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D. D. Eberl

Publications and source records attributed to D. D. Eberl.

At least 37 records · Page 2Linked to original sources
USGS2007

Microbial reduction of structural Fe3+ in nontronite by a thermophilic bacterium and its role in promoting the smectite to illite reaction

The illitization process of Fe-rich smectite (nontronite NAu-2) promoted by microbial reduction of structural Fe3+ was investigated by using a thermophilic metal-reducing bacterium, Thermoanaerobacter ethanolicus, isolated from the deep subsurface. T. ethanolicus was incubated with lactate as the sole electron donor and structural Fe3+ in nontronite as the sole electron acceptor, and anthraquinone-2, 6-disulfonate (AQDS) as an electron shuttle in a growth medium (pH 6.2 and 9.2, 65 ??C) with or without an external supply of Al and K sources. With an external supply of Al and K, the extent of reduction of Fe3+ in NAu-2 was 43.7 and 40.4% at pH 6.2 and 9.2, respectively. X-ray diffraction and scanning and transmission electron microscopy revealed formation of discrete illite at pH 9.2 with external Al and K sources, while mixed layers of illite/smectite or highly charged smectite were detected under other conditions. The morphology of biogenic illite evolved from lath and flake to pseudo-hexagonal shape. An external supply of Al and K under alkaline conditions enhances the smectite-illite reaction during microbial Fe3+ reduction of smectite. Biogenic SiO2 was observed as a result of bioreduction under all conditions. The microbially promoted smectite-illite reaction proceeds via dissolution of smectite and precipitation of illite. Thermophilic iron reducing bacteria have a significant role in promoting the smectite to illite reaction under conditions common in sedimentary basins.

American Mineralogist↗
USGS2006

An exploratory method to detect tephras from quantitative XRD scans: Examples from Iceland and east Greenland marine sediments

Tephras, mainly from Iceland, are becoming increasingly important in interpreting leads and lags in the Holocene climate system across NW Europe. Here we demonstrate that Quantitative Phase Analysis of x-ray diffractograms of the < 2 mm of marine sediment fraction (ie, sand, silt and clay) from Iceland and East Greenland can detect peaks in volcanic glass concentrations (weight%) even though discrete tephra layers are not visible; thus it provides a rapid overview of the probable location of volcanic glass within sediment sequences. Experiments in spiking samples from Baffin Bay and an artificial mixture of minerals with known weight% fractions of an Icelandic tephra (Hekla 4) demonstrate a significant correlation (r2 = 0.92 and 0.97) between known and estimated weight percentages, although the slope of the measured to observed weight% is around 0.65 and not 1.0 as expected. In core B997-321PC off North Iceland we identify tephras from point counting in the > 150 um fraction and identify these same peaks in XRD scans - two of these correlate geochemically and chronologically with Hekla 1104 and 3. At a distal site to the WNW of Iceland, on the East Greenland margin (core MD99-2317), the weight% of volcanic glass reaches values of 11% at about the time of the Saksunarvatn tephra. The XRD method identifies the presence of volcanic glass but not its elemental composition; hence it will assist in focusing attention on specific sections of sediment cores for subsequent geochemical fingerprinting of tephras. ?? 2006 SAGE Publications.

Holocene↗
USGS2006

Holocene history of drift ice in the northern North Atlantic: Evidence for different spatial and temporal modes

We present new high-resolution proxy data for the Holocene history of drift ice off Iceland based on the mineralogy of the <2-mm sediment fraction using quantitative X-ray diffraction. These new data, bolstered by a comparison with published proxy records, point to a long-term increasing trend in drift ice input into the North Atlantic from 6 to 5 ka toward the present day at sites influenced by the cold east Greenland Current. This feature reflects the late Holocene Neoglacial or cooling period recorded in ice cores and further terrestrial archives on Greenland. In contrast, a decrease in drift ice during the same period is recorded at sites underlying the North Atlantic Drift, which may reflect a warming of this region. The results document that Holocene changes in iceberg rafting and sea ice advection did not occur uniformly across the North Atlantic. Centennial-scale climate variability in the North Atlantic region over the last ???4 kyr is linked to the observed changes in drift ice input. Increased drift ice may have played a role in the increase of cold intervals during the late Holocene, e.g., the Little Ice Age cooling. Copyright 2006 by the American Geophysical Union.

