platinum group element distribution in the soils from urban areas of the campania region (italy)

Platinum group element distribution in the soils from urban areas of theCampania region (Italy)

D. Cicchella1, L. Fedele2, B. De Vivo2, S. Albanese2 & A. Lima2

1Dipartimento di Studi Geologici ed Ambientali, Università degli Studi del Sannio, Via dei Mulini 59/A, 82100Benevento, Italy (e-mail: [email protected])

2Dipartimento di Scienze della Terra, Università di Napoli ‘Federico II’, Via Mezzocannone 8, 80138 Napoli, Italy

ABSTRACT: This paper represents a detailed study to assess the platinum groupelement (PGE) content of topsoils from urban areas in the Campania region (Italy),following on from previous work. Samples were collected from residual andnon-residual soils from flowerbeds in the urban areas of Avellino, Benevento andCaserta (characterized by low population density, LPD), and in Salerno (a city withhigh population and high automobile traffic densities).

The soils (<100-mesh size fraction, i.e. <150 µm) were analysed for Pt, Pd and Rhby fire assay ICP-MS and for 37 other elements by ICP-AES and ICP-MS after amodified aqua regia digestion. In LPD cities, PGE concentrations were close tobackground values (with the exception of the industrial areas), but Salerno proved tobe contaminated by PGEs. Platinum, Pd and Rh concentrations are in the <0.1–278,<0.5–432 and 0.07–47 ppb range, respectively. Moreover, a high correlation amongPt, Pd and Rh (R=0.98), and between PGEs and other typical traffic-emitted metalssuch as Cr, Cu, Sb and Sn has been detected only in Salerno. Finally, the statisticalanalysis pointed out a lower background for PGEs in soils formed on sedimentaryrocks (in the eastern sector of Caserta, in Benevento and Salerno) compared to thoseformed on volcanic rocks (Avellino and the western area of Caserta).

KEYWORDS: platinum group elements, background concentration, urban soil, environmental pollution

INTRODUCTION

Catalytic converters (CCs) have been used in cars in westerncountries for the last 20 years (Barefoot 1999; Ely et al. 2001).These devices allow removal of pollutants such as CO, hydro-carbons and NOx, catalysing the reactions that convert theminto less toxic chemicals such as CO2, N2 and H2O. A modernCC is essentially a monolithic honeycomb support coated withan ‘activated’ alumina layer (the washcoat) upon which thecatalysts (Pt, Pd and Rh) are fixed. Different types of convertersexist and their characteristics depend on the type and size ofengine they are attached to.

Although CCs efficiently serve their purpose, an unwantedeffect of their use is the dispersion of dust containing platinumgroup elements (i.e. particulate matter (PM)-PGEs) in theenvironment. Release of PM-PGEs is caused by chemical andphysical stress of the washcoat surface during the discharge ofexhaust gases from the engine (König et al. 1992; Artelt et al.2000). Amounts and rates of PM-PGE emissions, whichaccount for more than 90% of the PGEs released in theenvironment by CCs (Ravindra et al. 2004), depend upon enginetype, car speed, fuel additives and type and age of the CC (Arteltet al. 2000; Ely et al. 2001). Barbante et al. (2001) have estimatedthat the annual Pt emission from automobile CCs alone can beas high as 0.5–1.4 tonnes per annum.

In recent years a number of studies have proved that theamount of PGEs along roadsides has increased since theintroduction of CCs, and hence further build-up should beexpected (Schäfer & Puchelt 1998; Barefoot 1999; De Miguel

et al. 1999; Petrucci et al. 2000; Ely et al. 2001; Jarvis et al. 2001;Cinti et al. 2002; Cicchella et al. 2003; Ravindra et al. 2004). WhilePGEs in metallic form are assumed to be inert with respect tobiological reactions, some platinum compounds are known tohave adverse consequences on human health and there is thepotential for PGEs to enter diverse ecosystems via adsorptionby flora and fauna (Zereini & Alt 2000; Ravindra et al. 2004, andreferences therein).

The objectives of this study were to:

(1) show the distribution of PGE concentration values and todetermine their background contents in the topsoils of theurban areas of Campania region;

(2) provide reliable analytical data to allow a quantitativeassessment of PGE pollution threat to ecosystem andhuman health;

(3) provide a sound basis to be used by policy-makers andlegislators for addressing public concerns regardingenvironmental pollution.

