UNIVERSITY of ALASKA
       COLLEGE, ALASKA 99701
      INSTITUTE OF MARINE SCIENCE
 Biological Effects  of Copper
    and Arsenic Pollution
      Cont. 18050 DLW
R71-8

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                      INSTITUTE OF MARINE SCIENCE
                         UNIVERSITY OF ALASKA
                            COLLEGE, ALASKA
          BIOLOGICAL EFFECTS OF COPPER AND ARSENIC POLLUTION
                             Prepared by

                     D.  K. Button and S. S. Dunker
                Principal Investigator:  D. K. Button
                         Final Report to the

                    Environmental Protection Agency

                        Contract No. 18050 DLW
Report No. R71-8                                                 D. W. Hood
April 1971                                                       Director

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                               ABSTRACT





     Inhibitory effects of copper toward marine microorganisms were studied.



Phosphate was found to prevent copper inhibition.  An organism capable of



metabolism at low phosphate concentrations was selected.  Growth and phosphate



flux kinetics were described.  These phosphate limited systems were found  to



be copper sensitive only under conditions of manganese deficiency.  Toxicity



occurred in this normally rather resistant yeast and in hydrocarbon oxidizing



microorganisms at about 10   M.  The protective influence in reagent grade



phosphate was traced to its usual contamination with trace amounts of manganese.



     Among a number of metabolic inhibitors found to inhibit phosphate transport



was arsenate.  Phosphate also competitively reduced arsenate uptake.  Reduced



phosphate uptake rates occurred at 10   M arsenate and high death rates in



cultures otherwise sustaining normal growth rates were Induced with 10"


     —8
to 10   M arsenate in phosphate deficient systems.  These levels are exceeded



in environmental and potable water systems.



     Evidence is presented consistent with the view that both arsenate and



phosphate are accumulated by the same active transport system.  The system



is peculiar in that velocities increase as the hydrogen ion is increased,



saturation of the system does not occur, and the transport temperature



coefficient is very large.



     Evidence suggests that both arsenate and copper are important at existing



concentrations in the environment.  When nutrients are dilute these anti-



metabolites prevent microbial metabolism thus affecting the steady state



chemistry which they control.



     It is abundantly clear that toxicity levels of antimetabolites depend



not only on populations and chelate concentrations but in a major way on free



nutrients and trace metal levels.

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                             INTRODUCTION






     It is well known that phosphate is actively accumulated by many




organisms (Blum, 1966; Goodman and Rothstein, 1968) and that the accumulation




is directly effected by arsenate  (Mitchell, 1964; Jung & Rothstein, 1965).




However little data exists describing phosphate incorporation kinetics in




the concentration range found in natural water systems.  One reason for




this is that organisms with the capacity to live in low phosphate natural




systems have sufficient affinity and capacity to satisfy their growth require-



ments at less than the usual background phosphate content of chemically defined




laboratory media.  This paper describes a method to handle nutrient uptake




kinetics and suggests that environmental levels of arsenate are such that




they make this phosphate analogue an important antimetabolite in population




dynamics.



     That heavy metals such as copper are inhibitory is also well known (Breslow



and Girotti, 1966; McBrien & Hassall, 1965; Steemann-Nielsen & Uiura-Anderson,




1969; Steeman-Nielsen & Wium-Anderson, 1970; Nielsen, 1969; Cabadaj & Gdoven,




1970; and Grande, 1966).  This paper further describes the strong influence the




availability of divalent metabolites such as manganese has on the level at which




copper becomes inhibitory.  Implications of the combined influence of these




antimetabolites are discussed.








                               METHODS






     A marine yeast was selected from the collection of Dr. K. Natarajan,




Institute of Marine Science, University of Alaska, on the basis of ease of growth




on low phosphate medium.  This pink yeast was isolated from Amukta Pass near




the Aleutian Islands.  It was found to be nitrate positive, lactose negative,




asporogenous and otherwise similar to Rhodotorula rubra.

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                                   -2-
     As with most yeasts the sodium chloride concentration  did not  affect



maximum growth rates and was maintained low for chemical  simplicity.  Other


constituents were maintained at near limiting values for  the  rather low



populations employed.  The constituents of the medium were  (per  liter):



glucose, 5 mg; NaCl, 40 rag; KC1, A mg; NH^SO^ 1 mg; MgSO^, 2.5  mg; CaCl2  •



2 H20, 5 mg; ZnSO^ • 7 H20, 70 yg; Fe(NH4>2S04 • 6 H20, 50  yg; MnS04  • 7 H20,



15 pg; Co(N03)2 • 6 H20, 0.15 ug; vitamins B^ B12 and biotin, 10~10 M in



distilled water followed by filtration.  Continuous culture was  in  a single



phase 250 cc stirred glass reactor at 25°C as previously  described  (Button


and Carver, 1956).



     Limiting substrate concentration and growth rates in continuous culture



were calculated from the usual relationships (Button, 1969) modified to


analyze conditions where limiting substrate concentration S is low  and ap-



proaches the quantity supplied as impurities in the feed  S..  Thus  at steady
state:
                               (Sa - Sb - S)                                (1)
where X is the cell population and Y the yield constant.  The yield constant



can be determined graphically from cell population at a range of added substrate



values according to equation 1 where S and S,  are constant.  The value of S,
                                            D                              b


is then given by the steady state population X,  when S  is zero.
                                              D       cl





                           Xb = Y (Sb - S)                                  (2)





A portion of added substrate was isotopically labeled so that the radioactivity



ratio, R, of extracellular steady state reaction medium to total isotope



concentrations gives S from the concentrations S  and S, :
                                                a      b




                           S = R (Sa + Sb)                                  (3)

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                                   -3-
     Substituting S, from equation 2 into equation 3 and solving for S:





                               R (S  -

                          S =  	rS—-
     The background substrate concentration S, was evaluated at the beginning



of each experiment according to equation 2.  The portion of total substrate



remaining outside the organism at steady state R was determined by a rapid



separation procedure.  Reactor contents were withdrawn with a syringe fitted



with a two way valve which allowed immediate filtration separation of the



dilute yeast population from surrounding medium.  The single phase reactor was



fitted with a temporary filtered air source to replace removed liquid during



sampling so that the sample was not diluted with unreacted feed.  The medium



supply system was shut down for a sufficient period to prevent rapid replacement



of the removed sample volume from appreciably disturbing the steady state.



     Initial rates of uptake were measured from the slopes of organism radio-



activity with respect to time, usually over a six minute period.  When the


                  -4
pH was altered, 10   M Tris buffer was added to the medium, otherwise similar



to that described.  Organisms for these experiments were provided by a phosphate



limited continuous culture at half maximum growth rate operated solely for this



purpose.  These systems were cleaned where necessary by exposing to a fresh



phosphate limited culture for phosphate scavenging.  No phosphate precipitates



or radiochemical exchange with the glassware could be detected below pH 7.0


                                                                    32
according to microfiltration and long term storage experiments with   PO,



labeled medium.



     Cell mass and volumes were calculated from an integration of electronic



counter and plate count population, size distribution and total volume from



electronic counter data, microbalance determination of dry weight in evacuated



heated chambers and checked by comparison vrlth glucose limited continuous

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                                   -4-
cultures according to the equation X = y  (S  - S)  (Button, 1969) where cell


yields, steady state populations and the  glucose distribution is known.


     A gamma spectrometer was used to count arsenate, scintillation or planchett


counting was used to count   P depending  on the radioactivity available.  Usual


scintillants and precautions were used throughout.




                               RESULTS



     During steady state growth phosphate controls growth velocity between

               _a
zero and 2 x 10   M at pH 4.0 as shown in Fig. 1.  The flux of phosphate


through the cell membrane can be calculated from initial uptake experiments


at concentrations greater than sufficient to achieve the maximum growth rate


of the organism, and thus measure the capacity of the phosphate transport


system.  This flux is shown in Fig. 2.  Arsenate is incorporated in a similar


manner and arsenate flux is also shown as calculated from initial uptake data.


Line slopes are approximately one throughout, indicating absence of a


saturation mechanism.  This lack of saturation indicates diffusion limitation


of phosphate and arsenate transport so the system was examined for an active


transport mechanism.  Recent data show that phosphate and arsenate show the


same affinity for the cell.

     As shown in Fig. 3 plunging cells exposed to 10   M phosphate into higher


concentrations loads the cells to such an extent that previously formed

phosphate pools leak out.  Preliminary experiments with high concentrations of


phosphate suggested this from the fact that initial uptake rates were very


high for the first minute, and then total radioactivity incorporated into the


cell decreased.


