June 1988
              BIOLOGICAL DEGRADATION OF CYANIDE BY
                  NITROGEN-FIXING CYANOBACTERIA
                               by

                        Dr. C.J. Gantzer
                         Dr. W.J. Maier
                     University of Minnesota
           Department of Civil and Mineral Engineering
                     Minneapolis,  MN  55455
                         Project Officer

                        James S. Bridges
Office of Environmental Engineering and Technology Demonstration
         Hazardous Waste Engineering Research Laboratory
                     Cincinnati,  OH  45268
                This study was conducted through

                Minnesota Waste Management Board
                      St. Paul,  MN  55108

                             and the

             Minnesota Technical Assistance Program
                     University of Minnesota
                     Minneapolis,   MN  55455
         HAZARDOUS WASTE ENGINEERING RESEARCH LABORATORY
               OFFICE OF RESEARCH AND DEVELOPMENT
              U.S. ENVIRONMENTAL PROTECTION AGENCY
                     CINCINNATI,  OH  45268

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                                  ABSTRACT
     This study examined the ability of  nitrogen-fixing Anabaena to biodegrade
cyanide in batch  reactors.   Mixed  second-order rate constants  were obtained
that described the biologically-mediated decrease in cyanide for reactors
containing initial cyanide concentrations of 3 ppo.   For Anabaena cultures not
previously exposed to cyanide,  the rate  constants were a function of pH.
Faster  rates of cyanide biodegradation were  observed at higher pH values.
Anabaena  cultures acclimated to the presence  of cyanide had rate constants
that were at least 10  times faster than rate constants  for unacclimated
cultures.

     Mixed second-order  rate  constants  were also obtained for the ability of
nitrogenase,  the enzyme  normally  responsible for nitrogen-fixation,  to reduce
hydrogen  cyanide  to methane and ammonia.   In batch reactors with  initial
cyanide concentrations of 30  ppb,  the rate constants for  methane production
were at least 10 times faster than expected based  on  literature values for
nitrogen  fixation, suggesting  that nitrogenase  will preferentially  use
hydrogen cyanide as a substrate as compared to  molecular nitrogen.  Also,  the
rate constants for methane production were of the same order of magnitude as
the rate constants for total cyanide removal, indicating nitrogenase as an
important mechanism for the biodegradation of trace concentrations of  cyanide.

     The magnitude of the cyanide biodegradation rate constants suggests that
the utilization of nitrogen-fixing  cyanobacteria  in  the treatment of  cyanide
wastes  can be a feasible process in some applications, i.e., secondary or
tertiary treatment at larger treatment facilities.
                                    iv

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This project was partially supported with a United States
Environmental Protection Agency cooperative agreement through the
Minnesota Waste Management Board and the Minnesota Technical
Assistance Program.


Although the research described in this report has been funded in
part by the United States Environmental Protection Agency through
a cooperative agreement, it haa not been subjected to Agency
review, and therefore does not necessarily reflect the views of
the Agency and no official endorsement should be inferred.

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                                   CONTENTS

 Abstract	iv
 Tables	vl
 Figures	vii

      1.   Introduction   	  1

      2.   Conclusions 	  4

      3.   Recommendations  	  7

      4.   Materials and Methods

          Experimental Overview   	  8

          Culture Media   	  8

          Experimental Procedures

               Growth Rate Experiments 	   10
               Total Cyanide Removal Experiments
                    Objective and Apparatus  	   12
                    Cyanide Mass Balances  	   12
                    Kinetic Parameter Determination  	   13
               Methane Formation Experiments
                    Objective and Apparatus  	   14
                    Kinetic Parameter Determination  	   15

          Analytical Procedures  	   17

     5.   Results and Discussion

          Growth Rate Determination  	   19

          Total Cyanide Removal Rates
               Limitations of Batch Experiments  	   23
               Rate Constants for Total Cyanide Removal  	   24
               Effect of Acclimation on Cyanide Removal Rates   	   32

          Methane Production Rates
               Rate Constants for Methane Production 	   33
               Comparison of Methane Production with Nitrogen Fixation  .  .   39

          Application of Kinetic Data to Cyanide Treatment  	   41

References	46

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                                    TABLES
Number

  1.  Cyanobacteria culture media
  2.  Extent of biodegradation and volatilization in
          selected batch experiments ................... 25

  3.  Overall volatilization rate constants (K^a) and
          mixed second-order rate constants (Kv) for
          total cyanide removal by unacclimatea Anabaena
          cultures in selected batch experiments ............. 26
  4.   Comparison of mixed second-order rate constants
          for total cyanide removal by unacclimated (batch
          number 4) and acclimated (batch number 5)
          Anabaena cultures in presence of thiosulfate .......... 33
                                      vi

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                                   FIGURES
Number                                                                    Page

  1.  Logarithmic increase in Anabaena biomass (X) as
          function of time, during a batch experiment  	 20

  2.  Changes in Anabaena biomass (X) versus time after
          the start of feed flow through the reactor.  The
          dotted line represents the expected decrease in X
          if dilution was the only removal mechanism	21

  3.  Decrease in total cyanide concentration (S) during
          batch test number 3.  The line represents the
          numerical solution of equation (3) using the
          Kf, and K^a values on Table 3	27

  4.  Relationship between log Kb [L/(ug chl hr)] versus
          time-averaged pH	29

  5.  Relationship between log Kb [L/(ug chl hr)] versus
          time-averaged ALPHA	30

  6.  Increase in headspace methane concentration with time.
          For the illustrated batch test, the initial cyanide
          concentration was 31.2 ug CN/L	34

  7.  Sensitivity of K_ obtained from equations (13) and (14)
          to inputted Kh values.  Both parameters have units
          of L/(ug chl hr)	37

  8.  Sensitivity of the ratio between Kn and Kb to inputted
          Kv values.  Both parameters have units of
          L/(ug chl hr)	38
                                     vii

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                                   SECTION  1



                                  INTRODUCTION





      The basic  premise of this study was that  the use of nitrogen-fixing



 cyanobacteria (blue-green algae) in the biological treatment of small



 concentrations  of  free cyanides (HCN and CN~) can be a cost-effective



 alternative  to  existing treatment processes.  A potential application of a



 cyanobacteria-based  process would be in  the  secondary treatment of the free



 cyanides that escape alkaline-chlorination.  Because the extent of cyanide



 oxidation in  alkaline-chlorination is an equilibrium-driven phenomena, use of



 a microbial  process  to detoxify the  last fraction of cyanide should result in



 lower alkaline-chlorination operating costs.  Another application of a



 cyanobacteria-based  process could be in the treatment of the cyanide



 associated with metal-cyanide complexes  via a two-step process.  The first-



 step  would release cyanide from the metal-cyanide complexes by exposing the



 complexes to  ultraviolet irradiation.  In the second-step,  cyanobacteria would



 detoxify the  released  cyanide.



     The use of nitrogen-fixing cyanobacteria in the treatment of cyanide



 wastes is a  new concept.  There are several potential advantages associated



 with  the use  of nitrogen-fixing cyanobacteria in the treatment of small



concentrations  of cyanide.   First, the biological  treatment of cyanide with



cyanobacteria should have much lower operating costs than alkaline-



chlorination. The  operating costs for the biological treatment of cyanide



wastes with  aerobic  heterotrophs  can be less than 10% the costs for alkaline-

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chlorination (Green and Smith,  1972).  The costs associated with providing
aeration and with  providing a supplemental  energy  source (organic  substrate)
for the maintenance of large amounts of aerobic heterotroph biomass make up a
considerable portion of the total operating costs for the traditional
biological treatment of hazardous wastes.  Because cyanobacteria are
photosynthetic, they do not require aeration for oxygen and do not require the
presence of organic substrates to maintain biomass (Kobayashi and Rittmann,
1982).   Thus,  in terms of operating costs, the use of nitrogen-fixing
cyanobacteria in the treatment of small amounts of cyanide should have an
economic advantage over the use of heterotrophic bacteria, and, consequently,
a significant economic advantage over  alkaline-chlorination.
     Second,  nitrogen-fixing cyanobacteria have the ability to survive in low
to moderate concentrations of hydrogen cyanide.  Hydrogen cyanide is toxic
because it inhibits the terminal cytochrome oxidase in respiration, which
normally reduces oxygen to water.   Cyanobacteria have several terminal
oxidases—some of  which  are resistant to cyanide inhibition (Fogg,  et al.,
1973;  Degn, et al., 1978;  Peschek,  1980;  Henry, 1981).   Cyanobacteria also
have several cyanide detoxification pathways,  i.e.,  enzymatic pathways that
transform free cyanides into a less  toxic form (Castric,  1981; Higgins, et
al.,  1984).  The most studied  and perhaps the most important detoxification
pathway is mediated by the enzyme rhodanese, which transfers a sulfur from a
donating compound  (e.g.,  thiosulfate) to  cyanide  to form  thiocyanate (Westley,
1981).  Other cyanide detoxification  pathways result  in the formation of amino
acids (Solomonson,  1981).   Thus, due to the presence of cyanide detoxification
pathways and cyanide-resistant respiration, cyanobacteria can survive in
solutions containing free cyanides.   For example, Howe  (1963, 1965) observed a