PGE concentration data only are discussed, while theremaining geochemical data produced were used to compile theenvironmental geochemical atlas of the urban areas of Avellino,Benevento, Caserta and Salerno (Albanese et al. 2007; Cicchellaet al. 2007; Fedele et al. 2007; Lima et al. 2007).

STUDY AREAS

This study was conducted in the urban areas of the Campaniaregion (Avellino, Benevento, Caserta and Salerno), following on

Geochemistry: Exploration, Environment, Analysis, Vol. 8 2008, pp. 31–40 1467-7873/08/$15.00 � 2008 AAG/ Geological Society of London

from previous work carried out in the city of Napoli, in thesame region, by Cicchella et al. (2003).

Avellino (60 000 inhabitants in an area of c. 30 km2, with apopulation density of 2000 inhabitants per km2) is an importantjunction for all the roads that connect the Adriatic with theTyrrhenian coastline, and the main connection between thecities of Benevento and Salerno (Fig. 1). The city stands atthe centre of a basin formed by Mt. Partenio and the Picentinimountains, along the Sabato Valley. This is an area full ofvegetation, especially walnut trees, vegetable gardens and fruittrees. Intense industrial activity has developed on the NW partof the territory. Soils have strong andic properties (Arnalds et al.2007) since they developed from pyroclastic deposits (vitricandosols) (Di Gennaro 2002).

Benevento (63 000 inhabitants in an area of c. 130 km2, witha population density of 485 inhabitants per km2) lies on a ridgebetween the Calore and the Sabato rivers, NE of Naples. It islocated at the centre of a large depression, surrounded to thenorth and west by the carbonate massifs of Matese, Taburnoand Avella, and to the east and south by the low ridges of theSannita Apennine. The Calore river and its tributaries (Miscano,Ufita, Tammaro and Sabato rivers) flow between these tworidges, along long valleys, to end in the Benevento depression.The city economy is essentially based on agriculture. The soilsin the urban centre developed on recent and present alluvialdeposits (fluvic-cambisols), or on ancient, terraced alluvialdeposits (cutanic luvisols). Soils developed on clays, with finetextures and with strong vertic properties (Isbell 1996), prevailin the north, while moderately fine-textured soils, which devel-oped on marls (haplic-calcisols), predominate in the south (DiGennaro 2002).

The city of Caserta (75 200 inhabitants in an area ofc. 56 km2, with a population density of 1343 inhabitants per

km2) is located at the eastern border of the fertile Campanianplain, at the base of the Tifatini mountains. It is an importantcommercial, tourist and industrial centre. Its territory is char-acterized by limestones and Mesozoic dolomitic limestonesoutcrops in the north, while hills made up of Mioceneterrigenous sediments occupy the NE. The remaining part ofthe territory is essentially flat and made up mostly of ignimbriticdeposits from Roccamonfina volcano. Most of the soils in thisterritory developed from ash fall and medium-textured pumicedeposits (vitric andosols) (Di Gennaro 2002).

The city of Salerno (138 200 inhabitants in an area ofc. 59 km2, with a population density of 2344 inhabitants perkm2), located in the northern part of the Salerno Gulf, isdeveloped parallel to the coast between the Tyrrhenian sea andthe inland hills. Salerno is an important street, railroad andmarine nexus for the Campania region and Italy. Soils of thedensely populated urban area are alluvial along the coastline,while the inland hills are covered by soils developed onconglomerates. Andisols prevail in the NW (Di Gennaro 2002).

METHODS

Soil sampling

A total of 163 soil samples were collected in the four urbanareas of Avellino (34), Benevento (40), Caserta (40) and Salerno(49). Since the bulk of the PGEs released in the environmentcomes from vehicle traffic (Ravindra et al. 2004), city centreswere sampled at a greater density than suburban areas, whichare clearly less affected by traffic.

Three sub-sites located at a distance of c. 10 m from eachother were sampled at each location. Approximately 3 kg of soilwere collected from between 0 and 15 cm below the surface,and stored in inert plastic bags (De Vivo et al. 2006).

Fig. 1. Location of investigated urban areas in Campania Region (Italy).