     Exchanged phosphate amounts to a minimum concentration of 5 x 10~  M


inside the cell concentrated from the 10   M external solution.  The actual


pool size is probably much larger, since  all free phosphate would not be expected

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                                   -5-
be  the case.   In  fact,  toluene  completely  stopped  phosphate incorporation

as  shown in Table I.
                               Table  1
                     Phosphate Uptake Inhibition
Inhibitor
_
Toluene

NaN3
1AA
DCCD
AsO."3
A
AsO,"3*
Q
Concentration
_

_5
10 M
10"5 M
10"5 M
10~7 M

10~7 M
10"8 M
Uptake rate
M/g cells/rain
12.6


1.6
8.7
11.3
4.3

0.4
5.1
Inhibition
0
100

56
31
12
36

94
20
     *10 minutes pretreatment with inhibitor
     Metabolic Inhibitors such as sodium azide were found to be inhibitory,

however, N, N-dicyclohexyldicarbodiimide (DCCD), a bound adenosine tripho-

sphotase inhibitor, was found to be relatively Ineffective.  Since this system

does appear to be an active transport system of sorts, ATP does not appear

to be involved as suggested above and phosphoenol pyruvate is thought to

drive some sugar transport systems, iodacetate was tested.  It is a well known

inhibitor of glyceraldehyde-3-phosphate dehydrogenase, a step preceding

phosphoenol pyruvate formation.  The degree of inhibition was some three times

that of DCCD at 10   M and it is conceivable that phosphate transport is

driven by this glycolytic intermediate.

     Most striking was the inhibition of phosphate transport by arsenate, a

phosphate analogue.  Arsenate treated cells yielded only 6% of control activity

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                               -6-
Fig. 1.  Steady state phosphate concentration as a function of
         growth rate.  Growth rates were calculated from continuous
         culture dilution rate and viability data.  The maximum
         growth rate w    is 0.175 hr~ .  Phosphate concentrations
         are calculated from extracellular radioactivity according
         to the relationship
                          R
                      s
         Data spread is shown as standard deviation from the results
         of approximately 10,000 hours of continuous culture operation
         data.

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  1.0
  .75
o .50
  .25
                     STEADY   STATE
                       PHOSPHATE
      I          2
PHOSPHATE,  M x I08
                                 10,000

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                            -8-
Fig. 2.  Arsenate and phosphate uptake as a function of



         concentration.  Solid symbols from initial uptake



         data, open symbols from steady state continuous



         culture data.  Velocity units, moles per mg cells



         dry wt per minute; concentration, molar.

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    8
CD
O
    10
   12
         10
              PHOSPHATE
  8


LOG
         ARSENATE

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                              -10-
Fig. 3.  Phosphate removed from cells by plunging cells




         equilibrated with 10~  M phosphate into higher




         concentrations to allow free or pool phosphate to




         exchange back out.  The first column shows radio-




         activity incorporated from labeled phosphate*  The




         second column shows the concentration of cold




         phosphate and the third column shows the phosphate



         radioactivity remaining in the filtrate as an



         indication of phosphate removed from the original




         concentration supplied.

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     PHOSPHATE   POOLS
          OOOO
          _Q_Q_QP..
     • '
        PO,
UPTAKE
                 / o
      COLD
      P04
                               COUNT
                             COUNT
EXCHANGE
  PQ4
PC,  REMOVED
 MOLES  XIO12
1723
1469
1270
333 *
288 *
IO'7M
lo-4
JO"2
lO'7
ID"2
2.7
5.5
5.6
2.5*
2.3*
      * HEAT  KILLED CONTROL

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                                   -12-
to exchange back out.  Hot ethanol as well as trichloracetic acid extrac-


                                                                     _2
tion by conventional techniques shows an internal concentration of 10   M


            32                  —6
extractable   P material from 10   M phosphate.



     Because these organisms are found at low temperatures and because our



studies of maltose transport  showed similar linear uptake kinetics and



operated very poorly at low temperature, we studied the effect of temperature



on the phosphate transport system.  Fig. 4 shows an Arrhenius plot of these



data which yields an activation energy of 52,000 cal per mole.  This value



also is high and suggests a mechanism more complex than simple diffusion and



one that requires reserve capacity for operation at low temperature.



     Mitchell (1954) has suggested that only one of the four possible phosphate



species might be transported.  Accordingly we studied the velocity of phosphate



transport with respect to hydrogen ion concentration as shown in Fig. 5.  Both



the initial uptake rate and the concentration at half maximum growth rate show



that the resistance to phosphate incorporation is greater when the pH is raised.


Most experiments were performed at pH 4 where the flux is maximum.  Another



reason for this choice of pH is the fact that NH_ is the only ligand present



with an appreciable binding constant, and this species virtually disappears



at pH 4.  This simplifies consideration of extracellular chemical complexation.



Recent observations show a similar pH dependence for arsenate uptake, that



is significantly higher at pH 4 than pH 7.


     A number of metabolic inhibitors were tested to see what sorts of anti-



metabolites effected transport from a medium 10   M in phosphate.  Organic



solvents such as ethanol, dimethyl sulfoxide and toluene were tested because



in some of our other systems showing similar kinetics, membrane disruptants



have been found to increase substrate flux .  This however, was not found to
 D. K. Button, unpublished data

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                                   -13-
if the cells were presented with 10   M arsenate 10 minutes before phosphate



uptake was measured as shown.



     Since phosphate uptake is inhibited by both arsenate and metabolic



inhibitors, part of the inhibition was probably due to reduced respiration of



this strict aerobe.  To see if arsenate inhibition was common with a phosphate



transport step the degree of arsenate transport inhibition by phosphate was



measured as shown in Fig. 6.  Since arsenate transport kinetics are linear,



concentrations and velocities are presented rather than their reciprocals as



normally used when describing saturatable systems.  The data show that arsenate



transport is reduced 50% by about 10   M phosphate.



     The effect of arsenate on the viability of low phosphate systems is



shown in Fig. 7.  Line slopes show that growth rates are slightly reduced by


  —8                       —7
10   M arsenate and that 10   M arsenate is sufficient to produce a death



rate of 0.15 hr~  from a control growth rate of 0.12 hr~ .



     Many marine isolates are inhibited by low levels of heavy metals.  Table



II shows some of the characteristics of hydrocarbon oxidizing organisms



selected mostly from Cook Inlet, Alaska.  Table III shows their sensitivity



to copper.  All showed reduced growth rates and most were killed by the



addition of 10   M copper as shown including £. rubra used in all of the



preceding experiments.  However early experiments showed that high phosphate



concentrations prevent copper inhibition of growth rates or viability at any



level and generated the need to understand phosphate incorporation kinetics



described in the foregoing.  This understanding allowed experimentation with



steady state continuous culture systems at low but not limiting levels of



phosphate.  Fig. 8 shows a pair of glucose limited continuous cultures popu-



lation data.  One set has a moderate (10   M) level of phosphate but trace



metals are at only the level provided by reagent grade chemical contamination.



The second set are with a full complement of trace metals but with added

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                              -14-
Fig. 4.  Initial rate of phosphate uptake measured over a six


                                                            -6
         minute period with respect to temperature from a 10



         M medium according to the Arrhenius equation.  Velocity



         is expressed as moles phosphate per gram cells dry weight



         per minute.  Temperature shown is degrees centigrade.



         Temperature plotted is the reciprocal of the absolute



         temperature.

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40°
     (I/T)

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                           -16-
Fig. 5.  Effect of hydrogen ion concentration on phosphate




         flux.  Open symbols, steady state concentration of




         phosphate in a continuous culture system diluted at




         0.09 hr"1.  Closed symbols, initial uptake rate from




         a 10   M phosphate solution.  Concentrations are




         expressed as total extracellular phosphate.

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            CONCENTRATION
           AT STEADY STATE
                               in
                               ^
                             X x
                             LU
O-CJ
CO
                      8
pH

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                            -18-
Fig. 6.  Initial rate of arsenate transport with respect



         to arsenate concentration with three concentrations




         of phosphate.

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UJ
o
<
a:
e>
UJ
UJ
O)
UJ


o
            0  PHOSPHATE
                            10
                       8
        ARSENATE  X 10° MOLAR

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                             -20-
Fig. 7.  Growth rates in low phosphate solution at various



         levels of arsenate.  Inoculation was from a phosphate



         limited continuous culture and populations measured



         by plate counting.

