‘Available online at www sciencedirectcom JOURNAL OF science Goimeors GEOCHEMICAL é EXPLORATION ELSEVIER Journal of Gechemisl Explorton £2 (2006) 1-15, sorvalbeereomfosfason Characterisation of a mining-related arsenic-contaminated site, Comwall, UK*™ G. Simon Camm**, Hylke J. Glass®, Derek W. Bryce”, Alan R. Butcher® "Combos Sl! of Mies Unive of it; Red Comal TRIS 86, UC “PS Anahi rr Hose, Cafes nda Exe Oring Ken, RS SHE OR CSIRO Nara, BO. Bos 88 Romar OID, fee Received 3 December 2002; scceptd 23 January 2004 Abstract ‘Arsenic contamination in Comwall is widespread due to th historic mining of polymeric ores and the calcination of oes. ns aess such as Cambome/Redruth and Hayle in West Comvall, arseni values typically exceed 100 mg kg” in sampled topsoil, with high values also being present inthe subsoil. To investigate the dispersion of arsenic from a caciner stack and fiom faptve dee, the New Ril site at Reseworthy, near Cambome, Comal wae chovsn for detailed invsatigaion. The it Contains a calener which was fed with handpicked ore anda refinery where arsenic Was refined t a salesble product. n total, sm area of 700% 600 m on a grid with spacing of 100 m was sampled. Seventy-eight soil samples were obtained from pts up (0 30 em deep and analysed by ICP-MS, while seven water samples were alzo analysed for arsenic. Two sol samples were smalysed in more detail, Measured properties were pH, particle size dishibution, the arsenic distribution inthe different size fnctions, andthe mineralogy of arsenic in the soil using XRD, SEM and QemSCAN. Twenty samples crossing the area were subjected to water extraction and speciation analysis by HPLC-HG-AFS. High values of total arsenic, above 4000 mg kg, were recorded in the soils in the valley oor adjacent tothe calciner. Lower values, close to 500 mg kg~' arseic, were ‘measured near the stack, with a background value of up to 125 mg kg”. Agricultural disturbance by ploughing and down-slope leeching has probably dispersed the arsenic contamination inthe sol. The majority of the arsenic contamination was found to cecrin the silt and sand fractions, Speciation ofthe water-soluble component revealed high values of As* plus AS™, between (134 and 1.7% ofthe total arsenic value, QemSCAN results indicat that coallcoke/Mly ach particulates area significant carer of wsenic contamination. Furdermor, locked and berated particles associated with silicates and oxides often contain asenic- ito oxide as rims and infilings. Water sample concentrations are below 50 jug I" indicating relatively low mobility of ersenic ‘contained in sols. This could be due tothe oxidation state of arsenic and redox conditions. However, a large reservoir of arsenic ‘ould be remobilse if there is a change in ambient conditions, allowing for potential rtoxication of the site (© 2004 Elsevier B.V, All rights reserved. epwors: Arsenic; Contamination; Ming; Caleina; Polio; Speciation; Comal! > Characterisation data obtined fom thi study is sable fw the authors by cootacting Prof, Glass a H.G-Glass@esm.exacuk * comespnding author. Tel: #4-1209-714866, fi +44-1208-710979 Ball eddrar §.Canmjeamexac.ak (GS, Can). (3767428 - se font mater © 2008 lever 8. All ight reserved . So:10 10165 explo 2003.0.0082 GS. Camm etal. / Jounal of Gsockenieal Exploration 82 2008) 1-13, 1. Introduction Arsenic in soils is increasingly drawing the attention of environmental scientists due to its potential toxicity to humans and fauna and flora in general. It may be derived from naturally occurring rminerals or be introduced anthropogenicaly by i Ausra) activities. Pact of this induswia activity is related to the mining and processing of metalliferous cores, There have been instances of arsenic poisoning, in various parts of the world due to the processing of arsenieal ores, or related to the residues of such ‘operations (Mandal and Suzuki, 2002). To assess the cavironmental impact, better methods are required for evaluation of such contamination (Ferguson et al. 1998), Te i now reongnised that exposure of humans to levated levels of arsenic should be avoided (Thorton ct al, 1986; Farago et al, 1997). Inorganic arsenste and arsenite are the most toxie natural forms. Of