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OPEN JOURNAL OF WATER POLLUTION AND TREATMENT VOLUME 1, NUMBER 1, JUNE 2014 OPEN JOURNAL OF WATER POLLUTION AND TREATMENT Sediment Geochemistry and Climatic Influences in a River Influenced by Former Mining Activities: the Case of Ribeira de Iguape River, SP-PR, Brazil Denis M. S. Abessa1 *, Lucas Gonçalves Morais1 , Fernando César Perina2 , Marcela Bergo Davanso3 , Valéria Guimarães S. Rodrigues4 , Letı́cia M. P. Martins5 , Joel BarbujianiSı́golo6 1 UNESP, Pça Infante Dom Henrique, s/n, São Vicente, SP, Brazil, 11330-900. IO-USP, Pça do Oceanográfico, 191, São Paulo, SP, Brazil, 05508-900. 3 Ministério do Meio Ambiente, Braslia, DF, Brazil. 70068-900. 2 4 EESC-USP, Av. Trabalhador São-carlense, 400, São Carlos, SP, Brazil, 13566-590. PROCAM-USP, Av. Prof. Luciano Gualberto, 1289, São Paulo, SP, Brazil, 05508-010. 6 IGc-USP, Rua do Lago, 562, São Paulo, SP, Brazil, 05508-080. *Corresponding author: [email protected] 5 Abstract: The Ribeira de Iguape River (RIR) was historically contaminated by residues from mining activities. These activities ceased in the late 1990’s, but the residues remained deposited along the river banks. This study aimed to evaluate the sediment characteristics of the RIR in different hydro-meteorological conditions and detect eventual changes in the geochemistry. Three sampling surveys were conducted, in which sediments were collected in 6 sites, and then analyzed for sediment textures and metals concentrations. Sediments were predominantly sandy, and samples collected downstream to the mining areas tended to be enriched by metals, especially Pb, Cr, Cu, Ni and Zn. Concentrations of metals in sediments tended to be higher after rainstorm episodes, evidencing the pollution sources are not totally controlled and that the stormwater runoff may carry metals to the RIR. Keywords: Environmental Recovery; Metals; Mining; Sediment; Toxicity 1. INTRODUCTION Climatic regime represents primarily the main factor to regulate hydrological balance of watersheds, since it controls the amounts of water flowing towards the rivers both by surficial runoff, tributaries and underground drainage [1, 2]. In special, extreme rainstorm episodes have potential to produce significant landscape and geomorphology changes, since they may redistribute sediments along the drainage basin, creating new or intensifying existing erosive and depositional areas, or even exporting material through the fluvial system [3, 4]. 43 OPEN JOURNAL OF WATER POLLUTION AND TREATMENT The geomorphologic impacts of an extreme event are closely related to factors such as the parent material erodibility, topography, vegetation cover and (historic) land use [5, 6]. Nevertheless, linkages between hill slope and river channel processes might be expected to be important, especially those concerning to removal of surficial sediments due to storm water runoff and eventual landslides [4]. Studies reported increasing inputs of sediments to watersheds related to rainstorm precipitations [3, 4]. In addition, the increase of water volumes and flow in watersheds are a secondary factor that may display sediment transport through the basin, since settled particles can be ressuspended as a physical consequence to the energy increase [7]. A further problem related to storm events is the contamination, as stormwater runoff may drag a series of contaminants deposited on soils or associate to sediment particles, as pesticides and metals, among others [8]. Such contaminants tend to be carried to low energy areas, as riverine lowlands, estuaries and the sea, where contaminated particles set, producing environmental contamination [9]. In the Southeastern Brazil, the Ribeira de Iguape River (RIR) basin represented an important region for mining activities, comprising nine major mines which mainly operated on lead extraction [10]. During mines operation, tailing and metallurgical slags of blast furnace [11] were directly dumped into the Ribeira de Iguape River till the early 1990’s decade, when the material started to be disposed directly on the ground, on the river banks, exposed to the weathering [11] and consequently to lixiviation. Mining activities have ceased in 1995, but about 89,000 m3 of metal rich residues were kept deposited on the ground, close to the river [12], representing source of metals, especially Pb, to RIR and to the lower portion of its basin, which is represented by the Cananéia-Iguape Estuarine Complex (CEIC), a sensitive region that was recognized as a World Natural Heritage. During the 1980 and 1990 decades, high levels of metals, especially Pb, were reported to RIR waters