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o
o
X
o
               TIME, HOURS

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                               -22-
Flg. 8.  Effect of heavy metals on the growth rate of IU rubra.



         Data are steady or transient state populations in



         continuous culture of two runs.  Circles are electronic



         counter counts, triangles are plate counts.  Both runs



         are glucose limited at 5 x 10~  M.  Medium used in the



         upper run contains 10**  M phosphate but no added zinc,



         manganese, cobalt or molybdenum.  The lower run medium



         contains these added trace elements but phosphate is



         reduced to 3 x 10   M.

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TIME.  DAYS

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                      Table II.  Hydrocarbon oxidizing organism characteristics.
Culture
54
72
80
114
179
181
197
198
Dimensions
Gram uM
+ 0.6 x 1.0
+ 0.5 x 2.0
+ 1.0 x 1.2
+ 0.6 x 3.0
+ 0.6 x 3.0
- 0.5
+ 0.5 x 20
+ 0.6 x 3
Shape
rod
rod
coccoid
rod
rod
cocci
branched
filaments
rod
Upper
temp.
limit
30
30
37
30
25
25
-
25
u u
max max
broth kerosene Ea
hr-1 hr'1 K/cal/mole
0.23
0.35 0.20 16.0
0.35 0.087
0.35 0.020 16.0
0.35 - 15.2
0.15
_
0.35 - 14.5
Emulsifi-
cation*
2
1
1
2
2
0.5
-
0.5
Type**
Mycobacterium
Nocardia
Arthrobacter
Nocardia
Nocardia
Micrococcus
Streptomyces
Mycobacterium
                                                                                                                 I
                                                                                                                NJ
**
Genus most closely resembling isolate.


Grams crude oil emulsified per gram dry weight of organism.

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                            -25-
                       Table  III
Culture
54
72
80
114
179
181
197
198
11. ruba
Added Cu"""
0 10"6 M 10"3 M
5 x 104* 0 0
3 x 10* 0 0
1 x 106 0 0
1 x 106 3 x 105 0
5 x 10* 1 x 103 1 x 103
70 0 0
70 - 5 x 103
70 0 0
370 20 0

10~4 M
0
0
0
1 x 104
1 x 102
0
0
0
0
*Cultures were grown in nutrient broth, harvested and suspended
in mineral mannose medium pH 7.2 except R. rubra which was
suspended in mineral salts glucose medium pH 4.0.  Columns above
report the population in broth culture 24 hr after inoculation
with various quantities of added copper shown.

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                                    -26-
phosphate at only  3 x  10~  M  so  that added  copper  at  10    M is  in  a  greater




than 1:1 ratio with remaining phosphate after population  growth.   It is  clear




that the trace metal deficient steady state is  repeatedly perturbed  by added




copper showing no  accumulated resistance and that  manganese and to a lesser




extent zinc reduce the Inhibitory effects of copper.  The low phosphate  high




trace metal system remains unperturbed under the same conditions of  perturbation




as shown in the upper  data set.  Atomic absorption analysis of  our stock




phosphate revealed a manganese peak of sufficient  size to provide  an alternate




manganese source and thus provide protection from  copper  inhibition  in high



phosphate systems.








                              DISCUSSION






     The isotope dilution bioassay technique presents a useful method to




handle nutrient incorporation kinetics of a  common metabolite incorporated




by a high affinity system.  The data spread  for phosphate  uptake appears




large but the absolute concentrations involved are extremely small,  less than




1% of that found in most marine systems.  Although it appears that phosphate




uptake rates extrapolated to a finite concentration at zero concentration,




extensive data collection (10,000 hours of continuous culture operation) did



not substantiate this point or reduce the data spread.  Initial uptake data




were obtained to evaluate the capacity of the phosphate transport  system




and are the basis for describing the phosphate incorporation system  in growing




systems as nonsaturatable.  The mechanism of phosphate uptake remains obscure.



However the linear concentration velocity relationship has appeared  before



and it may be a rather general type of incorporation kinetics.  Active



transport is clearly implicated in that internal free phosphate concentrations



are greater than external concentrations.   Metabolic inhibitors such as




iodoacetate and sodium azide also support the view that active transport is

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                                  -27-
involved, possibly driven by phosphoenol pyruvate hydrolysis since DCCD
appears ineffective.
     The fact that arsenate inhibits phosphate transport, phosphate inhibits
arsenate transport, and that the uptake kinetics are similar suggest that
this is another example of a transport system that cannot distinguish between
the two ions.
     If the mechanism involves diffusion limitation of a transfer process
across a membrane one might expect a low temperature coefficient for transport
and that membrane solubilizing agents might enhance the transport rate.  We
found neither to be the case and none of the usual transport models appear
attractive to explain the results presented.
     The environmental implications of these findings are interesting.  Table
IV shows some typical arsenate levels occurring in potable water and marine


                               Table IV
                                            Q
                       Environmental Arsenic
              Soil                           10,000 ppbb
              Hot springs                     8,500
              Lakes                           2-50
              Rivers                       0.2  - 25
              Desert ground water             8-27
              Sea water                       1-5
              Rain water                   0.02 - 14
                 ^feoephl, K. H., Handbook of Geo-
                  chemistry, New York, 1969, p. 33-
                  1-1.
                 v»                               —8
                  1 ppb is equivalent to 1.4 x 10   M

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                                  -28-
systems.  Dr. Michael Pilson  reports marine arsenic concentrations of between


  —8       7
10   and 10  M with the concentration in some areas exceeding that of phosphate.



Since arsenic is particularly effective in low phosphate systems it seems clear



that existing arsenic levels are sufficient to effect the metabolism rate of



at least part of a diversified population in low phosphate natural systems.



It seems likely that low levels of arsenate have had a role in contributing



to some of our experimental irreproducibility.  For example, sodium chloride



tolerance experiments using this organism probably more accurately reflected



the arsenate level in the reagent grade sodium chloride used than the salt



tolerance of the marine yeast.



     The survey of various hydrocarbon oxidizing marine organisms at hand



showed major copper toxicity at 10   M.  However most of the foregoing was an



effort to track down the rather variable sensitivity a rather resistant marine



yeast exhibited toward copper.  The final continuous culture shows that



copper inhibition is related in a major way to trace metal nutrition.  This is



not particularly surprising when one realizes that the prosthetic groups of



many enzymes can be replaced by heavy metals under certain conditions.  It



does however mean that many organisms sensitive to heavy metals are probably



even more sensitive than reported when in natural systems which are trace metal



and particularly manganese deficient.  Effects of this copper - manganese



interaction await careful quantitation.



     It seems likely that growth rates of organisms in the natural environment



are reduced by antimetabolites such as arsenate and heavy metals and at



existing concentrations so that blooms only occur when nutrient build-up has



been sufficiently great to provide a positive driving force to autocatalytic



microbial reproduction sufficient to overcome the negative influence of anti-









personal communication, Or. Michael Pilson, Univ. of R. I.

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                                  -29-
metabolites discussed.  It is interesting that this "bloom or bust" type




behavior of aquatic populations is probably one that maximizes the standing




crop from available nutrients.  The alternative of a stable slow growing




steady state population in the ocean for example would distribute available




nutrients so widely that major amounts of energy would be diverted to endogenous




metabolism in the smaller primary forms and to collection mechanisms in the




upper trophic levels.  The expected result would be a lower yield of fish for




example.  However some environmental arsenate levels may greatly exceed




threshold toxicity levels and seriously disturb the normal metabolic processes.




Reinforcement of these effects would be expected by additional antimetabolites




such as heavy metals.

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                                  -30-
                              REFERENCES





Blum, J. J.  1966.  Phosphate uptake by phosphate - starved Euglena.  J.



     Gen. Physiol., 49: 1125.



Breslow, E., and A. W. Girotti.  1966.  The interaction of cupric and zinc



     ions and the effect of cytidylic acid.  J. Biol. Chem. 241; 5651.



Button, D. K.  1969.  Thiamine limited steady state growth of the yeast,



     Cryptococcus albidus.  J. Gen. Microbiol., 58; 15-21.



Cabadaj, R., and T. Gdovin.  1970.  Tolerance of sheep to cupric sulfate



     (CuSO. • 5 H.O).  Vet. Med. (Prague), 15: 21-29.
          H      L                         ~~~


Goodman, J. and A. Rothstein.  1957.  The active transport of phosphate into



     the yeast cell.  J. Gen. Physiol., 40; 915.



Grande, M.  1966.  Effect of copper and zinc on salmpnid fishes.  Third Int.



