Environmental Pollution 157 (2009) 847–856

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Arsenic stability and mobilization in soil at an amenity grassland overlyingchemical waste (St. Helens, UK)

William Hartley a,*, Nicholas M. Dickinson a, Rafael Clemente b, Christopher French a,1,Trevor G. Piearce c, Shaun Sparke a, Nicholas W. Lepp a

a School of Biological and Earth Sciences, Liverpool John Moores University, Byrom Street, Liverpool L3 3AF, UKb Department of Soil and Water Conservation and Organic Waste Management, Centro de Edafolog a y Biologa Aplicada del Segura, CSIC, Apartado 4195, 30080 Murcia, Spainc Biological Sciences Division, Lancaster Environment Centre, Lancaster University, Lancaster LA1 4YQ, UK

Stabilization of alkali industry waste requires careful management to minimise soil arsenic mobilization and dispersal to the wider environment.

a r t i c l e i n f o

Article history:

Received 23 June 2008

Received in revised form7 November 2008

Accepted 9 November 2008

Keywords:

Brownfield

PhytoremediationArsenic

Soil

Risk assessment

a b s t r a c t

A 6.6 ha grassland, established on a former chemical waste site adjacent to a residential area, contains

arsenic (As) in surface soil at concentrations 200 times higher than UK Soil Guideline Values. The site isnot recognized as statutory contaminated land, partly on the assumption that mobility of the metalloid

presents a negligible threat to human health, groundwater and ecological receptors. Evidence for this isevaluated, based on studies of the effect of organic (green waste compost) and inorganic (iron oxides,

lime and phosphate) amendments on As fractionation, mobility, plant uptake and earthworm commu-nities. Arsenic mobility in soil was low but significantly related to dissolved organic matter and phos-

phate, with immobilization associated with iron oxides. Plant uptake was low and there was littleapparent impact on earthworms. The existing vegetation cover reduces re-entrainment of dust-blownparticulates and pathways of As exposure via this route. Minimizing risks to receptors requires avoidance

of soil exposure, and no compost or phosphate application.

2008 Elsevier Ltd. All rights reserved.

1. Introduction

Two centuries of industrialization have created a considerable

legacy of pollutionin St. Helens in North WestEngland. In 1862, thisarea around an alkali works near Merton Bank was described asone scene of desolation [where] three-fourths of trees are totallydead. Farms recently well-wooded, and with hedges in good

condition, have now neither tree nor hedge left alive; whole fieldsof corn are destroyed. orchards and gardens have not a fruit treealive . pastures are so deteriorated that graziers refuse to place

stock on them (Brenner,1974; Dingle, 1982). The Alkali Act of 1863that resulted from this scene of desolation is recognized as thefirst UK pollution control legislation (Hawes, 1995). Widespreadelevated soil arsenic (As) is a major component of this legacy,largely associated with development of the town around the

manufacture of glass, alkali chemicals, paints and numerousmetallurgical industries. Both glass manufacture and soda ashproduction (from the Le Blanc process) produced very large

volumes of waste containing arsenic as a major contaminant. Glasswastes, known locally as Burgy Banks (St. Helens, 2007), have anelevated As content because arsenic trioxide (As2O3) was added to

glass as a clarifying agent.St. Helens is also adjacent to large coal reserves that created

considerable areas of spoil until mining ceased in the 1970s; in thelast 20 years the colliery spoil heaps have been the focus of large

scale reclamation activity for environmental improvement andrevegetation in the context of UK community forestry (Hodge,1995; Rawlinson et al., 2004; Bell et al., 2007). Prior to this, in the

early 1980s, a former ill-defined chemical waste site at MertonBank (the location of the present study) in St. Helens was restoredto amenity grassland after more than a century of dereliction. Sincethen, the site has been managed as intensively mown grass withopen access that provides an important recreational area of urban

green space for local residents.For several years the Merton Bank site has provided a location

for research investigations into soil contamination, trace elementmobility (Hartley, 2002; Hartley et al., 2004; Clemente et al., 2008;

Hartley and Lepp, 2008a,b), brownfield land remediation (French,2005; French et al., 2005) and evaluation of soil quality and health(Dickinson et al., 2005; Hartley et al., 2008). Interest in the site has

been related to the known elevated soil As concentrations, with

* Corresponding author. Tel.: 44 1 151 231 2224.

