Effects of Organic Matter on Solubilities and Crystal Form of Carbonates

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1 AM. ZOOLOGIST, 9: (1969). Effects f Organic Matter n Slubilities and Crystal Frm f Carbnates YASUSHI KITANO, NOBUKO KANAMORI, AND AKIRA TOKUYAMA Water Research Labratry, Faculty f Science, Nagya Unixjersity, Chikusa-ku, Nagya, Japan SYNOPSIS. The results f a study f the rle f rganic cmpunds in the frmatin f carlxmate crystals in marine bilgical systems are reprted. In an increasing cncentratin f certain rganic cmpunds which cmplex calcium ins, the prprtin f aragnite decreases and that f calcite increases. In increasing cncentratins f magnesium ins the prprtin f aragnite increases and that f calcite and vaterite decreases. When the influence f rganic cmpunds is greater r smaller than that f magnesium ins, nly calcite r nly aragnite is frmed, respectively. Organic cmpunds frming a strng cmplex with calcium ins cause the frmatin f magnesium-rich calcite, and with an increase in temperature and the cncentratin f magnesium ins, the magnesium carbnate cntent f precipitated magnesian calcite increases. When the influence f rganic cmpunds is almst equivalent t that f magnesium ins, in increasing r decreasing temperatures, the prprtin f calcite decreases r increases, respectively, and the prprtin f aragnite increases r decreases, respectively. The cncentratin f magnesium ins in the bdy fluids f marine calcareus rganisms seems t differ little frm that f ther rganisms, and seems t be similar t that f sea water. Only the presence f certain rganic cmpunds brings abut the frmatin f the carbnate crystals bserved in marine bilgical systems. The very imprtant rle f rganic matter in the frmatin f crystals fund in skeletal carbnates is emphasized. A large amunt f carbnate sediments is distributed very widely n the surface f the earth. These sediments have cllected as carbnate fssils during a lng gelgic time. Mst sedimentary carbnates are derived frm the skeletal parts f calcareus marine rganisms. The majr cmpnent is calcium carbnate, which has three different crystalline frms: calcite, aragnite, and vaterite. In marine bilgical systems calcites (Mg-pr calcite and Mg-rich calcite) and aragnite are fund, but vaterite is nt (Kitan, 1964). Magnesium carbnate in skeletal calcites is present as a slid slutin between calcite and dlmite r magnesite (Kitan and Furutsu, 1959). And Mg-rich calcite (which is called magnesian calcite) and aragnite (pr in magnesium carbnate) are unstable relative t Mg-pr calcite under natural cnditins f temperature and pressure (Jansen and Kitan, 1963). The mineralgical cmpsitin f carbnate culd indicate the physicchemical nature f the envirnment, that is, the 681 temperature r the salinity f sea water in which the carbnate was frmed (Kitan, 1967). The crystal frm f carbnate greatly cntrls the cntent f minr elements f carbnate, a matter f great gechemical significance. In this regard, there is need t knw what factrs cntrl the frmatin f the three crystals in marine bilgical systems. Tw appraches have been used in the past t determine these factrs: (1) field bservatins t learn the relatinships between the crystal frms f carbnate skeletns cllected and the physicchemical nature f the envirnment in which the skeletns have been frmed; (2) labratry experiments n the synthesis f carbnate crystals fund in marine bilgical systems frm simple slutins the prperties f which are very clse t thse f media fr calcificatin in marine bilgical systems. In the present investigatin the authrs studied the cntrlling factrs using the secnd apprach. Certain characteristics which are very difficult t bserve in inrganic systems, but are familiar in bilgical systems, e.g., the frmatin f Mg-rich calcite at lw