D. Cicchella et al.32

Chemical analysis

All samples were air-dried and sieved to <100-mesh fraction(<150 µm). Analyses for Pt, Pd and Rh were carried outby Acme Analytical Laboratories Ltd (Vancouver, Canada)accredited under ISO 9002.

Pulp splits of 30 g were weighed into fire-assay crucibles. Thesample aliquot was custom-blended with fire assay fluxes, PbOlitharge and an Ag inquart. Firing the charge at 1050�C liberatesAu�PGEs that report to the molten Pb-metal phase. Oncecooled, the Pb button is recovered and fired in a MnO cupel at950�C to give an Ag�Au�PGEs dore bead. The bead isweighed and parted (i.e. leached in 1 ml of hot HNO3) todissolve Ag; 10 ml of HCl is then added to dissolve theAu�PGEs. A Rh fire assay requires inquarting with Au forquantitative analysis. Lower Au, Pt and Pd detection limitsare achieved by a longer determination time on the Elan6000 ICP-MS. Rhodium determined from an Au inquartgives a quantitative analysis whereas Rh by Ag inquart issemiquantitative owing to the limited solubility of Rh in Ag.

Quality assurance/quality control (QA/QC) protocol incor-porates: a sample-preparation blank (SI or G-1) carried throughall stages of preparation and analysis as the first sample; a pulpduplicate to monitor analytical precision; a �10-mesh ‘rejects’duplicate to monitor sub-sampling variation; two reagent blanksto measure background; and aliquots of in-house controlreference material FA-100S to monitor accuracy. Group 3B-MSof Acme incorporates new crucibles and additional reagent

blanks to allow accurate analysis at very low concentrationlevels.

Precision is calculated on eight blind duplicates submitted bythe authors. Raw and final data undergo a final verification bya British Columbia Certified Assayer who signs the AnalyticalReport. Table 1 lists the elements determined, instrumentaldetection limits, accuracy errors and precisions of thegeochemical data.

Statistical analysis and geochemical mapping

In order to show the single-element geochemical distribution, adetailed univariate analysis has been performed. A value corre-sponding to 50% of the instrumental detection limit (IDL) wasassigned to all data reported as below the IDL in order to allowinclusion in the statistical analysis. All data were normalized bylogarithmic conversion (log10). Table 2 presents all the calcu-lated statistical parameters. Table 3 shows, for each urban area,the correlation matrix between PGEs and other elemental dataconcentration.

The maps showing sampling sites and Pt, Pd and Rhdistributions have been generated using the ArcView andGeoDas programs (Cheng 2000). The multifractal inversedistance weighted algorithm has been utilized as the interpola-tion method to compile the geochemical maps (Cheng 1999a,b). In order to determine the PGE background values in theinvestigated urban areas (Table 4) the concentration–area fractalmethod (C-A) has been utilized (Cheng et al. 1994, 1996, 2000,2001; Lima et al. 2003; Cicchella et al. 2005).

The C-A method was developed by Cheng et al. (1994) forgeochemical anomaly separation. C-A is a fractal method thatcan be used to separate anomalies from background on thebasis of geochemical concentration values, spatial variability ofgeochemical values and geometrical and scaling properties. Itinvolves a plot of concentration values (c) against the area withconcentration value above a cutoff (Figs 2, 3, 4, 5). From amultifractal point of view, the extreme values, which areanomalous from a geochemical point of view, may follow a

Table 1. Detection limits, accuracy error and precision for Pt, Pd, Rd determined by fireassay ICP-MS.

Element Detection limit (ppb) Accuracy �(%) Precision (% RPD)

Pt 0.1 3.9 15Pd 0.5 3.3 22Rh 0.05 21 54

RPD, relative percentage difference

Table 2. Statistical parameters for soil samples from Avellino, Benevento, Caserta and Salerno. All values in ppb.

Min. Max. Mean Median Geometric mean 25th percentile 75th percentile Std dev. No. samples No. samples b.d.l.