and sediments [10, 13–15]. On the other hand, there are indications that the Pb contents in waters and sediments from RIR have been decreasing along time [16–19]; however, high concentrations of metals have been found in bivalves [20, 21] and suspended sediments [11] from RIR indicating the persistence of environmental problems in the river. Moreover, high concentrations of metals have been observed in sediments collected in the CIEC [13, 22], indicating transport of contaminated material downstream. This investigation aimed to evaluate the sediment characteristics of the RIR in different hydrometeorological conditions, as during a dry period, after an extreme rainstorm episode and after moderate rain precipitations, detecting eventual differences in the geochemistry. 2. MATERIAL AND METHODS 2.1 Study area The study area is inserted into the Ribeira de Iguape River Basin, comprising the cities of Cerro Azul and Adrianópolis, in the state of Paraná, and Iporanga, Ribeira, Eldorado, SeteBarras, Juquiá and Registro, in the state of São Paulo. The region is known as Ribeira Valley, is situated between 24 00’S - 24 45’S and 47 30’W - 49 30’W (Figure 1). The Ribeira de Iguape River Basin is mainly situated in the Coastal Province, with a small portion within Atlantic Uplands, presenting rugged topography and abrupt altitude variations [23]. Mostly, topography hilly, with slopes higher than 15% and local amplitudes from 100 to 300m or >300m. The local climate may be classified, according to Köppen, as following: 5% of basin are classified as wet tropical without dry season, 50% belong to the wet subtropical type with warm summers and the resting (45%) presents wet subtropical type with cool summers; however, these climatic limits are not well defined and vary inter-annually [24]. The region is influenced by two main water masses; Tropical 44 Sediment Geochemistry and Climatic Influences in a River Influenced by Former Mining Activities: the Case of Ribeira de Iguape River, SP-PR, Brazil Figure 1. Map of the studied area (Ribeira de Iguape River basin) indicating the sampling sites. Atlantic (which influences on rain distribution) and Polar Atlantic, responsible for lower temperatures. However, the Tropical Atlantic is more influent. The mean precipitation is about 1,400 mm/year, but it may reach up to 2,300 mm/year. The weather is characterized by a very rainy season, from October to March, with mean precipitation rates above 120 mm/month, and a drier season, from April to September, in which the monthly precipitation rates drop to about 70 mm. The Ribeira de Iguape River Basin occupies about 28,000 km2, between the NE of Paraná and the SW of São Paulo [17]. According to Theodorovicz & Theodorovicz (2007) [23], 61% from the basin belongs to São Paulo, whereas 39% in at Paraná. The river length is 470km, between its spring head (east from Paranapiacaba Ridge, at Paraná), and its mouth, in the Atlantic Ocean and close to the city of Iguape. The main tributary of RIR is the Juquiá River. Close to the spring, the river is named Ribeirinha, flowing eastward until receiving the contribution of Açunguı́ River, close to the city of Cerro Azul, at 380m altitude. From this point, the river starts to be named as Ribeira de Iguape, and flow through valleys, presenting higher slopes and several waterfalls. After the city of Itaóca, the topography becomes a less slope and the river exhibits a meandering pattern, producing depositional areas [14]. Close to the mouth, the lowlands become wide, and the river forms flooding areas, close to the city of Iguape, and already starts to be influenced by the tides and estuarine waters. 45 OPEN JOURNAL OF WATER POLLUTION AND TREATMENT 2.2 Sampling The sampling sites comprised: (P1) or reference site, that was situated upper to mining activities and ore processing; (P2) located just after Rocha mine; (P3) close to Ribeira City; (P4) after Plumbum processing plant; (P5), after the confluence with Pardo River, and (P6), close to the city of Eldorado. Sampling surveys were conducted in October 2010, August 2011 and April 2012. The 1st sediment collection was made after a relatively dry period (e.g<35mm precipitation in the previous 20 days), whereas the 2nd sampling occurred after a severe rainstorm (>220mm precipitation in 24h), which caused extreme precipitation and destructive floods to cities and rural areas situated along the RIR. This rainstorm caused the RIR level to rise up 14m in 24h. The 3rd sampling survey was conducted after weak to moderate rains that did not cause flood in the region (approximately 65mm precipitation). The techniques used to collect, transport and store the sediments followed the procedures established by National Guidelines [25]. Surficial sediment samples (2-cm surface layer) were collected with small plastic shovels from the river banks, at the water level, and conditioned in sealed plastic bags. Immediately after collection, samples were transferred to thermic containers with ice, and transported to the laboratory. In laboratory, sediment samples to chemistry analyses were frozen at -20 C. In August 2011, a sample of the metallurgical wastes disposed on the ground, produced during the smelting process of ore by Plumbum Company, was collected and analyzed aiming to compare concentrations of metals to those obtained previously by [15]. 