A-000

CHEMICAL AND MINERALOGICAL CHARACTERIZATION OF UNDISTURBED SOILS

FROM ZACATECAS (MEXICO)

R. Pardo, A. López, E. Escareño, L. Debán, M. Vega

Department of Analytical Chemistry and Institute of Sustainable Processes, Faculty of Sciences,

University of Valladolid, Paseo de Belén 7, 47011 Valladolid (Spain)
e-mail corresponding author: rpardo@qa.uva.es

Toxic trace elements, also known as heavy metals, are a very hazardous group of pollutants
because of their toxic and accumulative characteristics: they are non-biodegradable and
undergo global eco-biological cycles, so their circulation amongst the different environmental
compartments is a main concern. Soils can act as temporary reservoirs from which those
elements could be released back, and the real environmental risk must consider the total
concentrations as well as their mobility/availability.
Whereas total concentrations can be determined by non-destructive analytical techniques, such
as Neutron Activation Analysis (NAA) or X-ray fluorescence (XRF), the available/mobilizable
(also known as pseudo-total) contents are usually determined after a non-total digestion of the
soil sample with concentrated acids. This is the approach followed by US-EPA 3051A norm, the
de facto standard, that proposes a microwave assisted acid digestion with concentrated nitric
or/and hydrochloric acids. The elements present in the resulting liquid extracts, are then
determined by using a technique adequate for trace analysis, such as Inductively Coupled
Plasma Optical Emission Spectrometry (ICP-OES) or Inductively Coupled Plasma Mass
Spectrometry (ICP-MS).
The analytical results (total or available/mobilizable contents) can be studied by univariate
(element to element) or by multivariate statistical techniques, such as Cluster Analysis (CA) or
Principal Component Analysis (PCA), that allow to find relationships amongst soils and/or trace
elements, not available at a first glance by the univariate approach.
In this communication, we describe the results of a survey carried out to assess the contents of
toxic trace elements in 25 undisturbed top-soils of Zacatecas (Mexico), an area known for its
large deposits of silver and other minerals, but with scarce and very old information toxic trace
elements. The 25 samples were initially characterized by X-Ray Diffractometry (XRD), finding
that most of the top-soils had a composition based on quartz and plagioclases, except for a few
calcite-based samples.
The investigated elements were As, Cd, Cr, Cu, Ni, Pb and Zn. Total concentrations were
determined with a Bruker S8 Tiger XRF spectrometer. For the available/mobilizable elements,
the EPA-3051A was carried out on a Milestone Ethos Plus microwave, analyzing the resulting
extracts with an Agilent 7500 ICP/MS spectrometer.
The average total contents of As, Cr and Ni ranged between 40-60 mg/kg 24-39 mg/kg; Cu, Pb
and Zn between 130-180 mg/kg whereas Cd was negligible. On the other side, the average
available/mobilizable contents of As, Cr and Ni were 24-39 mg/kg; Cu and Pb 70-100 mg/kg; Zn
was around 180 mg/kg and Cd around 2 mg/kg. In all the cases, the soils were classified as
suitable for ‘industrial’ and ‘residential’ uses, according to the NOM-147-SEMARNAT/SSA1-
2004 Mexican norm.
PCA and AC allowed to separate the information due to the samples from that corresponding to
the analyzed elements. Three different toxic trace element associations were found for both
total and pseudo-total concentrations: Cr-Ni, As-Cu-Zn y Cd-Pb. In the case of the top-soil
samples, both PCA and AC located some samples with higher contents in the studied elements.

Authors wish to thank Junta de Castilla y León for the financial support (Ref. VA068G18)