Avellino

Pt 1 6.1 2.4 2.1 2.2 1.8 2.9 1 34 0Pd <0.5 38 2.2 1 1 0.7 1.7 6.4 34 7Rh <0.05 0.61 0.06 <0.05 <0.05 <0.05 <0.05 0.13 34 31

Benevento

Pt 0.4 18.4 2 1 1.2 0.7 2 3.3 40 0Pd <0.5 8.7 1.5 0.9 0.9 0.5 1.8 1.8 40 9Rh <0.05 0.6 <0.05 <0.05 <0.05 <0.05 <0.05 0.09 40 36

Caserta est

Pt 0.1 3.2 1 0.7 0.8 0.5 1.1 0.8 19 0Pd <0.5 1.7 0.5 <0.5 <0.5 <0.5 0.6 0.4 19 13Rh <0.05 0.29 0.06 <0.05 <0.05 <0.05 <0.05 0.08 19 15Caserta west

Pt 0.4 13.5 4.2 2.3 2.5 0.9 6.2 3.8 21 0Pd <0.5 30.8 3.8 1.1 1.3 <0.5 3.6 6.8 21 8Rh <0.05 2.45 0.6 0.32 0.2 <0.05 1.1 0.75 21 7

Salerno

Pt <0.1 278 13.1 2.1 2.8 0.7 10.3 40.4 49 2Pd <0.5 432 15.3 2.4 3 1.3 7.2 61.6 49 6Rh 0.07 47 1.79 0.28 0.48 0.23 0.93 6.7 49 0

b.d.l., below detection limit.

Platinum group element distribution in soils 33

fractal rather than a normal or log-normal distribution. The C-Aplot facilitates the distinction of anomalies from background onthe basis of concentration values (i.e. a frequency distribution of

values), as well as the spatial and geometrical properties ofgeochemical patterns. A C-A plot on log–log paper can beused to establish power-law relationships between the areasA(A � c) with the concentration values greater than c andthe concentration value c itself. A number of straight-linesegments can be manually or automatically fitted to the valuesof A(A � c) versus c for various values of c plotted on thelogarithmic scale, each representing a power-law relationshipbetween the area A and the cutoff concentration value c. Theintersections of these straight-line segments provide a set ofcutoff values for subdividing the concentration scale intodiscrete classes. On the map, these classes are zones that oftenhighlight the effects of underlying geochemical processes suchas mineralization and alteration, as well as patterns that are dueto regional geological processes. Further details can be found inCheng et al. (1994, 1996, 2000, 2001), Lima et al. (2003) andCicchella et al. (2005).

Table 3. Correlation coefficients of elemental concentration in soils from Avellino, Benevento, Caserta and Salerno.

Avellino PtPt 1 PdPd 0.69 1 RhRh 0.13 �0.04 1 CdCd �0.10 0.14 �0.11 1 CrCr �0.14 0.06 �0.01 0.07 1 CuCu 0.02 �0.06 0.01 0.01 0.27 1 HgHg 0.01 0.14 �0.06 0.46 �0.05 0.28 1 MoMo 0.51 0.44 0.12 0.25 �0.17 0.15 0.24 1 PbPb 0.24 0.43 �0.14 0.60 0.06 0.14 0.26 0.50 1 SbSb 0.28 0.58 �0.08 0.69 �0.01 0.02 0.39 0.61 0.87 1 ZnZn �0.08 0.06 �0.16 0.51 0.03 0.38 0.52 0.29 0.63 0.57 1

Benevento PtPt 1 PdPd 0.21 1 RhRh 0.82 0.14 1 CdCd 0.09 0.13 0.03 1 CrCr 0.17 0.20 0.03 0.46 1 CuCu 0.19 0.15 0.02 0.48 0.35 1 HgHg 0.43 0.20 0.07 0.23 0.15 0.30 1 MoMo 0.53 0.54 0.36 0.39 0.38 0.47 0.33 1 PbPb 0.25 0.41 0.08 0.54 0.20 0.37 0.50 0.59 1 SbSb 0.35 0.41 0.15 0.73 0.48 0.47 0.40 0.72 0.76 1 ZnZn 0.30 0.35 0.09 0.78 0.35 0.50 0.47 0.64 0.71 0.83 1