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"luxuriant" growth of cyanobacteria  on  the  filter stones of a  biological
reactor  that  was treating wastes containing 300 ppra cyanide.
      Third, in  addition  to  the  above pathways,  the  nitrogen-fixing
cyanobacteria can destroy hydrogen cyanide  with the enzyme nitrogenase.  While
normally responsible for the reduction  of molecular nitrogen  (dinitrogen)  to
ammonia, nitrogenase can also reduce hydrogen cyanide to methane and ammonia
(Hardy and Knight, 1967;  Hardy  and Burns, 1968; Biggins and Kelley,  1970;
Haystead, et  al., 1970; Hwang and Burris, 1972; Hwang, et al., 1973; Zumft and
Mortenson,  1975;  Stewart, 1980; Li,  et  al., 1982).   In fact,  nitrogenase will
preferentially  reduce hydrogen  cyanide  instead of its normal substrate,
dinitrogen (Li,  et al.,  1982).   Some  researchers have proposed that  the
original role of  the nitrogenase system was to detoxify the cyanide  and
cyanogen found  in the primitive biosphere when the  earth had a reducing
atmosphere (Silver and Postgate,  1973;  Postgate,  1982).
     Despite the considerable amount of information indicating that
cyanobacteria are able to survive in  the presence of cyanide and are able  to
detoxify cyanide, the kinetic data required to assess the feasibility of
utilizing cyanobacteria in the  treatment of cyanide wastes does  not  exist.
This study provides an initial assessment of the rate at which nitrogen-fixing
cyanobacteria are able to degrade free cyanide.  In particular, the mixed
second-order rate constants for the  biologically-mediated removal of cyanide
by unacclimated cultures  of  Anabaena were determined  in batch  reactors.  A
second set of batch experiments determined the mixed second-order rate
constants for the reduction  of  hydrogen cyanide  by  nitrogenase.

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                                  SECTION 2



                                 CONCLUSIONS




     In batch reactors with initial cyanide concentrations of 3 mg/L, the



mixed second-order rate constants (Kb) for the removal of cyanide by nitrogen-



fixing Anabaena cultures was a function of pH.  The biodegradation rate



constants increased with increasing pH for unacclimated Anabaena cultures,



i.e., cultures not previously exposed to cyanide.  At a pH of 8.4 and a



temperature of 25°C, the observed rate constant in terms  of  chlorophyll  (chl)



concentration was  5.0* 10~"  L/(ug  chl hr).   When the pH was increased  to  9.5,



Kj, increased to 2.2-10~* L/(ug chl hr).  The observed  relationship  between Kj,



and pH suggested that the ratio of hydrogen cyanide to total free cyanide



concentrations,  [HCN]/([HCN]+[CN~]),  influenced biodegradation rates.   Because



HCN is much more toxic and inhibitory than CN~, and because  an increase in pH



would reduce HCN concentrations, the faster biodegradation rates observed at



higher pH values was probably due to a reduction  in inhibition.



     When previously exposed to cyanide, Anabaena biodegraded cyanide at a



faster rate.   The Kj, value  for  an acclimated Anabaena culture was 10 times



greater than that for an unacclimated Anabaena culture.  Thus, reactors



operating under steady-state conditions should have faster cyanide removal



rates than those observed in the batch experiments.
                                       «


     The mixed second-order rate constant for the reduction  of cyanide to



methane by nitrogenase (Kn) was  determined in small gas-tight batch reactors



with initial cyanide concentrations of 30 ug/L.  A typical value of Kn was

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 2.6-10"* L/(ug  chl hr),  which was at  least an order of magnitude  greater  than
 t

 expected based on existing nitrogen-fixation kinetic data.  The larger  than


 expected Kn  supported  the  j.n_ vitro  observation that nitrogenase will


 preferential!/ reduce hydrogen cyanide rather than its normal substrate of


 molecular nitrogen.  Based on the amount of methane produced during the batch


 tests,  nitrogenase activity reduce* cyanide concentrations from 30 ug/L down


 to  20 ug/L.  Because few cyanide destruction processes are able to attack


 cyanide at such low  concentrations, the  utilization of nitrogen-fixing


 cyanobacteria  in the treatment of trace-levels of cyanide is worth further


 examination.


     Based on  the total cyanide  biodegradation rate constants  (Kjj) obtained


 from batch experiments, use of nitrogen-fixing cyanobacteria in the secondary


 or  tertiary  treatment of cyanide wastes  could be a feasible process, provided


 that the treatment process has adequate mean cell residence time.   With a net


 specific growth rate of 0.8 d~^f  the unacclimated Anabaena culture can have


 faster growth kinetics and trace-contaminant removal rates than existing


 biological treatment processes.  Because cyanobacteria are photosynthetic, the


amount  of biomass in a  reactor is not a  function of organic substrate


concentration.   Thus,  the volumetric size of the reactors required to treat


low concentrations of cyanide would be small compared to traditional aerobic


processes for treating dilute wastes.   For example,  a  chemostat model using


conservative rate and biomass parameters predicted that a hydraulic retention


time of  only 5  days is  required to  reduce an influent cyanide concentration of


4 mg/L  by 93 percent.  In comparison,  the 90 percent reduction  of  a 10 mg/L


influent BOD concentration in an aerobic chemostat would require a hydraulic


retention time of 21 days,  based  on  typical BOD kinetic parameters (Metcalf

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and Eddy,  1979).  However,  the  required  size  of  the  BOD  chemostat would be
reduced if supplemental substrates were added to the reactor to increase
biomass concentrations.
     Because of the potential to attack trace-concentrations of cyanide and of
the potential for low operating costs, the use of nitrogen-fixing
cyanobacteria In the biological treatment of cyanide wastes may be an
attractive alternative to exiting cyanide treatment technologies.  However,
the capital costs and the requirement for trained personnel associated with
biological treatment processes, may make the cyanobacteria process unsuitable
for small-volume cyanide-waste generators.  The cyanobacteria process is
probably better suited for larger cyanide treatment facilities.

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                                  SECTION 3



                               RECOMMENDATIONS





     This stud/ demonstrated  the ability of nitrogen-fixing cyanobacteria to



biodegrade low concentrations of free cyanides in batch reactors.  Future



studies need to examine  the ability of the cyanobacteria to degrade cyanide



under steady-state conditions and to determine the stability of the steady-



state reactors to slight perturbations in cyanide concentrations.  If such



laboratory-scale experiments  continue to demonstrate the attractiveness of



utilizing nitrogen-fixing cyanobacteria in the treatment of low cyanide



concentrations,  then a pilot-scale study  should be performed to determine the



economic and technical feasibility of the process.

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                                  SECTION 4



                            MATERIALS AND METHODS





EXPERIMENTAL OVERVIEW



     The objectives of the study were 1) to determine the rates at which a



cyanobacteria culture removed free cyanides (HCN + CN~),  and 2) to determine



the rate at which HCN was  reduced to methane by the activity of the enzyme



nitrogenase.  Rates of total cyanide removal were determined  in a 1.3-liter



reactor under batch conditions.   Attempts were also made to determine total



cyanide removal  rates under  continuous-feed  conditions,  i.e.,  in a chemostat.



