Carbon Monoxide in the Biosphere:
                CO Emission by Fresh-Water  Algae
                       FINAL REPORT TO:

                  Coordinating Research  Council
                     Thirty  Rockefeller  Plaza
                   New York, New York  10020
                              and
                 Air  Pollution Control  Office,  EPA
Principal Investigators;
  H. L Crespi  and J.  J. Katz

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         Carbon Monoxide in the Biosphere:  CO Emission


                      by Fresh-Water Algae*
      H. L. Crespi, Doris Huff, H. F. DaBoll and J. J. Katz

                       Chemistry Division

                  Argonne National Laboratory

                     Argonne, Illinois 6C439
 ..
  This work supported by Coordinating Research Council--U.S.
Environmental Protection Agency and under the auspices of the
U.S. Atomic Energy Commission.  Work  performed  during the
year  1971.  Final  report,  October,  1972.

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                               -2-
                             SUMMARY



     The chemical processes associated with the biosynthesis

and degradation of the photosynthetic pigments in algae produce

large amounts of CO.   Senescent cells are found to produce CO

in excess of that that can be accounted for only from degrada-

tion of chlorophyll indicating the existence of additional plant

sources of CO.  Our results indicate that plants may be the
            o
source of 10  tons or more of CO per year.

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                               -3-
     An accurate assessment of the role of carbon monoxide in



the atmosphere requires that all large natural sources of car-



bon monoxide be detected and the magnitude of their CO contri-



butions to the atmosphere be determined.  The discovery of



large and previously unknown natural sources of carbon monoxide



would obviously have considerable impact on the generally held



opinion that the carbon monoxide of the atmosphere is largely



man-made  (1).  We believe, on the basis of experimental work



described here, that the biogenesis, and, particulary the degra-



dation, of photosynthetic pigments are such large and previously



unsuspected contributors to CO in the atmosphere.  The older lit-



erature contains intimations to this effect.  Thus, there are



reports that higher plants  (2) and marine algae  (3) evolve CO.



Ocean waters appear to act as a natural source of CO (4,5).



An atypical fresh-water blue-green alga has also been shown to



produce CO  (6).  The relationship between these observations and



the generality of the phenomenon have, however, not been made



explicit.



     There are at least two pathways by which CO can be produced



by algae and higher plants.  Blue-green algae have two character-



istic photosynthetic pigments called phycocyanin and phycoerythrin,



whose prosthetic groups, phycocyanobilin and phycoerythrobilin,



result from the oxidation of a tetrapyrrole  macronucleus such as



chlorophyll (6).  (See Figure 1 for the structural formula of

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                               -4-
these tetrapyrrole compounds. )   The chemistry of this process



probably is similar to the conversion of the heme of hemoglobin



in animals to the bile pigments, a process which, as is well



known (7), produces one molecule of CO for each molecule of heme



transformed to bile pigment.  The macrocycle ring is opened by



oxidation of the carbon atom at the a bridge position to yield



a linear tetrapyrrole and a molecule of carbon monoxide.  The



chemical relationship between chlorophyll and algal bilins is



very similar to that of heme and bile pigment, and each molecule



of tetrapyrrole  converted to bilin would produce one molecule of



CO (6).  Thus, as the blue-green algae grow, they evolve CO.



It would be expected that as all blue-green algae contain phyco-



cyanin and/or phycoerythrin, all would produce CO.  However,



under our culture conditions,  production of CO by blue-green



algae by this process turns out to be strongly species specific,



and for no very obvious reason.



     The degradation of chlorophyll in dying plant material is



a second way for.,plants to produce CO, for the degradation of



chlorophyll might also follow a course analogous to the degrada-



tion of heme.  All photosynthetic organisms that fix carbon



dioxide and produce oxygen, without exception, contain chlorophyll



a.  Thus, it might be supposed  that the degradation of chlorophyll



in algae and in higher green plants could produce large amounts



of CO.

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                               -5--
     Th e work described here shows that the catabolism of



chlorophyll in algae does indeed make a large contribution to



the carbon monoxide content of the atmosphere.  This is a



previously unrecognized large natural source of CO that will



have to be taken into account in describing the inventory of CO



in the atmosphere.  Our observations furnish an initial basis



for the interpretation of the CO isotope studies of Stevens (8),



which appear to require the existence of a large, unknown nat-



ural source of CO.








                   Techniques of Algae Culture




     Both green and blue-green algae were cultured by the



techniques described by DaBoll et al. (9) and Crespi et al. (10).



The nutrient solutions contain a standard mix of salts (9) and



carbon dioxide is fed to the cultures as a mixture of 5$ COp-95^



Np.  The feed gas is passed over Hopcalite (a manganese-copper



oxide catalyst) to remove all traces of CO.  The light intensity



is controlled by means of neutral density screens.  As a culture



grows from a small inoculum, the light intensity is increased in



steps of from 12.5 to 25 to 50 to 100 percent of the maximum



light intensity.  All cultures are thermostated for temperature



control.  Figure 2 is a photographic view of the "algae farm".