     Conf. on Water Pollution Res., Munich, Germany.



Jung, C. and Rothstein.  1965.  Arsenate uptake and release in relation to



     the inhibition of transport and glycolysis in yeast., 14; 1093-1112.



Mitchell, P.  1954.  Transport of phosphate across the osmotic barrier of



     Micrococcus pyogenes;  specificity and kinetics.  J. Gen. Microbiol.,



     11: 73.



Nielsen, L. K.  1969.  Influence of copper on the photosynthesis and growth



     of Chlorella' pyrenoidosa.  Dan. Tidsskr. Farm., 43; 249-254.



Steeman-Nlelson, E., and S. Wium-Anderson.  1969.  The effect of deleterious



     concentrations of copper on the photosynthesis of Chlorella pyrenoidosa.



     Physiol. Plant., 22i 1121-1133.



Steemann-Nielson, E., and S. Wium-Anderson.  1970.  Copper ions as poison in



     the sea and fresh water.  Marine Biol., £: 93-97.

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                  -31-
              APPENDIX I
DATES AND TITLES OF CONTINUOUS CULTURE
         BUNS AND EXPERIMENTS

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                                  -32-
                       CONTINUOUS CULTURE DATA
Run
        Dates
Experiments (Rh-rubra)
 76


 77



 79



 80


 81



 86


 87


 88


 90



 91



 92



 94



 95
 5/15/68 -  5/26/68


 6/6/68  -  7/8/68



 8/1/68  -  8/23/68



 9/4/68  - 10/7/68


10/15/68 - 12/18/68



11/10/69 -  1/17/69


 3/13/69 -  2/24/69


 3/13/69 -  4/4/69


 4/9/69  -  5/12/69



 5/19/69 -  6/19/69



 6/24/69 -  7/8/69



 7/8/69  -  7/23/69



 8/6/69  -  9/9/69
Cu   inhibition @ low constant
phosphate concentration.

Added Cu4*, P6C12, HgCl2, ZnSo4
to observe effect on phosphate
limited culture.

Effect of copper on glucose
limited steady state continuous
culture.

Glucose limited steady state
culture w/o copper.

Added MnSo4, varying amounts of
substrate - glucose and copper to
reactor @ 50% maximum growth rate.

Phosphate limited steady state
continuous culture.

Phosphate limited steady state
continuous culture with P-^.

Phosphate limited steady state
continuous culture with p32.

Phosphate limited steady state
continuous culture with respect to
pH and determination of S.

Determination of S @ phosphate
limited steady state continuous
culture @ rO.3, rO.5 + rO.8.

Phosphate limited steady state
culture determination of S @ differ-
ent pH values.

Increasing amounts of phosphate
added to phosphate free steady state
continuous culture.

Phosphate limited steady state
continuous culture samples taken for
S @ rO.3, rO.5 + rO.8.

-------
                                   -33-
Run
        Dates
Experiments (Rh-rubra)
 96


 96R



 96Rx2



 100
 101



 105



 106



 107

 110


 113


 114



 120


 127
 9/23/69 - 10/6/69


10/6/69  - 10/23/69



10/23/69 - 12/8/69



12/4/69  -  1/8/70




 1/16/70 -  2/12/70



 2/16/70 -  2/26/70



 3/2/70  -  3/14/70



 3/2/70  -  4/11/70

 4/15/70 -  5/8/70


 6/8/70  -  6/13/70


 6/22/70 -  7/9/70



 8/18/70 -  9/14/70


10/7/70  - 11/11/70
Low phosphate steady state
continuous culture•

Phosphate limited steady state
continuous culture with respect to
pH.

Various sampling method for S in
steady state continuous culture
phosphate limited @ rO.3.

Phosphate limited steady state
continuous culture and determination
of S @ rO.3, rO.5 + rO.8 using new
quick sampling method.

Phosphate limited steady state
continuous culture c determination
for S @ rO.8.

Low phosghate steady state continuous
culture c determination for S @
rO.8.

Phosphate limited steady state
continuous culture c determination
for S @ rO.8.
            ^_l_
Effect of Ni   on K  for phosphate.
                   S
                          1^1
Determination of S with Ni  ,
@ rO.5.

Determination of S with copper, @
rO.3.

Phosphate limited continuous culture
@ steady state c sample taken for S
@ rO.5.
                         14
Determination of_S with_C   and copper
samples taken @ rO.5 + rO.8.

With a phosphate limited continuous
culture contamination of effect of
CU++ MnSO. + ZnSO..
         4       4

-------
                                 -34-
                    D. K. Button - FROM NOTEBOOKS
Ref.
Date
Expt.
DKB B4
P13
DKB B4
P14
DKB B4
P31
DKB B6
P4
DKB B6
P6
DKB B6
P9
DKB B6
P10
DKB B6
DKB B6
P14
DKB B6
P15
DKB B6
P16
DKB B6
PI 7
DKB B6
P18
DKB B6
P19
DKB B5
P32
DKB B5
P56
1/5/68
1/11/68
1/20/68


6/9/70
6/10/70
7/2/70
7/2/70
7/17/70
7/20/70
7/22/70
7/24/70
7/28/70
11/11/69
1/20/70
Inoculation + isolation of a low
phosphate requiring organism.
Set up culture in yeast extract, isolated
3 colonies and transferred to low glucose
media and allowed to grow through one log
phase.
A check for amounts of phosphate in
media salts.
Copper inhibition test for hydrocarbon
microbacterium isolate.
Copper inhibition of continuous culture @
steady state @ pH7.
Copper/ inhibition of continuous culture
using 64cu.
The use of low pH copper to prevent clumping
copper @ 3 x 10~6 H.
N.N'-Dicyclohexylcarbodiimide inhibition of
phosphate transport.
Initial uptake of phosphate c glucose
5 mg/1.
A viability check with phosphate + copper.
Initial uptake from continuous run, using
phosphate @ concentrations of 1 x 10"^ M •*
1 x 10~8 M.
Effect of pH on phosphate uptake.
Phosphate uptake of C. utilis + C. Albidus.

Phosphate concentration gradient in Rh
rubra.
Phosphate uptake in synthetic media.
Expt . for Rh rubra mutant .

-------
                                   -35-
Ref.            Date	Expt.
0KB B5
P66
DKB B5
P67
DKB B5
P73
2/25/70
2/27/70
5/4/70
Low phosphate transport of mutants.
Continuation of phosphate mutant expt.
Preparation of phosphate transportless
mutants .

-------
                                  -36-
                  INITIAL UPTAKES (HEAVY METALS)
 Ref.
DaCes
Expts.
SSD BK2
P9
SSD BK2
P10
SSD BK2
P14/15
SSD BK2
P69-73
SSD BK3
P32
SSD BK3
P33
SSD BK3
P35
SSD BK3
P38
SSD BK3
P45
SSD BK4
P33
8/12/70

8/13/70

8/17/70

12/2/70 ->
12/7/70
12/21/70

12/29/70

12/30/70

11/7/71

1/14/71

3/22/71

Copper inhibition of phosphate uptake
pilot run.
Copper inhibition of phosphate uptake
pilot run 11.
Copper inhibition of phosphate uptake
run III.
As-04 @ 10"6 M, 10"5 M, 10~7 M, 10~8 M +
10-9 M pilot expts.
As-73 c AsO, initial uptake.

Phosphate inhibition of AsO, uptake.

Comparison of As-0, + phosphate flux
under identical conditions.
AS-73 pool concentration expt.

AS-0, toxicity to Rh rubra.

Effect of pH on AS-0, uptake.

Notes:  * » day, * = expts. were repeated

-------
             -37-
INITIAL UPTAKES (OTHER)
Ref.
SSD BK2
P12
SSD BK2
P13
SSD BK2
P16
SSD BK2
P17
SSD BK2
P18
SSD BK2
P19
SSD BK2
P27
SSD BK2
P35
SSD BK2
P37
SSD BK2
P39
SSD BK2
P44
SSD BK2
P47
SSD BK2
P53
SSD BK2
Pll
Dates
8/14/70
8/17/70
8/18/70
8/20/70
8/21/70
8/21/70
8/31/70
9/14/70
9/21/70
9/29/70
10/2/70
10/7/70
10/22/70
8/13/70
Expts.
Phosphate concentration gradient a range
of dilutions from 1 x 10~6 M phosphate •*
10-7 M phosphate.
Effect of temperature on phosphate uptake,
5°C. 15°C, 25°C.
Effect of temperature on phosphate uptake,
5°C, 15°C, 25°C.
Phosphate concentration gradient a range
of dilutions from 1 x 10"^ M phosphate •*•
5 x 10~6 M phosphate.
Effect of temperature on phosphate uptake,
10°C, 20°C + 25°C.
Phosphate inside Rh rubra cells (pools) .
Glucose requirement of phosphate transport.
Effect of temperature on phosphate uptake,
1°C.
Initial uptake regarding pH c phosphate
limited cells.
Effect of sodium + potassium.
Effect of pH on phosphate limited cells
(final expt.).
Repeat of salt concentration effect using
sodium and potassium c phosphate limited
cells.
Effect of pH on phosphate limited cells c
tris buffer.
INHIBITORS
N.N'-dicyclohexyldicarbodiimide (DCCD) effe
on phosphate uptake.