these, ausenite is considered to be more acutely toxic than arsenate (National Academy of Sciences, 1977; Naqvi etal, 1994). A provisional drinking water guideline, WHO (1993), recommends a value of 10 ug 17> Recently published Soil Guideline Values (SGV’s) (2002) in the UK specify 20 mg kg~' per dry weight of soil for residential areas and allotments while the value for commercial or industrial land is 500 mg kg per dry weight of soil If levels exceed these values, farther assessment ofthe site is required. Tnorganic arsenic occurs ether as pentavalentarse- nate (As*) or trivalent arsenite (As"*) while organic forms of arsenic are mainly methylated compounds and carbohydrate derivatives. Methylated arsenic oxy- acids, found in soils (Masscheleyn et al, 1991), are less mobile than inorganic arsenic (Xu et al, 1988). Arsenic in water and soil can undergo a series of transformations, including oxidation-reduction reac- tions, ligand exchange and biotransformation (Mitch- ail and Barr, 1995). Arsenite predominates when tie redox potential is low or when the soil is waterlogged (Sadig, 1997), Haswell et al. (1985) reported that over 90% of the dissolved arsenic in aerobic soils occured 28 arsenate. This drops to 15% to 40% in the water- logged conditions prevalent in southwest England. At a pH of 5.8, As* is slightly more mobile than ‘As As pH increases, the mobility of both species increases with As’ becoming the more motile species. In environmental studies, however, the distinction between the arsenic species is often overlooked: arsenic is usually reported as total ‘Arsenic in the natural environment may oocur in both organic and inorganic forms. While the global average concentration of arsenic in uncontaminated ‘01 is 5 to 6 mg kg™! (Adriano, 1986), values forthe UK are between 2 and 53 mg kg~', with a median value of 10 mg kg"! (Archer and Hodgson, 1987). Concentrations in Comwall in areas away from for- met mining activity can range between 29 and 51 mg kg"! (Culbard and Johnson, 1984) or between 26 and 67 mg kg~! (Elghali, 1994), In contaminated areas such as the area around Camborne/Redruth/Hayle in ‘West Cornwall values reach 727 mg kg in sampled topsoils. and a maximum of 500 mg ke in the subsoil (Abrahams and Thorton, 1987) Historic non-ferrous metalliferous mining and ore concentration has resulted in the contamination of large tracts of Comwall by metals and metalloids (Thomas, 1980), Contamination was identified in stream sediments (Hosking et al, 1965; Aston et al., 1975; Web et al, 1978; Thornton, 1979), soils (Colburn et al, 1975; Abrahams, 1983; Xu and Thomton, 1985; Abrabams and Thornton, 1987; Li and Thornton, 1993; Mitchell and Barr, 1995; Camm and Moon, 2001), soil pore waters (Haswell ot a. 1985), estuarine sediments (Pirrie et al., 1997, 1999a,b, 2000), acid mine drainage (Jobnson and Thomton, 1987; Moon, 1993; Brown et al, 1994 Hunt and Howard, 1994; Hamilton et al, 1999; Brown et al., 2002) and bioavailability studies (Kava- nagh et al, 1997). The metalloid part of the contam- ination is derived from the calcination of arsenical cores and concentrates (Earl, 1983, 1996), either to remove the arsenic and/or for arsenic recovery. Dur- ing the period from 1860 to 1900, Cornwall was the world’s major producer of arsenic (Thornton ct al, 1986). Airbome dispersion of wseuie eau be taved 10 the plumes of ealciner stacks, waste product dumps, and the activity associated within the calciner site, including the transport of the raw or refined product. Waterborne pollution stems from particulate and soluble components. Abrahams and Thornton (1987) state that 11.9% of the total area surveyed by soil and stream sediment sampling in southwest England is contaminated by heavy metals or metal-GS. Camm etl / Journal of Geocheieal Exploration 82 2004) 1-18, 3 loids. Cornwall therefore isan excellent area to study the long-term impact of mining related activity on the environment. A site in West Comwall (Fig. 1) was chosen for a Aetiled characterisation study. The sit allows inves- tigation of the contaminant piume-trom the caleiner stack, the effet of ealciner “fugitive” dusts (Davies, 1983) from former industrial activity, and spillage of ‘material