The methane production experiments were conducted in small  0.037-liter, gas-



tight vials under batch conditions.





CULTURE MEDIA



     The cyanobacteria used in the cyanide degradation  experiments were



Anabaena sp. obtained from Carolina Biological Supply  Co. (Burlington, NC,



catalog number 151710).   None of the cultures used in the study were axenic,



i.e., none were free of  bacteria.



     The media used to maintain Anabaena cultures and used  in the cyanide



degradation experiments was the Hughes-Gorham-Zehnder media described in Allen



(1973).  The chemical composition of  the media is shown on  Table  1.  To



increase the buffering capacity  of the media at pH values slightly greater



than the pKa for  hydrogen cyanide for media used in the batch experiments



0.186 grams  of  H603 was  added to each liter of media (3 mN) .   Adjustments in



pH were performed by the addition of either 1M NaOH or HC1. Prior to its use,





                                      8

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TABLE 1.  CYANOBACTERIA CULTURE MEDIA
Macronutrients
K2HP04
MgS04-7H20
CaCl2-2H20
Na2C03
NaSi03-H20
Citric Acid
EDTA
Ferric Citrate
Micronutrient Solution
Micronutrient Solution
H3B03
MnS04-H20
ZnS04-H20
(NH4)Mo7024-4H20
Co(N03)2'6H20
Na2W04-2H20
Or
KI
Cd(N03)2-4H20
NiS04-6H20
V205
A12(S04)-»'K7SOA-24H-,0
grams/liter
0.369
0.075
0.036
0.020
0.058
0.006
0.001
0.006
0.08 mL
grams/liter
3.10
1.69
0.287
0.088
0.0167
0.33
0.119
0.083
0.154
0.138
0.018
0.474

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the media  was autoclaved.   Ferric citrate was autoclaved separately from the
rest of the media  to  prevent  the precipitation  of  ferric phosphates.  Because
no fixed-nitrogen  was added to  the  media,  the Anabaena had heterocysts and
relied on  the  fixation of dinitrogen for their  nitrogen  needs.
     Maintenance cultures were  grown in autoclaved 100-ml Erlenraeyer flasks
that were  stoppered with cheese-cloth-wrapped cotton plugs.   The maintenance
cultures were  illuminated by  cool-white fluorescent light, and were not
continuously agitated nor was air bubbled through  the media.  Probably due to
C02 limitations, the  Anabaena in the maintenance cultures had slow growth
rates.
     The Anabaena used in the total cyanide removal and the methane production
batch tests were not directly transferred  from maintenance culture to
respective batch reactors.   Instead, an inoculum from a maintenance culture
flask was  placed into a 500-mL gas wash bottle  that contained fresh media.
The media  was  agitated by the introduction of filtered air passing through a
porous glass diffuser.  In addition to providing agitation,  the air bubbles
released by the diffuser provided a continuous  supply of C02 to the system.
Anabaena in the gas wash bottle  had rapid  growth rates (doubling times on the
order of 1 day).  Upon reaching a desired biomass  (chlorophyll) concentration,
portions of the gas-wash-bottle cultures were transferred to the batch
experiment reactors.

EXPERIMENTAL PROCEDURES
Growth Rate Experiments
     Anabaena growth rates were determined in a New Brunswick Scientific
(Edison, NJ) Bioflo Chemostat  Model C32 with a Pyrex reaction vessel that held
1.3 liters  of  media.   During the initial growth rate experiments, the reactor

                                     10

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 was operated in batch mode (no continuous feed) and no cyanide was present.


 Temperatures were maintained at 25°C.  Air was supplied at a rate of 15 L/hr.


 Increases  in biomass were determined by monitoring the increase in


 chlorophyll-a (chl) concentrations with respect to  time.  The  rate of  increase


 in  biomass was assumed to be first-order with respect to biomass, i.e,


                                   dX
                                   — =uX                                (1)
                                   dt


 in  which X is the chlorophyll-a concentration (ug  chl/L), t  is time  (hr), and


 u is  the net specific growth  rate  (hr~*).  The value of u was  obtained  by


 determining the slope (least-squares  fit) of the line produced  when  the


 natural logarithm  of  X (In X)  was plotted versus time.   The amount of time


 required for the value of X to double was determined from


                                        0.693

                                  td	                               (2)
                                         u


 in which t
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Total Cyanide Removal  Experiments

Objective  and Apparatus—

     The objective  of  the total cyanide removal experiments was  to determine

the  mixed-second order rate constants for the biologically mediated  removal of

free cyanides from  the 1.3-liter reactor operated in a batch mode.   These

batch experiments were of short duration (4 to  5  hours),  so that during  the

course of  the experiment  any  increases in Anabaena biomass due to growth would

be negligible.  Initial total cyanide concentrations were approximately  3000

ug CN/L.  Water  temperatures  were  maintained at 25°C.  Filtered  air  was  added

to the reactor at a rate of 15 L/hr. and air exiting the reactor was drawn

through a  gas-wash  bottle containing  a  1 N  solution of NaOH to capture any HCN

that was volatilized from the reactor.

Cyanide Mass Balances—

     The two mechanisms responsible for the decrease in  total free cyanide

concentrations in the  1.3-L reactor were biodegradation of HCN and CN~ and

volatilization of HCN.   Based on these two mechanisms, the mass  balance

equation for the batch reactor is

                         dS
                         — - - Kb  X0 S - Kra ALPHA S                      (3)
                         dt

in which S is the concentration  of free  cyanide (HCN + CN~) in the reactor

(ug CN/L),  Kb is the mixed second-order rate constant for the biodegradation

of free cyanides  by the microorganisms (L/(ug chl hr)), XQ is the

concentration of Anabaena in the reactor at the start of the batch experiment

(ug chl/L), K^a  is the  overall mass transfer coefficient for the movement of

HCN from the liquid phase to  the gas  phase  (1/hr), and ALPHA is  the  ratio of

HCN to the total amount of free cyanide in  solution,
                                     12

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                                         [HCN]
                             ALPHA =	 .                         (4)
                                     [HCN]  + [CN-]

The ALPHA  parameter must be included in the volatilization term,  because HCN

is the  only  form of free cyanide that is subject to  volatilization.   ALPHA  is

a function of  the pKa of HCN and of the pH of  the  solution.  Because  the pKa

of HCN  at  25°C is 9.3, values of  ALPHA  can be obtained from  (Snoeyink and

Jenkins,  1980)

                                          10-PH
                             ALPHA =	                         (5)
                                     IO-PH  +  i
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being set at the same  values.  Thus, both Kb and l^a had to be determined from
the experimental data  for each batch test—So,  X0,  S(t),  pH(t), and Mf.
     The values of Kb and l^a for each batch test were obtained via a trial
and error algorithm utilizing the Runge-Kutta method  to  solve equation (3).
First, an approximate  value of KLa  was determined by  setting  Kb to zero and
finding the K^a value that predicted the amount of cyanide collected in the
gas-wash bottle at the end of the batch experiment  (Mf).  This approximate
value of KLS accounted for changes  in pH.   Second, this approximate value of
K^a was increased and Kb  values were increased until the Runge-Kutta model
approximated the observed decrease  in total cyanide concentration (S) with
time.   Third,  values of KLa and Kb were then adjusted to yield the best
description of observed Mf  and  S(t) values.
Methane Formation Experiments
Objective and Apparatus—
     The objective of the  methane experiments was to determine the mixed-
second order rate constant for the conversion of HCN by nitrogenase to methane
and ammonia by monitoring the increase in headspace methane concentrations in
gas-tight reactors that were operated in a batch mode.  The batch tests were
of short duration (1 to 2  hours),  so that increases  in Anabaena biomass or
changes in environmental conditions during the course  of  the experiment would
be insignificant.  The  Anabaena  used in  the methane  production experiments had
not previously been exposed to cyanide.   Initial total cyanide concentrations
were approximately 30  ug  CN/L.  To  minimize the volatilization of HCN, Initial
pH values were adjusted to 10.   Water, temperatures during the experiments were
2S°C.   Methane concentrations were  determined by  injecting 100 uL samples of
headspace gas into a Hewlett-Packard 5340A gas chromatograph with a flame-
                                     14

