U.S. Geological Survey sediment preparation procedures

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Method synopsis

Extraction of iron and manganese from sediments using 0.5 N HCl with hydroxylamine hydrochloride in anaerobic conditions, followed by ICP-AES analysis. This method targets metals associated with reducible phases in sediments.

Synthesized from method descriptions across 3 papers using this protocol.

Procedure from a recent peer-reviewed implementation

Steps below were extracted from the most recent peer-reviewed implementation of this protocol in the corpus — Reactive iron, not fungal community, drives organic carbon oxidation potential in floodplain soils (2023), Soil Biology and Biochemistry. Implementations in other papers (listed below) may differ.

1. Metal content analysis
   Total metals measured by Carlo Erba NA1500 Elemental Analyzer after acid digestion. Samples ground with Wig-L-Bug grinder, placed in plastic capsules, suspended in isopropyl alcohol, transferred to thin film for X-ray analysis. Reactive Mn and Fe extracted using 0.25 g freeze-dried soil in 75 mL acid-washed glass serum vials with 20 mL 0.5 M HCl, sealed with butyl septa, shaken 2 h at 145 rpm.
   Quantities: 18-22 mg soil for elemental analysis, 0.25 g for reactive metal extraction, 20 mL 0.5 M HCl extraction volumeDuration: 2 h shaking for reactive metal extraction at 145 rpmConditions: Acid-washed glassware, 0.5 M HCl for reactive metals, freeze-dried samples
   Equipment: Carlo Erba NA1500 Elemental Analyzer, Wig-L-Bug grinder, orbital shaker (VWR), acid-washed glassware

Typical Equipment

• HDPE bottles
• 0.5 N HCl
• 0.25 N hydroxylamine hydrochloride
• 0.45 μm filters
• ICP-AES

Output Measurements

• extractable iron concentration
• extractable manganese concentration

Papers Using This Protocol (3)

Species Studied With This Protocol