during transportation ofthe raw and refined products. Lint of metamorphic Grate [=] senare: 060s easements [] ror kes DO rae Fg |. Location map of west Cornwall shoring the sty area west of the Camboroe=Reduth oreild. and thermal metamorphic fente ofthe Cammenellis Gate ‘The objectives of this study are: (8) to characterise the spatial distribution and concen- trations of arsenic in soil and the soil pH around a caleiner site and stack, (©) to determine the concentrations of arsenic in te sand, silt and silt clay soil grain size fractions, (©) to examine the mineralogy of selected soil size fractions by X-ray diffraction (XRD) and soan- ‘ning electron microscopy (SEM), (@) to determine the arsenic speciation of the water- soluble component at selected sample sites within the study area. 2, Historical background Comwall has a very long history of metallferous mining dating back to the Bronze Age. During its peak in the 1800s, it was the largest producer of tin and copper inthe world (Dines, 1956). Arsenic occurs in the tin and copper lodes primarily as arsenopyrite (FeAsS) with minor amount of lallingite (FeAs,) and enargite (3Cu,S.As,S;). In addition, associated sec- ondary minerals occur in the upper oxidised parts of the lode structures. High levels of arsenic in concen- trates had a detrimental effect onthe smelting of such ores, Roasting or calcination of ores to remove arsenic ‘and sulphur probably began in the 1700s when placer and gossan ore supply was naturally replaced by the primary, more sulphidic ore types. Sulphidic ore is reduced in size and roasted with coal or coke as a fuel and arsenic driven off as an oxide, condensing on cooler surfaces. The recovery of arsenic is therefore primarily connected to the processing of tin ores as these are intimately associated with arsenic minerals, Concentrates were roasted to remove the metalloid as well as the sulphur component. From the 1860s, arsenio recovery and refining became more extensive (Earl, 1983, 1996). When arsenic became valuable due to the discovery of pigments, especially ‘Paris Green’ and ‘Kings Yellow”, and ater as an insecticide (Galcium-arsenate) and as a glass decolouriser, mine ‘waste dumps were handpicked for arsenic-bearing ores and arsenic-ich ore was purposely mined. The roasting process to remove the arsenic, with discharge to the atmosphere, was gradually replaced by the recovery of arsenic by the implementation of elaborate‘ GS. Comm et al. / Journal of Geocherileal Exploration 82 2004) 11S condensing features. Large areas were therefore high- ly contaminated by arsenic before the Alkali Inspec- torate introduced controls of 2.9 g of arsenious oxide per eubje metre of air in the late 1800s. ‘The metalliferous mining activity in Comwall let tailings and rock dumps and has produced soil (Abrabams and Thornton, 1987) or supertcr deposits, including river and estuarine sediments @irvie et al., 1997, 2000; Pirie and Camm, 1999). In practice, these are contaminated with arsenic and heavy metals, For example, some 410 km? in the Hayle~Cambomne~Redruth~St, Day-St, Agnes area is contaminated (Abrahams and Thomton, 1987). Besides contamination from anthropogenic sources, soils may be enriched from natural weathering of a parent rock containing elevated arsenic values (Thomton, 1979; Camm and Moon, 2001). To in- vestigate the contamination of soils from calcination lone without the over or underprint of tailings or other hardrock mining activity related material, a site was chosen at New Mill, Roseworthy near Camborne {for examination. ‘The New Mill calciner was constructed in 1889 for refining of arsenic soot from mines in the area as well asthe calcination of handpicked arsenical ore from the rine waste dumps. Historically, the site was chosen due to its close proximity to the Redruth Camborne orefiel, its access to waterpower, and its distance from habitation, Arsenic recovery was effected by shaft furnaces and waste products were dumped to the north of the caleiner on the west bank of the Reens River ‘which could handle a coarse feed from durnp material ‘mixed with coal/coke, The calciner complex continued ‘until circa 1923 as the English Arsenic Works. Pro- duction data from this calciner are, however, not available. The site is now derelict withthe condensing chambers and residue dump stil visible near the valley floor and with the stack on the hill above. 