Fractionation of Ni, Cr and Cu from Soil by Sequential Extraction Procedure and Determination by Inductively Coupled Plasma Optical Emission Spectrometry

Abstract Sequential selective extraction techniques are commonly used to fractionate the solid-phase forms of metals in soils. This procedure provides measurements of extractable metals from media, such as acetic acid (0.11 M), hydroxyl ammonium chloride (0.1 M), hydrogen peroxide (8.8 M) plus ammonium acetate (1 M), and aqua regia stages of the sequential extraction procedure. In this work, the extractable Pb, Cu, Mn, Sr, Ni, V, Fe, Zn, and Cr were evaluated in street dust samples from Sakarya, Turkey, between May and October 2009 using the three-step sequential extraction procedure described by the Community Bureau of Reference (BCR, now the Standards, Measurements, and Testing Programme) of the European Union. The sampling sites were divided into 10 categories; a total of 50 street dusts were analyzed. The determination of multielements in the samples was performed by inductively coupled plasma-optical emission spectrometry. Validation of the proposed method was performed using BCR 701 certified reference material. The results showed good agreement between the obtained and the certified values for the metals analyzed.

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Identification and Speciation of Nanoscale Silver in Complex Solid Matrices by Sequential Extraction Coupled with Inductively Coupled Plasma Optical Emission Spectrometry

Analytical Chemistry ◽

10.1021/acs.analchem.0c04741 ◽

2021 ◽

Vol 93 (4) ◽

pp. 1962-1968

Author(s):

Aimei Hong ◽

Qing Tang ◽

Ashfeen Ubaid Khan ◽

Maozhong Miao ◽

Zhenlan Xu ◽

...

Keyword(s):

Sequential Extraction ◽

Inductively Coupled Plasma ◽

Optical Emission ◽

Optical Emission Spectrometry ◽

Emission Spectrometry ◽

Inductively Coupled ◽

Solid Matrices ◽

Plasma Optical Emission Spectrometry

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Optimization and assessment of a sequential extraction procedure for calcium carbonate rocks

Environmental Monitoring and Assessment ◽

10.1007/s10661-021-09300-x ◽

2021 ◽

Vol 193 (9) ◽

Author(s):

Janin Scheplitz ◽

Sarah Koopmann ◽

Henning Fröllje ◽

Thomas Pichler

Keyword(s):

Sequential Extraction ◽

Inductively Coupled Plasma ◽

Extraction Procedure ◽

Optical Emission ◽

Sequential Extraction Procedure ◽

Emission Spectrometry ◽

Inductively Coupled ◽

Analyte Signal ◽

Carbonate Sample ◽

Sample Ratio

AbstractSequential extraction analyses are widely used for the determination of element speciation in sediments and soils. Typical sequential extraction protocols were developed to extract from low-carbonate samples and therefore are not necessarily suitable for high-carbonate samples. In this study, we tested increased reagent to sample ratios to adjust an existing sequential extraction procedure to analyze high-CaCO3 samples with concentrations ranging from 70 to above 90 %. Complete dissolution of the CaCO3 phase, and a higher extraction efficiency of manganese associated with the carbonate phase, was achieved when using four times the original reagent to sample ratio in the 2nd extraction step. This increase of reagent did not compromise the extraction of subsequent phases as shown by unaffected Fe concentrations in a low-carbonate sample. Hence, an essential outcome was that increasing the solution to sample ratio did not lead to the dissolution of other sedimentary phases, such as hydrous and crystalline iron oxides or sulfides. Thus, compared to other extraction protocols that use a lower reagent to sample ratio in the carbonate dissolution step, the new protocol allowed the complete extraction of oxide and sulfide phases in the following extraction steps. Furthermore, the study demonstrated the benefit of replacing Na-acetate with NH4-acetate to extract exchangeable ions and carbonates. We observed increased intensities for several analytes, i.e., trace metals such as Mo and As, due to less suppression of the analyte signal by NH4-acetate than by Na-acetate during analysis by inductively coupled plasma optical emission spectrometry (ICP-OES).

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