Caserta PtPt 1 PdPd 0.50 1 RhRh 0.77 0.81 1 CdCd �0.18 �0.18 �0.15 1 CrCr �0.22 �0.24 �0.28 0.64 1 HgHg 0.09 0.17 0.06 �0.02 �0.10 1 MoMo 0.12 �0.04 0.03 �0.06 �0.07 0.01 1 NaNa 0.57 0.64 0.64 �0.15 �0.41 0.39 0.02 1 PbPb 0.08 0.01 0.18 0.13 �0.04 0.26 0.28 0.37 1 SbSb 0.06 0.11 0.17 0.23 0.10 0.14 0.71 0.15 0.53 1 ZnZn 0.00 0.09 0.03 0.01 �0.07 0.57 0.17 0.27 0.57 0.34 1

Salerno PtPt 1 PdPd 0.98 1 RhRh 0.98 0.98 1 CrCr 0.77 0.80 0.77 1 CuCu 0.88 0.89 0.89 0.88 1 HgHg 0.29 0.30 0.27 0.35 0.32 1 MoMo 0.37 0.39 0.38 0.46 0.52 0.14 1 PbPb 0.32 0.28 0.26 0.34 0.35 0.24 0.20 1 SbSb 0.68 0.67 0.66 0.78 0.84 0.34 0.52 0.54 1 SnSn 0.65 0.65 0.63 0.80 0.80 0.50 0.44 0.63 0.86 1 ZnZn 0.38 0.33 0.33 0.61 0.48 0.31 0.28 0.49 0.61 0.72 1

Table 4. Background concentration values in ppb for PGEs in urban soils from Avellino,Benevento, Caserta, Salerno and Napoli.

Pt Pd Rh Soil type

Avellino 3.2 2.8 <0.05 Soils formed on volcanic rocksBenevento 1.3 1.1 <0.05 Soils formed on sedimentary rocksCaserta east 1.1 0.9 <0.05 Soils formed on sedimentary rocksCaserta west 2.7 2.3 0.3 Soils formed on volcanic rocksSalerno 1 1 0.4 Soils formed on sedimentary rocksNapoli 6 10 – Soils formed on volcanic rocks

Napoli data from Cicchella et al. (2003).


RESULTS AND DISCUSSION

A dot and interpolated map for every urban area is shown inFigures 2, 3, 4, and 5 together with the relative C-A plot.Comparing these maps with those in Figure 1, the relationshipbetween the high PGE concentrations and the areas of highpopulation density or the main traffic routes becomes evident.Low concentrations are instead found in areas of low popu-lation density or low traffic intensity.

Average PGE concentrations in Avellino (Table 2) aremoderate and very close to background values (Table 4 andFig. 6A). Similar situations are recorded for Benevento andCaserta. High PGE levels and high Rh concentrations wererecorded in Salerno (Fig. 5) and in the western area of Caserta(Fig. 4), respectively.

The soils of all urban areas are enriched with both Pt and Pd(Fig. 6B). However, this enrichment is much higher for Pt and

Pd (>5) in Avellino (Fig. 2) and the western area of Caserta(Fig. 4) than in Salerno (Fig. 5) and Benevento (Fig. 3) urbanareas and in the eastern sector of Caserta (Fig. 4). The high Ptand Pd enrichment of Avellino soils is similar to that found inthe urban area of Napoli (Cicchella et al. 2003; De Vivo et al.2006).

Platinum and Pd enrichment in soils from Avellino, westernCaserta and urban areas of Napoli (which translates into higherbackground for these elements) is due to their common originfrom pyroclastic rocks originating from Vesuvius and differentignimbrite events in the Campania Plain (De Vivo 2006). Soilsin other urban areas developed from sedimentary rocks.

In Avellino (Fig. 2) only two samples showed Pt concen-trations >4 ppb (which are considered anomalous). Thesesamples were taken in the city centre and near highways. Theonly sample with a high Pd concentration (38 ppb, almost 15times the local background value) was taken in the centre of the

Fig. 2. Pt, Pd and Rh geochemicalmaps of municipal area of Avellino andfractal concentration–area (C-A) plot.


urban area near an intersection where cars are often forced intoa ‘stop and go’ mode, which strongly reduces the performanceof CCs. Most samples show Rh concentrations of <0.05 ppb, avalue considered equal to the local background.

In the urban area of Benevento (Fig. 3) almost 70% of thesamples have concentrations close to or below the localbackground for Pt, Pd and Rh (Table 4). For high concentrationsamples, Pt, Pd and Rh show different spatial concentrations.Palladium values are more elevated in the urban area, whereasPt and Rh are concentrated in the industrial area.