3. Location, physiography and geology The calciner is situated some 4 km to the WSW of ‘Camborne in Comwall, southwest England. The in- dustrial site lies on the western side of the valley floor ‘in a cut into the hillside adjacent to the Reens River, which is 2 tributary of the Red River (Fig. 2). The chimney is at an elevation of some 50 m above ordinance datum or 35 m above the valley loor and is positioned on an interluve between two small streams, feeding down to the main river. The main river catchment includes the most westerly extent of the Cambome-Redruth orefield, and as such would have been a conduit for mine tailing discharge in the 1300s through to the ari part of the 190s. Lhe area is partially farmed with the majority of the rea as pasture, slong with some arable and areas of serub and semi-managed woodland (Fig, 3). Natura soils are usually slightly acidic. Soils in both the pasture and arable land have been enriched with amendments in the form of calcareous beach sand and fertilisers and disturbed by ploughing. The soil type in the area is generally a high clay loam (brown earths) with alluvium in the valley bottom (Staines, 1979). Pre- vailing winds are westerles and the average rainfill i 1400 mam per annum. The solid geology of the study area is dominated by the Devonian Mylor Slate Formation with fine silt laminae and rare thin beds of sandstones and interbedded metabasites (Goode and Taylor, 1988). Although on the edge of the metamorphic aureole and associated mineralisation, there is a record of a small mine named Rose-in- Valley Mine Hamilton Jenkin, 1963), mining two east-west copper, zine end lead bearing lode struc- tures in the area. Litle evidence ofthis mining activity snow remains. 4, Previous studies ‘The site mainly consists of agricultural land with the exclusion of one small area containing the calciner. It was first investigated by Abrahams (1983) with SWINE traverse sampling. Metal and rmetalloid contamination due to past mining activity is reported in Thomton et al. (1986) and Abrabains and Thorton (1987). A total of 51 out of $8 samples showed arsenic values exceeding the moderately con- taminated threshold of 110 mg ke™' (Fig. 6). Loca- tions adjacent to the stack and to the calciner on the valley floor gave values between 600 and 2200 mg g"!, respectively, with unexplainable outliers shove 59,000 and 1200 mg kg™' to the southwest. It was concluded thatthe contamination was widespread end ‘worthy of further investigation. Samples for arsenic determination were anslysed by ICP-AES.GS. Camm et al / Journal of Geocherical Rsploaton #2 (2004) I-15 8 = aaa aa a. me NEESER A my Saiee nL Fig. 2. Topography and area of intrest showing the Reens River valley and ste ofthe caeiner and stack Li and Thornton (1993) studied part of the New Mill site near the chimney. Topseil (0-15 cm) and subsoil (15-30 cm) were sampled. Three soil samples were extracted using a 2.5 om soil auger to produce a composite sample of nine borings within a 2 mx2 m square, while two subsoil samples consisted of three sub samples. The arsenic concentration ranged be- tween 210 and 925 mg kg"! in the topsoil (0. 15 ‘m), 257 to 962 mg kg arsenic in the subsoil (15-30 ‘m) and 190 to 236 mg kg arsenic in the subsoil (60-45 om) Frizzel (1993) used 2 90 m transect at the calciner site to extract soil samples of 10 em depth. High levels of arsenic were measured in the direct vicinity of the caleiner and adjacent buildings, with values between £800 mg kg™' and 16% from soil samples. 