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See detailElemental composition of soils and sediments by using portable X-ray fluorescence (pXRF) spectroscopy: a preliminary study
Alberti, Roberto; Falsone, Gloria; Gironda, M. et al

Poster (2017, December)

Portable X-ray fluorescence spectrometry (pXRF) provides rapid and low-cost analysis in laboratory and field conditions for a wide range of environmental applications. Its successful application in soils ... [more ▼]

Portable X-ray fluorescence spectrometry (pXRF) provides rapid and low-cost analysis in laboratory and field conditions for a wide range of environmental applications. Its successful application in soils requires a good instrument calibration and the possibility to implement custom calibrations and methods using known samples as well as reference materials. In the present study two set of samples, one from pedogenized sediments of a basin in Marradi (Italy; n=13) and the other from agricultural land in Meuse valley (Belgium; n=10), were analyzed by using a portable X-ray fluorescence (pXRF TRACER 5i made by Bruker) to detect and quantify the element species (Al, Si, Ca, Fe, Mg, K, Mn, P, S, Ba, Cd, Co, Cr, Cu, Mo, Pb, Sb, Sn, Sr and Zn). Element concentrations results were compared with analytical results from aqua regia extractions (AQ) followed by ICP-OES analysis. The aim of this work was to verify and find the best instrument setup for the specific matrix, elements and their concentration range with the purpose of using the pXRF technique directly insitu for the screening of sites potentially polluted. A standard factory calibration for soil applications was used for samples from Meuse valley, while a custom calibration for P, S, Ca and Fe quantification with the coefficient correction method was developed and used for pedogenized sediments from Marradi, as well as for Cu and Cr quantification in both sites. Comparing portable XRF and AQ results, elements could be grouped in three classes: 1) elements where the content determined by both methods is not correlated (p>0.05; Al, Si, and K); 2) elements strongly correlated (0.84<r<0.99, p<0.001; P, S, Mn, Fe, Ca, Cu, Cr, Zn and Pb); 3) elements with a weaker correlation (0.67<r<0.78, p<0.01; Mg and Sr). A further class of elements (Co, Mo, Cd, Sn, Sb, and Ba) was not evaluable because their concentration was below the detection limit of the pXRF. The measured concentrations and the relationship between pXRF and AQ were obviously affected by the elements form in the soils. The value of macroelements commonly related to the silicate phase measured by portable XRF is higher than that determined by AQ, which does not allow the destruction of Si-O and Al-O bounds (explaining the uncorrelation in the class 1 elements). The elements related to the organic matter (P and S, r2>0.60), carbonates (Ca, r2>0.55) and oxy(hydr)oxides (Fe and Mn) have instead comparable concentrations between pXRF and AQ. Preliminary results showed that portable XRF can quickly provide data for some elucidations of important pedogenic processes involving many elements (class 2) in the studied soils. Alternative methods offer results after expensive and time-consuming analytical procedures. Moreover for environmental and human health purposes, the pXRF should be a valid tool for a rapid screening of heavy metals, such as Cu, Cr, Zn and Pb. A larger set of soil samples and further custom calibration will be tested. [less ▲]

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See detailImpacts de contaminations sur la végétation et la faune du sol
Liénard, Amandine ULiege

Conference given outside the academic context (2017)

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See detailTreatment MEthodology and MOnitoring for sequenced Reallocation of severely polluted Industrial Sites (MEMORIS) project
Duprez, Marie-Eve; Castro, Cristiana; Devalckeneer, Aude et al

Poster (2017, May)

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See detailTransfert sol-plante et Procédés de phytoremédiation (Memoris)
Liénard, Amandine ULiege

Conference given outside the academic context (2017)

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See detailCharacterization of metallic trace elements in soils by portable X-ray fluorescence spectrometry
Rosière, Clément; Godin, Bruno; Liénard, Amandine ULiege et al

Poster (2017)

1. Introduction X-ray Fluorescence Spectrometry (XRF) is undeniably a valuable asset for the simultaneous determination of mineral elements. This is a fast, non-destructive and inexpensive method in ... [more ▼]

