Limitations of the ferrozine method for quantitative assay of mineral systems for ferrous and total iron

Anastácio, Alexandre S.; Harris, Brittany; Yoo, Hae-In; Fabris, José Domingos; Stucki, Joseph W.

doi:10.1016/j.gca.2008.07.009

Cited by 69 publications

(44 citation statements)

References 30 publications

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“…Phenanthroline was employed in preference to the commonly employed Fe(II) colorimetric agent ferrozine since, at low pH, ferrozine can induce the reduction of Fe(III) and therefore interfere with the reliable measurement of Fe(II) (Anastacio et al, 2008). Furthermore, phenanthroline can be used to quantify the concentration of Fe(II) in the presence of EDTA and citrate, with no interference due to complex formation (Wang et al, 2013) and forms an extremely stable Fe(II) complex with a stability constant of 10 21.3 (Banks & Bystroff, 1959); stronger than that of Fe(II)-EDTA (Morel & Hering, 1993).…”

Section: Analysis Of Fe(ii)mentioning

confidence: 99%

Ferrous iron oxidation by molecular oxygen under acidic conditions: The effect of citrate, EDTA and fulvic acid

Jones

Griffin

Waite

2015

Geochimica et Cosmochimica Acta

113

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Section: Analysis Of Fe(ii)mentioning

confidence: 99%

Ferrous iron oxidation by molecular oxygen under acidic conditions: The effect of citrate, EDTA and fulvic acid

Jones

Griffin

Waite

2015

Geochimica et Cosmochimica Acta

113

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“…Caveats about matrix interferences in spectrophotometric determination of total Fe and Fe 2+ have been raised in the past (Skogerboe and Wilson, 1981;Anastácio et al, 2008), but the problem is not universal because environmental samples can vary widely in their matrix components (Perdue, 1998). Additionally, there is no consensus as to whether the effectiveness of different Fe quantitative methods varies with matrix characteristics, particularly for samples containing highly humified, complex DOM.…”

mentioning

confidence: 99%

“…For example, Pentrák et al (2013) recommended that o-P is applicable for Fe quantitation in minerotrophic wetland (fen) sediments and soil pore water, based on the quantitative recoveries of Fe compared with another Fe assay, the ferrozine method. Anastácio et al (2008) compared the performance of o-P with that of the ferrozine method and also recommended o-P across a wide range of ecosystems, including systems with clay-sorbed amorphous Fe oxides. Lipson et al (2010) reported total Fe recoveries in Arctic peat soil using o-P that were not significantly different from direct quantitation using ICP-OES Methods.…”

mentioning

confidence: 99%

Ionic Liquid Extraction Unveils Previously Occluded Humic‐Bound Iron in Peat Soil Pore Water

