 generation. When necessary, Freon extractables generally are reducible to about 10 ppm or less
 ay the addition of more electrolytically dissolved iron to the system at a small increase in cost.
     Preliminary economics look favorable and overall results  are  quite encouraging so that
 further scale-up of the process is recommended.
     This  report was  submitted  in  fulfillment of  Grant No. S-804174 by Ford Motor Company
under the sponsorship of the  U.S. Environmental Protection Agency.  The report covers the period
May 18, 1976 to August 17,  1978, and work was completed as of August 17, 1978.	
 7.
                               KEY WORDS AND DOCUMENT ANALYSIS
                 DESCRIPTORS
                                              b.lDENTIFIERS/OPEN ENDED TERMS
                                                                        c.  COSATI Field/Group
 OILY WASTEWATER    WATER  POLLUTION

 INDUSTRIAL  WASTES
                                              ELECTROLYTIC  PROCESS
                                              EMULSIFIED OIL RE-
                                              MOVAL FROM WASTEWATER
68D
18. DISTRIBUTION STATEMENT

  RELEASE  TO  PUBLIC
                                              19. SECURITY CLASS (ThisReport)

                                               ITMTT
                                                                         21. NO. OF PAGES
                                              2O. SECURITY CLASS (Thispage)
                                               UNCLASSIFIED
                                                                        22. PRICE
EPA Form 2220-1 (R«v. 4-77)    PREVIOUS EDITION is OBSOLETE
                                                           •if U.S. GOVERNMENT PRINTING OFFICE: 1980--657-765/0024

-------