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 ionization  detector  (FID).
      The reactors used in methane experiments consisted of a 40-mL Wheaton
 serum bottles fitted  with a Supelco Mini-Valve stopper.  The stopper was a
 combination value and septum that provided a means of sampling  the headspace
 of the bottle, while  being  gas-tight when  the headspace was  not being  sampled.
 To maintain a uniform distribution of  Anabaena in the media, a small Teflon-
 coated magnetic  stir-bar was placed inside the bottle and the bottle was
 placed on top of a stirring plate.  During the batch experiments, the bottle
 contained 25  mL  of media and  had a headspace volume of 12 mL.  The stem of the
 stopper occupied the  remaining  3  mL.
 Kinetic Parameter Determination —
      Each mole of methane appearing in the headspace of the serum bottle was
 assumed to be produced from the reduction of one  mole of hydrogen cyanide to
 methane and ammonia by nitrogenase.  Thus, the molar concentration of methane
 in the headspace corresponds to  a  mass concentration  of  cyanide that was
 reduced  by nitrogenase,
                                [CH4] --                         (7)
                                            Vwater
in which P is the cyanide concentration in the water phase corresponding to
the mass of methane produced  (ug CN/L), [CH^] is the molar concentration of
methane in the headspace gas (umoles Cfy/L of gas),  MWCH4 is the molecular
weight of methane,  MW^ is the molecular weight of  the cyanide  function group,
Vgas is the voiune  of the  headspace  (0.012 L),  and Vwater is the volume of the
water phase in  the  serum bottle (0.025 L).  Because  P represented another  way
of describing methane concentration  (the product of nitrogenase activity),  the
value of P increased with  time during  the  methane batch  tests.
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     The rate of methane production by nitrogenase was assumed to follow mixed
second-order kinetics,
                                 dP
                                 — = Kn X0 S                               (8)
                                 dt
in which P is the water-phase  concentration of  cyanide corresponding to the
mass of methane produced (ug CN/L), t is time (hr), Rn is the mixed second-
order rate constant for the production of methane  by  nitrogenase expressed  in
terms of chlorophyll-a concentration  (L/(ug chl hr))t  X0 is the concentration
of Anabaena at  the  start  of the  batch test (ug  chl/L), and S  is the total
cyanide concentration at  time  t (ug CN/L).
     Because nitrogenase was not the only biological mechanism for reducing
cyanide concentrations (S) in  the vials,  the determination of Kn required that
the decrease in S in equation  (8) reflect these additional mechanisms.  The
total rate at which S decreases with time due to biological activity can be
described by
                                dS
                                	 *b xo s                              (9)
                                dt
in which Kjj is  the  mixed  second-order rate constant for  the biodegradation  of
free cyanides by Anabaena  cultures (L/(ug chl hr)).  Integration of equation
(9) yields
                            S  - S0 exp[-Kb X0 t]                          (10)
in which So is  the  initial cyanide  concentration (ug  CN/L).   Substitution of
equation (10)  for S in equation (8) yields the  following equation:
                         dP
                         — =•  Kn X0 S0 exp[-Kb  X0  t]  .                    (11)
                         dt
Integration of  equation (11) from t=0 and P»PO««0 to t»t  and P=P produces
                                     16

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                             Kn So
                         P -- {l-exp[-Kb  X0  t]J                      (12)

                              Kb


 which describes methane concentration as a function of time.


      The goal of the methane  batch experiments was to determine  the  value  of


 KU for the nitrogen-fixing Anabaena  culture.  For each  batch test, all of  the


 parameters in equation (12) were known,  except  for Kn.  The value of the


 overall biodegradation rate  constant (K^) was determined from  the batch


 experiments examining total cyanide  removal.  When an independent variable


 (RHS) is defined for each sampling time  by




                          RHS-— (1 -exp[-KbX0 t]J ,                    (13)

                                Kb

 equation (12) is reduced  to a linear relationship,


                                  P = Kn  RHS .                              (14)


 Thus,  the value of Kn for each batch test was calculated from  the slope of a


 linear  least-squares  fit  of  the P(t) and RHS(t) data points collected during


 the batch  test.  The y-intercept for equation (14)  should equal zero, because
ANALYTICAL PROCEDURES


     Cyanide and chlorophyll measurements  followed  the  procedures  presented in


Standard Methods  (APHS,  1980).


     Prior to analysis, cyanide samples were distilled in a commercially-


available cyanide distillation apparatus.  In the boiling flask, the cyanide


sample was subjected to  acidic conditions  and  to a  magnesium chloride reagent.


This solution was re fluxed  for 1 hour.  The volatilized hydrogen cyanide was


collected in a gas-wash  bottle  containing 1.25 N NaOH solution.


     For samples with  cyanide concentrations greater than 1 mg CN/L, the




                                     17

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cyanide concentrations in the alkaline distillate were determined by the



titrimetric method.  The distillate was titrated with a standard silver



nitrate (AgNOj) solution to form a soluble cyanide complex,  Ag(CN~>2.  As soon



as all the CN had been completed and a small excess concentration of Ag+ had



been added, the excess Ag+ was detected by the silver-sensitive indicator,



paradimethylaminobenzalrhodanine, which turned from a yellow to salmon color



(APHS, 1980).



     For samples  with concentrations  less than 1 rag CN/L, the cyanide content



of the alkaline distillate was determined by the colorimetric method.  First,



the pH of a distillate sample was adjusted to approximately 8 with the



addition of a phosphate buffer.  Second, chloramine-T  was added,  which



converted the CN~ in the distillate to CNC1.   Third,  with the addition of a



pyridine-barbituric reagent,  the CNC1 formed a red-blue dye.  The absorbance



of the aqueous dye at 578 nm was linearly proportional to CN concentration in



the distillate (APHS,  1980).



     The concentration of chlorophyll-a in a sample was used as an indicator



of Anabaena biomass concentration.   Chlorophyll-a concentrations  were



determined by the cold acetone extraction method.  A known volume of the



cyanobacteria suspension with a small amount of MgC03 was drawn through a



0.45-um membrane filter.  The filter was placed was placed into a centrifuge



tube,  and a small known volume of a 90% acetone (v/vwater) solution was added



to the centrifuge tube.  The  acetone  solution was allowed to extract the



chlorophyll from the Anabaena for 24 hr at a temperature  of  A°C.  After



centrifugation,  the chlorophyll-a  concentration in the supernatant was



calculated from the supernatant's  absorbances at 663,  645, and 630 nm  (APHS,



1980).  Absorbances were  measured  with a Beckmann Spectrophotometer.
                                     18

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                                   SECTION  5



                             RESULTS  AND  DISCUSSION





 GROWTH RATE DETERMINATION



      For batch growth experiments conducted  at pH values ranging from 8.0 to



 9.5 in the absence of cyanide, the average net specific growth rate  (u) of the



 Anabaena was 0.832  d~^,  which corresponded to a doubling time (tj) of 20  hr.



 The fastest  observed  net  growth  rate was 1.07  d"1 (td=15.6 hr);  the growth



 curve for this batch  experiment  is shown on  Figure  1.  These growth rate



 values were  comparable to growth rates described  by others (Stewart,  1977;



 Fay,  1983;  Bothe, et. al.,  1984).



      The Anabaena did  not survive  in  maintenance  cultures buffered at pH



 values of 10 or greater.



      While the batch growth experiments  yielded actively growing Anabaena



 populations, attempts  to develop steady-state populations of Anabaena in a



 chemostat failed.  The chemostat studies were performed in the same reactor



 and under the same environmental conditions as the batch growth experiments,



 except that a  continuous feed was  added  to the reactor.  When the reactor was



 subjected to a  continuous feed, the concentration of chlorophyll in the



 reactor  decreased at a rate faster than would be  predicted based on the



 hydraulic dilution rate (D) for  the  reactor.