-------
                                 -38-
Ref.
Dates
Expts.
SSD BK2
P56
SSD BK2
P58
SSD BK2
P74
SSD BK2
P75
SSD BK3
P21
SSD BK3
P36
SSD BK4
P7
SSD BK4
P8
SSD BK4
P12
SSD BK4
P14
SSD BK4
P25
SSD BK4
P26
11/11/70
11/13/70
12/7/70
12/11/70
12/16/70
1/4/71
2/16/71
2/17/71
2/22/71
2/24/71
3/8/71
3/9/71
Icdoacetic acids, effect on phosphate
uptake.
Sodium azide's effect on phosphate
uptake.
Sodium dichromate effect on phosphate
uptake.
Effect of high temperature on phosphate
uptake, 25°C, 30°C + 35°C.
Effect of high temperature on phosphate
uptake, 25°C, 408C + 50°C.
Effect of low temperature on phosphate
uptake, 25°C, 40°C, 50°C, 1°C.
Phosphate inhibition of AS-0, uptake,
25°C, 40°C, 50°C, °C. *
Phosphate uptake c sodium chloride.
Saline inhibition check for viability.
Phosphate inhibition @ low temperature,
5°C, 158C + 25°C.
Effect of EtOH on phosphate transport.
Repeat of EtOH on phosphate transport
and including effect of dimethylsulfoxide
                                (DMSO) 20%.

-------
                          -39-
                    APPENDIX II
EFFECT OF CLAY ON THE AVAILABILITY OF DILUTE ORGANIC
 NUTRIENTS TO STEADY-STATE HETEROTROPHIC POPULATION
   SOME FACTORS INFLUENCING KINETIC CONSTANTS FOR
         MICROBIAL GROWTH IN DILUTE SOLUTION

-------
                        -41-
                                Made in the United States of America
                               Reprinted from LIMNOLOGY AND OCEANOGRAPHY
                                    Vol.  14, No. 1, January 1969
                                        pp. 95-100
   EFFECT OF CLAY ON THE AVAILABILITY OF
 DILUTE ORGANIC NUTRIENTS TO STEADY-STATE
          HETEROTROPHIC POPULATIONS
                   BY D. K. BUTTON
Reprinted  from Limnology and Oceanography. _14_(1): 95-100
(1969),  by permission of the Editor.

-------
                                        -43-
            EFFECT  OF CLAY ON THE AVAILABILITY OF
          DILUTE  ORGANIC  NUTRIENTS  TO  STEADY-STATE
                     HETEROTROPHIC  POPULATIONS1


                                  D.  K. Button"
               Institute of Marine Science, University of Alaska, College  99701

                                     ABSTRACT
       The effect of clays on the availability of small organic  molecules  to  microorganisms
     was  determined.  Recovered suspended sedimentary material and Bentonite was tested
     for its ability to compete with yeast and bacteria for thiamine or glucose in continuous
     culture systems at low  organism  concentrations.  The added clays do not render the
     organics tested unavailable to microorganisms or remove them from solution to a detectable
     or significant extent.  The addition of clays can,  however,  effect a perturbation to the
     steady system, possibly by altering the inorganic chemistry of the dissolved phase.
              INTRODUCTION
  Chemical  analyses  of certain  systems
have been interpreted to show that  clays
and sediments are effective in adsorbing
organic compounds  from solution. These
clay-organic  associations  include starch
(Lynch, Wright, and Cotnoir  1956), pro-
teins and amino acids (Sieskind and  Wey
1959), and carbohydrates (Bader, Hood,
and Smith 1960).  The amount of adsorp-
tion determines the  effect of clays on the
dissolved organic  chemistry of sediment-
laden water systems. Suspended sediment
loads normally run  from 0.5  to  100 mg/
liter in the glacier-fed  bays and inlets of
southeast  Alaska  and  even  higher  in
streams draining areas of intensive mining
or other earth-moving activities.
  The extent of the clay-organic associa-
tion was  further investigated by  measur-
ing the influence of clay particles on the
nutrient  adsorption  kinetics of some het-
erotrophic cultures.   This was done  by
subjecting steady-state low population nu-
trient-limited cultures  to perturbation  by
injected clay.
  1 Substantial support for this work was provided
by U.S. Department of Interior, Office of Water
Resources and  Federal Water Pollution  Control
Administration,  Grants A-007-ALAS and WP-
1240-01. Institute of Marine Science Contribution
No.  48.
  21 am indebted to Emma Dieter who provided
technical assistance.
                 THEORY
  In a  nutrient-controlled continuous  cul-
ture system, the limiting  nutrient governs
the steady-state  cell population  (Monod
1950; Herbert, Elsworth, and Telling 1956;
Button  and Carver  1966) and  is divided
between the growing organisms and extra-
cellular solution according to the equation:
               = Y(S0-S),
(1)
where S0 is the initial limiting nutrient con-
centration and Y the yield constant, grams
of organisms  produced per gram  of lim-
iting substrate used, (S0-S). In continu-
ous culture at 100% viability the average
growth  rate is  numerically equal  to  the
dilution rate and is  set by the concentra-
tion of S at a  particular temperature.  This
rate  increases as a  monotonic increasing
function of  substrate  concentration  fre-
quently approximated by the Michaelis-
Menten equation:
                   K. + S-

Thus one can determine changes in avail-
able substrate concentration,  S, by observ-
ing changes in the steady-state concentra-
tion of organisms, X, at a particular rate.
If one  chooses a  value  of  S0 near the
Michaelis constant for growth, K,, and sets
the dilution rate (which is  equal  to the
growth rate at 100% viability and perfect
population dispersal)  at  a large fraction
                                        95

-------
                                        -44-
96
D.  K. BUTTON
of the maximum growth rate, j^mnv, small
changes in available limiting substrate are
reflected by large changes in the cell popu-
lation. For example, K, for Escherichia coli
is 4 mg glucose/liter (Monod 1950), about
the same as  for  most  heterotrophs near
their  upper  temperature  limit under usual
laboratory conditions. If one operates at a
dilution or growth rate of 0.5 /imnx,  where
S = K,,  and  sets  S0 at 5 mg/liter,  the
resulting  population  at  Y =  0.5  will  be
0.5 mg/liter,  according  to  equation (1).
Under these  conditions  a 10% reduction
in available substrate would reduce  the
steady-state bacterial population to half its
original value.

            CLAY PREPARATION
  Initial nutrient  adsorption  experiments
were  run with  sediments collected from
routine hydrographic stations  in southeast
Alaska. Sufficient seawater was filtered to
obtain a few hundred mg of sediment. The
sediment  was weighed,  resuspended,  and
autoclaved  15 min at 121C.  This  sterile
suspension was  cither introduced  into the
feed  chamber (a  20-liter carboy) or  the
culture vessel (a 250-ml boiling flask) of
the continuous culture apparatus,  depend-
ing on  the  experiment.  Sterile  conditions
were  maintained by injecting the suspen-
sions  with a syringe through rubber cov-
ered ports.  Standard clay was prepared by
grinding Montmorillonitc No.  27 (Benton-
ite.  Belle Fourche, S. Dak., Ward's Natu-
ral Science  Establishment, Inc.,  Rochester,
N.Y.)  in  a porcelain  mortar and pestle.
This  was  fractionated   by  sedimentation
and  a cut  of approximately  1.2 X 10-I3-g
particles  was obtained  with  90% of  the
particles between  1.5 and 2.5 /u in  diam-
eter.  These particles  remained  indepen-
dent  from  one another  and  from  the
microorganisms, this was clear in  phase
contrast examination of the suspensions.