5. Field methods Given that the calciner site was previously ide fied as highly contaminated and containing ‘made ‘ground’, no samples were taken there, Sampling was restricted to the area with ‘natural’ soils. Most of the soil has been in egricultural use. Official guidance on patial oampling atratogica is not very helpful (Pereu- son, 1992). Because the site contains two potential sources, the stack and calciner site, a staggered square ‘grid on 100 m centres, with # 50 m interval between, staggers was designed. This produced a grid patter, ‘which covered the largest area (700%600 m) with a W pattern and allowed for infill if required (Fig. 3) ‘Sample positions were initially located using com- pass, tape, and ranging poles using the field hedge‘ GS. Comm et ak / Journal of Ceochonieal Exploration 82 (2004) I-15 Yeoso0 140400 140700 408s 140n00 181000 61100161200 A ES COE es z ron sexo 0200 000 m4 } soi00 como 4 L so 29900 9900 9000 00 vwosco —16osoo— 0700160000 veovon-—vetomD «161100161200 TB butcing N Eas] Pox B53 wotercourse [se] Soil sample FER] Cotciner/stock [BB] Woter sarc a — 200 Fig 3. Land we and soar sample postions within the study rs boundaries as locators and with a beck up of a Garmin 48 handheld GPS. Each sample was given a Unique alphanumeric number with the grid origin to the southwest of the area of interest. A total of 78 sample sites were obtained with only six samples ‘moved from their grid locations due to obstructions or ‘availability, teach sample site, 3030 em pit was excavated by spade to the subsoil or to a maximum of 30 em (deep plough depth) if the subsoil had not been encountered. A channel sample of the soil was then cut using a stainless steel trowel 8 cm wide, ranging to the organic layer atthe top. Soil depths were measured, the soil type observed and recorded, and the samplesG5. Camm et al. / Journal of Geochemical Exploration 82 (2004) I-18 7 (epproximately weighting 250 g) placed into Kraft bags. At two sites, 9EON in the valley floor and SESN on the hill near the calciner stack, further samples were taken for characterisation for “down- profile’ As values and particle size analysis. Channel sampling for size analysis cut a sample of approxi- rately 250 g. Using a 10-cm-wide fat stainless steel scoop soil samples Were cut at 10cm increments tothe botiom ofthe 30 em pits for down-profile values. The samples were placed in Kraft bags. To assist withthe characterisation study, samples were cut into the bank on the westside ofthe river adjacent to the calciner fiom an exposure ofthe calciner residue dump. To determine the aqueous contamination, water samples were taken at seven locations NMI to NM7 fiom the two streams and the river running through the area Fig. 3). Acid-cleaned 1 | plastic containers were used forthe purpose of water collection 6. Laboratory methods Soil samples for analysis were air dried at 30 °C, weighed, diseggregated in a porcelain mortar and pestle and sieved at 2 mm through a stainless steel sieve. The oversize from sieving was bagged and retained and the undersize weighed, split by rifler to one quarter of the volume for size reduction, and the remainder retained. The quarter split was ground ina Tema mill wth a chrome-steel barel to ~100 um, ‘The ground sample was riffle spit into two parts, one for analysis and the other for retention as a replicate. Samples for determination of the sand, silt and clay fractions were Kept in the natural state, mixed and agitated with demineralised water and wet sieved through 2 mm and 63 jum stainless steel sieves using «vibrating shaker. The +2 mm fraction was thorough- ly washed with demineralised water and discarded ‘while the +63 jum fraction was washed by using demineralized water and tranefered to a toy for air ‘ying. The ~63 um fraction and wash water were transferred to 5 1 beakers and made up to 5 1 with demineratised water. Four drops of 0.05% Calgon were added and agitated before solids were allowed to settle. The 2 jum clay fraction was decanted and the silt and clay fractions transferred to trays for air drying. Samples were weighed and recorded prior to sample preparation, Sized samples (SESN and 9E9N) of the sand, silt and clay were disaggregated in a porcelain mortar and pestle prior to riffle splitting One-half of the sample was retained in the natural state for XRD and SEM analysis, the other ofthe sand and silt ground to ~100 ym in a Tema mill for analysis. The clay fraction was disaggregated in a porcelain mortar and pestle, riffle split into two samples, one for geochemical analysis and the other for XRD and SEM examination, All soit samples were analysed using Inductively Couple Plasma-Mass Spectrometry (ICP-MS) for 