Paleoceanography↗
USGS2006

Influence of layer charge and charge distribution of smectites on the flow behaviour and swelling of bentonites

The influence of layer charge and charge distribution of dioctahedral smectites on the rheological and swelling properties of bentonites is examined. Layer charge and charge distribution were determined by XRD using the LayerCharge program [Christidis, G.E., Eberl, D.D., 2003. Determination of layer charge characteristics of smectites. Clays Clay Miner. 51, 644-655.]. The rheological properties were determined, after sodium exchange using the optimum amount of Na2CO3, from free swelling tests. Rheological properties were determined using 6.42% suspensions according to industrial practice. In smectites with layer charges of - 0.425 to - 0.470 per half formula unit (phfu), layer charge is inversely correlated with free swelling, viscosity, gel strength, yield strength and thixotropic behaviour. In these smectites, the rheological properties are directly associated with the proportion of low charge layers. By contrast, in low charge and high charge smectites there is no systematic relation between layer charge or the proportion of low charge layers and rheological properties. However, low charge smectites yield more viscous suspensions and swell more than high charge smectites. The rheological properties of bentonites also are affected by the proportion of tetrahedral charge (i.e. beidellitic charge), by the existence of fine-grained minerals having clay size, such as opal-CT and to a lesser degree by the ionic strength and the pH of the suspension. A new method for classification of smectites according to the layer charge based on the XRD characteristics of smecites is proposed, that also is consistent with variations in rheological properties. In this classification scheme the term smectites with intermediate layer charge is proposed. ?? 2006 Elsevier B.V. All rights reserved.

Applied Clay Science↗
USGS2005

Direct observation of heavy metal-mineral association from the Clark Fork River Superfund Complex: Implications for metal transport and bioavailability

Two sets of samples from riverbeds and adjacent floodplains, separated by 80 river kilometers, were collected from the Clark Fork River Superfund Complex, Montana, (the largest Superfund site in the United States), and studied primarily with transmission electron microscopy (TEM) with several supporting techniques to determine heavy metal-mineral association. Seven of the eight samples studied were strongly influenced by material that once resided in mining and smelting dumps and impoundments; this material was transported downstream sometime during the last century and a half from the Butte/Anaconda areas. The eighth sample was from a deeper floodplain level and dates to premining days. The TEM observations afford a direct look, down to the nanometer level, at secondary mineral formation as a result of the breakdown of sulfides and silicates in the acid environment of this massive mine-drainage system. In the shallow, oxic floodplain sediments, heavy metals of concern in this system (As, Cu, Pb, and Zn) are taken up by the formation of sulfates (particularly Pb in jarosite), as well as hydrous metal oxides (As, Cu, Pb, and Zn in and on ferrihydrite, and a possibly new vernadite-like mineral). The oxides are long-lived in these systems, as they were also found in the anoxic riverbeds. Metals are also taken up by the formation of sulfides in sulfate-reducing environments as observed in the formation of nanoclusters of chalcopyrite and sphalerite. In all samples, clays make up between 5 and 20% of the sediment and carry significant amounts of Cu and Zn. The hydrous oxides, secondary sulfides, and clays provide several routes for metal transport downstream over long distances. Besides the potential bioavailability of heavy metals exchanged on and off the hydrous metal oxides and clays, nanometer-sized sulfides may also be highly reactive in the presence of biologic systems. Copyright ?? 2005 Elsevier Ltd.