     A typical  response between chlorophyll concentration and time after the



start of feed flow is  shown  on Figure 2.  After 22 hr of flow, the chlorophyll



concentration  in the once-through  reactor increased from 220  to 300 ug chl/L.
                                     19

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           1000
                                        In X • 1.071
                                          r 2. 0.981
2.12
                                   t (day)
                                                           6
Figure 1.   Logarithmic increase in Anabaena biomass (X)  as  function of time,
           during  a  batch experiment.
                                    20

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    300-'
    200"
           0                   30

                                 Time  (hr)

Figure 2.  Changes in Anabaena biomasa (X) versus time after the start of feed
          flow through the reactor.  The dotted line represents the expected
          decrease in X if dilution was the only removal mechanism.
                                 21

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This biomass  increase  was equal to the increase predicted by the average net




specific growth rate (u)  minus the dilution rate  (D),  i.e.,




                             Xt =  XQ exp[(u-D)  t]                          (15)



in which Xt is  the  chlorophyll concentration at time t (ug/L), X0 is the



chlorophyll concentration when flow was started (ug/L), u is the average  net



specific growth rate for Anabaena obtained from the batch growth experiments



(0.0347 hr'1),  D is  the dilution  rate  for the  reactor (0.0211 hr'1), and  t is



the time since  start of flow through the reactor (hr).  Thus, for the  first



22 hr of feed addition, the transient chlorophyll concentrations followed the



predicted growth curve for a  once-through reactor.



     After 22 hr, the transient chlorophyll concentrations no longer followed



the predicted trend.  Instead of continuing to  increase or of plateauing  at a



steady-state value,  the concentration of chlorophyll in the once-through



reactor decreased with time  (Figure 2).  The rate of chlorophyll decrease was



1.5  times greater than the  dilution rate (D).



     Possible explanations for the  observed decrease in chlorophyll



concentrations included an Anabaena die-off or  the presence of a selective



mechanism for removing the Anabaena trichomes from the reactor.  An Anabaena



die-off could have occurred, due either to cell lysis  caused by  the lack  of



nutrients or to a rapid increase in the concentration  of grazers.  Because



Anabaena die-offs did not occur during the batch growth experiments, and



because the batch growth experiments were of longer duration and obtained



higher chlorophyll concentrations  than the situation displayed in Figure 2,



the die-off hypothesis was not  considered a strong possibility.



     The selective removal mechanism explanation was based  on the fact that



the flow exited from the reactor through an overflow weir.  Any mechanism that
                                     22

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 accumulated Anabaena in the neustron or in the upper regions of the reactor
 would have allowed the chlorophyll concentrations to decrease at a rate faster
 than predicted by the dilution rate.  Possible mechanisms  included the
 entrainment of the filamentous Anfbaena on rising air bubbles and the buoyancy
 conferred on Anabaena due to the presence of  gas  vesicles.   An  interesting
 observation was that significant portions of  the  Anabaena  collected in  the
 overflow-collection vessel were buoyant.   However, the observed  buoyancy could
 have arisen from the different environmental  conditions  provided in the
 overflow-collection vessel.
      Regardless of  the  mechanism,  it was not  possible to establish steady-
 state conditions in the once-through  reactor  either  in the presence of  or in
 the  absence of  cyanide.  Chlorophyll concentrations always decreased at a rate
 faster than predicted by  the dilution rate, despite variations in feed flow
 rate,  agitation  speed, air  flow  rate, light intensity, and method of reactor
 start-up.  Because the available reactor could not function as a chemostat for
 the  Anabaena cultures,  the  kinetic coefficients for the degradation of cyanide
 were determined from short-term batch experiments.

TOTAL  CYANIDE REMOVAL RATES
Limitations  of Batch Experiments
     The mixed  second-order rate constants (K^) describing the biologically-
mediated decrease in total  cyanide concentrations by the Anabaena cultures
were  determined via short-term batch  experiments.  The initial objective of
the batch experiments was to provide kinetic information for the setup of the
chemostat experiments.  With inability  of  the available once-through reactor
to establish steady-state conditions, the results of  the batch experiments,  as
the only source of kinetic information,  became more important than originally

                                     23

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intended.



     The short-term batch experiments were performed with Anabaena cultures



that had not previously been exposed to cyanide.  Because the cultures were



not acclimated  to  the presence of cyanide (i.e., the optimal concentrations of



cyanide degrading enzymes were not  developed),  the reported rate constants for



total cyanide removal are probably slower than  would be observed for



acclimated Anabaena cultures.  Another reason why the reported rate constants



underestimate cyanide removal  potential is that the maximum inhibitory effects



of cyanide on respiration and enzyme activity were expressed during a batch



test (i.e., protection mechanisms and pathways  were not  allowed to become



fully operational).   Thus,  a steady-state tertiary cyanide treatment process



utilizing Anabaena should have faster rate constants for the degradation of



cyanide than the reported values.



Rate Constants for Total Cyanide Removal



     The two mechanisms responsible for reducing total cyanide concentrations



during a batch test were biodegradation and  volatilization.  The length of the



batch tests listed on Table 2  was 4 hours, with the exception of batch test 1



which was 5 hours  long.  The extent of biodegradation and volatilization



varied considerably between the batch tests.  With the exception of batch test



1, the extent of cyanide loss due to volatilization increased as the time



averaged pH value decreased.   For  example,  for  batch test 2 with a time-



averaged pH value of 8.44, 1112 ug CN was volatilized,  while the amount of



cyanide volatilized during batch test 3 with a  time-averaged pH of  9.5 was 138



ug CN.   This was the expected  result, because as pH dropped the fraction of



cyanide existing as volatile hydrogen cyanide increased.  In contrast, the



extent of biodegradation increased as the time  averaged pH value increased
                                     24

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             TABLE 2.  EXTENT OF BIODEGRADATION AND VOLATILIZATION
                         IN SELECTED BATCH EXPERIMENTS



Batch
Number
1
2
3
4*
5**


Time
Ave.
PH
9.59
8.44
9.50
9.00
9.00
Initial
Biomass
*o

(ug chl/L)
412
4926
203
560
367
Total
Mass CN
Removed

(ug CN)
752
1188
443
360
583
Volatilized
Mass of
Cyanide

(ug CN)
534
1112
138
324
410
Biodegraded
Mass of
Cyanide

(ug CN)
218
76 .
305
36
173
           *   media  for this  batch test  included 0.5 ppm  thiosulfate

          **   re-exposure  of  biomass  in  batch test #4 to  cyanide and
                thiosulfate
(for this observation ignore batch test 5, which is a batch test examining the

potential for acclimation).  For example,  at a  time-averaged pH of 8.44  (batch

test 2), biodegradation accounted for the removal of 76 ug CN.  At a time-

averaged pH of 9.5 (batch test  3),  biodegradation  accounted for the removal of

305 ug CN.  Batch test 3 had a greater extent of biodegradation than batch

test 2, despite it having only 4% of the biomass.  These observations suggest

that pH played an important role in determining rate of total  cyanide removal,

whether the removal mechanisms was predominantly  by volatilization or by

biodegradation.

     The biodegradation and volatilization rate constants  in equation (3) were

determined from a computer algorithm.  The resulting rate constants provided
                                     25

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the simultaneous best fit of two sets of data:  the decrease in cyanide
concentration with  time  in  the  reactor  and  the  mass of  cyanide collected in
the gas-wash bottle.  The calculated Kb and Yi^a values  for batch tests 1
through 4 are listed on Table 3.  As shown on Figure 3  for batch test 3,  the
calculated values of Kj, and K^a described the decrease  in total cyanide
concentration.   Similar fits of the data were obtained  for the other batch
tests.
TABLE 3. OVERALL VOLATILIZATION RATE CONSTANTS (Kia) AND MIXED SECOND-ORDER
RATE CONSTANTS (KO FOR TOTAL CYANIDE REMOVAL BY UNACCLIMATED ANABAENA
CULTURES IN SELECTED BATCH EXPERIMENTS
Batch
Number
1
2
3
4*
Time
Averaged
pH
9.59
8.44
9.50
9.00
Time
Averaged
ALPHA
0.339
0.879
0.387
0.666
KLa
(hr-1)
0.17
0.22
0.052
0.075
Kb
[L/(ug chl hr)]
8.5-10-5
5.0-KT6
2. 2 -10-*
8.0- 10'6
           *  media for this batch test included 0.5 ppm thiosulfate

     Examination of Table 3 indicates  that the fitted  values  of  Kb  and
varied considerably between the 4 batch tests.  Because the effect  of temporal
changes in pH on volatilization rates  were accounted for by the  ALPHA term  in
equation (3),  the 4-fold variation in the calculated K^a values was due  to
differences in aeration rates and agitation intensities.  These  differences
existed, despite the mechanical settings on the experimental  reactor being  the
same for each batch test.
                                     26

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   3300
u
53
   2900
   2500
                                                    O sample
                                                    — equation (3)
                                   2           3
                                     Tim® (fw)
  Figure 3.  Decrease  in total cyanide concentration (S) during batch test
            number 3.  The line represents the numerical solution of equation
            (3) using the Kb and KLa values on Table 3.
                                    27

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     The mixed  second-order biodegradation rate constants (Kb)  for  the

unacclimated  Anabaena cultures ranged from  5.0-10~6  to  2.2-10'4 L/(ug chl hr).