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                               -6-
                   Analysis of GO,  Chi,  Bilin




     An P and M Model 700 gas chromatograph with a flame ioni-



zation detector was modified for the  detection of low concen-



trations of carbon monoxide (11).   A  gas sampling system was



added so that the sample can be swept directly from a collection



tube into the chromatograph gas carrier  stream.   A catalyst



tube with furnace and hydrogen supply was placed bewtween the



chromatographic column and the detector  to convert CO to methane



(CO may be determined directly with a thermal conductivity



detector,, but the sensitivity is low).  A nickel catalyst is used



for this conversion.  Carbon dioxide  is  removed by a COg absor-



ant positioned before the sample collecting tube, and Linde 5A



molecular sieve is used for the GC column packing to retain any



residual trace of carbon dioxide and to  separate methane, if any,



from CO.  An absolute sensitivity of 0.005 microliters  (1 ppm



CO in a 5 ml sample) is readily attained, with a precision of



ħ 10$.  Our standard gas mixtures (Matheson) have also been



analyzed manometrically.  Chlorophyll was extracted and analyzed



according to the methods of Strain and Svec  (12) and phycocyano-



bilin was determined as phycocyanin  (13).







                     Results and Discussion




     The results of a survey for CO  evolution of algae under



routine culture in our laboratory are shown  in Table 1.

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            Table 1.  CO Production by Various Algae
      Species                       Type               Co Evolved




Phormidium luridum               Blue-green                +



Fremyella diplosiphon            Blue-green



Synechococcus lividus            Blue-green



Chlorella vulgaris                 Green                   +



Scenedesmus obliquus               Green                   +
     The blue-green alga  Phormidium luridum produces CO at the



rate of 100-300 |_ig per gram of new growth, a CO production rate



that correlates with the rate of biosynthesis of the photosyn-



thetic pigment phycocyanin.  However, the blue-green algae



Syne choc oc cus_ lividus and Fremyella diplosiphon evolve CO at very



much lower levels or perhaps not even at all.  As all these blue-



green algae contain phycocyanin, it would appear that either



different biosynthetic pathways are used for the production of



phycocyanin, or that the algae differ from each other in their



ability to utilize endogenously produced CO.  It is entirely pos-



sible that CO in these organisms is being fixed, as recent



reports (14) indicated that many soil organisms are able to fix



CO.  The environmental impact of blue-green algae may thus involve



both large-scale emission and fixation of CO.

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                               -8-
     Figure 3 is a plot that shows CO evolution by a culture of



the blue-green algae Phormidium luridum.   CO was evolved



throughout the culture cycle at a rate dependent on light in-



tensity and at a level consistent with the amount of CO expected



from the extent of phycocyanobilin biosynthesis.  An average of



about 50 x 10~3 p,l/min of CO were evolved during the approxi-



mately 160-hour lifetime of the culture.   Integration over this



time period gives a total of ^80 jj,l or 600 u.g total CO evolved



by this culture.  At harvest, our Phormidium cultures contain



6.0 grams of newly formed algae of which about 8 percent is



phycocyanin.  Since phycocyanin is 4 percent bilin by weight,



the culture will have generated 19.2 milligrams of bilin from



which 925 |_ig of CO is expected to be evolved.  This number is



somewhat higher than the measured value of 600 |j,g, but the CO



that was evolved is probably due to bilin biosynthesis, as the



rate of CO evolution appears related to light intensity is shown



by Figure 3, and therefore to biosynthetic activity.



     Figures 4 and 5 illustrate the growth and CO emission of



Phormidium luridum under conditions similar to the cultures  shown



in Figure 3, but over a longer time period.  As the culture  be-



came very dense, the rate of CO evolution increased to levels



much higher than those expected from bilin biosynthesis only.


                    -S
A total of 7-10 x 10 -" moles of CO were emitted during the course

                                             _c
of each of these experiments.  About 2-3 x 10 J moles of CO  is

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                               -9-
                                                                 _
expected from bilin synthesis, which leaves an excess of 5-7 x 10 J

moles of CO.  While this number corresponds clearly to the total

amount of chlorophyll in these cultures, there is no evidence

of chlorophyll degradation during the course of the experiment.

These results indicate a source of CO other than bilin synthesis

or chlorophyll degradation.   It is possible that Ph. luridum, a

filamentous organism, some form of cell senescence occurs

throughout the growth cycle.  It has been observed in this Lab-

oratory  (J. Norris, personal  communication) that Ph. luridum

cells often generate a very weak electron spin resonance photo-

signal,  an indication of possible cellular degradation.  We have

also found that the "typical" results depicted in Figures 3-5 are

not consistently reproducible, so that one must postulate processes

involving carbon monoxide other than those associated with the

simple scheme outlined for  tetrapyrrole metabolism.