2.3 Sedimentological analyses The grain size distribution was obtained by dry sieving method [26]. Initially, 150g aliquots from each sediment sample and the slag were previously dried at 60 C for at least 72h. Then, the material was sieved for 10 minutes in a set of different mesh sizes (2mm, 1.7mm, 1.18mm, 600µm, 150µm, 75µm and < 75µm) installed on a shaker. The fractions retained in each mesh were weighted in analytical balance and recorded. The analysis of organic matter was made by the method of loss by ignition in a muffle and gravimetry [27]. 2.4 Chemical analyses Sediment samples were analyzed by inductively coupled plasma optical emission spectrometry (ICPOES) [28, 29], after acid extraction by acquaregia. Concentrations of aluminum (Al), arsenic (As), cadmium (Cd), lead (Pb), copper (Cu), chromium (Cr), iron (Fe), manganese (Mn), nickel (Ni) and zinc (Zn) were measured. For sediments, QA/QC consisted of analyzing a standard sample fortified with metals (Standard Soil – RTC – CRM023) and blanks; QL were 0.5 mg/kg for most of elements and 0.05 mg/kg for Cd. Recoveries were within the acceptable ranges, and ranged between 90 and 110% for most elements and 82% for Cd. The laboratory is accredited by ISO17025 standard. The same procedure was used to evaluate chemical composition of the sample of the metallurgical wastes from Plumbum. The metals concentrations in sediments were compared to Canadian Sediment Quality Guidelines (SQG) for freshwater [30], considering TEL (threshold effect level) and PEL (probable effect level), and to the background values proposed tor RIR basin [31, 32]. 46 Sediment Geochemistry and Climatic Influences in a River Influenced by Former Mining Activities: the Case of Ribeira de Iguape River, SP-PR, Brazil Table 1. Mean Concentrations of Metals (mg/kg) in Residues from Mining Activities in the Upper Portion ofRIR Basin. Residue type Tailings from Rocha Mine Tailings from Panelas (Plumbum) Mine Slags from Plumbum Plant Slags from Plumbum Plant Pb Zn Element Cu 9435.27 429.09 421.82 6366.70 8817.00 110.90 34018.00 118004.33 2730.33 26615.00 100087.00 1357.00 Cr Ba Source 117.45 nm [15] 42.10 111624.20 [15] 214.17 3656.00 [11] 64.00 nm This study 3. RESULTS AND DISCUSSION 3.1 Characterization of Primary Sources of Metals The primary contamination sources to RIR consists of residues from mining activities (tailings from ore processing) and metallurgical wastes (slags), which were better studied and described previously [11, 15]. Although mining has ceased, residues from such activities are still deposited close to the former mines and to the metallurgical plants. Two main old mines still presented tailings deposited directly on the ground (Rocha and Panelas mines, respectively located on Adrianópolis and Ribeira municipalities) [15]. Tailings from Rocha Plant were deposited close to the Rocha creek, and present an approximately volume of 3,000m3 . In their turn, the residues from Plumbum (Panelas mine) were deposited on the RIR riverbank, with a volume of about 89,000m3 [12]. The residues of metallurgical activities (from Plumbum Plant) were formerly discharged into the RIR (along 40 years), but during the 1990’s decade these slags were deposited directly on the RIR riverbanks, totalizing 200,000m3 [12] of residues with As, Cd, Pb, Cu, Cr and Zn. Guimarães [15] evaluated the chemical composition of slags from Rocha and Panelas mines, and observed high concentrations of Pb and other elements (Table 1). Guimarães&Sı́golo [11] analyzed the slags from the Plumbum Plant and detected much higher concentrations. Results obtained in the present study for these slags also showed very high concentrations of some metals, which were similar to those previously observed [11]. Considering their higher volume and higher contamination, the slags from Plumbum may be considered the more relevant source of metals to RIR. 3.2 Sediment Geochemistry Grain size distribution analyses showed that sediments