In the urban area of Caserta, two different PGE backgroundscan be defined. The soils of the western sector, developed fromignimbritic volcanic rocks (De Vivo et al. 2001; Rolandi et al.2003), show a higher background than those of the eastern area(developed from sedimentary rocks: limestones and dolomitic

limestones). The eastern area, which is also the one with higherpopulation density, has higher concentrations of PGEs, whileaverage values in the western sector resemble the local back-ground (Fig. 6A, B).

Among the four urban areas investigated, the highest PGEconcentrations were monitored in Salerno (13, 15 and six timesthe local background for Pt, Pd and Rh, respectively; Figs 5 and6A). In one sample, Pt, Pd and Rh reach values of 278, 432 and47 ppb, respectively, which are extremely high even when com-pared to PGEs in soils from larger urban areas of Europe andMexico (Fig. 7). In almost 25% of the soils from the Salernourban area, Pt and Pd concentrations are <1 ppb, correspond-ing to the local estimated background (Fig. 5). Rhodium con-centration is <0.4 ppb, corresponding to the local estimatedbackground, in 60% of the samples (Table 4).

Fig. 3. Pt, Pd and Rh geochemicalmaps of municipal area of Beneventoand fractal concentration–area (C-A)plot.


It is evident that all the Salerno areas with low populationdensity and low traffic intensity have PGE concentrations closeto background values, while the industrial and the highlypopulated coastal area show concentrations from ten to severalhundred times higher than the background.

A strong correlation between Pt, Pd and Rh (R = 0.98), andbetween PGEs and Cr, Cu, Sb and Sn (typical traffic emitters)was found in Salerno (Table 3). Although previous studies havefound a strong positive correlation between PGEs and Pb(Schafer & Puchelt 1998; Ely et al. 2001; Cicchella et al. 2003),no strong association of Pb with any of the PGEs was observedin this study (Table 3).

SUMMARY AND CONCLUSIONS

PGE concentrations in topsoils from four major urban areas ofthe Campania region (Italy) were determined. The data wereanalysed using univariate and multivariate techniques. A new

multifractal inverse distance weighted algorithm was utilized asthe interpolation method to compile geochemical maps (Cheng1999a), while a fractal method was used to determine the PGEbackground values (Cheng et al. 1994, 1996, 2000, 2001; Limaet al. 2003; Cicchella et al. 2005).

Data analysis revealed that (1) PGE background values arehigher in soils formed on volcanic rocks than in those formedon sedimentary rocks, and (2) in Avellino, Benevento andCaserta, high PGE values are found only in industrial and highlypopulated areas. Soils from Salerno show high PGE contents,with Pd, Pt and Rh levels, respectively, reaching averageconcentrations 15, 13 and six times higher than the localbackground values. The highest values for these elementscorrespond to the location of emission sources (i.e. roads).Geochemical maps highlight the positive correlation betweenPGE concentrations and road distribution (i.e. high trafficflow). High PGEs are found mainly in samples collected alongthe coastline in a densely populated area, where PGE levels

Fig. 4. Pt, Pd and Rh geochemicalmaps of municipal area of Caserta andfractal concentration–area (C-A) plot.


Fig. 5. Pt, Pd and Rh geochemicalmaps of municipal area of Salerno andfractal concentration–area (C-A) plot.

Fig. 6. (A) Arithmetic mean versusestimated background values.(B) Estimated background values versusupper continental crust concentration(UCCC).


reach concentrations hundreds of times higher than the localbackground. The high correlation between PGEs and othertraffic-related elements, such as Cr, Cu, Sb and Sn, confirm therelationship between high traffic flow and high PGE levels.

The areas polluted by CC-emitted PGEs are quite large, andconsidering the present emission rates, they will most likelyincrease in the near future. Considering that CCs have beenmandatory in Italy only since 1993, and given the concen-trations detected in soils, it can be estimated that accumulationrates have probably increased very quickly. This is likely tocreate a significant health risk for humans and vegetation in thenear future.

This research was supported by PON fund to Professor B. De Vivo(Project PETIT-OSA; OR10). We wish to express many thanks tothe reviewers of the manuscript, Simon Pirc and Claudia Colombo,for their helpful comments.

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platinum group element distribution in the soils from urban areas of the campania region (italy)

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