2 682 YASUSHI KITANO, NOBUKO KANAMORI, AND AKIRA TOKUYAMA ; --n KJC ' The crystal frm f carbnate in the skeletns f the three representative grups f marine calcareus rganisms is pltted in Figure 1. Represented are (1) rganisms which secrete skeletal parts cmpsed nly f aragnite in the range f bilgical temperatures, and (2) rganisms which frm calcite in the same range f temperature. With increasing sea water temperatures, the magnesium carbnate cntent f calcite increases. The rate f increase in the magnesium carbnate cntent with temperature varies with the phylgenetic level f the rganism. Furthermre, with increasing cncentratin f magnesium ins in sea water, the magnesium carbnate cntent f skeletal calcite increases. (3) Certain rganisms which depsit calcite in ne prtin and aragnite in anther prtin f their skeletns are included. With increasing temperature f the sea water, the prprtin f aragnite increases, that f calcite decreases, and the magnesium carbnate cntent f the calcite prtin increases. The frmatin f the three carbnate crystals is cntrlled by bilgical species, temperature, and the cncentratin f magnesium ins in sea water. Temp IIC. I. A plt f per cent aragnitc vs. envirnmental temperature in the skeletal parts f marine calcareus rganisms., Framiniferans, spnges, echinderms, asterids, phiurids, crinids, crustaceans, barnacles, alcynarian crals, pelagic algae, hrachipds, and thers: O, Madreprian crals, gastrpds, pelecypds, bryzans, benthic algae, annelids, and thers; X, Serpulids, Schizprella, Mytilus, I.ittrina, pelecypds, annelids, gastrpds, bryzans, and thers. temperatures and pressures, are dependent n the presence f rganic substances in the parent medium. The present paper reprts the results f a study f the rle f rganic materials in the parent medium n the frmatin E carbnate crystals in marine bilgical calcificatin. OBSERVATIONS RESULTS OF LABORATORY EXPERIMENTS The frmatin f carbnate as either aragnite, Mg-pr calcite, r Mg-rich calcite is prbably influenced by the fllwing factrs (Kitan, 1964): (1) the presence f certain inrganic ins and cmpunds in the parent slutin, (2) the presence f certain rganic matter in the parent slutin, (3) the temperature, (4) enzymes (carbnic anhydrase) and bacteria, (5) the mechanical cnditins fr frming carbnate, including the rate f frmatin, (6) nuclei fr frming carbnate, and (7) the transfrmatin f the crystal f carbnate after the carbnate has been frmed. Factrs 1-6 are related t the rate at which carbnate is frmed. The fllwing basic chemical reactin was used fr making calcium carbnate, t learn the influence f the factrs listed abve: carbnate was precipitated frm calcium bicarbnate slutin with escape f carbn dixide gas t the atmsphere. The reactin was used because it is ne f the hmgeneus precipitatin reactins, and calcium bicarbnate slutin des nt disslve any ther matter than calcium and carbnate. The crystal frms f precipitated carbnate were identified and cmpared with thse f skeletal materials. The calcium bicarbnate parent slutin shuld cntain inrganic materials present in sea water and rganic matter fund in the bdy fluids f marine calcareus rganisms. Enzymes were nt added t the parent slutin in the present

