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Crystal Chemistry of the Zeolites Erionite and Offretite

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Crystal Chemistry of the Zeolites Erionite and Offretite American Mineralogist, Volume 83, pages 577±589, 1998 Crystal chemistry of the zeolites erionite and offretite E. PASSAGLIA,1 G. ARTIOLI,2,* AND A. GUALTIERI1 1Dipartimento di Scienze della Terra, UniversitaÁ di Modena, via S. Eufemia 19, I-41100 Modena, Italy 2Dipartimento di Scienze della Terra, UniversitaÁ di Milano, via Botticelli 23, I-20133 Milano, Italy ABSTRACT Many known occurrences of the zeolites erionite and offretite have been characterized by electron probe microanalysis, X-ray powder diffraction, and optical microscopy. For the ®rst time, a substantial amount of experimentally consistent and homogeneous chemical and crystallographic data have been evaluated for these natural zeolites. Systematic anal- ysis of the data, performed by statistical multivariate analysis, leads to the following con- clusions: (1) the two zeolites have well-de®ned compositional ®elds in the chemical space describing the extraframework cation content, best illustrated in a Mg-Ca(1Na)- K(1Sr1Ba) diagram; (2) no discrimination is possible on the basis of the framework Si/Al ratio because of the extensive compositional overlap between the two species, however the Si-Al content in the framework tetrahedra is the major control on the unit-cell volume dimensions, particularly in erionite; (3) the crystal chemistry of the Mg cations is a major factor in controlling the crystallization of the mineral species; (4) cation compositions at the boundary of the recognized compositional ®elds might be due to chemical averaging of two-phase intergrowths, although these mixed-phase occurrences are much less common than previously thought; (5) the sign of optical elongation is not a distinctive character of the two phases, it is related to the Si/Al ratio in the framework tetrahedra of each zeolite type and cannot be used for identi®cation purposes; (6) the zeolite mineral species epitax- ially overgrown on levyne in all cases is identi®ed as erionite; in a few cases offretite was found to be overgrown on chabazite; (7) erionite samples epitaxially overgrown on levyne are substantially more Al-rich and Mg-poor than the erionite samples associated with other zeolites. INTRODUCTION of the two mineral zeolites, whereas offretite occurrences Erionite and offretite are natural zeolites having differ- are scarce. Typical occurrences, morphological and opti- ent topologies ([ERI]- and [OFF]-topological codes fol- cal features, and earlier crystal chemical studies are well lowing Meier and Olson 1992). Both zeolites are found described in the literature (Sheppard and Gude 1969; in vugs of volcanic massive rocks, and available literature Wise and Tschernich 1976; Gottardi and Galli 1985; descriptions include: one-phase occurrences and epitaxial Tschernich 1992). The present study stems from two ma- intergrowths of the two species (Pongiluppi 1976; Rinaldi jor problems commonly encountered in the characteriza- 1976; Wise and Tschernich 1976; Hentschel and Schricke tion of erionite-offretite mineral samples: (1) The identi- 1976; Betz and Hentschel 1978; Rychly et al. 1982), ep- ®cation of mineral species is troublesome, due to the itaxial overgrowth of both erionite and offretite on levyne structural and crystal chemical similarities of the two ze- (Shimazu and Mizota 1972; Passaglia et al. 1974; Shep- olites; and (2) the literature descriptions available to date pard et al. 1974; Wise and Tschernich 1976; England and do not provide clear discriminatory parameters for the Ostwald 1979; Birch 1989; Kile and Modreski 1988), and de®nition and the distinction of the two minerals, unless epitaxial overgrowth of offretite on chabazite (Passaglia a complete structural study is performed. and Tagliavini 1994; Passaglia et al. 1996). Only erionite The ®rst point is readily justi®ed: In the literature it is is also found as an authigenic mineral in volcanoclastic possible to ®nd several cases where the minerals were silicic layers and tuffs diagenetically altered in continen- misidenti®ed by simple routine mineralogical analysis. tal (Staples and Gard 1959; Sheppard and Gude 1969; An example is the sample from Beech Creek, Oregon, Sheppard et al. 1965; Gude and Sheppard 1981; Boles which was originally identi®ed as an offretite overgrowth and Surdam 1979; Surdam and Eugster 1976) and marine on levyne on the basis of optical elongation sign and X- (Shameshima 1978) environments. Given the wider range ray powder diffraction data (Sheppard et al. 1974), but for conditions of formation, erionite is the more common was subsequently rede®ned as erionite on levyne on the basis of thorough X-ray and electron diffraction analysis * E-mail: [email protected] and adsorption capacity measurements (Bennett and Grose 0003±004X/98/0506±0577$05.00 577 578 PASSAGLIA ET AL.: CRYSTAL CHEMISTRY OF ERIONITE AND OFFRETITE FIGURE 1. Compositional diagram showing the reliable (1965); Sheppard and Gude (1969); Staples and Gard (1959); chemical analyses of erionite (open circles) and offretite (solid Surdam and Eugster (1976), Wise and Tschernich (1976). About circles) from the literature. Sources of the data: Batiashvili and half of the erionites are reported to be ``hydrothermal,'' and half Gvakhariya (1968); Belitskiy and Bukin (1968); Birch (1988, are sedimentary. M 5 (Na 1 K); D 5 (Ca 1 Mg 1 Sr 1 Ba). 