E-mail address: [email protected] (W. Hartley).1 Present address: Parsons Brinckerhoff Ltd, Manchester Technology Centre,

Oxford Road, Manchester M1 7ED, UK.

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0269-7491/$ see front matter 2008 Elsevier Ltd. All rights reserved.doi:10.1016/j.envpol.2008.11.017

Environmental Pollution 157 (2009) 847856
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hotspots above 4000 mg kg1 dry wt. that critically exceed the UKContaminated Land Exposure Assessment (CLEA) Soil Guideline

Value (SGV)of 20mg kg1 total inorganic As for residential land use(DEFRA, 2002b) as well as the SGV of 500 mg kg1 that applies tocommercial and industrial land uses. Concentrations of As inuncontaminated UK soils are generally in the range of 2

53 mg kg1 [median 10 mg kg1] (Archer and Hodgson, 1987). Themetalloid is a USEPA Group A human carcinogen, with soil inges-tion being a critical issue in assessing health risks. Baseline riskassessment studies use the assumption that As is bioavailable

although it is known, for example, that both soil pH and speciationsignificantly affect this property (Datta and Sarkar, 2005).

This paper is a collation of data obtained from Merton Bank that

assesses the significance of elevated As concentrations in surfacesoil and questions the assumption that As has low mobility andbioavailability. This is the first paper that focuses specifically on thisparticular site. We evaluate (i) the consequences of Monitored

Natural Attenuation (relying on natural processes to reduce themobility and concentration of contaminants) and aftercarefollowing typical methods of landscape engineering used in the UK

until the 1980s, and (ii) the likelihood that future use of the site ordiffering management practices may alter As mobility and transferto receptors such as humans, groundwater or soil biota.

2. Methods

2.1. Study site

The site at Merton Bank, 16 km east of Liverpool, is situated in an urban resi-dential housing area bounded by the Sankey Brook (a tributary of the River Mersey),

a Phragmites wetland and a small industrial and commercial area ( Fig. 1). In 1849,

this was the site of a reservoir that supplied water to nearby mills that was laterdrained. An alkali works was present on part of the site in 1873, although this had

been removed some 20 years later. It is reported that, on cessation of production,

the site consisted of two large conical tips of alkali waste with a central area of

rubble. and has remained untreated for over 70 years (Murphy, 1979). There is

a historyof refineries, alkali, other chemicaland copper (Cu)works in theimmediate

vicinity of the site, but declining industrial activity and a conversion to residential

development occurred in the area during the 1960s. In 1978, the alkali waste was

leveled and used to contour the site which is now raised up to 15 m above

surrounding land with slopes of 412. A 20 cm layer of imported acidic colliery

spoil was then applied to the surface to ameliorate extreme alkalinity after which

thesurfacewasrippedto 60 cm.A thin layerof soil (apparently limitedto about5 cm

Fig.1. Merton Bank in St. Helens, Merseyside, with three experimental plots marked. The site is bordered to the north by a footpath and brook (above Plot 2) and to the south by thestrip of shrubs and trees (W of Plot 2).

W. Hartley et al. / Environmental Pollution 157 (2009) 847856848


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depth) and fertilizers were applied to the soil in 1980 prior to seeding of the site for

amenity grassland, with small patches of trees and shrubs planted in deeper soil

(Murphy, 1979). The site has no formal drainage system but appears to be generally

well drained, at least partially into the adjacent watercourse.