35, ‘elements using 0.5 g of split sample leached in hot (95 °C) Aqua Regia before analysis at the ACME Labora tories, Vancouver, Canada. The samples were digested in a 2:2:2 mixture of ACS grade concentrated HCI, ‘concentrated HINOs; ad demincralised water, is added. to cach sample. Samples are digested for 1 b in a hot water bath (>95 °C), The OA/OC protocol requires simultaneous digestion of two reagent banks randomly inserted in each batch, Sample solutions were aspirated into a Perkin Elmer Elan 6000 ICP mass spectrometer, Limits of detection for arsenic were 0.5 mg kg~'. One in 10 samples was sent in as duplicates while two certified soil reference materials (GBWO7405, GBW 07402) were twice sent as controls. Comparison of the 8 duplicate analyses revealed an average difference of 2.7% in the arsenic concentration, The analysis of the four control samples showed an average error of 2.2% in the arsenic concentration Ure and Davidson (1995) state that the chemical form, the distribution within the soil/sediment phases, the mobility and the bioavailability of contaminants determine the risk. Bioavailability is mostly related to the water-soluble fraction of the accumulated chemi- cal while the adsorbed or insoluble solid phase is generally not available for biological uptake (Sti- aliani, 1994). Hence, itis important to determine the speciation of the water-soluble (bioavailable) arsenic. ‘Twenty samples from locations crossing the field were ‘analysed in duplicate for the conceatratious vf eiscuie species. The method for speciating water-soluble arsenic is as follows: a 0.1 g sample is weighed into an acid-washed digestion vessel containing 10 em of deionised water and shaken overnight. The solutions ‘were passed through Watman $41 filter papers and diluted to 20 ml with deionised water before being. analysed. Extracted samples were then analysed by a hyphenated High Performance Liquid Chromatogra-‘ GS. Camm et al. / Journal of Geockemical Exploration 82 (2004) I-15, phy (HPLC), Hydride Generation (HG) and Atomic Fhuorescence Spectroscopy (AFS) system. HPLC sep- artes the arsenic species on a strong anion exchange column (Gomez-Ariza et al, 1998; Moreno et al., 2000; Le et al., 2000). The coupled HG-AFS was ‘obtained from PS Analytical. The detection limit for total arsenic is 2 ppt. For speciation, the limit of detection is 0.2 ng cm-*. Water samples were analysed by HPLC-HG-AFS by South West Water using a standardized protocol: 20 mi of unacidifed sample was placed into a poly- propylene screw capped container with 6 em* of HCL (dao 1.18) followed by heating to 80 °C for 30 min; afier cooling, 50% KI/10% is added at a ratio of 50:1 sample KV/ascorbie acid solution and left to stand for 30 min before analysis. All sirdried samples were tested for pH on soil pulps according to British Standard 1377 (1990). A 75 ‘mt of distilled water is added to 30 g of air-dried soil, stirred and left for 8 h. The suspension is stirred again before testing witha calibrated pH{ meter. Two or three readings are taken and these readings should agree to within 0.05 pH units before being accepted XRD analysis of the sized fractions was performed using a Siemens D5000X-ray diffractometer using CuKa radiation at 40 KV, 40 mA. Profiles were measured from 2-70" in step sizes of 0.02° per 1s giving a total time of 56 min. Major and minor minerals that are greater than 3% were identified using the DEFRACT programme. Clay samples from SESN and SEN were characterised on the XRD by the following method: one smear slide was examined untreated, and again after being heated over glycerol in an enclosed vessel for 2-2.5 h at 110 °C. The other smear slide was heated for 2h in a muffle furnace, first 1300 °C and then at 550 °C (De Kimpe, 1993). After each heating, the slide was cooled in a silica-gel dessicator and X-rayed. The diffractometer traces of each sample were then examined. ‘Automated mineral analysis was carried out using QemSCAN, a fully automated scanning electron mi- croscope (SEM), which provides rapid automated fully quantitative mineral analyses. The instrument is based on a LEO 438VP SEM fitted with an array of three Gresham energy dispersive spectrometers. Sam- ples were run using a QemSCAN automatic mineral analyser in particle mineralogical analysis mode (PMA). Up to 4000 individual particles were analysed in each sample, Arsenic-bearing minerals found auto- matically by QemSCAN were then investigated inter- actively, and EDS X-ray spectra collected for the main occurrences. 