Determining how environmentally important trace metalsare sequestered in soils at the molecular scale is critical todeveloping a solid scientific basis for maintaining soilquality and formulating effective remediation strategies.The speciation of Zn and Ni in ferromanganese nodules fromloess soils of the Mississippi Basin was determined by asynergistic use of three noninvasive synchrotron-basedtechniques: X-ray microfluorescence (
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XRF), X-raymicrodiffraction (
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XRD), and extended X-ray absorptionfine structure spectroscopy (EXAFS). We show that Ni isdistributed between goethite (
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-FeOOH) and the manganeseoxide lithiophorite, whereas Zn is bound to goethite,lithiophorite, phyllosilicates, and the manganese oxidebirnessite. The selective association of Ni with only ironand manganese oxides is an explanation for its higherpartitioning in nodules over the soil clay matrix reportedfrom soils worldwide. This could also explain the observedenrichment of Ni in oceanic manganese nodules. Thecombination of these three techniques provides a newmethod for determining trace metal speciation in both naturaland contaminated environmental materials.