No anoxic conditions were encountered when trial pits were dug and oxygen

values above 10% were recorded to depths of 1 m, suggesting that the most domi-

nant As species in the soil was arsenate (AsV). Surface soil was characterized as silt

loam (70% of samples), sandysilt loam (18%) loamy sand (10%) or clayloam (2%); the

latter used for one of the more recent detailed studies of As ( Hartley and Lepp,

2008b). Total nitrogen concentrations (range between plots 0.220.30%) weretypical for mineral soils. Extractable phosphate was particularly low (0.5 mg,

100 g1 in 73% of samples, n 33) for UK soils (Allen, 1989) although higher values

were determined in one study, carried out after green waste compost (GWC) had

been applied.

2.2. Site investigation and sampling

A site investigation was carried out in 1999 (The Mersey Forest, 1999); 35 trial

pits (all dimensions 1.5 m) were dug to provide descriptive profiles, with 1 kg bulk

soil samples removed for analysis (015 cm and two lower depths). Additional soil

sampling was carried out using hand augers to obtain 1 kg bulk samples to 7.5 cm

depth (25 samples)and 15 cm depth (10 samples).Early in 2000, three experimentalplots of short-rotation coppice woody plants were established at the site(Fig.1).The

plots were rotovated, followed by a glyphosate weed control treatment. Soils were

then sampled, using an auger, to 30 cm depth in a herringbone sampling design(DoE,1994); 72 samples per plot allowed identification of 1% hotspots (3 m 3 m).

The planting of Salix and Populus taxa, Betula pendula, Alnus incana andLarix eurolepis was part of a wider experimental trial at five brownfield sites,

reported elsewhere (French et al., 2005). Collections of soil for laboratory analyses

were obtained from hotspots within these plots (Fig. 2), following guidelines ISO

10381-1 and -2 (International Standards Organisation). Another post-graduate

(Ph.D.) laboratory-based project was also completed using soils from this site

(Hartley, 2002).

In 2002, earthworms were sampled within each of the three experimental

blocksby digging andhandsortingfrom25 25 cmpits.In late 2005further studies

focusing on a range of biological descriptors (Dickinson et al., 2005) were initiated,including a comparison of Merton Bank with 9 other remediated sites in North West

England (Hartley et al., 2008). In the latter study, sampling areas delineated by

0.25 0.25 m quadrats were excavated until there was no further evidence of

earthworm activity, sometimes at a depth of as little as 0.15 m. Numbers, weights

and functional groupings of earthworms [epigeics, non-burrowing in surface litter

and organic horizons; endogeics, sub-surface dweller in branching, horizontal

burrows; anecics, surface litter feeders in deep vertical burrows] (Bouche, 1977)

were recorded.

In early 2005, theexperimental blocks were coppiced and GWC of accredited UKstandard(BSI, 2005) was applied as a mulch,to a depthof 20 cm, in randomlyplaced

(approximately5 m) strips. In 2007, rhizon samplers were inserted at varyingdepths

to 20 cm in pits within composted and non-composted sections of the experimental

plots for monitoring of soil pore water, using methods reported elsewhere (Clem-

ente et al., 2008).

2.3. Laboratory and glasshouse investigations

Sub-samples of field-collected bulk soilswere homogenized in the laboratory by

handmixing.Air-driedsoil wascrushed and sieved (


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three weeks from May to September, providing five successive harvests. Plant

growth trials were carried out in a controlled glasshouse environment (21 2 C;

60% R.H.; 12 h light) with regular daily watering (distilled water) as required. The

soils were also used to grow two species of vegetable crop (data not shown in this

paper, Hartley and Lepp, 2008a).

Further pot trials (5 kg capacity; 32 cm diameter) investigated the effect of GWC

incorporation on water soluble organic carbon (WSOC) concentrations and arsenic

mobility. Green waste compost was applied to the soil at a rate of 30% v/v. Amended

soils were homogenized thoroughly by hand, moistened to 70% of the soil water

holding capacity (WHC) with distilled water and allowed to equilibrate in plasticbags at room temperature for 1 month prior to being transferred to the pots.