     Figures 6, 7, and 8 show the results of monitoring the CO

evolution by cultures of the  green alga, Scenedesmus obliquus.

Because  green algae contain no bilinoid pigments, no CO is ex-

pected from this source, and  no CO evolution is, in fact, ob-

served until after about 450  hours of growth, when a dramatic

output of CO begins.  CO emission begins as soon as the algae go

into the stationary phase of  growth and begin to die.  Table 2

shows the results of analysis of various portions of the curves

shown in Figures 6, 7, and 8.  During the initial phase of CO

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                               -10-
      Table 2.   Correlation of CO Emission with Chlorophyll
                   Disappearance in S.  obliquus
Experiment
  Culture
    Days
                                 Total  CO
                                 Emitted
                               (moles x 10
                                            5
                                                     Decrease in
 Chlorophyll
(moles x 105)
  Fig. 5
  Fig. 6
Fig. 6
  Fig. 7
  Fig. 7
     3
(Days 23-26)
     6
(Days 23-29)
     7
(Days 29-36)
     2
(Days 23-25)
     3
(Days 32-35)
                                    5.4
                                   11.0
                                    2.3
                                    5-5
                                                          9-9
     13.7
                                                          6.7
     10.0
      9.0
evolution and chlorophyll disappearance,  the amount of CO evolved
is equal to or lower than the amount of chlorophyll that has
disappeared (on a molar basis).   In the later stages of growth,
however, considerably more CO is evolved than can be accounted
for by chlorophyll degradation.   The data of Figure 8 indicate

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                               -11-
that CO evolution from S_. obliquus is related to plant senescence.



At day 26 the entire algal culture was centrifuged, washed and



resuspended in fresh nutrient medium.  Total chlorophyll content



then increased and CO evolution decreased as the cells became



more viable and at day 32 CO evolution abruptly increased as



chlorophyll content went sharply down.



     Figure 9 shows the CO evolved from a culture of Chlorella



vulgaris as a function of growth and chlorophyll content.  Unlike



the other green alga, S_. obliquus, the Chlorella culture emitted



CO at a low level through most of its life cycle and there is no



rapid emission of CO as chlorophyll content drops at senescence.



     These data are consistent with the following interpretation:



(1) the biosynthesis of bilinoid pigments in blue-green algae



yields CO;  (2) the degradation of chlorophyll in both blue-green



and green algae yields COj   (3) an additional unknown source of



CO exists in plants.  It is possible that additional CO is evolved



from the oxidation of phenolic types of compounds  (15,16) as it



has been shown that flavonoid degradation by molds yields CO (17).



Figure 10 summarizes our results.  The fact that some of the algae



examined here do not emit CO may be due to the fact that CO can



be fixed by many organisms (14).  Thus, the algae may fix the CO



that they generate, or the particular heterotrophic flora



supported by these cultures may fix CO.  Our results complement



those of C. M. Stevens and co-workers (8) who have observed CO

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                               -12-
emissions from trees.  These workers have observed, in the

northern hemisphere, an autumnal burst of CO that corresponds
                                     o
to an emission of the order of 5 x 10  tons of CO over a 1.5

month period.  Fogg  (18) estimates that the total annual world

yield of photosynthesis to be 25 x 1010 tons of organic matter.

If it is assumed that 0.5$ of this organic matter is chlorophyll,

chlorophyll degradation could yield 6 x 10^ tons of CO per year.

Bilin biosynthesis could account for about the same amount of
                                                              o
CO per year, so these two sources could emit a total of 1 x 10

tons of CO per year.  The data of Stevens e_t al. (8) indicate

natural sources of CO in addition to bilin biosynthesis and

chlorophyll degradation, and our data indicate that algae and

other plants are contributing in further unknown ways to the

large natural CO emissions.