This observed 44-fold variation in the Kb  values appeared to be a function of

pH.  As shown on Figure 4,  the biodegradation  rate constant increased as  the

time-averaged pH for  each batch test  increased.  The  observed relationship

between Kb and  the time-averaged pH value was approximated by the following

linear regression:

                            log Kb «, 1.44 ^H -  17.7                         (16)

                                  r2  = 0.836

in which Kb has the units L/(ug chl hr),  pH is the time-averaged pH value for

the batch test,  log is the base 10 logarithm, and r2  is the square  of the

linear regression  coefficient.

     Because Kb values increased as the time-averaged pH  increased,  the

observed Kb values were probably responding to  ALPHA,

                                        [HCN]
                            ALPHA =	                        (4)
                                    [HCN] + [CM~]

Since the initial total cyanide concentration for the batch tests were similar

(aprox. 3000  ug  CN/L), comparing Kb to the time-averaged ALPHA value would

indicate the effect of HCN on biodegradation rates.  The observed relationship

between Kb and the time-averaged ALPHA value suggested that for smaller

concentrations of HCN the rate of total cyanide biodegradation  by the Anabaena

cultures Increased (Figure 5).   The relationship between Kf, and ALPHA was

approximated by the following linear  regression:

                          log Kb = -2.91 ALPHA - 2.88                       (17)

                                  r2  - 0.862

in which ALPHA  was calculated from the time-averaged pH for each batch test.
                                     28

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             •4-
                      log Kb=l.44pH-l7,7
                          r2 » 0.836
Figure A.   Relationship between log Kb [L/(ug chl hr)]  versus
          time-averaged pH.
                                29

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                                           log Kh--2.91 ALPHA
                                                      -2.88
                                               r2a 0.862
Figure 5.  Relationship between log Kb [L/(ug chl hr)] versus
          time-averaged ALPHA.
                                 30

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     The  rate  at  which unacclimated Anabaena cultures reduced total cyanide



 concentrations was optimized by reducing the fraction of  the cyanide that



 existed as HCN (reduced ALPHA value).  This  observation is consistent with  the



 concept that HCN  is more toxic and inhibitory than CN~ (Doudoroff,  et al.,



 1966;  Doudoroff,  1976).  The  ALPHA value is  smallest  at pH values greater than



 the pKa for HCN.   Operating a reactor  at pH  values above  the pKa for HCN also



 reduces the rate  of volatilization.  These factors suggest that the



 biodegradation efficiency of  a  cyanide-treatment  process  based on nitrogen-



 fixing cyanobacteria would  increase  as the pH of  the  system  is increased.



 This improvement  in reactor efficiency with  pH would  occur only up  to pH



 values of  10,  because Anabaena  culture did not survive at pH values greater



 than 10.



     The maximum  observed Kb for the degradation  of cyanide  by unacclimated



 Anabaena cultures is  larger than the mixed second-order rate constants for



 existing biological  treatment processes.  Converting  the observed K^ for batch



 test 3 into  units of L/(mg VSS  d)  where  VSS  is volatile suspended solids, the



 maximum observed  rate constant was 0.0195 L/(mg VSS d).  In  comparison, the



 biodegradation  of  acetate by  methanogens (i.e., anaerobic heterotrophs that



 produce methane) can have a mixed  second-order rate constant of 0.0054



 L/(mg VSS d) (Rittmann and McCarty,  1980).  Thus,  the biodegradation of



 cyanide by unacclimated  Anabaena cultures can  have faster rate constants than



 the biodegradation of acetate by methanogens.  The observed  net specific



growth rate  for Anabaena under  optimum conditions was 0.832  d  ,  while the



 maximum specific growth rate  for the acetate-utilizing methanogens was



reported  as  0.25 d~* (Rittmann  and McCarty,   1980).  Because  Anabaena can have



faster  growth rates and contaminant removal  rates than methanogens,  and
                                     31

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because successful wastewater treatment facilities have been developed using
methanogens-,  there appears to be no kinetic limitation for the development of
biological treatment  processes  utilizing  Anabaena.  However, other factors may
limit process development, such as  construction costs.  As with the anaerobic
treatment of  wastes with suspended  microorganisms,  large reactors may be
required to provide adequate  cyanide removal and  to ensure  process  stability.
Effect of Acclimation on Cyanide Removal Rates
      By re-exposing an Anabaena culture to cyanide,  the impact of acclimation
on biodegradation rates was assessed.  Batch test 5 was a repeat of batch test
4 (Table 2).   Thiosulfate (0.5 ppm) was  added to the culture media used in
batch test 4  to induce the production of rhodanese, the enzyme that catalyzes
the formation of thiocyanate  from free  cyanide and  thiosulfate.  The addition
of thiosulfate was assumed to have  no effect on the K^  value for batch test  4.
However, the  induction of rhodanese  and other detoxification pathways during
batch test 4,  were expected to  increase the rate of total cyanide removal
during batch  test 5.   Comparison of the Kj, values for batch tests 4 and 5
would indicate the difference in cyanide biodegradation kinetics between
unacclimated  and acclimated Anabaena cultures.
     Several hours after completion of batch test 4, aeration and agitation
were shut off in the experimental reactor.   The Anabaena was allowed to settle
overnight.  The next morning  the supernatant was siphoned off and replaced
with new culture media containing thiosulfate.   Aeration and agitation were
restarted.  Two hours  later, the acclimated Anabaena culture was subjected to
a second cyanide batch experiment.
     The acclimated Anabaena culture reduced total cyanide concentrations 12
times faster  than the unacclimated  Anabaena culture (Table 4).  The acclimated
                                     32

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    TABLE 4.   COMPARISON OF MIXED SECOND-ORDER RATE CONSTANTS (Kb)  FOR TOTAL
     CYANIDE  REMOVAL BY UNACCLIMATED (BATCH NUMBER 4)  AND ACCLIMATED (BATCH
             NUMBER 5)  ANABAENA CULTURES IN PRESENCE OF THIOSULFATE


Batch
Number
4
5
Time
Averaged
pH
9.00
9.00
Time
Averaged
ALPHA
0.666
0.666
KLa
(hr-1)
0.075
0.085
Kb
[L/(ug chl hr)]
8.0-10-6
1.0- 10~4
Anabaena  culture  (batch test 5) had a mixed  second-order  rate  constant (K^)  °

1.0-10~4 L/(ug  chl hr),  while KJJ for the unacclimated Anabaena culture (batch

test 4) was 8.0-10~6 L/(ug chl hr).

     Thus,  when an Anabaena culture  has time for the induction of rhodanese

and other enzymatic  pathways,  the rate  constants  for cyanide biodegradation

increase.  Because the Anabaena in an operating cyanide-treatment process

would be acclimated  to a steady-state cyanide concentration, the rate

constants for cyanide biodegradation would likely be faster than those listed

on Table  3.


