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Processing of Bulk Nanocrystalline Metals at the US Army Research Laboratory
Published on: March 7, 2018
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Optimization of Field and Laboratory Sample Processing for Characterization of Metallic Residues at Military Training
J L Clausen1, T Georgian2, K H Gardner3
1Engineer Research Development Center, Cold Regions Research and Engineering Laboratory, U.S. Army Corps of Engineers, 72 Lyme Road, Hanover, NH, 03755, USA. Jay.L.Clausen@usace.army.mil.
Bulletin of Environmental Contamination and Toxicology
|March 14, 2018
Summary
This study found that Incremental Sampling Methodology (ISM) processing for small arms range metal contaminants in soil requires careful method selection. Milling and increasing digestion mass improved results, while field splitting techniques showed poor precision.
Area of Science:
- Environmental Science
- Analytical Chemistry
- Geochemistry
Background:
- Military ranges present unique challenges for soil contaminant characterization due to heterogeneous distribution of energetics and metals.
- Conventional grab sampling is insufficient for accurately assessing contaminants like lead (Pb), copper (Cu), antimony (Sb), and zinc (Zn) at these sites.
- While Incremental Sampling Methodology (ISM) is effective for energetic contaminants, its application to metal characterization at small arms ranges requires specific processing studies.
Purpose of the Study:
- To evaluate the effectiveness of different Incremental Sampling Methodology (ISM) processing steps for characterizing metal contaminants (Pb, Cu, Sb, Zn) in soils from small arms ranges.
- To assess field splitting techniques for reducing sample mass and their impact on data precision and distribution.
- To determine the necessity of milling and the optimal subsample mass for digestion in ISM soil sample processing.
Main Methods:
- Evaluation of cone-and-quartering and rotary sectorial splitting for field sample splitting.
- Comparison of milled versus unmilled soil samples for metal analysis.
- Assessment of increased digestion subsample mass (2 g to 10 g) on analytical results for both milled and unmilled samples.
Main Results:
- Cone-and-quartering and rotary sectorial splitting techniques resulted in poor precision and positively skewed data distributions.
- Unmilled soil samples exhibited the highest variability in results, irrespective of the subsample mass used for digestion.
- Increasing the digestion mass to 10 g showed potential benefits, but sample preparation (milling) remained a critical factor.
Conclusions:
- Standard field splitting methods are inadequate for precise characterization of metal contaminants at small arms ranges using ISM.
- Milling is a crucial step in ISM soil processing for accurate metal contaminant analysis.
- Optimizing digestion subsample mass in conjunction with appropriate sample preparation is essential for reliable ISM data at military ranges.
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