1. Introduction X-ray Fluorescence Spectrometry (XRF) is undeniably a valuable asset for the simultaneous determination of mineral elements. This is a fast, non-destructive and inexpensive method in comparison with conventional analysis methods. The recent development of portable spectrometers (pXRF) further increases the potential of the XRF technique in environmental purposes by bringing the device to the field. This work focused on trace elements determination (Cu, Zn, Pb, Ni, Cr and As), most of which are subject to specific regulations, especially for sewage sludge (expect As) and contaminated soil management. In Wallonia, the reference method is based on aqua regia (HCl+HNO3, ISO 11466) digestion followed by Atomic Absorption Spectrometry (AAS) or Inductively-coupled plasma atomic emission- or mass- spectrometry (ICP-AES/ICP-MS). It is established that aqua regia digestion-based analysis underestimates the total content of elements because it does not completely digest silicates, while XRF is supposed to measure total content. To assess the performance of a pXRF (S1 Titan 600, Bruker), we compared the prediction values with the values from the aqua regia digestion for some reference values in soils. 2. Material and methods Seventeen soils (mainly agricultural soil), all of which were already evaluated for concentration of some metallic trace elements, were analyzed by pXRF in desktop configuration with XRF cells (Ø 40 mm, Prolene film 4µm) according to a validation process and were compared to their current aqua regia digestion-AAS values. Soil selection was based on results of a principal component analysis (PCA) using metallic trace elements and major elements (Ca, Mg, K, P, Fe) aqua regia contents, followed by a hierarchical cluster analysis (Ward’s method) to extract samples as diversified as possible. In addition, three inter-laboratory reference materials from BIPEA were subjected to the same protocol to carry out checks on the laboratory experiments. All samples were air-dried, sieved and crushed to 200 µm. Time measurement was set to 30 seconds in dual phase (60 seconds total). In order to assess the validity of the pXRF, the accuracy profile’s method [1] was chosen. Under intermediate precision conditions (5 days and 3 repetitions/day), results were calculated as the mean of 3 successive readings. The accuracy profile allows determining an interval which will contain 95% of the measurements. This interval was then compared to an acceptability interval, which was fixed at ± 20% of the reference value, to vouch for the validity. Reference values of each metallic trace element were calculated as the mean of 5 series of measurements according to an aqua regia digestion-AAS method. For the purpose of improving the trueness, two types of regression were applied between XRF and reference values: a simple linear regression and a FREML regression [2]. The advantage of the latter is that it can take into account errors on both X and Y variables. Dataset was split into one calibration set (2/3) and one validation set (1/3). In addition, the performance of the pXRF was compared to a laboratory wavelength-dispersive X-ray fluorescence spectrometer (WDXRF) supposed to give more reliable results and total contents. 3. Results and discussion Strong linear correlations were found in soils for Cu, Zn or Pb (R² > 0.99) between pXRF and aqua regia digestion-AAS. This linear correlation was very poor for Cr, probably due to internal calibration issues. Figure 1 shows the Zn accuracy profile, where the underestimation by pXRF can be seen. A simple slope and y-intercept correction of pXRF data could generally restore the trueness (bias) to improve the accuracy on a larger concentration range. However, concentration levels close to detection limits have a higher degree of random variability. This can be explained by the Horwitz curve where random variability increases with lower concentrations. This emphasizes the need of multiplying the number of measurements/readings. The comparison made of the pXRF with the WDXRF showed that the pXRF underestimates the metallic trace elements content. Indeed, the pXRF results were lower than WDXRF results. But, in terms of prediction of the reference values, the pXRF seems to be only slightly worse than the WDXRF. This shows the power of the portable XRF to predict AAS reference values at a low cost. Figure 1. Zinc Accuracy profile. Red short dotted line: Acceptance limits. Orange long dotted line: Tolerance limits 4. Conclusions S1 Titan XRF is an interesting tool and easy to use for the prediction of metallic trace elements content in soils. However, to predict reference values (aqua regia digestion-AAS) with sufficient accuracy, direct measurements are not suitable and a specific XRF calibration is recommended. A simple linear or FREML regression is adequate to improve the accuracy of the measured values in some cases, depending on the wanted future application. 5. References [1] M Feinberg, M Laurentie 2010. Validation des méthodes d’analyse quantitative par le profil d’exactitude. Cah. Tech. l’INRA No Special, 139, 2010. [2] Analytical Methods Committee (AMC). Fitting a linear functional relationship to data with error on both variables [technical brief no. 10]. R. Soc. Chem. 1(10), 2002. [less ▲]

