Digestion Methods for Total Heavy Metals in Sediments and Soils

Water Air and Soil Pollution (Impact Factor: 1.55). 11/2002; 141(1):189-205. DOI: 10.1023/A:1021302405128


The objectives of this study were to analyze the total contents of Cd, Cr, Cu, Ni, Pb, and Zn in the freshwater sediments
and the arable and non-arable soils of Taiwan, and to compare the different digestion methods for their determination. Two
hundred and thirty-nine freshwater sediments were collected from the Fei-Tsui Reservoir Watershed (FTRW) in northern Taiwan.
Forty-two surface (0–15 cm) and subsurface (15–30 cm) soil samples were likewise collected from 21 representative arable soils
derived from various parent materials and with varying weathered degrees in different regions of Taiwan. In addition, one
hundred and ninety-four non-arable soils were collected from the different forest regions, industrial parks, resident areas,
and commercial areas. Several digestion methods including the aquaregia and different combinations of concentrated acids (HClO4, HNO3, H2SO4, or HF) were compared. All samples were digested both by the aqua regia method and the Baker and Amacher method for Cd, Cr, Cu, Ni, Pb, and Zn. The Reisenauer method was used for Cr and the Burau
method for Pb further. The results indicate that the best digestion methods to analyze the total contents of heavy metals
in the sediments and soils were recommended as follows: the Baker and Amacher method for Cd, Cr,Cu, Ni, and Zn; the Reisenauer
method for Cr, but for simplicity the Baker and Amacher method is also recommended as the flexible method for the total analysis
of Cr; the aqua regia method for Cu, Ni, and Zn; and the Burau method for Pb.

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Available from: Zeng-Yei Hseu, Oct 11, 2015
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    • "of homogenized sediment were digested with aqua regia (3:1 v/v, HCl to HNO 3 ) and H 2 O 2 at 100 °C (Hseu et al., 2002). The extracts were centrifuged, diluted to 25 ml with deionized water and stored in polyethylene bottles. "
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    ABSTRACT: Water and sediment samples were collected in the Samborombón Bay, outer Río de la Plata estuary to evaluate the dynamics of trace metals along the fluvial–marine transition. This estuarine environment presented strong salinity (0.11–31.4) and turbidity (21 to 4999 mg L-�1) gradients with a consistent turbidity maximum zone (TMZ:41 g suspended solids L�-1) in the low salinity region. Suspended particulate metals showed different spatial patterns: homogeneous distributions (Fe, Zn) and progressive enrichment from the TMZ to the maritime area (Cu, Ni). The influence of the TMZ is clearly reflected by the enrichment of flocculated clays which in turns control the distribution of sedimentary TOC and trace metals resulting in a prevailing decreasing land–sea gradient. Mn has a particular behavior along the salinity gradient denoting intense dissolved-particulated phase changes both in the water column and bottom sediments. An average 36% drop of particulate Mn observed in parallel with a strong dissolved peak suggests a rapid Mn desorption/dissolution in the water column whereas bottom sediments display an average 72% Mn enrichment in the TMZ relative to the riverine sector reflecting the diffusive escape from anoxic sediments and reprecipitation in oxic surface layers.
    Continental Shelf Research 01/2015; 96:27-33. DOI:10.1016/j.csr.2015.01.007 · 1.89 Impact Factor
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    • "This complete dissolution process—termed acid digestion—is required for element determination . The effectiveness of closed (pressure) digestion using a combination of HNO 3 , HClO 4 , and HF has been demonstrated for bulk-certified reference materials of marine sediments, in which both HNO 3 and HClO 4 are oxidizers; the HNO 3 prevents explosive reactions of the organic matter with HClO 4 while HF attacks silicate minerals to form gaseous SiF 4 (Hseu et al., 2002; Begum et al., 2007). The solutions from the extractable and residual fractions were evaporated to dryness, and clear solutions were generated using 10 ml of 1% HNO 3 . "
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    ABSTRACT: We sampled two box-core sediments from the slope of the eastern South Korea Plateau (SKP) in the East Sea (Sea of Japan) at water depths of 1400 and 1700 m. Two chemical fractions of extractable (hydroxylamine/acetic acid) and residual rare earth elements (REEs) together with Al, Ca, Fe, Mg, Mn, P, S, As, Mo, and U were analyzed to assess the post-depositional redistribution of REEs. Extractable Fe and Mn are noticeably abundant in the oxic topmost sediment layer (<3 cm). However, some trace elements (e.g., S, As, Mo, U) are more abundant at depth, where redox conditions are different. Analysis of upper continental crust (UCC)-normalized (La/Gd)UCC, (La/Yb)UCC, and (Ce/Ce*)UCC revealed that the extractable REE is characterized by middle REE (MREE) enrichment and a positive cerium (Ce) anomaly, different from the case of the residual fraction which shows slight enrichment in light REEs (LREEs) with no Ce anomaly. The extractable MREEs seem to have been incorporated into high-Mg calcite during reductive dissolution of Fe oxyhydroxides. In the top sediment layer, the positive Ce anomaly is attributed to Ce oxide, which can be mobilized in deeper oxygen-poor environments and redistributed in the sediment column. In addition, differential concentrations of Ce and other LREEs in pore water appear to result in variable (Ce/Ce*)UCC ratios in the extractable fraction at depth.
    Journal of Asian Earth Sciences 03/2014; 82:66–79. DOI:10.1016/j.jseaes.2013.11.019 · 2.74 Impact Factor
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    • "Sample digestion is often a necessary step before determining metal concentrations. Around the world, many studies have evaluated the heavy metal concentrations in sediments in soils using the aqua regia digestion procedure [11] [12] [13]. The aqua regia (3:1, v/v, HCl to HNO 3 ) digestion procedure is considered adequate for analyzing the total-recoverable heavy metals in soils and sediments. "
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    ABSTRACT: The aim of this study was the evaluation of the trace element contamination level in sediments of the most important rivers in Serbia and their tributaries. The determination of the aqua regia soluble contents of 12 micro- and macro-elements (Ca, Cd, Co, Cr, Cu, Fe, Mn, Pb, Ni, Zn, Be and V) in sediments was developed by the microwave digestion technique combined with inductively coupled plasma atomic emission spectrometry. Correlation analysis and principal component analysis distinguishes factors of lithogenic and anthropogenic origins. The Fe, Mn, Be and V contents are controlled by a regional lithogenic high background factor, while Cd, Cr, Pb, Ni, Zn and Cu are recognized as tracer of pollution. For Co, mixed sources from both lithogenic and anthropogenic inputs were evidenced.The investigated sediment of the major rivers and their tributaries in Serbia showed high concentrations of metals, especially of Cd, Pb, Cu and Zn, which may cause serious environmental impacts. Rivers which flow into the Danube from its entrance into Serbia significantly influence the chemical load of the water and sediments.The experimental study was conducted using two BCR standard reference materials. The calculated accuracy and precision confirmed the good performance of the adopted procedures.
    Microchemical Journal 11/2011; 99(2):492-502. DOI:10.1016/j.microc.2011.06.027 · 2.75 Impact Factor
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