7. Results 7.1. Water samples ‘Water samples from locations indicated in Fig. 3, produced values below the recommended WHO val- ues of 50 ug I”, The stream to the north had values from 1.3 yg I" (NMI) to 7.9 yg I~! (NM2) and the cone to the south 2.2 to 5.9 wg. 17" (NMA), In the Reens River running past the calciner site, the values ran from 11 pg I~! (NM) upstream, 18 pg I-’ (NM6) adjacent to the calciner, to 21 yg I" (NMS) just downstream of the site 7.2. Soil mineralogy Samples SESN, near the stack on the hillside, and EON on the valley floor, were sized into the sand, silt and clay fractions. The XRD examination shows that the predominant mineralogy for both samples and size fractions is quartz, chlorite and muscovite minor illite and kaolinite in the clay fraction. The manganese mineral sergeevite (CagMg),(CO3)i3-10H0) was identified in the clay ffaction of SESN and in semple SEN send fraction, trace amounts of cassiterite (Gn0,) and rutile (Ti02), and in the sit fraction of the same sample the manganese mineral pyrochrorite (Mn(OH)2). The result of the clay XRD analysis are major quartz, illite, minor kaolinite, very minor chlo- rite, K feldspar and plagioclase. The QemSCAN examination revealed arsenic- bearing minerals in most samples. Typically up to 10 arsenic-containing particles were found in each 30 mm polished block. The main arsenic species found were arsenic-oxide and iron-arsenic-oxide. These ar- senic minerals were found in the following textural settings: inclusions in silicate-rich fragments, in-flls and rims associated with coke/fly ash fragments (Fig, 4), on the boundaries of silicate rock fragments, in the form of liberated arsenic-oxide grains and as inclu- sions in and on boundaries of liberated Fe-oxide particles.GS. Comm etal. / Journal of Geocetnicl Exploration 82 (2004) I-15 ° Analysis 1 Analysis 2 Fig. 4 Seaning electron microscope images of particulates and EDS profile forthe bright areas which ae Fe—Asondes (a) Backscattered Cleeton image showing Fe~As-onide in ookeliy ash, (b) Backscattered elacron image showing As-—Fe-oxide rim sound feldspar pares. 73. Soil geochemical values Background values for arsenic from sedimentary rocks ranges from § to 10 mg kg~' (Webster, 1999) or for Comwall between 22 and 28 mg kg! (K. Reid pers. comm.). Background values for soils from uncontaminated areas in Comwall range from 26 to 6 mg kg” (Elghali, 1994) with values of 63, 40, 84 mg kg™" for histols, uvisols and gleysols, respec- tively, for England (Ferguson, 1990). Soils in Com- wall have an average of 90 me ke”! arsenic (DoE, 1980) but can range up to 750 mg kg~' in contam- inated areas such as the land around Camborne! Redruth/Hayle (Abrahams and Thomton, 1987. sols and dusts sources can be grouped into three classes; continuous point sources, such as stacks; area sources such as waste tips or industrial activity; and Tine sources, such as the roads that the raw or refined material was transported along (Davies, 1983). ‘According to the criteria above, the area of New Mill is severely contaminated by arsenic fom the calciner stack, a point source; the calciner furnace sit ‘an area source; and transported material spills, line source. The spatial distribution of arsenic in the soil is shown in Fig. 5. Values of up to 4466 mg kg! were ‘obtained from soils in the valley bottom downwind of the ealciner and 456 mg kg~" just downwind of the stack. High values of up to 1830 mg kg”! to the southeast, and slightly elevated values up to 218 mg kg™' to the southwest of the site, are interpreted as spills, or a line source, from either the transportation of the raw feed or refined product, High values of arsenic were found in samples close to tracks to the site and in the valley adjacent to the caleiner site. This is attributed to fugitive dust ftom the caleiner waste

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