            CULTURE METHODS
  Nutrient  adsorption by clay  was mea-
sured in a single-phase continuous culture
apparatus of the type described by Button
and Carver (1966). Cryptococcus albidus,
       o
       z
       "*  c
       m  O
       a
       o
       
-------
                                       -45-
                            CLAY-NUTH1ENT ASSOCIATION
                                                                                97
  A third organism was selected for use in
experiments involving low buffer capacity
and high pH—the only one of those tested
that would tolerate these conditions.  This
organism, a pink yeast tentatively identi-
fied as belonging in the genus Rhodotorula,
was isolated from  Amukta Pass  near the
Aleutian Islands by K. Natarajan.  It pos-
sessed the requisite characteristics of high
growth rate and stable  behavior in con-
tinuous culture without  adhering  to  glass
surfaces. Culture conditions were 25C, pH
6.5 in the medium described above except
that Na2HPCvH2O was  reduced to 3 mg/
liter.  This is referred to  as the "low phos-
phate" medium.

          COUNTING AND SIZING
  Populations were counted on plates pre-
pared from the liquid culture medium plus
1.5%  agar.  Where possible  an electronic
counter (Coulter Counter Model  B,  Hia-
leah, Fla.) was used for counting and sizing
the organisms  and the  clay.  Agreement
between methods was normally within sta-
tistical error when more than  1,000  colo-
nies were counted.  Yeast cells could be
counted in the presence of clay  with the
counter owing to their greater average vol-
ume;  however,  all populations  reported in
the presence of clay were determined  from
plate  counts. Populations for the K, mea-
surement  were  determined  from  optical
density in a 5-cm cell at  625 Tap..

                RESULTS
  A thiamine-limited continuous culture of
C. albidus was maintained at steady  state
at half maximum growth rate of 0.132 hr1
corresponding to a doubling time of 5.25 hr
at 25C.  The  feed contained 2 X 10-12 M
thiamine,  and the  Michaelis  constant (ex-
tracellular concentration at (j. = 0.5uma,) for
this nutrient was  4.7 X  10'13 M  (unpub-
lished  data).  This resulted in a  reactor
population  of  2.0 X 107   cells/liter.  Clay
recovered from  Glacier  Bay, Alaska, was
then injected into  the feed  to a  level of
10 mg/liter  of medium.  This remained in
suspension owing  to  the agitation  caused
by air bubbles from  the sparger  used to
saturate  the  feed  medium with air. The
time allowed for equilibration was  48  hr,
during which 6.3 volumes of  feed flushed
through the 500-ml reactor. The final pop-
ulation  in  the  reactor  after  equilibration
was 2.4 X107  cells/liter,  essentially  the
same as  before adding  the clay. A  fall in
the cell population had  been  expected due
to the addition of the clay-thiamine (vita-
min Bj)  term in the equilibrium:

Clay - B!
  + Cells ^ Clay + BI
           + Cells^Clay + Cells-B,. (3)

  However, since the above evidence indi-
cated a low binding constant  for the clay-
thiamine association, the binding ability of
clay was further tested with the  carbon
source—glucose.  Experimental  conditions
to test the affinity of clay for glucose were
the same as  above except that thiamine
was added to  10-° M,  and  glucose was
added  to 6 mg/liter. Under  these  condi-
tions, the Michaelis constant for glucose is
3.0 mg/liter as  shown in the  plot of equa-
tion (1)  in Fig. 1 according to the method
of Button and Carver (1966). The reactor
population before and after adding 140 mg
of Bentonite  of 10  liters of feed is shown
in  Fig.  2. The  upward  portion  of the
curve indicates that  the experiment was
terminated before a true steady state was
reached. However,  the glucose removed
by  the clay cannot have exceeded 0.7 mg/
liter and appears to approach zero.
  Since pH is  a factor in the chemistry
and charge of  the  clay surface  (Sieskind
and Wey 1959), the apparent lack  of ad-
sorption was tested again at neutrality. For
this purpose E. coli was set up in continu-
ous culture at  pH 7, with a  feed glucose
concentration of 6 mg/liter and at a dilu-
tion or growth  rate of 0.35 hr1. The yeast
used in  the  experiments above was not
used here  because  its  glucose  transport
system apparently fails  above pH 5. The
total lack of effect of  Bentonite particles
injected  directly  into the reactor on the
steady-state cell  population   is shown  in
Fig. 3.  As the clay particle  concentration
changed from  zero to  1012  particles/liter

-------
                                         -46-
                                    D.  K. BITITON
           8     9    10
               TIME, DAYS
12
  FIG.  2.  Steady-state population  of Cryptococ-
cits albidus, glucose limited at 6 nig/liter growing
at 0.132 hr'1 before and after adjusting the level
of clay in the feed to 14 mg/liter.
and then exponentially towards  zero  the
bacterial population remained unchanged.
A monomolecular glucose layer on the clay
would have reduced the dissolved glucose
level 4 mg/liter  to 2 mg/liter and caused
immediate and complete  washout of  the
culture.
   Phosphate was the only nutrient in large
excess in these experiments.  To  rule  out
the possibility of phosphate protecting  the
clay  from associations with the  organic
compounds,  the low  phosphate  medium
was used with the pink  yeast described
above.  This yeast possessed  characteristics
allowing low population culture techniques
without buffers or crielates, and it behaved
very well in continuous culture.  It has a
thiamine requirement  that is satisfied by
something less than the 9 X 104 molecules/
organism  required  by  C.  albidus at  half
maximum growth rate.
   The chemical species having the highest
binding  capacity for  cations in  the  low
phosphate medium is NH3 which is present
at only 9 X 10"7 M at pH 6.5. The steady-
state population in the presence of the 2 X
10"5 M phosphate,  or  low phosphate  me-
dium, is shown in Fig. 4.  The initial addi-
tion of Bentonite to the reactor at 4.5 days
caused  a temporary 80% decrease in the
cell population.  The level added was 20
mg  of clay/liter.  However,  subsequent
additions  of 10 and 100 mg/liter of clay
PARTICLE CONCENTRATION per liter
O Q. 0 o
_ .0 ^ „= K3
. !
^
I ci
\
\
\ ORGANISMS
-O. ~ \
\
S
s
.AY \
\
. V
) 10 20
TIME, HOURS


30
       Fie.  3.  Steady state of population  of Esch-
     erichia  coli growing at 0.35 hr1 before  and after
     the introduction of 10" clay particles/liter into the
     reactor.
     to the feed had no effect on the population.
     Under  these  conditions, there was some
     coalescing of the-clay in the feed vessel
     so that the reactor clay concentration was
     somewhat lower than the feed concentra-
     tion.  In Fig. 5, the effect of 100 mg of clay
     added to one of duplicate batch  cultures
     9 hr  after inoculation is shown. The cul-
     tures were  limited to about 2 X 107 orga-
     nisms/liter  by the 3  mg/liter of  glucose
     present initially. The added clay  had no
     effect on  the final cell population;  the two
     cultures behaved as duplicates within  the
     normal variability of batch cultures.

                     DISCUSSION
       The vitamin thiamine is a cation in solu-
     tion with  a positive charge residing at  the
     nitrogen (3-position) of the thiazolium ring
     under the conditions  reported  here.  Since
     clays have  been reported  to  possess  ion
     exchange  capacity for cations  (Hendricks
     1941)  and to  have  surface  affinity  for
     neutral molecules (Bader et al. 1960), it is
     surprising that  no  binding of glucose or
     thiamine was detected in any of the experi-
     ments reported  here.