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See detailSite expérimental du Martinet - Premiers résultats
Liénard, Amandine ULiege; Colinet, Gilles ULiege

Conference given outside the academic context (2016)

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See detailAssessment of vertical contamination of Cd, Pb and Zn in soils around a former ore smelter in Wallonia, Belgium
Liénard, Amandine ULiege; Colinet, Gilles ULiege

Conference (2016, September 14)

Examples of sites contaminated by atmospheric fallouts are numerous across former industrial areas, among which the valleys of Sambre and Meuse in Wallonia hosted metal ore treatment factories. We have ... [more ▼]

Examples of sites contaminated by atmospheric fallouts are numerous across former industrial areas, among which the valleys of Sambre and Meuse in Wallonia hosted metal ore treatment factories. We have studied the fate of Cd, Pb and Zn in soils affected by atmospheric deposition in the vicinity of old smelters. The importance of vertical redistribution of contaminants in soils is questioned and the aims of this paper are to i) characterize the vertical distribution of TEs and soil properties along diverse soil profiles, ii) evaluate enrichment or impoverishment of TEs along the profiles to discriminate anthropogenic or geogenic origin of contaminations and iii) evaluate whether soil type or land use influenced the mobility of contaminants in the selected profiles. Concentrations of trace elements (Cd, Co, Cr, Cu, Ni, Pb, and Zn) and major elements (Ca, Mg, K, Fe, Al, and Mn) as well as pHKCl and TOC were measured on 22 profiles located in a 3 km radius of a former ore treatment plant in Wallonia (Belgium). Enrichment factor (EF), vertical impoverishment factor (VIF), and availability ratio (AR) were used as diagnostic tools of contamination and migration of Cd, Pb, and Zn in profiles. Data revealed that soil profiles are significantly contaminated. The ranges of enrichment factors for Cd (17-3570), Pb (1-2883), and Zn (2-309) are very broad with the higher EF in the topsoil of profile. VIFs of subhorizons are rarely above 1. In a few remaining cases with VIF > 1, the main factor explaining is soil type (especially, Colluvic Regosols, Luvisols, and, Cambisols with shale load). Cd, Pb and Zn ARs are strongly correlated with TOC and to a lesser extent with pHKCl. Pb and Zn ARs are influenced by soil type and land use only plays on Zn AR. The Cd availability is independent by these two factors. The contents of trace elements measured in soil profiles are very high especially in topsoil. Until now, the Cd, Pb, and Zn vertical distribution shows a low migration from topsoil up to depth. However, we must not minimize the hazard of a future potential transfer. [less ▲]

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See detailCaractérisation multiscalaire de contaminations en éléments traces dans les sols : distribution spatiale et verticale, évaluation du transfert sol-plante-vers de terre et gestion potentielle par amendements organiques
Liénard, Amandine ULiege

Doctoral thesis (2016)

Human economic and technological development has a negative impact on the environment. The soil is not spared from this growing threat through its role in the environmental interface. Once degraded as a ... [more ▼]