3 SOLUBILITIES AND CRVSTAL FORM OF CARBONATES 683 experiment, and the rate f carbnate frmed was cntrlled by changing the rate f escape f carbn dixide frm the slutin mechanically. The labratry experiments shwed that the mst imprtant factrs are 1-3. The influences f varius inrganic ins and cmpunds such as H +, Li+, Na+, K+, Rb+, Cs+, Mg 2 +, Cu 2 +, Zn 2 +, Mn 2 +, Hg 2 +, Ca 2 +, Sr2+, Ba2+, Pb 2 +, OH- C1-, NO 3 - SO 4 2 -, HCO,,-, CO/- and CO 2 n the crystal frm f precipitated carbnate were reprted by Kitan (1962«). In the experiment, calcium carbnates were precipitated frm calcium bicarbnate slutins int which inrganic ins and materials had been added in varius prprtins, and the crystal frms f precipitated carbnates were identified. Frm the previus wrk it was expected that inrganic ins having a pssible influence in marine bilgical systems wuld be sdium, magnesium, chlride, sulfate, and bicarbnate ins in the parent slutin. The results indicate that magnesium ins in the parent slutin have the greatest influence (Fig. 2). Magnesium ins favr the frmatin f aragnite, and hinder the frmatin f calcite and vaterite (Kitan and Hd, 1962; Kitan, 1962&). In the labratry experiment, the prprtin f aragnite increases and that f calcite decreases with increasing temperature, as bserved in skeletns (Kitan, 19626) g 1 < NCI FIG. 2. Salt cntent in calcium bicarbnate mther slutin, mcq/l. Influence f salt in mther slutin n crystal type f frmed calcium carbnate (28 ± 3 C)'. SO Ci't e,pyfuvie / *"" ^^Glutamte - -" Galctse,Aceiatt V\ Dextr se. Serine Glycine '. Turine Organic material in mther slutin (g/ ) ( 27+2*C) FIG. 3. Plymrphic cmpsitin f calcium carbnate frmed frm calcium bicarbnate slutin cntaining rganic material and magnesium chlride. Kitan and Hd (1965) reprted the results f preliminary experiments cncerning the influence f rganic matter present in a parent slutin n the crystal frm f precipitated carbnate (Fig. 3). Selectin f varius rganic cmpunds used in the experiment was based n previus reprts n the mechanism f calcificatin and the distributin f rganic matter in calcareus rganisms. Calcium, bicarbnate, rganic cmpunds, and magnesium chlride slutins were mixed in varius prprtins in an Erlenmeyer flask, plugged with cttn, and allwed t stand at rm temperature fr 2 t 8 weeks. The rate cnstants in the reactin with the first type rder were calculated (Fig. 4). The fllwing results were btained: (a) Organic cmpunds such as citrate, malate, pyruvate, and glycgen frm a cmplex with calcium ins, enlarge the slubility f calcium carbnate (Fig. 5), reduce the rate f precipitatin f carbnate, and favr the frmatin f the stable frm, calcite, even in the presence f magnesium ins which greatly hinder the frmatin f calcite. This wuld suggest the pssibility f the precipitatin f magnesian calcite at lw temperatures and pressures. In the labratry, calcites culd be frmed frm calcium bicarbnate slutins cntaining magnesium ins and certain rganic cmpunds

4 684 YASUSHI KITANO, NOBUKO KANAMORI, AND AKIRA TOKUYAMA Organic material added (g/l ) PIG. 4. Rate-cnstant in the reactin Ca (HCO 3 ). -» rganic cmpunds (temperature 27 ± 2 C). CaCO 3 + CO 2 f -f H 2 O in the presence specific such as sdium citrate, malate, r pyruvate by allwing the slutins t stand still at lw temperatures and pressures (Kitan and Kanamri, 1966). The precipitated calcites frm the slutins cntained magnesium carbnate. The values fr the difference in spacing f (0114) reflectin between pure calcite and precipitated calcites were pltted against magnesium carbnate cntent as chemically determined (Fig. 6). The linear relatinship between these variables indicates magnesium carbnate is cntained as a frm f a slid slutin between calcite and dlmite (magnesian calcite). Figures 7 and 8 shw the magnesium carbnate cntent f magnesian calcites precipitated frm calcium bicarbnate slutins cntaining magnesium chlride and sdium citrate. The figures indicate that an increase in the cncentratins f magnesium ins and rganic cmpunds, such as citrate, and an increase in temperature, cause a Mg-richer calcite. The presence f sdium citrate r malate favrs the frmatin f Mg-rich calcite, prbably by cmplexing calcium ins, enlarging the O O O AIR ORGANIC MATERIAL ADDED (g/l) FIG. 5. Slubility f calcium carbnate in slutins cntaining specific rganic cmpunds in cntact with ne atmsphere f CO 2 gas and air.