Geochimica et Cosmochimica Acta↗
USGS2005

Control of Fe(III) site occupancy on the rate and extent of microbial reduction of Fe(III) in nontronite

A quantitative study was performed to understand how Fe(III) site occupancy controls Fe(III) bioreduction in nontronite by Shewanella putrefaciens CN32. NAu-1 and NAu-2 were nontronites and contained Fe(III) in different structural sites with 16 and 23% total iron (w/w), respectively, with almost all iron as Fe(III). Mo??ssbauer spectroscopy showed that Fe(III) was present in the octahedral site in NAu-1 (with a small amount of goethite), but in both the tetrahedral and the octahedral sites in NAu-2. Mo??ssbauer data further showed that the octahedral Fe(III) in NAu-2 existed in at least two environments- trans (M1) and cis (M2) sites. The microbial Fe(III) reduction in NAu-1 and NAu-2 was studied in batch cultures at a nontronite concentration of 5 mg/mL in bicarbonate buffer with lactate as the electron donor. The unreduced and bioreduced nontronites were characterized by X-ray diffraction (XRD), Mo??ssbauer spectroscopy, and transmission electron microscopy (TEM). In the presence of an electron shuttle, anthraquinone-2,6-disulfonate (AQDS), the extent of bioreduction was 11%-16% for NAu-1 but 28%-32% for NAu-2. The extent of reduction in the absence of AQDS was only 5%-7% for NAu-1 but 14%-18% for NAu-2. The control experiments with heat killed cells and without cells did not show any appreciable reduction (<2%). The extent of reduction in experiments performed with a dialysis membrane to separate cells from clays (without AQDS) was 2%-3% for NAu-1 but 5%-7% for NAu-2, suggesting that cells probably released an electron shuttling compound and/or Fe(III) chelator. The reduction rate was also faster in NAu-2 than that in NAu-1. Mo??ssbauer data of the bioreduced nontronite materials indicated that the Fe(III) reduction in NAu-1 was mostly from the presence of goethite, whereas the reduction in NAu-2 was due to the presence of the tetrahedral and trans-octahedral Fe(III) in the structure. The measured aqueous Fe(II) was negligible. As a result of bioreduction, the average nontronite particle thickness remained nearly the same (from 2.1 to 2.5 nm) for NAu-1, but decreased significantly from 6 to 3.5 nm for NAu-2 with a concomitant change in crystal size distribution. The decrease in crystal size suggests reductive dissolution of nontronite NAu-2, which was supported by aqueous solution chemistry (i.e., aqueous Si). These data suggest that the more extensive Fe(III) bioreduction in NAu-2 was due to the presence of the tetrahedral and the trans-octahedral Fe(III), which was presumed to be more reducible. The biogenic Fe(II) was not associated with biogenic solids or in the aqueous solution. We infer that it may be either adsorbed onto surfaces of nontronite particles/bacteria or in the structure of nontronite. Furthermore, we have demonstrated that natural nontronite clays were capable of supporting cell growth even in medium without added nutrients, possibly due to presence of naturally existing nutrients in the nontronite clays. These results suggest that crystal chemical environment of Fe(III) is an important determinant in controlling the rate and extent of microbial reduction of Fe(III) in nontronite. Copyright ?? 2005 Elsevier Ltd.

Geochimica et Cosmochimica Acta↗
USGS2004

Quantitative mineralogy of the Yukon River system: Changes with reach and season, and determining sediment provenance