Human economic and technological development has a negative impact on the environment. The soil is not spared from this growing threat through its role in the environmental interface. Once degraded as a result of contamination, it can no longer fulfill its ecosystem functions such as the protection of ecosystems, food production or preservation of the quality of surface water and groundwater. The studies presented in the thesis are on soil contaminated by atmospheric fallouts enriched by trace elements. This type of contamination increases the natural levels of contaminants in soils and particularly in surface horizons to exceed the maximum levels set by legislation. The first axe of research concerns the assessment of contamination at a landscape scale around a former zinc-lead ore-treatment plant. The spatial distribution of cadmium, lead and zinc in the topsoil (0-20 cm) was characterized using 247 samples taken in crop, grassland and forest on three major types of loam soils representative of the study area Sclaigneaux (Wallonia, Belgium). The distribution of contaminants is explained by the distance to the source of contamination, direction of dominant winds, land use and soil type. Subsequently, 22 soil profiles were sampled within the study area to estimate the vertical transfer of contaminants. Based on various indexes of contamination, no migration along the profiles has been demonstrated. Only some more clay horizons presented contaminant levels that increased relative to their upper horizons. The second approach studied the soil-plant transfer and soil-plant-worm transfer of contaminants. First, a field study of the quality of grains of barley (Hordeum vulgare L.) harvested in the study area Sclaigneaux was performed. It appears that the concentration of cadmium in the grain meets quality standards for placing the cereals on the market. However, 78% and 94% of zinc and cadmium, respectively, concentrations measured in grains exceed the expected levels of a non-impacted environment by human activity. Secondly, a study on microcosms was conducted with soils of agricultural parcels around Sclaigneaux on which two crops (faba bean, Vicia faba L. and corn, Zea mays L.) were grown and where earthworms (Eisenia fetida (Savigny)) were introduced. The life traits of E. fetida such as mortality and adult weight were not affected by the levels of contaminants unlike the presence of plants which limit their reproduction (weight and number of cocoons). Moreover, the presence of E. fetida in microcosms influenced the mobility and bioavailability of contaminants. The third approach deals with metal contaminations in vegetable gardens and their management using organic amendments. This method of stabilization aims to decrease the labile fraction of soil contaminants and further reduce their transfer to plants. To do so, two vegetables (spinach, Spinacia oleracea L. and lettuce, Lactuca sativa L.) were grown on contaminated garden soils enriched in various amendments sold in garden centers. The major finding of this study is that management by amendments does not allow a systematic decrease in the soluble fraction contaminants. This is mainly due to the direct intake of rapidly mobilized trace elements produced by the addition of some of the studied amendments. [less ▲]

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See detailPédologie - Concepts de base
Liénard, Amandine ULiege

Conference given outside the academic context (2016)

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See detailAssessment of vertical contamination of Cd, Pb and Zn in soils around a former ore smelter in Wallonia, Belgium
Liénard, Amandine ULiege; Colinet, Gilles ULiege

in Environmental Earth Sciences (2016), 75

Concentrations of trace elements (Cd, Co, Cr, Cu, Ni, Pb and Zn) and major elements (Ca, Mg, K, Fe, Al and Mn) as well as pHKCl and total organic carbon (TOC) were measured on 22 profiles located in a 3 ... [more ▼]

Concentrations of trace elements (Cd, Co, Cr, Cu, Ni, Pb and Zn) and major elements (Ca, Mg, K, Fe, Al and Mn) as well as pHKCl and total organic carbon (TOC) were measured on 22 profiles located in a 3 km radius of a former ore-treatment plant in Wallonia (Belgium). The enrichment factor (EF), vertical impoverishment factor (VIF) and availability ratio (AR) were used as diagnostic tools of contamination and migration of Cd, Pb and Zn in profiles. The data revealed that the soil profiles are significantly contaminated. The ranges of EFs for Cd (17–3570), Pb (1–2883) and Zn (2–309) are very broad with the higher EF in the topsoil of the profiles. VIFs of subhorizons are rarely above 1. In the few cases with VIF > 1, the main factor explaining is the soil type (in particular, Colluvic Regosols, Luvisols and Cambisols with shale load). Cd, Pb and Zn ARs are strongly correlated with TOC and to a lesser extent with pHKCl; Pb and Zn ARs are influenced by soil type while land use only has an effect on Zn AR. The Cd availability is independent of these two factors. The contents of trace elements measured in soil profiles are very high, especially in topsoil. At present, the Cd, Pb and Zn vertical distribution shows a low migration from topsoil to deeper levels. However, we must not discount the hazard of a future potential transfer. [less ▲]

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See detailEarthworms Eisenia fetida affect the uptake of heavy metals by plants Vicia faba and Zea mays in metal-contaminated soils
Lemtiri, Aboulkacem ULiege; Liénard, Amandine ULiege; Alabi, Taofic ULiege et al

in Applied Soil Ecology (2016), 104

Earthworms increase the availability of heavy metals in some situations and aid in maintaining the structure and quality of soil. The introduction of earthworms into metal-contaminated soils has been ... [more ▼]

