Hupfer,M., Zak,D., Roβberg,R., Herzog,C. and Pothig(oの頭に¨),R.(2009): 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. Limnology and Oceanograpgy: Methods, 7, 399-410.

『方解石に富む湖堆積物において使われる十分確立した連続リン分別法の評価::燐灰石形成による人工物の同定と防止』


Abstract
 Speciation of particulate phosphorus in soils and aquatic sediments by sequential extraction techniques is commonly used to address both fundamental and applied problems. It has been suggested, however, that sequential extraction techniques can produce misleading results due to the generation of new solid phases during the extraction process. In this study, a well-established fractionation technique introduced by Psenner et al. (1984) for crystalline sediments was reevaluated in four calcite-rich lake sediments using a set of additional extraction tests and structural analyses. Extended tests using a sediment artificially enriched with Al and Ca, regarded as model sediment, showed a distinct overestimation of Ca-bound P (HCl-TP) and concomitant underestimation of metal oxide-bound P (NaOH-SRP). The formation of new solid phases during extraction was evident by P addition to the alkaline extract, change of volume-to-solid ratio, and variation of extraction time. Examination of the model sediment with infrared and X-ray spectroscopy demonstrated that Ca-bound P was not present before the NaOH step. Apatite structures were detected by IR spectroscopy in the model sediment after NaOH extraction. In contrast, in the three natural calcite-rich sediments with high HCl-TP portions, underestimations of NaOH-SRP were not detected with the standard protocol. Therefore, a modification of the Psenner method does not appear necessary for most conditions. In hardwater lakes, however, especially those restored with al and Fe salts, a shift from NaOH-SRP to HCl-P cannot be excluded. Our study provides helpful tools to identify such artifacts and thus to prevent misinterpretation of fractionation results.』

Acknowledgments
Introduction
Materials and procedures
 Sequential phosphorus extraction
 Analysis with X-ray and infrared spectroscopy
 Sampling sites
Assessment
 Extraction tests
 Structural analysis
Discussion
Comments and recommendations
References

表1.Psenner et al(1984)に従って修正された連続リン抽出法および画分中に期待されるリン(他の研究者らによる修正を含む)

抽出剤/画分

時間
(時間)

分析されたリン

期待されるリン化学種
1M NH4Cl(脱酸素化された) 0.5 TP 孔隙水中のP表面にゆるく吸着したP(例えば、FeOOHやCaCO3の表面)
0.11M BD(bicarbonate/dithionite) 1 TP 酸化されたFeとMn化合物に主に結合した酸化還元に敏感なP
1M NaOH

16
SRP OH-イオンに対して交換可能なP〔例えば、AlとFe(オキシ)水酸化物に吸着したP〕および塩基中で可溶な無機P化合物〔FeとAl(水酸化)リン酸塩〕
NRP ポリリン酸(poly-P)と砕屑物中の有機Pとフミン化合物に結合したPを含む微生物中のP
0.5M HCl 16 TP Caリン酸塩鉱物および酸に可溶の有機P
残渣P(Residual-P、Res-P   TP 溶けにくい(refractory)有機Pおよび抽出できない(nonextractable)鉱物P
NRP=非反応性リン(nonreactive phosphorus)、SRP=可溶の反応性リン(soluble reactive phosphorus)、TP=全リン(total phosphorus)


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