The mineralogy of Yukon River basin sediment has been studied by quantitative X-ray diffraction. Bed, beach, bar, and suspended sediments were analyzed using the RockJock computer program. The bed sediments were collected from the main stem and from selected tributaries during a single trip down river, from Whitehorse to the Yukon River delta, during the summer of 2001. Beach and bar sediments were collected from the confluence region of the Tanana and Yukon Rivers during the summer of 2003. Suspended sediments were collected at three stations on the Yukon River and from a single station on the Tanana River at various times during the summers of 2001 through 2003, with the most complete set of samples collected during the summer of 2002. Changes in mineralogy of Yukon River bed sediments are related to sediment dilution or concentration effects from tributary sediment and to chemical weathering during transport. Carbonate minerals compose about 2 wt% of the bed sediments near Whitehorse, but increase to 14 wt% with the entry of the White River tributary above Dawson. Thereafter, the proportion of carbonate minerals decreases downstream to values of about 1 to 7 wt% near the mouth of the Yukon River. Quartz and feldspar contents of bed sediments vary greatly with the introduction of Pelly River and White River sediments, but thereafter either increase irregularly (quartz from 20 to about 50 wt%) or remain relatively constant (feldspar at about 35 wt%) with distance downstream. Clay mineral content increases irregularly downstream from about 15 to about 30 wt%. The chief clay mineral is chlorite, followed by illite + smectite; there is little to no kaolinite. The total organic carbon content of the bed sediments remains relatively constant with distance for the main stem (generally 1 to 2 wt%, with one exception), but fluctuates for the tributaries (1 to 6 wt%). The mineralogies of the suspended sediments and sediment flow data were used to calculate the amount of mineral dissolution during transport between Eagle and Pilot Station, a distance of over 2000 km. We estimate that approximately 3 wt% of the quartz, 15 wt% of the feldspar (1 wt% of the alkali and 25 wt% of the plagioclase), and 26 wt% of the carbonates (31 wt% of the calcite and 15 wt% of the dolomite) carried by the river dissolve in this reach. The mineralogies of the suspended sediments change with the season. For example, during the summer of 2002 the quartz content varied by 20 wt%, with a minimum in mid-summer. The calcite content varied by a similar amount, and had a maximum corresponding to the quartz minimum. These modes are related to the relative amount of sediment flowing from the White River system, which is relatively poor in quartz, but rich in carbonate minerals. Suspended total clay minerals varied by as much as 25 wt%, with maxima in mid July, and suspended feldspar varied up to 10 wt%. Suspended sediment data from the summers of 2001 and 2003 support the 2002 trends. A calculation technique was developed to determine theproportion of various sediment sources in a mixed sediment by unmixing its quantitative mineralogy. Results from this method indicate that at least three sediment sources can be identified quantitatively with good accuracy. With this technique, sediment mineralogies can be used to calculate the relative flux of sediment from different tributaries, thereby identifying sediment provenance.

American Mineralogist↗
USGS2004

Killer clays! Natural antibacterial clay minerals

The clay chemical properties that may be important in medicine were investigated. It was found that natural clay minerals can have striking and very specific effects on microbial populations. The effects can range from potentially enhanced microbial growth to complete sterilization. This paper presents evidence that natural clay minerals can be effective antimicrobial agents.

Mineralogical Society Bulletin↗
USGS2003

On the origin of size-dependent and size-independent crystal growth: Influence of advection and diffusion

rystal growth experiments were conducted using potassium alum and calcite crystals in aqueous solution under both non-stirred and stirred conditions to elucidate the mechanism for size-dependent (proportionate) and size-independent (constant) crystal growth. Growth by these two laws can be dis- tinguished from each other because the r elative size difference among crystals is maintained during proportionate growth, leading to a constant crystal size variance ( b 2 ) for a crystal size distribution (CSD) as the mean size increases. The absolute size difference among crystals is maintained during constant growth, resulting in a decrease in size variance. Results of these experiments show that for centimeter-sized alum crystals, proportionate growth occurs in stirred systems, whereas constant growth occurs in non-stirred systems. Accordingly, the mechanism for proportionate growth is hypothesized to be related to the supply of reactants to the crystal surface by advection, whereas constant growth is related to supply by diffusion. Paradoxically, micrometer-sized calcite crystals showed proportionate growth both in stirred and in non-stirred systems. Such growth presumably results from the effects of convection and Brownian motion, which promote an advective environment and hence proportionate growth for minute crystals in non-stirred systems, thereby indicating the importance of solution veloc- ity relative to crystal size. Calcite crystals grown in gels, where fluid motion was minimized, showed evidence for constant, diffusion-controlled growth. Additional investigations of CSDs of naturally occurring crystals indicate that proportionate growth is by far the most common growth law, thereby suggesting that ad ection, rather than diffusion, is the dominant process for supplying reactants to crystal surfaces.