-------
                                       -47-
                             CLAY-NUTHIENT ASSOCIATION
                                                                                  99
   0  I
234  56789  10  II
     TIME, DAYS
  FIG. 4.  Steady-state yeast population, glucose
limited in unbuffered medium, as clay was added
to the reactor and to the feed.
  Temporary reduction of a yeast popula-
tion owing  to the addition of clay in the
low phosphate experiments  was  detected.
Since the populations returned to the ini-
tial  steady-state  level and did not again
decrease when subsequent and even larger
clay additions were made to the  feed, die
effect could not have been due to nutrient
removal.  The temporary reduction in cell
population was not surprising since biolog-
ical membranes  are particularly  sensitive
to perturbation  when not stabilized with
a buffer  such as phosphate or a  chelate
ligand.  The failure of subsequent  additions
of clay to cause similar perturbations can
be  explained by  the  normal  capacity of
microorganisms  to respond  to  new situa-
tions after   a  suitable  induction  period
(Horecker,  Thomas,  and Monod 1960).
Thus it seems likely that a chemical change,
such as a rise  in concentrations of free
heavy metals,  caused the temporary re-
sponse  shown in Figs.  2 and  4.  Recent
experiments' (unpubh'shed)  have  shown
similar  temporary  inhibition by  injected
copper at 10~7 M in a medium of low buffer
capacity.  Stotzky and  Rem (1967) reported
the absence of  an inhibitory effect in ex-
periments using a  clay  culture  medium;
this was  probably due  to the protection
afforded  by the yeast extract  component
of their basal medium.
  Under  the various  experimental condi-
tions described  here,  the data show that
                                                      10
                                                                        40
                    20       30
                 TIME, HOURS
  Fie.  5.   Duplicate  batch  cultures of  yeast,
glucose limited at low phosphate concentrations.
Arrow indicates the addition of clay to a level of
100 ing/liter to one of the cultures.


the equilibrium constant  between free or-
ganics and those bound to suspended sedi-
mentary material lies far in the direction
of the  dissolved state.  The  experimental
conditions included a range of pH, neutral
and charged substrates, media of high and
low  buffer capacity,  and  different types
of clay  preparations  and  concentrations.
Thus, it seems  unlikely that in natural sys-
tems  the  level  of  suspended  organisms
using small organic molecules is materially
influenced by the level of suspended sedi-
mentary material. The data do show evi-
dence  that clays cause temporary  reduc-
tion  of the growth rates  of the organisms
used, which is probably due to the solution
of some component.

               REFERENCES
BADEK,  R.  C., D. W.  HOOD, AND J. B.  SMITH.
    1960.  Recovery of dissolved organic matter
    in sea-water  and organic sorption by particu-
    late material.  Geochim.  Cosmochim. Acta,
    19: 236-243.
BUTTON, D.  K., AND ].  C. CARVER.  1966.  Con-
    tinuous culture of Torulopsis ntilis. A kinetic
    study of oxygen  limited growth.   J. Cen.
    Microbiol., 45: 195-204.
HENDRICKS, S. B.  1941.  Base exchange of the
    clay mineral montmorillonite for organic cat-
    ions and its dependence upon adsorption due

-------
                                           -48-
100
                                        D. K. BUTTON
    to van der waals forces.   J. Phys. Chem., 45:
    65-81.
HERBERT, D.,  R. ELSWOHTH, AND  R. C. TELLING.
    1956.  The continuous culture of bacteria;  a
    theoretical and experimental  study.   J. Gen.
    Microbiol., 14: 601-622.
HORECKER, B.  L., J. THOMAS, AND  J.  MONOD.
    1960.   Galactose  transport  in   Escherichia
    colt.  I.  General properties as  studied in  a
    Galactokinaseless mutant.  J. Biol.  Chem.,
    235: 1580-1585.
LYNCH, D. L., L. M.  WRIGHT, AND L. J. COTNOIR,
    JR.  1956.  The adsorption of carbohydrates
    and  related  compounds  on  clay minerals.
    Soil  Sci. Soc. Am. Proc., 20: 6-9.
MONOD, J.   1950.  La technique de culture con-
    tinue.  Th6orie et applications.   Ann.  Inst.
    Pasteur, 79:  390-399.
NATAHAJAN, K. V., AND  R.  C.  DUGDALE.   1966.
    Bioassay and distribution of thiaminc  in the
    sea.  Limnol.  Oceanog., 11: 621-629.
SIESKIND, O., AND R. WEY.  1959.   Sur 1'adsorp-
    tion d'acides amines par  la montmoiillonitc-H.
    Influence  de  la  position  relative  des deux
    fonctions-NH, et  -COOH.  Compt.  Rend.,
    248:  1652-1655.
STOTZKV, G., AND  L.  T.  REM.  1967.  Influence
    of clay  minerals on  microorganisms.   IV.
    MontmonUonite and kaolinite on fungi.  Can.
    J.  Microbiol., 13:  1535-1550.

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                                  -49-
                 Organic Matter In Natural Waters, ed D. W. Hood

                 lust Mar. Sci.. U. of Alaska, Pub. No. 1. 1970
    SOME  FACTORS  INFLUENCING KINETIC CONSTANTS  FOR
           MICROBIAL GROWTH  IN  DILUTE SOLUTION

                             D. K. Button
                       Institute of Marine Science
                         University of Alaska
                        College, Alaska  99701

      A growing microorganism reproducing in dilute aqueous environments
such as our natural water systems is faced with the problems of recognizing
and  concentrating desired nutrients,' preventing the concomitant entry of
chemical species not required and retaining desired components within itself.
This is successfully accomplished by simple diffusion accompanied by a set
of transport systems, each capable of recognizing a required  species and
carrying it across the cell wall to a site of chemical modification so that the
nutrient  cannot move  back by the same  path. The nutrient molecules a
species of microorganism  can  recognize are genetic parameters and some
transport systems can be produced or omitted in response to the chemical
environment. These  systems are sufficiently enzyme-like to behave in  a
similar kinetic  fashion  and can be described  with maximum velocities,
apparent Michaelis  constants   and  inhibition  constants. These  kinetic
constants are a measure of effective collision frequency at the site of the
growth rate limiting step as compared with the growth rate when that step is
saturated.
      The rate  limiting step for a microorganism grown in dilute solution
can therefore be nutrient diffusion through the aqueous environment to the
cell surface, transport of recognized nutrients through the cell surface into
the organism or a subsequent slow step in the conversion of the nutrient into
useful biochemical forms. The  kinetics of each step except the  first can be
affected  by the  external  environment of  the  organism. The following
observations describe how growth  velocity can be affected by nutrient
concentration, mixing, temperature, pH and heavy metal concentration.
      Growth   velocity is  normally an  increasing function  of  limiting
substrate concentrations. This can be hyperbolic, linear or logistic depending
on the rate limiting mechanism. The bottom curve of Fig. 1 shows how the
growth velocity of a yeast cell  Cryptococcus albidus varies with the vitamin
thiamine  at  the  cell  surface.   The  curve  is  computed  from  the
Michaelis-Menton  equation, the variation in cell yield with growth rate, the
variation in organism  size with growth rate and  the apparent  Michaelis
constant for growth experimentally determined  and  reported elsewhere
(Button, 1969).  The  upper  curve  is based  on  a computation  of the
concentration of  thiamine required  in the bulk of the medium to supply
thiamine at the cell surface at the required rate assuming no  mixing and
Flickian  diffusion.  A  convenient equation  presented  by Borkowski and
Johnson  (1967) for  this purpose is presented below. As one can see, the
effective concentration at the  cell surface is about half that in  the bulk of
the medium in  an unmixed system. Normal growth rates of yeast, bacteria
and  algae are  indicated to provide  a reference scale. These  data would


                                •537-


  Reprinted from Organic Matter in  Natural Waters,  ed. D. W.
  Hood,  Inst. Mar.  Sci., U. of Alaska, Pub. No. 1,  1970,  by
  permission  of the  Editor.

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                              -50-
                           YEAST and BACTERIA
    10-18
                 123456

                 GROWTH  RATE,  SECT'XIO8
Fig. 1.       The lower curve represents the thiamine concentration at the surface of
            the organism, Cryptococcus albidus, computed from the Michaelis Menton
            equation, Ks 4.4 x 10"' 3M, and the changes in cell volume and yield with
            growth rate. The upper curve represents the thickness of the diffusion film
            in a non-mixed solution computed from equation 1.
                                 •538-