5 SOLUBILITIES AND CRYSTAL FORM OF CARBONATES j "s 0.03 I 0.02 c CD' cp slubility f calcium carbnate and n the rate f carbnate precipitatin, have little effect n the crystal frm f precipitated carbnate. (c) Organic cmpunds which enlarge the slubility f calcium carbnate and reduce the rate f carbnate precipitatin t a mderate degree have nly a mderate influence n the crystal frm. Their influences were different: chndritin sulfate, succinate, and lactate favr the frmatin f calcite, and taurine favrs the frmatin f aragnite n Weight per cent MgCO- FIC. 6. The relatin between magnesium carbnate cntent and interplanar spacing. slubility f calcium carbnate, reducing the rate f frmatin, giving a stable calcitic lattice cnfiguratin and causing a capture f magnesium in the calcitic lattice. Many ther rganic cmpunds were examined fr cntent f magnesium carbnate (Kitan and Kanamri, 1966). It is knwn that the cntent f magnesium carbnate differs with the kind and the cncentratin f rganic cmpund. (b) Cmpunds such as galactse and dextrse, which have little effect n the '\ 800 mj/500 ml Mg' f, 600 mg/500 ml Mg'+ 400 mj/500 ml -O- Mg H. 200 mg/500 nil 0 100!C SCO 10CO W0 Na citrate cncentratin (citrate ins cntent, mj/500 mil in the mther slutin (500 mil CalHCftl, + MgCI. + Na citrate FIC. 7. MgCO 3 cntent f magnesian calcite frmed frm the Ca (HCO 3 ) 2 slutin cntaining MgCl 2 and sdium citrate (20 ± 1 C). S 10»p 9 I 8 I 1 I f 4 " 2» 1 citrate ins 200mg/500.ml citrate ins 100mg/500ml citrate ins 50mg/500ml Temperature ( C) f mther slutin FIG. 8. MgCO 3 cntent f magnesian calcite frmed frm the calcium bicarbnate mther slutin (500 ml) cntaining MgCl 2 (Mg 2 *, 400 mg/500 ml) and sdium citrate (citrate ins, mg/500 ml). These results were btained when the parent slutin was undisturbed during the prcess f precipitatin. When the slutin was stirred, the results were nt s simple; the effects f stirring n the crystal frm and the mechanism remain unslved. Cncerning the rle f rganic cmpunds disslved in a parent slutin, the fllwing interesting facts have been bserved first in ur labratry experiment. Heavy metal ins such as cpper, zinc, nickel, r manganese favr the frmatin

6 686 YASUSHI KITANO, NOBUKO KANAMORI, AND AKIRA TOKUYAMA 0D0I FIG. 9. Mineralgical cmpsitin f carbnate frmed frm calcium bicarbnate slutin cnlain- f aragnite much mre than d magnesium ins in a parent slutin (Fig. 9). The extent f their influence n the frming f aragnite increases in the fllwing sequence, althugh the influences f zinc and manganese disslved in the parent slutin are very cmplex: Cu 2 +> Zn 2 +> Ni 2 +> Mn 2 +> Mg 2 +. This sequence is in agreement with that f the secnd inizatin ptential value, in ther wrds, that f the value f the stability cnstant f cmplex between metal ins and carbnate ins in slutin. Thus, we wuld expect that metals disslved as bth cmplex and free inic frms are much mre favrable fr aragnite frmatin than thse disslved in either cmplex r inic frm. We have examined als the influence f metal ins, cexisting- with rganic matter which frms cmplexes with the metal ins, n the crystal frm f precipitated carbnate. Figure 10 shws a plt f the prprtin f aragnite in precipitated carbnate against the cncentratin f zinc disslved in the calcium bicarbnate parent slutin with glycine. The value f the stability cnstant between zinc ins and glycine, [Zn 2 + ] X [Glycine-]-y[Zn-Glycine 2 "], is 10-»- 4. Figure 10 shws that the influence f zinc in the parent slutin n the frmatin f Me'(m q/i) in" metal nitrate at C. aragnite increases with increasing cncentratin f glycine added t the parent slutin up t a certain cncentratin, and then decreases with a further increase in the cncentratin f glycine. This indicates that metal disslved in the parent slutin in bth cmplex and free inic frms is much mre favrable fr the frmatin f aragnite than in either cmplex r free inic frms alne. Althugh such an interesting mechanism has nt been clarified cmpletely, the basic data given here n the rle f rganic matter in a parent slutin seem t help in understanding the factrs cntrlling the frmatin f carbnate crystals in marine bilgical systems (Kitan, 1964). The majr factrs seem t be (1) the cncentratin f magnesium ins in a parent medium, (2) the cncentratin f certain rganic materials which cmplex calcium ins in a parent medium, (3) the temperature f a parent medium, and (4) the rate f depsitin f carbnate in relatin t the presence f enzymes such as carbnic anhydrase. With increasing cncentratin f certain rganic materials which cmplex calcium ins, and with decreasing temperature, the