American Mineralogist↗
USGS2003

Distinguishing palagonitized from pedogenically-altered basaltic Hawaiian tephra: Mineralogical and geochemical criteria

Palagonitization is a common, but imperfectly defined process that greatly modifies the physical and chemical properties of glassy basaltic tephra deposited in subaquatic/subglacial environments on Earth and perhaps Mars. It also results in textures and mineralogies that are distinct from other forms of (mainly pedogenic) low temperature alteration. Specifically, the process of palagonitization (1) initially results in the formation of 'palaginitized glass', a quasi- or nano-crystalline, rind-like material that contains smectite, as well as lesser amounts of other clays (e.g. serpentine), and (2) eventually results in consolidation of tephra, mediated through the accretion of palagonitized glass and later- formed authigenic cements. Conversely, pedogenic weathering of glassy basaltic tephra is characterized by disaggregation of tephra, and formation of a wide range of pedogenic products, including layer silicates (although not primarily smectite), short-range-order aluminosilicates and oxyhydroxides, whose composition reflects the intensity of the weathering environment. These mineralogical and textural properties can be readily recognized through a variety of techniques including electron microscopy/microprobe analysis, reflectance spectroscopy, X-ray diffraction and soil chemistry. Analyses of samples collected from the summit regions of Kilauea and Mauna Kea volcanoes on the island of Hawaii are presented here in order to illustrate differences between palagonitization and pedogenic weathering of glassy basaltic tephra. In the young Hawaiian tephras studied, palagonitization has occurred in response to hydrothermal activity shortly after deposition. Although some, non-hydrothermally affected tephras may eventually become palagonitized, those that have been strongly desilicated by intense pedogenic weathering will probably never become palagonitized.

Geological Society Special Publication↗
USGS2002

Characterization and modeling of illite crystal particles and growth mechanisms in a zoned hydrothermal deposit, Lake City, Colorado

Mean thickness measurements and crystal-thickness distributions (CTDs) of illite particles vary systematically with changes in hydrothermal alteration type, fracture density, and attendant mineralization in a large acid-sulfate/Mo-porphyry hydrothermal system at Red Mountain, near Lake City, Colorado. The hydrothermal illites characterize an extensive zone of quartz-sericite-pyrite alteration beneath two deeply rooted bodies of magmatic-related, quartz-alunite altered rock. Nineteen illites from a 3000 ft vertical drill hole were analyzed by XRD using the PVP-10 intercalation method and the computer program MudMaster (Bertaut-Warren-Averbach technique). Mean crystallite thicknesses, as determined from 001 reflections, range from 5-7 nanometers (nm) at depths from 0-1700 ft, then sharply increase to 10-16 nm at depths between 1800-2100 ft, and decrease again to 4-5 nm below this level. The interval of largest particle thickness correlates strongly with the zone of most intense quartz-sericite-pyrite alteration (QSP) and attendant high-density stockwork fracturing, and with the highest concentrations of Mo within the drill core. CTD shapes for the illite particles fall into two main categories: asymptotic and lognormal. The shapes of the CTDs are dependent on conditions of illite formation. The asymptotic CTDs correspond to a nucleation and growth mechanism, whereas surface-controlled growth was the dominant mechanism for the lognormal CTDs. Lognormal CTDs coincide with major through-going fractures or stockwork zones, whereas asymptotic CTDs are present in wallrock distal to these intense fracture zones. The increase in illite particle size and the associated zone of intense QSP alteration and stockwork veining was related by proximity to the dacitic magma(s), which supplied both reactants and heat to the hydrothermal system. However, no changes in illite polytype, which in other studies reflect temperature transitions, were observed within this interval.