METHANE PRODUCTION RATES

Rate Constants for Methane  Production

     For the methane production data shown on Figure 6, an unacclimated

Anabaena culture  (Xo»1146 ug chl/L) produced  14  ug  CH^/L  (gas  phase)  in 1.75

hours when  the initial  total cyanide concentration  in the vial was  31.2

ug CN/L (water phase).  This amount of methane production corresponded  to the

reduction of 11.0 ug CN/L (water phase)  by nitrogenase in 1.75 hours.   The

ability of nitrogen-fixing  cyanobacteria to reduce cyanide concentrations


                                     33

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      16
   3Q-T
   u
                                          I
                                      Tim«  (hr)
Figure 6.  Increase in headspace methane concentration with time.  For the
          illustrated batch test,  the initial cyanide concentration was

          31.2 ug CN/L.
                                   34

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 below 20 ug/L may be significant, because no cyanide destruction process
 has demonstrated the ability to reduce total cyanide concentrations to
 levels less than 25 ug/L (Brunker, 1980).   Thus,  nitrogen-fixing
 cyanobacteria may be well suited for  use in the  secondary or tertiary
 treatment of cyanide wastes.
      The suitability of utilizing the nitrogen-fixing capacity of
 cyanobacteria to treat  small concentrations of cyanide can be related to the
 mechanism by which nitrogenase  synthesis is regulated.  Nitrogenase synthesis
 is  induced by the lack  of ammonia (Stewart, 1977; 1980).   Thus,  the
 intracellular concentration of nitrogenase  is not a  function of substrate
 concentration (N2 or HCN),  but is a function of product concentration
 (ammonia).  By promoting the active growth  of cyanobacteria,  ammonia is kept
 in  short supply, which  results in the maintenance of maximal levels of
 nitrogenase  (Stewart, 1977),  regardless  of  cyanide concentration.   In
 constrast  to  nitrogenase, the synthesis  and maintenane of high intracellular
 concentrations of  rhodanese is a function of cyanide concentration (Atkinson,
 1975;  Atkinson,  et al.,   1975; Brunker, 1980).  The ability to maintain maximal
 activity levels  of nitrogenase at  low cyanide concentrations implies that
 nitrogenase may  be more effective in  the removal of low levels of  cyanide than
 cyanide-induced  enzymatic  pathways.
     The determination  of  the rate constant for the  reduction of cyanide by
 nitrogenase required the calculation of  the mixed second-order rate constant
 for the overall  removal of  cyanide from  the vial.  As the pH in  the vial  was
 10,  the value of mixed  second-order rate constant for  the  total  cyanide
 removal  rate  (Kb)  calculated from equation (17) was  4.33'10~* L/(ug chl hr).
This Kb value was used  in equations (13) and (14)  to  calculate the  mixed
                                     35

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second-order  rate  constant  (Kn)  for  the reduction of cyanide by nitrogenase.
For the methane production shown in  Figure 6,  the calculated Kn  value  was
2.58-KT4 L/(ug  chl hr).
     A quick  comparison of  the  calculated Kn and Kb values would suggest that
for an initial cyanide concentration (S0) of 31.2 ug CN/L,  the rate  of HCN
reduction by  nitrogenase  accounted for 60% of the total cyanide  removal rate.
One problem with this comparison is  that  the calculation  of Kb ^ro°  equation
(17) assumes  that  SQ 13 approximately 3000 ug  CN/L.   Because the value of Kb
was found to  increase with decreasing HCN concentration,  the use of  equation
(17) in the analysis of above methane  production experiment may  greatly
underestimate Kb.   Fortunately,  the  Kn value obtained from equations  (13) and
(14) was relatively insensitive  to changes in  Kb.   For  inputted  total  cyanide
biodegradation rate constants (Kb) ranging from 2.58-10~4 (all cyanide removal
due to nitrogenase)  to  I.O'IO"-*  L/(ug  chl hr)  (only 5% of  original cyanide
remained in reactor after 1.75 hr), the Kn values obtained  from  equations (13)
and (14)  only varied by a factor of  2 (Figure 7).   For  the inputted  range of
Kb values,  the ratio of nitrogenase  activity to  total cyanide  biodegradation
rates (Kn/Kb) ranged from 0.39  to  1.00 (Figure 8).  These  calculations suggest
that the reduction of HCN  to methane by nitrogenase is a significant mechanism
of cyanide biodegradation for unacclimated Anabaena cultures exposed to low
cyanide concentrations (SQ-31.2  ug CN/L).
     As the initial concentration  of  cyanide increased, the mixed second-order
rate constant for  nitrogenase activity (Kn)  appeared to decrease.  For a
methane production experiment with an initial cyanide concentration (SQ) of
400 ug CN/L and a  pH of 9.9, the calculated  Kn value was 2.62-10~6
L/(ug chl hr). This Kn value was 2 orders of magnitude slower than  the Kn
                                     36

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.0004- •
.0002- -
      -3.75
—I—
  -3.35
 log Kb
-235
Figure 7.   Sensitivity of Kn obtained from equations  (13) and (14) to inputted
          Kb values.  Both parameters have  units of  L/(ug chl hr).
                                37

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 i.o-
0.3
  oH—
   -3.73
                                 -3.33
                                 log
-2.95
Figure 8.  Sensitivity of the ratio between Kn and Kb to inputted
          Both parameters have units  of L/(ug chl hr).
                                                                  values.
                                    38

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 value calculated when SQ was 31.2 ug CN/L.  The decrease  in Kn with  increasing
 S0 was probably due to HCN  inhibition of  the ATP generating pathways in  the
 heterocysts,  because cyanide at  the  experimental concentrations has  no effect
 on the rate of electron flow through nitrogenase  (Li, et al.,  1982).  Thus,
 the effect of cyanide concentrations on Kn may diminish with acclimation.
 Comparison of Methane Production with Nitrogen Fixation
      The observed rate of HCN reduction (methane production) by nitrogenase
 was compared to literature  values of dinitrogen  (^)  reduction rates.  The
 dinitrogen reduction rates  were  converted to HCN reduction rates based on
 three assumptions.   First,  the rate  of electron flow  through nitrogenase is
 independent of  HCN  concentration, so  that the rate of electron flow  for
 nitrogen fixation is assumed  equal  to electron flow  for HCN reduction (Li, et
 al.,  1982).  This is a reasonable assumption for the experimental conditions
 described above.  Second, all of the cyanide inside the heterocyst is in the
 form  of  HCN.  This  is a reasonable assumption, because the pH inside of a
 heterocyst is 7.3 (Stewart,  1977), two pH units below the pKa for HCN.  Third,
 for each  mole dinitrogen  reduced there is the simultaneous reduction of 2
 protons  to make 1 mole of hydrogen  gas, i.e.,  8 electrons  must flow through
 nitrogenase for each mole of N2  fixed.  This is a conservative estimate of the
 moles of  H2 produced per mole of ^2  re^uced by nitrogenase (Burris and
Peterson, 1978; Lean, et al., 1973;  Postgate, 1982; Fay,  1983; Bothe, et al.,
 1984).
      Ramos, et  al.,  (1987) reported  that an Anabaena culture had a maximum
specific dinitrogen  reduction rate of 30  umole N2/(mg chl hr).   Based on the
above assumptions,  this corresponded to a  calculated  maximum specific HCN
reduction  rate (k) of 1.08 ug HCN/(ug chl hr).   This maximum rate  was adjusted
                                     39

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to account for the effect of ambient HCN concentrations by  the  following
modified Monod equation:
                                        k S
                                rHCN	                            (18)
                                       Km + S
in which FHCN is  the specific  HCN reduction  rate [ug  HCN/(ug chl hr)], k  is
the  maximum specific HCN reduction rate [1.08 ug HCN/(ug  chl hr)], S  is  the
ambient  HCN concentration (ug HCN/L),  and  Km  is the Michaelis-Menten  constant
for  the  production of methane  from HCN by nitrogenase (121,500  ug  HCN/L)  as
reported  by Li, et al.f (1982).  This  Km value included both the effect  of
enzyme affinity for  HCN and  of H2 production  on  r^of.  Because Km  is  much
larger than the ambient cyanide concentrations used in the methane production
experiments,  equation (18) can be reduced to
                                       k
                                rHCN = — S                               (W)
                                       Km
in which k/Km has the value 8.9-10~6  L/(ug chl hr).   Equation (19) is
equivalent to  the following  rearrangement of equation (8):
                                   1 dP
                                 	*„ S                             (20)
                                  X0dt
in which  K,, is the experimentally-derived mixed  second-order rate  constant for
the production of methane by nitrogenase  [L/(ug chl hr)].   The calculated k/Km
value was compared to the experimentally-derived Kn values.
     The observed values of Kn ranged from 2.62-10~6 L/(ug chl  hr)  when S0 was
400 ug CN/L to 2.58-10-4 L/(ug chl hr) when SQ was 31.2 ug CN/L.  The
calculated k/Km value of 8.9-10~6  L/(ug chl hr) lies between the two  observed
&n values.  Thus,  the observed  rates of methane production were reasonable
compared  to known in. vivo nitrogen-fixation rates and in,  vitro HCN reduction

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 rates.