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                                 -51-
                  kinetic constants and microbial growth
indicate  that  in this  case of vitamin limited growth, diffusion  to the cell
surface is the growth rate  limiting step. If that is the case,  the thiamine
utilization  rate  is  a  function of  mixing. We found  this to be the  case
experimentally (Button, 1969).
      Fig. 2 shows how the stagnant film thickness would vary with growth
rate if a concentration of nutrient equivalent to its apparent Michaelis
constant were provided in the nutrient medium. Curves shown were obtained
as described by  Borkowski  and Johnson  (1967). Using the experimentally
determined Michaelis constant for  thiamine limited growth of 4 x 10" ' 3 M
(center line) as the concentration at the cell surface, the film thickness  at
usual growth rates of 5 x 10s sec"1  is about one micron, which is within the
normal range of  stagnant  film  thicknesses.  The upper and lower lines
represent how the film thickness  would vary if the apparent Michaelis
constant were either ten times larger or ten times smaller than its actual
value.  The  divergence suggests  the existence of  a rational relationship
between the Michaelis constant for a substrate and the amount of substrate
required by  a microorganism.  This was  first noticed  in  tabulations of
published Michaelis constant data.  The resulting relationship js about what
one would  expect on  the  basis of molecular collision frequency  in the
Salmonella typhimurium system at published  concentrations  of  sulfate
binding enzyme (Drey fuss,  1964) and assumed values of sulfate flux. The
same relationship can be obtained  from the C. a/feidus-thiamine system by
substituting the  film  thickness at half the maximum growth  rate of 5.4 x
10~4  cm, obtained from Fig.  2,  into  the general equation for relating
diffusion limited nutrient concentration drops presented by Borkowski and
Johnson (1967).
where Cf and Cs are concentrations of nutrient in the bulk of the medium
and at the cell surface; n is the growth rate; x is the distance from the cell
center to the outside of the film in units of r,  the  cell  radius; D is the
diffusivity of the nutrient in the medium; and \ is the yield of cell mass from
nutrient provided. If  the experimental values of these constants for the C.
a/bidus-thiamine  system are substituted  into  equation  (1) the  following
relationship is obtained:
      A logarithmic plot of this equation is shown in Fig. 3. Notice that the
experimental values of  Wright and  Hobbie  (1965) and  Borkowski  and
Johnson (1967) for acetate and oxygen,  respectively, fall near this line,
although the yield constants are a factor of 106 lower than the thiamine data
used to formulate the relationship.
      Growth velocities  of microorganisms when the rate limiting step is
substrate saturated  follow the Arrhenius equation as shown in Fig. 4. Pena
(1955) suggested a similar relationship to temperature. Our values of Ks for


                                 •539-

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                             -52-
    14

I'2
cc
SK>
 LJ
 o
      8
 n:  2
                                                      :cf=f(iOKs)
                 I       23456
                    GROWTH RATE,  SECT'XIO6
Fig. 2.       The  center  curve (solid line) represents the  maximum diffusion film
            thickness that will allow the indicated growth rates with the concentration
            in the bulk of the unmixed medium equivalent to the Michaelis constant
            for thiamine in the thiamine requiring Cryptococcus albidus system. The
            darkened lines show the same maximum film thicknesses when the bulk
            medium is raised or lowered by a factor of ten.
                                 -540-

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       C9
       O
 7
 6
 5
 4
 3
 2
  I
 0
-I
                                                                                                        I
                                                                                                       ?
                  OXYGEN
                  ©   S*> ACETATE
o  ye
 i S  i
                       7    8    9    10   II     12   13   14
                             -LOG  Ks
Fig. 3.      Fit of experimental Ks data to equation 5. Points to the left of
           the line represent departure from diffusion limited systems.

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                             Tt CENTIGRADE

                        20            10
                        C.ALBIDOS
                         GLUCOSE
                                  R. MUCILAGINO
                                            GLUCOS
                                                                                                    i
                                                                                                    Ln
Fig. 4.     Arrhenius plot of Vmax for R. mucilaginosa (solid circles), and u. Ks vs.
          temperature (open circles).

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                                   -55-
                  kinetic constants and microbial growth
glucose at 1.6  C are shown along with the value of Ks for glucose at 25 C
with C. albidus and Pena's value for glycerol using C. u tilts at 15 C. The
values  for these yeast Ks data increase with temperature in the same way as
the maximum velocity of growth. Thus if


                          Umax =  Ae-E*/RT                       (3)

then

                           Ks  = AVEa/RT                        (4)

and from (1)

                        A-e-Ea/RT   =  _J_^
                                       7xl07X                     *  '

      Where growth rate is limited at the cell  surface  by nutrient transport
the system  can  be  likened to substrate competition for  passage through a
matrix of doors. These doors at the cell surface axe chemical in nature and
subject to closing (chemical modification) by inhibitory components of the
medium.
      Table 1 shows the  maximum growth rate of C. utilis after extended
growth at steady state in continuous culture. Population  was regulated by
flow rate at a low value so that the population remained at jumax. The rates
observed were  different  from  the corresponding batch growth rates and
much  slower after  the  first three days. Notice that  the  rate responds to
glycerol concentration in a different way at pH 4 than at pH 6, indicating a
Michaelis  constant of a higher order of magnitude at  pH 6. This difference
between batch and continuous culture data also occurred with C. albidus and
Rhodotorula glutmis and is under current consideration. The data show that
long term substrate limited growth  at low  population  can  respond to
concentration in a different way than short term substrate uptake.
      Fig.  5 shows  the  response of  R.  glutmis, a marine  pink yeast, to
copper. The yeast was selected because it grows well  in continuous culture
with no added chelates or buffers and only substrate quantities of phosphate
(Button, 1969). Under these conditions the  rate of growth  was sharply
reduced, about 70%, by  the addition  of copper to a final  concentration of
10~6 M. The copper  content of the continuous culture reactor decayed at the
rate shown  and  the population approached its original value of 1.5  x 10"
cells/liter. Succeeding additions of heavy  metals had progressively less effect
on the growth  rate. However,  the steady state population was reduced to
about  1  x  10s  cells/liter  as shown.  This  indicates a higher heavy metal
tolerance at the expense of a less efficient transport system which lowers the
total standing crop at a given level of nutrients.
      In   summary, mixing,   temperature,  nutrient concentration  and
inhibitor concentration all affect the efficiency and rate at which microbial
processes occur and  effects can be described in a rational manner.
                                 -543-

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                             -56-
Table 1.    The maximum growth rate of C. utilis after extended growth at
           steady state in continuous culture.
Glycerol
(mq/liter)
5
1000
5
1000
pH
4.0
4.0
6.2
6.2
wmax
(hH)
0.425
0.425
0.024
0.144
                                •544-

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                              -57-
       20
    r-
    '2
     x

     co 10
     o
     o
     X
ICT6M Cu'
.**
         I
         240   250  260   270  280

                       TIME, HOURS
 720   730
Fig. 5.     Effect of first and second addition of 10~6 M Cu" added to the
          reactor of a steady state continuous culture of a marine yeast
          (pink 1) growth at0.092/hr.
                             -545-

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                               -58-
                               Button
                            DISCUSSION

BELSER: Dr. Button, Dr. Jones reported alterations in cellular morphology
with the emergence of resistants. Have you observed a similar phenomenon
in these kinds of studies?

BUTTON: This is recent work. We have developed a theory of this over the
past couple of years and this was experiment number one. If I had had things
organized properly, we could have had size distribution prof iles throughout
this copper perturbation. The only yeast that will work for this has turned
out to be  tiny and  it was below our current facility for measuring size
distribution. We have the facility for answering your question but I do not
have an answer for your question. I think the probability of what you say, or
of what Dr. Jones said, happening, though, is certainly quite great.

JONES: Did the yeast concentrate the metals at all?

BUTTON: The ratio  between the copper concentrations and cell mass was
10£; in other words, if all of the copper had gone into the mass of the cell it
would  be one part in 106 copper. I do not have data, but I cannot see how
they could do otherwise. One has on the surface the type of material that
has ligands  of the type that binds things like heavy metals. As you  know, if
you do not have a really clean system and you try  inoculating,  as Dr.
Jannasch pointed  out, with a small inoculum, it is hard to get things going,
but if you use a large  inoculum, it is not so hard and this is probably because
the cell surfaces  are  good complexing agents which, of course, has been
demonstrated by many people.

                            REFERENCES

BORKOWSKI, J. D.,  and M. J. JOHNSON. 1967. Experimental evaluation
      of liquid film resistance in oxygen transport to microbial cells. Appl.
      Microbiol., 15:  1483-1488.

BUTTON, D. K.  1969.  Effect of clay on the availability of dilute organic
      nutrients  to   steady-state  heterotrophic  populations.  Limnol.
      Oceanogr., 14:  95-100.

BUTTON, D. K. 1969.  Thiamine limited steady state growth of the yeast
      Cryptococcusalbidus. J. Gen. Microbiol., 57: 777.

DREYFUSS,   J.   1964.    Characterization    of    a   sulfate    and
      thiosulfate-transporting  system in Salmonella typhimurium. J. Biol
      Chem., 239: 2292-2297.

PENA, C.  E.  1955.   The influence of temperature on  the growth of T.
      utills. M.S. Thesis, Univ. Wisconsin. Univ. Microfilms, Ann  Arbor,
      Michigan.


                                •546-

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                                -59-
                 kinetic constants and microbial growth
WRIGHT, R. T., and HOBBIE, J. E. 1965. The uptake of organic solutes in
     lake water. Limnol. Oceanogr., 10: 22-28.

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