Untreated soils were used as controls. Once filled with soil, a hole was drilled in the

side of each plastic pot (10 cm below the lip) and a rhizon soil pore water samplerwas inserted at a 45 angle. Samples were collected every 4 weeks over a 6-month

period and analysed for dissolved organic carbon (DOC) and As.

Accuracy of trace element concentrations in soils and soil extracts from previ-

ously unpublished analytical data was routinely checked by reference to interna-

tional certified standard water (NWRI-TMDA-62) and to digests of a standard

reference soil (CMI7004).

2.4. Statistical analysis

Statistical analysis was carried out using Minitab Ver.15. One-way ANOVAs and

GLMs combined with Dunnets Test were used to test for statistical significance.

3. Results and discussion

3.1. Contamination at Merton Bank

The surface soil at Merton Bank is highly polluted with As(Table 1), with a heterogeneous dispersion of hotspots of up to5000 mg kg1 (Fig. 2). Elevated concentrations of As were found atall locations sampled. In the most detailed survey (French et al.,

2005) arithmetic means varied between 642 and 879 mg As kg1

within the 3 plots. However, As tends to be relatively immobile insoil (Langdon et al., 1999; Milton and Johnson, 1999); for example,

soils and mine spoils in SW England contain respectively


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inner-sphere complexes on ferrihydrite (HFO), with binuclearbidentate complexes or mononuclear monodentate complexesforming at high or low surface coverage respectively (Mench et al.,

1998). Amendment of Merton Bank soil with iron grit redistributed

As to the residual fraction (Fig. 3a). However, incorporation of FeII

sulphate plus lime increased the concentration of As bound to theFe and Al fraction, thereby increasing the stabilization of the

metalloid in the soil, reducing potential mobility and hence soilplant transfer.

Whilst differences between treatments using sequential

extractions were marginal (Fig. 3a), longer-term leaching studies(Fig. 3b) show much more significant differences. The modifiedDutch Leaching Test showed that FeII and FeIII sulphates plus limesignificantly reduced the amount of As leached from Merton Bank

soil (Fig. 3b). The most effective treatment was amendment withFeIII plus lime; leaching of untreated soil was reduced from14,680 mg kg1 to 1110 mg kg1, equivalent to a 92% reduction inleachable As (Hartley et al., 2004). Other treatment formulations

also reduced As in leachates, but to a lesser degree; for example,reductions of 56% with goethite and 17% with iron grit. When lime

was applied to Merton Bank soil there was an 8% reduction in Asleached. This may be due to As binding with calcium (Ca2), and

thus reducing mobility (Hartley et al., 2004).Preliminary studies and analyses of soil pore water, collected

using rhizon samplers directly from the site at two soil depths

(15 cm and 30 cm), showed As concentrations to be in the range of40189 mg l1, which represents


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Reduction of AsV to AsIII is dependent on both pH and redoxpotential. In an oxidized soil, such as this, H 2AsO4

would change to

HAsO42 as pH increases, their concentrations being equal at pH

6.76. Sorption of arsenate then decreases as pH increases as isknown to occur for phosphate. Fulvic acid has been shown toincrease As leaching by out-competing the metalloid for binding

sites such as ferrihydrite whilst humic acid was suggested not to beinvolved in As leaching (Grafe et al., 2002). Hence the degree oforganic matter humification will affect As mobility due to the

presence of either high or low molecular weight organic acidshaving either low or high solubility respectively (Kumpiene et al.,2008).