      The observed Kn value for So=31.2 ug CN/L was almost 30 times larger than



 the calculated k/Km value.  This  suggests that Anabaena may  reduce  low



 concentrations of HCN at a more rapid rate than dinitrogen.   Such a conclusion



 agrees with the observation by Li, et al.,  (1982) that the activation



 requirements for nitrogenase to reduce HCN are  lower than the activation



 requirements to reduce dinitrogen. Because lower activation energies  usually



 translate into faster kinetics,  nitrogenase will preferentially reduce HCN.



 Thus,  if nitrogenase's  requirements for  ATP and  electrons can be continuously



 satisfied,  then the enzymatic apparatus in  Anabaena  normally responsible  for



 nitrogen-fixation may play an important  role in determining  the rate at which



 low concentrations of cyanide are biodegraded in a treatment process.  In the



 methane production experiments with So»31.2 ug CN/L,  the  rate of nitrogenase



 activity  was responsible for  at  least 39% of the total cyanide biodegradation



 rate (Figure 8).





 APPLICATION  OF  KINETIC  DATA TO CYANIDE TREATMENT



     The  purpose of this section is to predict the strength of a cyanide  waste



 that can  treated by a process  utilizing  suspended cultures of nitrogen-fixing



 Anabaena.  This prediction will assume steady-state conditions in a once-



 through competely-mixed reactor.   Because the kinetic data collected in this



 study were not  obtained under steady-state conditions, application of  the



 following discussion  to the design of an operating cyanide treatment process



 should be done  with  great  caution.



     Assuming mixed second-order  biodegradation kinetics and ignoring



 volatilization, the mass balance equation for cyanide in a completely-mixed



once-through reactor is as  follows:





                                     41

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                             dS
                           V_=QS1-QS-KbXS                      (21)
                             dt
 in  which V is the volume of the reactor (L),  S  is  the concentration of cyanide
 in  the  effluent  and  in  the reactor  (ug CN/L), SA is  the  cyanide concentration
 in  the  influent  (ug CN/L), t is time  (hr), Q is the volumetric  flow rate
 through the  reactor  (L/hr), X is the  concentration of Anabaena  in  the  reactor
 (ug chl/L), and Kb is the  mixed second-order  rate  constant  for  the
 biodegradation of cyanide  by Anabaena [L/(ug  chl hr)].   Under steady-state
 conditions  (i.e.,  dS/dt=0 and dX/dt=0),  the influent  concentration can be
 described by
                             S4 = S [1 +  Kb X 9]                           (22)
 in  which 9  is the hydraulic retention time (hr) and  is equal to V/Q.   Thus,  by
 assigning values  of  S, Kb, X and 9, the strength of the  cyanide waste  can be
 estimated  from equation (22).
     In  predicting the influent cyanide concentrations that can be treated by
 an Anabaena process,  the following parameters were assumed:
               pH - 9.5               temperature -  25°C
               X  = 500 ug  chl/L       S - 300 ug CN/L
               9  - 120 hr             Kb  = 0.00022 L/(ug chl hr)
The values of the above parameters  are considered  to be  conservative.   The
value of S is an  order of  magnitude smaller than the cyanide concentration at
which Kb was  determined.  The above Kb value assumes  an  unacclimated Anabaena
culture, under steady-state conditions Kb should be  larger.  The biomass
concentatlon (X)  is an order of magnitude  smaller than the  highest
concentration observed in  the experimental reactor.   A 9 of 120 hr (5  days)
provides a safety factor of 10 above  the average net  specific growth rate for
                                     42

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 Anabaena.   Substitution of the above parameters into equation (22) yields a SA
 of 4260 ug CN/L (4.26  mg CN/L).  Thus,  if a  steady-state  Anabaena
 concentration of 500 ug chl/L can be maintained in a chemostat  with a
 hydraulic retention time of 5 days, then the reactor should  be  able to reduce
 an influent cyanide concentration of 4.26 mg/L to  an effluent concentration of
 0.3 mg  CN/L,  a 93 percent reduction.  As the rate  of cyanide biodegradation is
 first-order with respect to cyanide concentration  (equation  22),  similar
 removal efficiencies should be observed for  lower  influent cyanide
 concentrations.
      The above calculations predict that a chemostat with a  hydraulic
 retention time (0)  of  5  days  is required to  achieve a 93% reduction in
 cyanide.  For some  cyanide-waste  generators,  the costs associated with the
 construction  of  a reactor large enough  to hold the volume of wastes generated
 in 5  days may be prohibitive.  However,  the  volumetric size  of a  cyanobacteria
 reactor could be reduced by using methods to make the mean cell residence  time
 (Oc) larger than the hydraulic retention time (0).
     One possible method for  increasing Oc involves the recycling of
 cyanobacteria biomass  in the effluent line to the  reactor.  The activated-
 algae reactor was originally proposed by McGriff and McKinney (1971).   The
 success  of the activated-algae reactor  is dependent on the ability to separate
 algal cells from the reactor effluent by settling.   Despite  the presence of
 gas vesicles, cyanobacteria will sink when their growth is limited by fixed
 nitrogen availability  (Kleiner,  et  al.,  1982).  Because nitrogen-fixing
cyanobacteria only  produce one mole of  ammonia per cyanide reduced instead of
 the two obtained from  dinitrogen, the availability of nitrogen may limit
cyanobacteria growth rates  in  reactors  used  to treat cyanide wastes.  While
                                     43

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cyanobacteria may  sink,  the  potentially-slow  settling  velocities of the



filamentous nitrogen-fixers  might  require clarifiers with  large surface  areas.


Thus, the reduction in construction costs for the activated-algae reactor


compared to a chemostat could be partially negated by the construction costs


for  a clarifier.


     Another method of increasing  9C would be the use of attached-growth


reactors instead of suspended-growth chemostats.  By growing cyanobacteria on


attached media steady-state  concentration of biomass becomes less dependent on


hydraulic flow rates.   One problem with a cyanobacteria biofilm reactor is


assuring that sufficient light intensity reaches all of the cyanobacteria


biofilms.  If the light availability problem can be solved, then the



combination of the large QC  associated with biofilm reactors and the ability


of nitrogenase to detoxify trace-concentrations of cyanide suggests that a


nitrogen-fixing cyanobacteria biofilm reactor would be well suited for the


secondary or tertiary treatment of cyanide wastes.


     In addition to providing adequate mean cell retention times,  another


concern is protecting  the cyanobacteria from fluctuations in cyanide


concentration.  Despite the acclimation of a microbial process to a given


cyanide concentration,  small short-term increases in cyanide concentrations


can be inhibitory to the microorganisms and, thus, disrupt the microbial


process (Gaudy,  et al., 1982).  One means of protection is  to  dampen the


magnitude of the influent cyanide concentration fluctuations by primary


treatment of the cyanide  wastes before biological treatment.   Primary
                                       «

treatment of the cyanide wastes would  also reduce the cyanide load to the


cyanobacteria process.  Thus, the  steady and small concentrations of cyanide


in the effluent of an  alkaline-chlorination or other primary treatment process
                                     44

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would be conducive to the maintenance of cyanobacteria in a secondary




treatment process.  Utilization of nitrogen-fixing cyanobacteria to detoxify



the last fraction of cyanide, instead of attempting to treat all of the



cyanide by the primary process, should result in lower operating costs for



larger cyanide treatment facilities.
                                    45

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