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Limits of Coprecipitation of Cadmium and Ferrous Sulfides

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Limits of Coprecipitation of Cadmium and Ferrous Sulfides I .- Table 111. Measurement Dlfferences Between Methods 2&7k& A&-- Data Mean and edd SO, Ppm SO2 Bla8. ppm So2 a palrs tPararosanll ne Moan and estd SO Max Anaheim 160 0.0057 f 0.0071 0.0050 f 0.0034 0.0008 f 0.0065 0.024 Los Angeles 101 0.0191 f 0.0081 0.0071 f 0.0050 0.0120 f 0.0072 0.045 San Bernardino 130 0.0064 f 0.0067 0.0024 f 0.0017 0.0040 f 0.0072 0.029 San Diego 25 0.0019 f 0.0030 0.0035 f 0.0034 -0.0016 f 0.0040 0.013 -a Conductimetric SO2 minus pararosaniline SO*. Literature Cited Table IV. Relative Bias at 0.04 ppm SO2 by Each Method (1) “Directory of Air Quality Monitoring Sites Active in lYS:l”, EPA-450/2-75-006, Mar. 1975. (2) Cooper, R. E., “Statistics for Experimentalists”, Pergamon Press, Conductimetric SO2 Pararosanlllne SO2 1969. Blas at Bias at (3) Blacker, J. H., Confer, R. G., Brief, 11. S., J. Air Pollut. Control 0.04 ppm Carrel 0.04 PP~ carrel Assoc., 23,525 (1973). Cond SO*,’ ppm cooff PRA S02, ppm coeff (4) Hocheiser, S., Santer, d., Ludmann, W. I?., ibid, 16. 2%; Anaheim 0.0282 0.65 0.0008b 0.08 (1966). Los Angeles 0.0267 0.79 0.0048 0.15 (5)~. Terabe. M.. Oomichi. S.. Benson. F. B.. Mewill. V. A.. Thomoson.., San Bernardino 0.0391 0.54 -0.0582c 0.40 J. E., ibid., i7,fjn (1967). San Diego 0.0258 0.55 -0.0301 0.67 (6) Staff Reo. 75-12-2. “Consideration of the California 24-Hour Mean 0.0300 -0.0207 ‘ Ambient kir Quality Standard for Sulfur Dioxide”, California Air Resources Board, June 11,1975. By linear regression. * Mean bias, not significant. 0.04 ppm is largest (7) Booras, S. G., Zimmer, C. E., J. Air Po‘Jut. Control Assoc., 18,512 meaningful negative bias. (1968). (8) Stevens, R. K., Hodgeson, J. A., Ballard, L. F., Decker, C. E., “Ratio of Sulfur Dioxide to Total Gaseous Sulfur Compounds and Ozone to Total Oxidants in the Los Angeles Atmosphere--An In- strument Evaluation Study”, in “Determination of Air Quality”. Conclusions G. Mamantov and W. D. Shults, Eds., pp 83-108, Plenun;, New Estimated bias between the conductimetric and pararos- York, N.Y., 1972. (9) “Air Qualitv Criteria for Sulfur Oxides”. National Air Pol1ut;on aniline methods at 0.04 ppm SO2 by the conductimetric ControiAdmin., Jan. 1969. method ranges to the order 0.04 ppm. (10) Katz. M.. “Inorpanic Gaseous Pollutants”, in “Air Pollution”. Estimated random measurement error ranges (99.7% con- ’ A. C. Stern,’Ed., 2iid ed., Chap. 17, Academic Press, New Yorlc. fidence) are f0.02 and f0.006 ppm for the conductimetric and N.Y., 1968. (11) Neuscheler, R. C., “Selection uf Continuous Sulfur Dioxide pararosaniline methods, respectively. Monitors for Ambient and Source Concentration Levels”, “In- The conductimetric method is unsuitable €or determining strumentation for Air Monitoring”, ASTM STP 555, pp 9-19, compliance with 0.04 or 0.05 ppm 24-h average ambient air American Society for Testing Materials, 1973. quality standards for SOZ. (12) Purdue, L. J., “Performance Evaluation of SO:! Monitoring In- struments”, ibid., pp :3--5. (13) “The Environmental Protection Agency’s Research Program with Primary Emphasis on the Community Henlth and Environ- Acknowledgment mental Surveillance System (CHESS):An Investigative Report”, for Committee on Science and Technology, US. House of Repre- N. R. Crawford and F. W. Morgan’s statistical advice and sentatives, Nov. 1976. assistance ant1 E. G. Loffay and J. R. Ugolini’s computer data handling were invaluable. Received /or review July 22, 1977. Accepted October 25, 1977. Paul E. Framson* and James 0. Leckie Environmental Engineering and Science, Department of Civil Engineering, Stanford University, Stanford, Calif. 94305 ID Cadmium was precipltatcd from aqueous sulfide to as- mium in the Corpus Christi, Tex., estuarine system demon- certain the of sulfide pre- strate that those sediments act alternately as a sink during the cipjtated in aquatic ecosystems. Monitoring cell-dimension summer months when high concentrations of sulfides are trends of cadmium sulfides precipitated from thioacetarlli& present in the surficiai sediments and as B source during the so!utiogs df increasing ferrous corltent allowed estimation of winter when more oxidizing conditions prevail (1).In uno& nrr ,lpper bound 3.5 f 1 x 10 -4 for the distribution coeffi- benthic marine, estuarine, and freshwater environments, cient describing F~Wcocrysta!lization with greenockite. ~1~i~sulfate-reducing bacteria can generate total uqueous sulfrde restilt suggeststhat cadmiurn prcciplbtes primarily ttlrclugh as high as millimolar concerrtration i2,3). Under sml‘ficiently surface exchange with ferrous monosulfide substrates and as reducing conditions* srdimenq mi~~dPhw essentially cnsubstituted CdS in natural sulfidic systems. such as hydrous oxides and bydroxidcs are repkced by SUI+ fides. The PI& of the heavy metal sulfides rmge fram z%? I for ZnS(s) to 53.2 for HgSiu) (2).Hence, a