Fast and inexpensive detection of total and extractable element concentrations in aquatic sediments using near-infrared reflectance spectroscopy (NIRS)

PLoS One. 2013 Jul 29;8(7):e70517. doi: 10.1371/journal.pone.0070517. Print 2013.

Abstract

Adequate biogeochemical characterization and monitoring of aquatic ecosystems, both for scientific purposes and for water management, pose high demands on spatial and temporal replication of chemical analyses. Near-infrared reflectance spectroscopy (NIRS) may offer a rapid, low-cost and reproducible alternative to standard analytical sample processing (digestion or extraction) and measuring techniques used for the chemical characterization of aquatic sediments. We analyzed a total of 191 sediment samples for total and NaCl-extractable concentrations of Al, Ca, Fe, K, Mg, Mn, N, Na, P, S, Si, and Zn as well as oxalate- extractable concentrations of Al, Fe, Mn and P. Based on the NIR spectral data and the reference values, calibration models for the prediction of element concentrations in unknown samples were developed and tested with an external validation procedure. Except Mn, all prediction models of total element concentrations were found to be acceptable to excellent (ratio of performance deviation: RPD 1.8-3.1). For extractable element fractions, viable model precision could be achieved for NaCl-extractable Ca, K, Mg, NH4 (+)-N, S and Si (RPD 1.7-2.2) and oxalate-extractable Al, Fe and P (RPD 1.9-2.3). For those elements that showed maximum total values below 3 g kg(-1) prediction models were found to become increasingly critical (RPD <2.0). Low concentrations also limited the performance of NIRS calibrations for extracted elements, with critical concentration thresholds <0.1 g kg(-1) and 3.3 g kg(-1) for NaCl and oxalate extractions, respectively. Thus, reliable NIRS measurements of trace metals are restricted to sediments with high metal content. Nevertheless, we demonstrated the suitability of NIRS measurements to determine a large array of chemical properties of aquatic sediments. The results indicate great potential of this fast technique as an analytical tool to better understand the large spatial and temporal variation of sediment characteristics in an economically viable way.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Geologic Sediments / analysis
  • Geologic Sediments / chemistry*
  • Metals / analysis
  • Metals / chemistry
  • Netherlands
  • Oxalates / analysis
  • Oxalates / chemistry
  • Rivers*
  • Sodium Chloride / analysis
  • Sodium Chloride / chemistry
  • Spectroscopy, Near-Infrared*
  • Water / standards
  • Water Pollutants, Chemical / analysis
  • Water Pollutants, Chemical / chemistry

Substances

  • Metals
  • Oxalates
  • Water Pollutants, Chemical
  • Water
  • Sodium Chloride

Grants and funding

Part of this work was carried out within the Water Framework Directive Innovation Project ‘Maatregelen Baggeren en Nutriënten (BAGGERNUT)’ which was financed by the Ministry of Economic Affairs/Agentschap NL (The Netherlands). The funders had no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript. No additional external funding received for this study.