1889); Boles and Surdam (1979); England and Ostwald (1979); All data normalized to 72 framework O atoms. Horizontal dis- Gude and Sheppard (1981); Harada et al. (1967); Kile and Mod- crimination lines based on Si/Al ratio are after Sheppard and reski (1988); Noh and Kim (1986); Passaglia et al. (1974); Pas- Gude (1969) [±´±´±], Wise and Tschernich (1976) [- - - -], and saglia and Tagliavini (1994, 1995); Pongiluppi (1976); Rinaldi Rinaldi (1976) [´´´´´´´´]. Sub-vertical line (D 5 M) is the discrim- (1976); Rychly et al. (1982); Sameshima (1978); Sheppard et al. inant after Sheppard and Gude (1969). 1978). Several of the samples obtained for the present natory diagram based on the above chemical parameters study were also misidenti®ed by the original authors: The (Fig. 1), it is evident that none among the proposed cri- close relationship between the crystal structures of the teria satisfactorily de®nes appropriate compositional two minerals (Bennett and Gard 1967) is the cause for ®elds apt to describe the literature information. Chemical such frequent misidenti®cations. Although both crystal analyses are considered to be reliable if (Si 1 Al) ø 36, structures are now reasonably well de®ned, at least in on the basis of 72 O atoms; and balance error E # 10%, terms of major crystallographic features (Staples and where E% (Passaglia 1970) is Gard 1959; Kawahara and Curien 1969; Gard and Tait 1972, 1973; Alberti et al. 1996; Gualtieri et al. 1998), the 100 3 [(Al 1 Fe)ob2Alth]/Alth (1) available crystal chemical characterizations are incom- Al 5 Na 1 K 1 2 3 (Ca 1 Mg 1 Sr 1 Ba). (2) plete and often inconsistent. This is the cause of the sec- th ond problem listed above: Based on the present literature, The situation is even more confused if we try to plot it is impossible to de®ne universal discrimination criteria the available data describing the extraframework cation applicable to all reported erionite and offretite samples. content of the two zeolites, using the same literature Problems exist because earlier discrimination parame- sources (Fig. 2). We assume that the lack of discrimina- ters were based on a limited number of samples. Shep- tory compositional ®elds for the two zeolites is due to pard and Gude (1969) proposed species distinction based several factors: First of all, several minerals in the liter- on the optical sign of elongation (positive in erionite, neg- ature could be simply misidenti®ed; second, several of ative in offretite, a widely used identi®cation parameter the analyses may have been carried out on mixed-phase in subsequent studies) and on chemical parameters [eri- samples. onite: Si/(Al 1 Fe) . 2.9 and (Na 1 K) . (Ca 1 Mg)]. The present work attempts to rede®ne the crystal Subsequently, Wise and Tschernich (1976) and Rinaldi chemistry of erionite and offretite minerals. We collected (1976) proposed a distinction based on the Si/Al ratio, as many available samples as possible from different lo- the former de®ning as erionite the mineral having Si/Al calities, identi®ed the associated minerals, and eventually . 3.0, the latter de®ning as erionite the mineral having separated pure erionite and offretite samples. For each Si/Al . 2.4. sample, we performed electron microprobe analysis If all reliable chemical analyses of erionites and offre- (EMPA), thermal gravimetric analysis, X-ray powder dif- tites available in the literature are inserted in a discrimi- fraction, and optical microscopy. Statistical analysis of PASSAGLIA ET AL.: CRYSTAL CHEMISTRY OF ERIONITE AND OFFRETITE 579 FIGURE 2. Compositional diagram showing the extraframework cation content of reliable chemical analyses of erionite and offretite minerals in the literature. Sources of the data and symbols as in Figure 1. the internally consistent and homogeneous chemical and rated for preliminary X-ray diffraction analysis by long crystallographic data was used to evaluate and interpret exposures (up to 24 h) using a Gandol® camera. The non- possible discrimination parameters between the two zeo- destructive technique allowed identi®cation of the sepa- lites. A companion study (Gualtieri et al. 1998) presents rated crystals and guaranteed integrity of the crystals for the full structural characterization
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