Iia-ga fratxi aqueous heavy metai contammmnt~is likely kmmd as Sediments possess the interesting ability to act as both n menhry sulfids under anaembic condition sink and a source for many trace contaminants. For example, Certain human activities such iL9 dredging, which dimp significant spatial and teinporal variations in zinc and cad- sediments, can effect oxidative diwlution of Ferrous sulfides, 00 13-936X/78/0912-0465$0 1.30/0 G) 1978 American Chemical Society Volume 12, Number 4, Aprd 1978 465 I prompting concern that associated heavy metals may also be where dB and dA represent increments of R+ and A+ pre- released from their sulfide phases. To resolve this concern, we cipitated, and [B+]and [A+] represent their aqueous con- must first ascertain the chemical nature of the heavy metal centrations. The heterogeneous distribution coefficient sulfide phase precipitated under natural conditions. describes cocrystallization resulting in a heterogeneous dis- Cadmium was selected as the subject in the endeavor to tribution of foreign species within the host lattice when answer this question due to the relatively extensive informa- aqueous solution composition changes during the course of tion concerning the aqueous and surface chemistry of cad- precipitation. X approaches D as the precipitation rate ap- mium and because Cd is known to be toxic. Because in aquatic proaches zero, sediments, iron sulfides are the dominant sulfides, cadmium Surface reaction constitutes not only a critical step in co- will exist in intimate aswciation with iron in the sulfide solid crystallization, but in and of itseif, a prominent course of phase. The possiliilities for cadmium precipitation as its sul- coprecipitation. Most widely documented of sulfide surface fide are: cadmium surface exchange with or adsorption onto reactions is the exchange reaction conforming to the me- iron(I1) sulfide substrate; solid solution formation of ferrous tathetical equilibrium and cadmium sulfide: cocrystallization as cadmium sulfide K host phase substituted with Fe2+,or cocrystallization as fer- A2/,,,S + 2/1zB+~ 2/mA+m + R2/,,S; rous sulfide host phase substituted with Cdz+; and precipi- - tation as esseiitially pure cadmium sulfide. This study K = K$;/K,:; (7) suggests which of thse phenomena are most probable. whereby aqueous cation B+, displaces cation A +*I from the Tizeory solid sulfide when the solubility of B,/,,S is less than that of We first consider the general thermodynamic boundaries A2/,,,S. Accordingly, ferrous sulfide, nearly the most soluble of equilihrium cocrystallization. The substitution of a foreign of the heavy metal sulfides, has been enlisted as an effective cation I?+ into the host solid AX may be considered a two-step analytical adsorbent for other heavy metal cations incliidir.fr process of wrface exchange followed by diffusion and incor- Cd2+ (51, whereas cadmium sulfide was found to remove froin poration into the crystal latticc (4), aqueous solution Fez+ most feebly among seven cations studied (6). A+(ads)+ Ij+(aq)*+ R+(ads) + A+(aq) (1) The metathetical reaction typically proceeds by rapid for- mation of a mono- to trilaver coating of the displacing cation. fl+(ads)+ AX(solid) ** R,Y(solid) A+(adsf + (2) whereas subsequent formation of a new sulfide crystalline the overall equilibrium heing phase proceeds much more slowly reflecting low solid state diffusion rates. Phillips and ICraus (7) document formation AX(mlid) + H+(aq) - BX(&lid) -I- A+(aq) (3) of new crystalline phases by Ag+ and Cu2+conversion of zinc, The ecluiiihrium distribrition coefficient D for Equation 3 is cadmium, lead, arsenic, or cupric sulfides. Garidin et al. (8) defined as also find Ag+ to convert zinc sulfide to a new crystalline phase, notably rejecting mixed crystal formation a5 a mechanism for this process. (4) James and Parks (9)find two models to describe moderately where x denotes mole fraction in the solid phase. Assuming well the nonmetathetical reaction of aqueous Zn2+with solid HgS. The first model postuiates a simple adsorption reaction LA:( 2 1,U can be forrnulaiedfrom thermodynamic parame- ters as whose driving force arises from electrostatic attraction be- tween surface and adsorbate. change in the solvation energy of adsorbate, and modification of the chemical free energy of the adsorbate; the other model postulates an exchange be- where K,, is the equilibrium ion activity product, y2 the mean tween adsorbed H+ and Zn2+ in the sulfide surface layer. aqueous activity coefficient product, f the solid state activity To speculate on the degree to which coprecipitation in the coefficient, R the universal gas constant, and T the absolute Fe-Cd-S system involves not only surface phenomena but temperature. AGAxequals the modification of the free energy crystal lattice phenomena as well, a brief examination of the of the AX latt,ice due to the suhstitution of R+, or through crystal chemistry of pertinent solids in that system is useful slight refor:nitlation.
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