Evaluation of a well‐established sequential phosphorus fractionation technique for use in calcite‐rich lake sediments: identification and prevention of artifacts due to apatite formation

Hupfer, Michael; Zak, Dominik; Roβberg, Reingard; Herzog, Christiane; Pöthig, Rosemarie

doi:10.4319/lom.2009.7.399

Cited by 47 publications

(30 citation statements)

References 49 publications

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“…Phosphorus in soils and sediments has traditionally been divided into different fractions based on the components of soils and sediments. These fractions usually include aqueous phosphorus, exchangeable, and organic phosphorus; ironphosphorus (FeÀP; operationally defined as phosphorus bound by iron oxides and its hydroxides); and calcium phosphate (referred as phosphate bound by calcium carbonate [CaCO 3 ]) (Golterman,1996;Hupfer et al, 2009;Ruban et al, 1999;Ruttenberg, 1992;). In this study, FIP in sediments of Fubao Bay of Dianchi Lake was estimated to range from 23.4 to 39.8% of total phosphorus, which was higher than some previously identified phosphorus factions (Chang et al, 2010;Gao et al, 2005).…”

Section: Discussionmentioning

confidence: 99%

“…These techniques, however, are not able to separate FIP from ferric iron phosphorus. A sequential extraction method similar to that proposed by Chang and Jackson (1957) has been widely used to distinguish phosphorus species in sediments (Aydin et al, 2010;Golterman, 1996;Hupfer et al, 2009;Ruban et al, 1999;Ruttenberg, 1992). However, because FIP is not considered to be an independent fraction, it is assigned to different phosphorus fractions through reagent-defined extraction procedures.…”

Section: Introductionmentioning

confidence: 99%

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Ferrous Iron Phosphorus in Sediments: Development of a Quantification Method through 2,2′‐Bipyridine Extraction

Li¹,

Wang²,

Bartlett³

et al. 2012

Water Environment Research

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The role of ferrous iron in the phosphorus cycle of an aquatic ecosystem is poorly understood because of a lack of suitable methods to quantitatively evaluate ferrous iron phosphorus (FIP) phases. Using sediments sampled from Fubao Bay of Dianchi Lake in China, a novel extraction method for FIP using 2,2 0 -bipyridine was explored. Total phosphorus and iron in the sediments ranged from 1.0 to 5.0 mg/g (dry weight) and 28.5 to 90.6 mg/g, respectively. Organic content (as indicated by loss on ignition or LOI) and iron(II) ranged from 3.1 to 27.0% and 26.5 to 64.9 mg/g, respectively. The dissolution dynamics of FIP extraction with a low solid/liquid ratio (1:25) indicated that a single application of 0.2% 2,2 0 -bipyridine extracted both iron(II) (Fe(II)) and phosphorus (as PO 4 3À ) in sediments with different organic contents with low efficiency. The extraction efficiency of Fe(II) was improved by alteration of the solid/liquid ratio, but the effect was limited. However, addition of a 1:1000 solid/liquid ratio of 0.5 M potassium chloride to a 0.2% 2,2 0 -bipyridine solution significantly accelerated extraction of FIP with the release of Fe(II) and phosphorus toward equilibrium at approximately 150 hours. Further investigation demonstrated that 2,2 0 -bipyridine exhibited a higher selectivity in distinguishing FIP from phosphorus bound to ferric (Fe(III)) oxides or precipitated by calcium (Ca 2þ ). Air-drying sediments significantly decreased the amount of extracted FIP, which indicates that fresh, wet sediment should be used in this type of FIP extraction. Based on experimental results using the proposed extraction protocol, (1) FIP in sediments of Fubao Bay had a predominant status in the lake sediment and accounted for 23.4 to 39.8% of total phosphorus, and (2) Fe(II) FIP released in the extraction is directly proportional to phosphorus FIP (Fe(II) FIP ¼ 2.84 3 P FIP þ 0.0007; R 2 ¼ 0.97) with an average molar ratio of Fe(II) FIP /P FIP of 2.7. This study shows that FIP extraction with 2,2 0 -bipyridine is a robust method for releasing ferrous iron associated with phosphorus. Further, the high percentage of FIP in total phosphorus (40%) measured in the study site using this extraction method suggests that FIP might have been often underestimated in previous studies. Water Environ. Res., 84 2037 (2012.