presented a preponderantly sandy composition, with variable percentages of gravel and fines, and predominance of fine and very fine sands (Table 2). The organic matter (OM) contents were generally low, ranging between 0.39% (P6) and 4.96% (P3). There were no clear spatial or temporal patterns concerning to OM distribution and variations or to grain size. The data obtained in this investigation are compatible to that available in the literature.The monitoring program made by State Environmental Agency has systematically registered values lower than the background for the majority of analyzed elements; however, at same time, Pb concentrations exceeding the TEL values have been frequently observed by such monitoring [18, 33–40] in RIR sediments. On the other hand, low concentrations of Pb in sediments from RIR were found by Melo et al. [41], whereas Guimarães&Sı́golo [11] detected high concentrations of Pb and other elements in sediments from RIR, which were lower than those observed in a recent past [13]. 47 OPEN JOURNAL OF WATER POLLUTION AND TREATMENT Figure 2. Concentration of metals (mg/kg) in sediments from RIR (2010, 2011 and 2012). Yellow and red-brownish lines show respectively TEL and PEL values [30], whereas black lines show background values [31, 32]. 48 Sediment Geochemistry and Climatic Influences in a River Influenced by Former Mining Activities: the Case of Ribeira de Iguape River, SP-PR, Brazil Table 2. Grain Size Distribution and Organic Matter in Sediments from Ribeira de Iguape River in the 2010, 2011 and 2012 sampling surveys. Grain Size Distribution (%) and Organic Matter October 2010 G P1 P2 P3 P4 P5 28.21 3.86 1.46 1.08 15.44 VCS CS MS FS VFS Fines OM (%) 3.19 2.82 2.35 27.03 27.10 2.67 9.86 17.12 32.10 23.67 0 5.03 10.79 31.16 31.62 4.48 8.72 7.02 41.70 15.44 1.43 2.02 5.97 24.73 30.39 9.30 10.72 19.94 5.56 20.01 1.74 1.21 4.96 1.41 0.85 August 2011 G VCS P1 0.34 5.15 P2 0 2.58 P3 4.58 4.44 P5 0 0.31 P6 23.8 33.56 G VCS CS 8.52 19.08 6.6 1.70 19.07 CS MS FS 16.29 41.20 32.00 32.09 5.35 34.35 28.50 52.69 12.88 6.03 April 2012 MS FS VFS Fines OM (%) 22.33 13.90 39.42 16.18 4.39 11.86 3.05 15.19 8.11 5.28 1.24 0.58 2.01 2.60 0.39 VFS Fines OM (%) P1 1.84 10.71 18.35 19.79 37.05 11.69 5.60 0.95 P2 0 0.65 10.12 28.08 46.95 13.83 3.75 1.04 P3 0 0.10 0.18 3.81 51.69 43.65 10.69 2.82 P4 0.58 0.26 0.65 10.73 58.91 28.41 11.18 1.53 P5 3.45 1.25 1.50 11.80 59.05 22.45 11.87 0.70 P6 0.17 0.18 0.78 42.76 49.01 6.88 4.15 0.73 G = gravel; VCS = very coarse sand; CS = coarse sand; MS = medium sand; FS = fine sand; VFS = very fine sand; and OM = organic matter. Previous studies [42–46] have shown that areas under influence of mining activities present environmental fragilities or contamination. In this study, positive correlation between sandy fractions and metals may be related to the nature of the mining residues, which are thick and are comminuted when residues are transported downstream [15]. On the other hand, the grain size distribution analyzes showed that the samples were predominantly composed by fine and very fine sands, indicating the sampling sites did not constitute depositional areas. The upper RIR region is hilly, being characterized by steeper slopes, which attribute more energy to the system and make the river channel to be seated in the relief, hindering the formation of the depositional areas. The low concentrations of the majority of metals in sediments possibly could be explained by the sandy nature of sediments and the high energy in the system. Some enrichment by metals could be observed in the sites located downstream, suggesting the influence of former mining activities, especially at P4, P5 and P6. The sediment from P4 exhibited enrichment trends for other elements present in mining residues, as Cu and Zn. The worse conditions observed at P4 for Pb probably were related to the concentrate residues of Plumbum plant. In the second sampling campaign, concentrations of metals in sediments tended to be slightly higher than those observed in the first campaign, but generally levels were below TEL and close to background values [31, 32]. Pb concentrations exceeded the PEL in P5, and Cr levels exceeded the TEL in samples from P2 and P6. The sediment from reference area exhibited concentrations of Cu, Zn and Cr slightly above the background values, in the sampling survey conducted in 2011, after an extreme rainstorm episode. In the third sampling campaign, levels were again generally low and close to background levels. The 49 OPEN JOURNAL OF WATER POLLUTION AND TREATMENT TEL values were exceeded for Pb in P5 and for Cr in P2, whereas background values were exceeded for Pb (P5), Ni (P4 and P5), Cr (P2), Cu (P1, P2, P3, P4 and P5) and Zn (P4 and P5). The results of each campaign were observed separately. In 2010, the concentrations of metals in sediments were relatively low (Figure 2). The lowest Pb concentration was observed in the reference sample (3.5 mg/kg), which was also lower than the proposed background for RIR basin, that is 12-16 mg/kg [31, 32]. The sediment sample from P4 presented the highest concentrations of all analyzed elements; in this sample, the concentration of Pb was above the local background and about 7x greater than the concentration measured in the reference sediment (P1). The Cd levels were below the quantification limits for all samples. Comparing the obtained concentrations to the Canadian SQGs [30], the concentrations of all analyzed metals were below TEL. Regarding to the contents of metals, concentrations were generally low (i.e., below the TEL and/or the background values) and tended to increase downstream (Figure 2), especially Pb, Ni, Cu, Zn and Mn. For Pb, lowest concentrations were observed in the reference sample, which was lower than the proposed background for RIR basin [31, 32]. On the other hand, the sediment sample from P5 presented the highest concentrations of Pb, exceeding TEL (2010 and 2011) and PEL (2011). The Cd levels were below the quantification limits for all samples. For Cr, concentrations above TEL were detected in P2 and P6.Concentrations of Cu, Zn and Ni eventually were found above the background values. The results of this investigation are also coherent to the published data, as literature suggests that metals levels in RIR sediments are decreasing along time [16–18, 38, 39]. Thus, the results corroborate, at least partially, the official reports from the State Environmental Agency on natural attenuation in RIR catchment [18]. Natural restoration has been observed worldwide in rivers contaminated by metals from mining activities [47–49]; but this process may be slow and depends on several factors [50]. On the other hand, literature indicates that the restoration process is not complete, as suspended sediments seem to be still enriched by Pb [11], and bioaccumulation of metals in burrowing bivalves has been reported [20, 21]. This is corroborated by the remaining enriched levels of metals in sediments from RIR, especially Pb, which suggests a residual influence of mining contamination. Mahiques et al. [22] detected a continuous enrichment of Pb and Cr in the sediments from the Estuarine Complex of Iguape and Cananéia, at the mouth of RIR, which was, in its turn, directly related to the former mining activities, situated upper RIR. Moraes et al. [14] estimated that about 840,000 tons of Pb are transported downstream RIR each year, mostly associated to fines. Such transport of metals may explain the enrichment in sediments along RIR, especially in its lower portion and in the downstream estuarine areas [13, 22]. In addition, our data showed that the concentrations tended to be higher in the 2nd and 3rd sampling surveys, which were conducted after rainstorms. According to Costa et al. [51] the rainstorms have major role in removing surface soils and contaminants along the RIR basin. In a study conducted in the Yellow River, Xu (2002) [52] demonstrated that strong rainstorms may cause hyper concentrated flows of suspended sediment concentrations of more than 300 kg/m3. If such suspended solids are contaminated, they would be the carriers of contaminants to the watercourse. The increase of concentrations of metals and nutrients in the sediments of a RIR tributary during the rainy season was observed by Cunha et al. [53]; these authors stated that rainstorms were related to an increase in the adsorption and complexation reactions between fines, organic matter, metals and nutrients. Corsi& Landim [10] have indicated that the lixiviation process is related to the increase of metals inputs from mining areas to some RIR tributaries, which could explain the data obtained in the present investigation. In summary, in spite of the natural restoration process which is in progress along RIR, there is still enrichment by Pb and other elements in its sediments, especially downstream of the former mining activities, and the rainstorms still have a role in carrying metals to the RIR catchment. 50 Sediment Geochemistry and Climatic Influences in a River Influenced by Former Mining Activities: the Case of Ribeira de Iguape River, SP-PR, Brazil ACKNOWLEDGEMENTS The authors thank São Paulo Research Foundation (FAPESP) (grants2009/52762-6 and 2008/54607-5) and CNPq for the financial support. 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