Colorado↗
USGS2002

On geological interpretations of crystal size distributions: Constant vs. proportionate growth

Geological interpretations of crystal size distributions (CSDs) depend on understanding the crystal growth laws that generated the distributions. Most descriptions of crystal growth, including a population-balance modeling equation that is widely used in petrology, assume that crystal growth rates at any particular time are identical for all crystals, and, therefore, independent of crystal size. This type of growth under constant conditions can be modeled by adding a constant length to the diameter of each crystal for each time step. This growth equation is unlikely to be correct for most mineral systems because it neither generates nor maintains the shapes of lognormal CSDs, which are among the most common types of CSDs observed in rocks. In an alternative approach, size-dependent (proportionate) growth is modeled approximately by multiplying the size of each crystal by a factor, an operation that maintains CSD shape and variance, and which is in accord with calcite growth experiments. The latter growth law can be obtained during supply controlled growth using a modified version of the Law of Proportionate Effect (LPE), an equation that simulates the reaction path followed by a CSD shape as mean size increases.

American Mineralogist↗
USGS1999

Crystal growth mechanisms in miarolitic cavities in the Lake George ring complex and vicinity, Colorado

The Crystal Peak area of the Pikes Peak batholith, near Lake George in central Colorado, is world-renowned for its crystals of amazonite (the blue-green variety of microcline) and smoky quartz. Such crystals, collected from individual miarolitic pegmatites, have a remakably small variation in crystal size within each pegmatite, and the shapes of plots of their crystal size distributions (CSDs) are invariably lognormal or close to lognormal in all cases. These observations are explained by a crystal growth mechanism that was governed initially by surface-controlled kinetics, during which crystals tended to grow larger in proportion to their size, thereby establishing lognormal CSDs. Surface-controlled growth was followed by longer periods of supply controlled growth, during which growth rate was predominantly size-independent, consequently preserving the lognormal shapes of the CSDs and the small size variation. The change from surface- to supply controlled growth kinetics may have resulted from an increasing demand for nutrients that exceeded diffusion limitations of the system. The proposed model for crystal growth in this locality appears to be common in the geologic record, and can be used with other information, such as isotopic data, to deduce physico-chemical conditions during crystal formation.

American Mineralogist↗
USGS1998

Deducing growth mechanisms for minerals from the shapes of crystal size distributions

Crystal size distributions (CSDs) of natural and synthetic samples are observed to have several distinct and different shapes. We have simulated these CSDs using three simple equations: the Law of Proportionate Effect (LPE), a mass balance equation, and equations for Ostwald ripening. The following crystal growth mechanisms are simulated using these equations and their modifications: (1) continuous nucleation and growth in an open system, during which crystals nucleate at either a constant, decaying, or accelerating nucleation rate, and then grow according to the LPE; (2) surface-controlled growth in an open system, during which crystals grow with an essentially unlimited supply of nutrients according to the LPE; (3) supply-controlled growth in an open system, during which crystals grow with a specified, limited supply of nutrients according to the LPE; (4) supply- or surface-controlled Ostwald ripening in a closed system, during which the relative rate of crystal dissolution and growth is controlled by differences in specific surface area and by diffusion rate; and (5) supply-controlled random ripening in a closed system, during which the rate of crystal dissolution and growth is random with respect to specific surface area. Each of these mechanisms affects the shapes of CSDs. For example, mechanism (1) above with a constant nucleation rate yields asymptotically-shaped CSDs for which the variance of the natural logarithms of the crystal sizes (??2) increases exponentially with the mean of the natural logarithms of the sizes (??). Mechanism (2) yields lognormally-shaped CSDs, for which ??2 increases linearly with ??, whereas mechanisms (3) and (5) do not change the shapes of CSDs, with ??2 remaining constant with increasing ??. During supply-controlled Ostwald ripening (4), initial lognormally-shaped CSDs become more symmetric, with ??2 decreasing with increasing ??. Thus, crystal growth mechanisms often can be deduced by noting trends in ?? versus ??2 of CSDs for a series of related samples.