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                           REFERENCES
 1.   L.  S. Jaffe, Ann. N. Y. Acad. Sci.  174,  76  (1970)-
 2.   S.  Wilks, Science 129, 964  (1959).
 3-   C.  C. Delwiche, Ann. N. Y.  Acad. Sci.  174,  116  (1970).
 4.   J.  W. Swinnerton, V. J. Linnenbom  and  R.  A.  Lamontagne,
     Science 167, 984  (1970).
 5-   D.  F. Wilson, J. W. Swinnerton  and R.  A.  Lamontagne,
     Science 168, 1577  (1970).
 6.   R.  F. Troxler, A. Brown, R. Lester and P. White,  Science
     167, 192  (1970).
 7.   T.  Sjostran, Ann. N. Y. Acad. Sci.  174,  5 (1970).
 8.   C.  M. Stevens, L. Krout, D. Walling, A.  Venters,
     A.  Engelkemeir and L. E. Ross,  Earth and Planetary
     Sciences  Letters, In press.
 9.   H.  F. DaBoll, H. L. Crespi  and  J.  J. Katz,  Biotech.  Bioen^
     ;4,  281  (1962).
10.   H.  L. Crespi, H. F. DaBoll  and  J.  J. Katz,  Biochem.
     Biophys.  Acta 200, 26  (1970).
11.   J.  W. Swinnerton and V. J.  Linnenbom,  J.  Gas Chromatog.
     5,  570  (1967).
12.   H.  H. Strain and W. A. Svec,  in The Chlorophylls,  L.  P.
     Vernon  and  G. R. Seely, Eds., Academic Press, N.  Y.,  1966,
13.   H.  L. Crespi, U. Smith and  J. J. Katz, Biochemistry "]_,
     2232 (1968).

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14.  R. E. Inman, R. B. Ingersoll and E. A.  Levy,  Science



     172, 1229  (1971).



15.  S. Miyahara and H. Takahashi, J. Biochem.  69,  231 (1971).



16.  T. Matsuura, H. Matsushima and H. Sakamoto,  J.  Am.  Chem.



     Soc. 89, 6370  (1967).



17.  D. W. S. Westlake, J. M. Roxburgh and  G. Talbot,



     Nature 189, 510  (1961).



18.  G. E. Fogg, Photosynthesis, The English Universities



     Press, Ltd., London, 1968.

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                         FIGURE LEGENDS




Figure 1 -- Structural formulas of heme, bilirubin, chloro-



            phyll a,, phycocyerobilin, and phycoerythrobilin.



Figure 2 -- View of the algae farm showing Lucite rocking



            trays and associated equipment.



Figure 3 -- The production of carbon monoxide by the blue-



            green alga Phormidium luridum.  Culture conditions



            are as described in the text, with 5$ COp-95^ N~



            being fed at a rate of 18 ml/min.  As the light



            is stepped up in intensity, CO emission increases,



            a reflection of an increased rate of bilin synthesis,



            At about 95 hours, the lights were turned off, and



            at 100 hours, turned on again.



Figure 4 — Growth and CO production by the blue-green alga



            Phormidium luridum under standard culture condi-
            tions, but with a 5$ CO^-^fo N2 feed rate of 9



            ml/min.  As compared to the culture described by



            Figure 1, there is a large CO output as the cul-



            ture ages .



Figure 5 -- Growth, CO production, chlorophyll and bilin levels



            during the course of culture of Ph. luridum



            under culture conditions as for the culture of



            Figure 3-  There are large CO emissions without



            concommitant disappearance of chlorophyll.

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Figure 6 -- Growth,  CO and chlorophyll production by the green



            alga Scenedesmus obliquus.  CO production corre-



            lates with cessation of growth and a decrease in



            chlorophyll content of the cells.



Figure 7 — Growth,  CO and chlorophyll production by S_.



            obliquus followed far into the stationary phase



            of growth.  Even after disappearance of most of



            the chlorophyll, CO is being emitted at a rapid



            rate.



Figure 8 — Growth,  CO and chlorophyll production by a culture



            of S_. obliquus thas was centrifuged, washed, and



            resuspended in fresh nutrient medium at day 26.



            Although the culture was in the stationary phase



            of growth at the time of resuspension, cell den-



            sity increased further in the fresh medium, as did



            the chlorophyll content, and CO emission dropped.



            After a few days, the normal processes of



            senescence resumed.



Figure 9 -- Growth,  CO and chlorophyll production by the green



            alga Chlorella vulgaris.  Small amounts of CO are



            emitted throughout the life cycle.



Figure 10 - A schematic picture of CO emission by algae.

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                  CH=CH2
                               H2C = CH
       Heme
                         CH 3
                                                  CH3
      CH2
      I
R02C-CH2   CH3 0

      Chlorophyll
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            H
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OH3  CH2
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Bilirubin
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FIGURE 2

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         Light Intensity (% of maximum)

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                                    feed gas at 18 m l/min.
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                      Days of  Growth
                CO  Production  by  Phoridium luridum
                                          FIGURE 3

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Light Intensity (% of maximum)
12 25 50 100
0
6     8      10     12
Days  of  Growth
14
16
 Growth  and CO Production by Phormidium  luridum
                                                      FIGURE 4

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         Growth, CO and Chlorophyll Production by C.  vulgaris
                                                          FIGURE 9

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Chlorophyll

Precursors
                                  Senescence
                      Chlorophyll	*•  CO
                          t
Growth
                            Green  and
                            Blue-green  Algae
                            Blue-green
                            Algae
                    Bilins and  CO
                                    FIGURE 10

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