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Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Ferrous Iron Phosphorus in Sediments: Development of a Quantification Method through 2,2′‐Bipyridine Extraction

Li¹,

Wang²,

Bartlett³

et al. 2012

Water Environment Research

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“…Soil and sediment samples (~2 g) were sequentially fractionated at room temperature using modified methods from Hupfer et al. (). Twenty‐five milliliters of the following extractions were used: 1 M NH 4 Cl shaken for 30 min extracting loosely bound and pore water P; 0.11 M NaHCO 3 Na 2 S 2 O 4 (buffered dithionite, BD) shaken for one hour extracting Fe‐bound and redox sensitive P; 1 M NaOH shaken for 16 h extracting Al‐bound P and organics; and 0.5 M HCl shaken for 16 h extracting Ca‐bound P. A separate pore water extraction was not possible due to limited water content and samples were subjected to only one cycle of reagent and shaking per step.…”

Section: Methodsmentioning

confidence: 99%

Two‐Stage Agricultural Ditch Sediments Act as Phosphorus Sinks in West Michigan

Kindervater

Steinman

2019

J American Water Resour Assoc

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Phosphorus (P) and sediment inputs from agricultural drainage contribute to the development of hypereutrophic conditions in lakes across the world. Two‐stage (2‐S) ditches, an agricultural best management practice gaining acceptance in the Midwestern United States, increase floodplain area within drainage ditches to help capture nutrients and sediment. While denitrification has been shown to increase on 2‐S benches, less is known about their P retention ability. This study assessed the abiotic and biotic P retention of two separate 2‐S ditches compared to their corresponding traditional reaches directly upstream within the Macatawa watershed, located in West Michigan. Soluble reactive P export was significantly reduced in 2‐S baseflow of both ditch systems. Equilibrium P concentration values suggest retention of P within the 2‐S sediment. P was bound within stable fractions in both 2‐S and traditional reaches. An analysis of P stock within the ditches revealed sediment held over 96% of total P (TP) within each reach compared to <4% in bench vegetation and periphyton combined. Turbidity, but not TP, was reduced in one study ditch, whereas TP, but not turbidity, was reduced in the other study ditch. Geomorphic stability may have been responsible for differing P retention between ditches. Ability to retain P appears to be impacted by physical as well as biogeochemical characteristics; hence, structure and age of 2‐S reaches influence P retention.

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“…For each extractant SRP was determined based on a separate calibration curve. As recommended by Hupfer et al [71] for calcite rich sediments, we employed enhanced volume-to-solid ratio (50:1) in the fractionation procedure, which is at least 2 times higher as originally proposed (12.5:1-25:1; [70]). This helps to avoid shifts from mobile fractions to the HCl-P pool.…”

Section: Chemical Analysismentioning

confidence: 99%

Phosphorus Inactivation in Lake Sediments Using Calcite Materials and Controlled Resuspension—Mechanism and Efficiency

et al. 2020

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The efficiency and mechanism of orthophosphate—soluble reactive phosphorus (SRP)—inactivation in eutrophic lakes using controlled resuspension and calcite application into the sediment were investigated in this study. Two calcite materials, industrially produced precipitated calcium carbonate (PCC) and natural ground limestone (GCC), were tested in short-term batch experiments and long-term sediment incubations under oxic and anoxic conditions. Maximum SRP adsorption capacity calculated using Langmuir model for PCC (3.11 mg PO43− g−1) was 6 times higher than of GCC (0.43 mg PO43− g−1), reflecting substantial difference in the surface area of calcite materials (12.36 and 1.72 m2 g−1, respectively). PCC applied into the sediment during controlled resuspension reduced SRP release by 95% (oxic) and 78% (anoxic incubation) at medium dose (0.75 kg m−2) and suppressed it completely at high dose (1.5 kg m−2) for at least 3 months, irrespectively of incubation conditions. The maximum achieved reduction of SRP release using GCC was also meaningful: 78% under oxic and 56% under anoxic conditions, but this required very high doses of this material (6 kg m−2). Mechanisms of SRP inactivation by calcites were: (1) adsorption of SRP during application into the resuspended sediment and (2) precipitation of calcium-phosphate compounds (Ca-PO4) during subsequent incubation, which was reflected in a substantial increase in the HCl-P fraction (phosphorus extractable in 0.5 M HCl) in sediments enriched with calcite, irrespectively of oxygen presence. However, anoxia strongly promoted the formation of this fraction: the rise of HCl-P was 2–6 times higher in anoxic than in oxic conditions, depending on the dose and form of calcite applied. The results showed that SRP inactivation using the controlled resuspension method is only successful if highly efficient reactive materials are used, due to large amount of SRP being released from sediment during resuspension. Thus, calcite materials exhibiting high adsorption capacity should be used in this lakes’ restoration technology to ensure fast and sufficient SRP inactivation. The rise in the HCl-P fraction in sediment suggests SRP inactivation through precipitation of relatively stable Ca-PO4 minerals, which makes calcite a suitable agent for sustainable, long term SRP inactivation. As anoxic conditions promoted formation of these compounds, calcite seems to be a promising SRP inactivation agent in highly reductive sediments.

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Evaluation of a well‐established sequential phosphorus fractionation technique for use in calcite‐rich lake sediments: identification and prevention of artifacts due to apatite formation

Cited by 47 publications

References 49 publications

Ferrous Iron Phosphorus in Sediments: Development of a Quantification Method through 2,2′‐Bipyridine Extraction

Ferrous Iron Phosphorus in Sediments: Development of a Quantification Method through 2,2′‐Bipyridine Extraction

Two‐Stage Agricultural Ditch Sediments Act as Phosphorus Sinks in West Michigan

Phosphorus Inactivation in Lake Sediments Using Calcite Materials and Controlled Resuspension—Mechanism and Efficiency

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