American Journal of Science↗
USGS1998

Hydrothermal synthesis of ammonium illite

Synthetic gel and glass of illitic composition, natural kaolinite, and mixed-layer illite-smectite were used as starting materials for hydrothermal synthesis of ammonium illite. Ammonium illite was prepared from synthetic gel by hydrothermal treatment at 300??C. The onset of crystallization began within 3 h, and well-crystallized ammonium illite appeared at 24 h. Increasing reaction time (up to four weeks) led to many illite layers per crystal. In the presence of equivalent proportions of potassium and ammonium, the gel was transformed to illite with equimolar contents of K and NH4. In contrast, synthesis using glass under the same conditions resulted in a mixture of mixed-layer ammonium illite-smectite with large expandability and discrete illite. Hydrothermal treatments of the fine fractions of natural kaolinite and illite-smectite produced ammonium illite from kaolinite but the illite-smectite remained unchanged.

American Mineralogist↗
USGS1996

MUDMASTER: A Program for Calculating Crystalline Size Distributions and Strain from the Shapes of X-Ray Diffraction Peaks

Particle size may strongly influence the physical and chemical properties of a substance (e.g. its rheology, surface area, cation exchange capacity, solubility, etc.), and its measurement in rocks may yield geological information about ancient environments (sediment provenance, degree of metamorphism, degree of weathering, current directions, distance to shore, etc.). Therefore mineralogists, geologists, chemists, soil scientists, and others who deal with clay-size material would like to have a convenient method for measuring particle size distributions. Nano-size crystals generally are too fine to be measured by light microscopy. Laser scattering methods give only average particle sizes; therefore particle size can not be measured in a particular crystallographic direction. Also, the particles measured by laser techniques may be composed of several different minerals, and may be agglomerations of individual crystals. Measurement by electron and atomic force microscopy is tedious, expensive, and time consuming. It is difficult to measure more than a few hundred particles per sample by these methods. This many measurements, often taking several days of intensive effort, may yield an accurate mean size for a sample, but may be too few to determine an accurate distribution of sizes. Measurement of size distributions by X-ray diffraction (XRD) solves these shortcomings. An X-ray scan of a sample occurs automatically, taking a few minutes to a few hours. The resulting XRD peaks average diffraction effects from billions of individual nano-size crystals. The size that is measured by XRD may be related to the size of the individual crystals of the mineral in the sample, rather than to the size of particles formed from the agglomeration of these crystals. Therefore one can determine the size of a particular mineral in a mixture of minerals, and the sizes in a particular crystallographic direction of that mineral.

Open-File Report↗
USGS1991

Infrared spectroscopic examination of the interaction of urea with the naturally occurring zeolite clinoptilolite

Infrared spectroscopy has shown for the first time that the naturally occurring zeolite clinoptilolite can absorb urea, (NH 2 ) 2 CO, under ambient conditions from either aqueous or ethanolic solutions. The two strongest NH stretching bands at 3441 and 3344 cm −1 in pure, solid urea shift to higher frequency (about 3504 and 3401 cm −1 ) after absorption. Two of the four urea bands in the 1800-1300 cm −1 range (at 1683 and 1467 cm −1 ) undergo marked downward shifts to about 1670 and 1445 cm −1 . The other two bands show little change in frequency. The strong band at 1602 cm −1 , however, diminishes in intensity to little more than an ill-defined shoulder on the 1626-cm −1 peak. When clinoptilolite is heated to 450 °C and then treated with molten urea (ca. 140 °C) for several minutes, and finally washed twice with ethanol to remove excess unreacted urea, further changes become apparent in the spectrum of the urea-treated clinoptilolite. The two NH stretching bands broaden without significant change in frequency. Two new bands appear in the midfrequency range at 1777 (weak) and 1719 (medium strong) cm −1 . Of the four original midfrequency peaks, the one at 1602 cm −1 is now absent. Two others (1627 and 1440 cm −1 ) exhibit little change, while the fourth has broadened and shifted down to 1663 cm −1 , where it appears as a shoulder on the band at 1627 cm −1 . Both treatments clearly induce interaction between urea and the zeolite which seems to result in significant modifications in the nature of the hydrogen bonding of the substrate.

Microchemical Journal↗