The current requirement to divert biodegradable wastes from

landfill has led to increased useof GWC as a mulch and soil-formingmaterial on brownfield land (Saebo and Ferrini, 2006; Gadepalleet al., 2007; van Herwijnen et al., 2007a; Sere et al., 2008 ). Whilst

generally beneficial to degraded soils, there is some concern thatcontaminant solubility may be increased through the formation ofsoluble organic complexes due to incorporation of carbon-richcomposts (Zhou and Wong, 2001; Mench et al., 2003; van Her-

wijnen et al., 2007b). Negatively charged dissolved organicsubstances appear to have higher potential to compete with As for

adsorption sites in soils, leading to increased As mobility (Lin et al.,2008). It has also been suggested that added organic matter acts asa food source for microbes that enhance As leaching as themetalloid is biotransformed and reduced to AsIII (Mandl et al., 1992;Turpeinen et al., 1999), although rates of formation are likely to besmall in most circumstances (DEFRA, 2002b). Conversely, othershave found reduced mobility after compost application (Xu et al.,

1991; Cao and Ma, 2004; Perez-de-Mora et al., 2007). The effect ofpH is a major controlling factor and it has been reported that in thepresence of organic matter, oxyanion adsorption is increased as pHdecreases (Sposito, 1989). In the present study where the soil pH of

6.57.6 was already relatively high, addition of GWC (30% v/v)appears to release a proportion of the bound As from the Fe and Aloxide fraction which is redistributed to less strongly bound phases

(surface-adsorbed and water soluble), thereby increasing As inthese fractions by more than 10% (Fig. 5a).

Incorporation of larger amounts of GWC (50% v/v) doubled theleachable As concentrations in the last four fractions of the modi-fied Dutch Leaching Test (Fig. 5b). Overall, GWC increased the

amount of As leached by 18%, thought in this case to be possibly dueto increased fulvic and humic acids (Kumpiene et al., 2008). Thepresent findings suggest that release of As from sorption sites maynot occur immediately within the soil, as this test attempts to

simulate trace element leaching over a greater timescale (upwardsof 3 years) implying that application of GWC may affect As mobi-lization in the long term. Results from short-term pot trials showGWC-treated soil to increase WSOC together with slightly elevated

As concentrations (Fig. 6). It has been observed that a small but

substantial increase in arsenic mobility in wetland soils is associ-ated with high DOC, brought about by formation of aqueous

arsenic/dissolved organic matter (DOM) complexes either bypositively charged amino groups in DOM (Saada et al., 2003) or bymetal cation bridges (Redman et al., 2002).

3.4. Biological impacts

Sufficient experimental work has been carried out at Merton

Bank to allow a preliminary evaluation of potential ecotoxicology ofAs at the site. Glasshouse plant investigations using L. perenne (thedominant grass species at Merton Bank) showed that As concen-trations in plants were not raised substantially above background

concentrations of 0.11.0 mg kg1 (Fig. 7) normally expected at

uncontaminated sites (Allen, 1989). Arsenic uptake was highest insoil amended with lime (1% w/w) but soilplant As transfer

0

10

20

30

40

50

1 2 3 4 5 6 7

Fraction (K)

As(mgkg-1)

0

200

400

600

800

1000

Untreated GWC

As(mg

kg-1)

a

a

b

a

b

Water Sodium bicarbonate (0.5 M)

Sodium hydroxide (0.1 M) Hydrochloric acid (1 M)

Nitric acid (14 M)

Fig. 5. a. Arsenic fractionation in Merton Bank soil amended with green waste

compost (GWC, 30% v/v), using the method of Shiowatana et al. (2001) [previously

unpublished data], key as in Fig. 3a, and b. Changes in labile As in untreated Merton

Bank soil , and Merton Bank soil amended with green waste compost (50% v/v) ,

assessed during the modified Dutch Leaching Test (n 3, standard deviations)

[previously unpublished data].

0

0.1

0.2

0 50 100

WSOC (mg l-1)

As(mgl-1)

Fig. 6. Relationship between concentrations of pore water As and water soluble

organic carbon in untreated (B) and GWC (30% v/v) treated (:) Merton Bank soil[previously unpublished data].