7 SOLUBILITIES AND CRYSTAL FORM OF CARBONATES g FIG. 10. Mineralgical cmpsitin f carbnate frmed frm calcium bicarbnate slutin cntain- «sptted circle duble circle A X ttal glycine Zn (mea/l) ing metal nitrate and glycine at 36 ± 2 C. Cncentratin f glycine (meq/1) : 0 x i- 3 X 10" X 10i X 10i X 10= glycine" X X X 10" X lo-i 2.3 X 10 1 prprtin f aragnite decreases and that f calcite increases. With increasing cncentratins f magnesium ins in a parent medium, the prprtin f aragnite increases and that f calcite and vaterite decreases. When the influence f rganic material is greater r smaller than that f magnesium ins, nly calcite r nly aragnite is frmed, respectively. And it is nted that rganic material frming a strnger cmplex with calcium ins in a parent medium causes the frmatin f a Mg-richer calcite, and that with increase in the temperature and the cncentratin f magnesium ins in a parent medium the magnesium carbnate cntent f precipitated magnesian calcites increases. When the influence f rganic material is almst equivalent t that f magnesium ins, with increasing r decreasing temperature, the prprtin f calcite decreases r increases, respectively, and the prprtin f aragnite increases r decreases, respectively. The cncentratin f magnesium ins in the bdy fluids f marine calcareus rganisms seem little different frm that f ther rganisms. It seems t be similar t that in sea water. If the term "bilgical species" in the sectin n "Observatins" is exchanged fr the phrase "kind and cncentratin f rganic material in a parent medium", the bserved facts are cmpletely in accrdance with the results f the labratry experiments (Kitan, 1968). Only the presence f certain rganic materials accmplishes the frmatin f carbnate crystals bserved in marine bilgical systems. We must emphasize the very imprtant rle f rganic material in the frmatin f crystals fund in skeletal carbnates.

8 688 YASUSHI KITANO, NOBUKO KANAMORJ, AND AKIRA TOKUYAMA REFERENCES Jansen, (., and Y. Kitan The resistance f recent marine carbnate sediments t slutin. J. Oceangr. Sc. Japan 18: Kitan, Y., and T. Furutsu The state f a small amunt f magnesium cntained in calcareus shells. Bull. Chem. Sc. Japan 33:1-4. Kitan, Y. 1962a. The behavir f varius inrganic ins in the separatin f calcium carbnate frm a bicarbnate slutin. Bull. Chem. Sc. Japan 35: Kitan, Y. 1962i>- A study f the plymrphic frmatin f calcium carbnate in thermal springs with an emphasis n the effect f temperature. Bull. Chem. Sc. Japan 35: Kilan, Y., and D. W. Hd Calcium carbnate crystal frms frmed frm sea water by inrganic prcesses. J. Oceangr. Sc. Japan 18: Kitan, Y On factrs influencing the plymrphic crystallizatin f calcium carbnate fund in marine bilgical systems, p In Recent researches in the fields f hydrsphere, atmsphere and nuclear gechemistry. Maruzen C., Ltd., Tky. Kitan, Y., and D. VV. Hd The influence f rganic material n the plymrphic crystallizatin f calcium carbnate. Gechim. Csmchim. Acta 29: Kitan, Y., and N. Kanamri Synthesis f magnesian calcite at lw temperatures and pressures. Cechem. J. 1:1-10. Kitan, Y Pale-chemical cmpsitin and pale-temperature f cean water. Kagaku, Iwanami C., Ltd. 37: Kilan, Y Factrs cntrlling the crystal frm and the minr element cntent f carbnates frmed in marine bilgical systems the gechemical significance f carbnate fssil. Chem. and Chem. Industry 21:

Step 3: The nitrates and nitrites are used by plants to make amino acids which are then used to make plant proteins.

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