Veverica

Kane

Marcarelli

et al. 2016

Soil Science Soc of Amer J

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Globally, peatland ecosystems store tremendous amounts of C relative to their extent on the landscape, largely owing to saturated soils which limit decomposition. While there is still considerable uncertainty regarding CO 2 production potential below the water table in peatland ecosystems, extracellular Fe reduction has been suggested as a dominant pathway for anaerobic metabolism. However, colorimetric methods commonly used to quantitate Fe and partition between redox species are known to be unreliable in the presence of complex humic substances, which are common in peatland pore water. We evaluated both the standard o-phenanthroline (o-P) Method and an ionic liquid extraction (ILE) Method followed by quantitation with inductively coupled plasma optical emission spectrometry (ICP-OES) to compare total Fe recovery and Fe 2+ /Fe 3+ ratios in four distinct peatland ecosystems, ranging from rich fen to bog. While total Fe concentrations measured with ILE and o-P were correlated, the ILE method proved to be superior in both total Fe quantitation and in separately quantifying ferric (Fe 3+ ) and ferrous (Fe 2+ ) iron. In peat pore water, the o-P Method underestimated Fe 3+ by as much as 100%. A multivariate approach utilizing fluorescenceand ultraviolet (UV)-visable (Vis) spectroscopy identified indices of dissolved organic matter (DOM) humification and redox status that correlated with poor performance of the o-P Method in peat pore water. Where these interferences are present, we suggest that site-specific empirical correction factors for quantitation of total Fe by o-P can be created from ILE of Fe, but recommend ILE for accurate appraisals of iron speciation and redox processes.Abbreviations: DI, deionized; DOC, dissolved organic carbon; DOM, dissolved organic matter; EEMs, excitation-emissions matrices; FI, fluorescence index; H p , index of humification; ICP-OES, inductively coupled plasma optical emission spectrometry; ILE, ionic liquid extraction; o-P, o-phenanthroline; PARAFAC, parallel factor analysis; PCA, principal component analysis; RI, index of redox dissolved organic matter status; TEA, terminal electron acceptor; UV, ultraviolet; Vis, visible. P eatlands represent critical terrestrial C stores that are preserved by a combination of hypoxic and anoxic soil environments. These conditions present an energetic challenge for microbial consortia in anaerobic environments which utilize alternative (to oxygen) terminal electron acceptors (TEAs) during heterotrophic metabolism. In anaerobic conditions, microbes preferentially reduce several alternative TEAs for respiration, with thermodynamic yield declining in the order: NO 3 -, Mn 4+ , Fe 3+ , SO 4 2-, and ultimately CO 2 (see review by Megonigal et al., 2004). Although there is wide agreement that alternative TEA reduction is important for anaerobic decomposition, variation in the magnitudes of anaerobic CO 2 production across studies suggests that there is high variability in facultative and obligate anaerobic processes that occur below the water table (M...

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“…The 1,10-phenanthroline method is based on total digestion of the mineral with HF-H 2 SO 4 and has been demonstrated as an effective approach for measuring total Fe(II) in layer silicates (Amonette and Templeton, 1998;Anastacio et al, 2008).…”

Section: Fe(ii) Analysis and Cell Countsmentioning

confidence: 99%

Low-temperature feldspar and illite formation through bioreduction of Fe(III)-bearing smectite by an alkaliphilic bacterium

et al. 2015

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Biogenic mineral assemblages that form from circumneutral microbial reduction of iron in smectite have been suggested as biosignatures in the geological record. However, mineralogical transformation of smectite mediated by microbes under extreme pH condition is still poorly known. The objective of this study was to understand the reduction capacity of structural Fe(III) in iron-rich smectite (nontronite, NAu-2) by a novel anaerobic alkaliphile (strain CCSD-1) isolated from the deep subsurface, and associated mineralogical changes. The experiments with CCSD-1 were conducted in a growth medium containing the electron shuttle anthraquinone-2,6-disulfonate (AQDS) at pH 9.4. The Fe(II) concentration was monitored over the course of the experiment via wet chemistry, and unreduced and reduced nontronites were characterized with X-ray diffraction (XRD), and scanning and transmission electron microscopy (SEM and TEM). The results indicate that strain CCSD-1 utilizes proteinaceous substrates (yeast extract and tryptone) to reduce structural Fe(III) in smectite with the maximum reduction extent of 26.2%. Mineralogical analysis confirmed that biogenic plagioclase (Na-Ca feldspar) and illite were formed after bioreduction. Our work shows that the interaction between alkaliphile and iron-bearing smectite could account for low-temperature feldspar and illite formation and these minerals may be used as biosignatures in sedimentary rocks.

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Limitations of the ferrozine method for quantitative assay of mineral systems for ferrous and total iron

Cited by 69 publications

References 30 publications

Ferrous iron oxidation by molecular oxygen under acidic conditions: The effect of citrate, EDTA and fulvic acid

Ferrous iron oxidation by molecular oxygen under acidic conditions: The effect of citrate, EDTA and fulvic acid

Ionic Liquid Extraction Unveils Previously Occluded Humic‐Bound Iron in Peat Soil Pore Water

Low-temperature feldspar and illite formation through bioreduction of Fe(III)-bearing smectite by an alkaliphilic bacterium

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