Earthworms increase the availability of heavy metals in some situations and aid in maintaining the structure and quality of soil. The introduction of earthworms into metal-contaminated soils has been suggested as an aid for phytoremediation processes. In Wallonia, Belgium, a century of industrial metallurgic activities has led to the substantial pollution of soils by heavy metals, including copper (Cu), zinc (Zn), lead (Pb) and cadmium (Cd), due to atmospheric dusts. Two plant species, Vicia faba and Zea mays, and earthworms (Eisenia fetida) (Savigny, 1826) were exposed to different concentrations of long-term-contaminated soils for 42 days. The soil samples, which were collected from the land surrounding a former Zn-Pb ore-treatment plant, exhibited different levels of heavy metals. Our aim was to evaluate the role of earthworms E. fetida on the availability of metals in soils and their effects on metal uptake by V. faba and Z. mays plants at different soil concentrations. The results suggest that earthworms and plants modified the availability of metals in contaminated soils after 42 days of exposure. Earthworm life-cycle parameters were affected by metal contamination and/or the addition of plants; cocoon production and weight were more responsive to adverse conditions than earthworm survival or weight change. The concentrations of Pb and Cd in earthworm tissues decreased in the presence of plants. Results showed that metal accumulation in plants depended on the metal element considered and the presence of earthworms. However, the presence of earthworms did not change the concentrations of metals in plants, except for Cd. In the presence or absence of earthworms, V. faba accumulated higher concentrations of Cu and Zn compared with Z. mays, which accumulated higher concentrations of Cd. These findings have revealed that earthworm activities can modify the availability of heavy metals for uptake by plants in contaminated soils. Moreover, the study results show that the ecological context of phytoremediation should be broadened by considering earthworm-plant-soil interaction, which influence both the health of the plant and the uptake of heavy metals by plants. [less ▲]

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See detailEvaluation of the contamination of the soil and forage by heavy metals in the pastureland of the north west of Tunisia
Riahi, Thameur; Colinet, Gilles ULiege; Said, S et al

Poster (2015, November)

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See detailCaractérisation des systèmes sols-plantes dans les collines de l’arc cuprifère du Katanga (synthèse bibliographique)
Kaya Muyumba, Donato ULiege; Liénard, Amandine ULiege; Mahy, Grégory ULiege et al

in Biotechnologie, Agronomie, Société et Environnement = Biotechnology, Agronomy, Society and Environment [=BASE] (2015), 19(2), 204-214

Introduction: The Copper belt of Katanga presents huge resources of Cu and Co-ore. On the copper hills, mineralized rocks outcrop and a specific flora did develop as a response to the high levels of Cu ... [more ▼]

Introduction: The Copper belt of Katanga presents huge resources of Cu and Co-ore. On the copper hills, mineralized rocks outcrop and a specific flora did develop as a response to the high levels of Cu and Co in soil. Soil-vegetation relationships need to be understood in order to elaborate biodiversity conservation programs prior to industrial mining of the copper hills. Literature: This paper reviews knowledge about soil characterization in the copper hills of Katanga and makes proposals for further research about the influence of the very specific chemical conditions of contaminated soils on the vegetation. The focus was put on the geochemical background and the bioavailability of Cu and Co. A lot of progress has been made recently about identification of soil-vegetation relationships. Conclusion: However, the issue of Cu and Co mobility within soil-plant systems is not entirely solved. [less ▲]

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See detailSynthèse bibliographique sur la mobilité des éléments traces dans les sols et l’utilisation de la stabilisation physico-chimique comme technique de gestion in situ des sites contaminés
Liénard, Amandine ULiege; Colinet, Gilles ULiege

in Biotechnologie, Agronomie, Société et Environnement = Biotechnology, Agronomy, Society and Environment [=BASE] (2014), 18(2), 273-289

Industrial activities have deeply impacted the quality of biophysical environment at places. This review focuses on consequences of soil contaminations by metallic trace elements: what conditions the ... [more ▼]

Industrial activities have deeply impacted the quality of biophysical environment at places. This review focuses on consequences of soil contaminations by metallic trace elements: what conditions the mobility of contaminants in soils and what are the remediation practices based upon physico-chemical stabilization? This technique is an in situ remediation which aims at limiting the dispersion of metals in the environment by use of soil conditioners and amendments in contaminated sites. First of all, we reviewed the concepts of mobility of trace elements and their indicators. Then, we compiled the different kinds of amendments applied to stabilize contaminants in soils and the processes involved. [less ▲]

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See detailHazards of plant contamination around former Zn-Pb industries in Wallonia
Liénard, Amandine ULiege; Colinet, Gilles ULiege

Poster (2014, February 26)

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