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coefficients (Tc) for ryegrass grown in untreated soil were low(0.01) (Hartley and Lepp, 2008a) and at the lower end of publishedtypical transfer values of between 0.01 and 0.1 (Kloke et al., 1984),

and 0.0007 and 0.032 (Warren et al., 2003). Overall, Fe-oxides wereshown to be effective in situ amendments that reduced Asbioavailability, although soilplant transfer of As was not

completely halted by any amendment (Hartley and Lepp, 2008a).Mortality of woody biomass species at Merton Bank was the

highest, and productivity was the lowest, when comparing 5brownfield sites located in North West England that were studied

intensively by French et al. (2005). Varying yields of 1.5, 3.5 and5.5 dry t ha1 annum1 in the 3 plots probably reflecting higherproduction on north-facing slopes with less sun exposure and lesswater shortage during the summer. Uptake of As into foliage and

woody stems of plants was insignificant (300 mgkg1), and 200 earthworms of 7 species inless contaminated areas of the plots (As warm spots,


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99% of samples exceeding SGVs for As of 20 mg kg1 for residential

land uses (DEFRA, 2002b). Less conservative SGVs are set forcommercial and industrial land uses at 500 mg As kg1. Furtherstatistical guidance on comparing soil contamination data with

critical concentrations has been provided more recently (CL:AIRE,2008).There are uncertainties about the human health risks of As

ingestion from soil. UK guidance uses an estimate that a daily

intake of 1 mg As averaged over a lifetime would increase cancer

risks between 2.7 104 and 6 105 (DEFRA, 2002a,b). An IndexDose of minimal risk is derived from combined oral and inhalation

pathways of 0.302 mg kg1 body weight day1. In practical termsthis dosage would require a daily ingestion of just 0.04 g MertonBank soil day1 (from 500 mg As kg1 hotspots, by a 70 kg adult).The difficulty of digesting soil and absorbing As from the digestive

system mitigates to some degree against this concern.The potential for increased exposure of human, groundwater

and ecological receptors in the future largely depends on the long-

term stability of As in surface soils and underlying wastes. Atpresent, UK guidance only considers ecological receptors at siteswith designated nature conservation status. Currently, however,the soil at Merton Bank appears to support a diverse community of

soil fauna. The site is free draining with no evidence of water-logging and, together with a low soil phosphate status (with theexception of the plots treated with GWC), this would help toimmobilize the metalloid; the grassland is not irrigated or routinely

fertilized. Relatively high soil pH (6.57.6) may enhance themobility of As.

4. Conclusion

A realistic interpretation of the evidence is that surface soil atMerton Bank is significantly contaminated with As, but currentlyappears to be relatively stable in terms of environmental mobility

of this element. The metalloid generally is not mobile and isstrongly adsorbed in soil. The current extremely high As content ofshallow surface soils must reflect mixing and some degree ofupward movement of contaminants from underlying wastes during

site engineering and the first 25 years of pedogenesis, even thougha generally low clay content would suggest restricted binding sitesin the surface soils.

The reclamation carried out at Merton Bank in 1980 falls below

acceptable modern standards (Foxet al.,1998;Wong and Bradshaw,2002), but the site appears to have remained relatively stable for

the past 28 years. In common with many brownfield sites in thisregion and elsewhere in the UK, the approach to management isthrough Monitored Natural Attenuation (Environment Agency,2004). Natural processes are unlikely to adequately resolve thepollution issues, but there is no evidence that suggests any exac-

erbation of risk. This site is not currently monitored in any form.Surface soils will naturally accumulate organic matter from

vegetation over time and potentially this could increase Asmobility. Amending the site with recycled GWC or fertilizing with

phosphate would not appear to be sensible options for sustainablesite management. In terms of future management, iron oxides areworth considering as an amendment to reduce As mobilization tothe wider environment. To date, As mobility into deeper layers of

the waste has not been investigated which is a major shortcomingof the existing site characterization. More detailed studies ofdownward As migration, particulate re-entrainment and ecologicalmonitoring are required.

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0

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40

60

80

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Environmental Pollution 157 (2009) 847–856