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Sulfur Speciation in the Surface Sediments of Lakes from Different Regions, China: Characterization by S K-Edge XANES Spectroscopy

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Sulfur Speciation in the Surface Sediments of Lakes from Different Regions, China: Characterization by S K-Edge XANES Spectroscopy Hindawi Publishing Corporation Journal of Chemistry Volume 2016, Article ID 3672348, 9 pages http://dx.doi.org/10.1155/2016/3672348 Research Article Sulfur Speciation in the Surface Sediments of Lakes from Different Regions, China: Characterization by S K-Edge XANES Spectroscopy Wang Jingfu,1 Chen Jingan,1 Dai Zhihui,2 Yang Haiquan,1 and Ma Chenyan3 1 State Key Laboratory of Environmental Geochemistry, Institute of Geochemistry, Chinese Academy of Sciences, Guiyang 550081, China 2State Key Laboratory of Ore Deposit Geochemistry, Institute of Geochemistry, Chinese Academy of Sciences, Guiyang 550081, China 3Institute of High Energy Physics, Chinese Academy of Science, Beijing Synchrotron Radiation Facility, Beijing 100049, China Correspondence should be addressed to Chen Jingan; [email protected] Received 9 March 2016; Accepted 28 April 2016 Academic Editor: Stanislav Franciˇ ˇskovic-Bilinski´ Copyright © 2016 Wang Jingfu et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. X-ray absorption near edge structure (XANES) spectroscopy affords the opportunity to determine redox status for element S in the aquatic ecosystems. However, there have been relatively few studies of S XANES spectroscopy in the terrestrial aquatic ecosystems. In this study, XANES technology was used to examine changes in S speciation in the sediments collected from Taihu Lake, Qinghai Lake, Dianchi Lake, Caohai Lake, and Hongfeng Lake located in distinct geological background areas of China. The results showed that sedimentary S in Qinghai Lake has a high proportion of sulfate averaged 88.9% due to physical weathering of watershed rocks, while deposited S in Taihu Lake has a high fraction of intermediate S (36.5%), which may be the response of the agricultural nonpoint source pollution in drainage basin. The three lakes located in Southwest China have similar composition characteristics of S species, indicating similar S sources including chemical weathering of carbonate and atmospheric deposition. 60–90% of S compounds in the surface sediments were in the form of sulfate and FeS. In deeper layers, the ratio of FeS2 and the intermediate S significantly increased, suggesting rapid processes of sulfate reduction and sulfide reoxidation with the increasing depths. 1. Introduction determine redox status and coordination environment for a wide variety of elements, including sulfur, carbon, and nitro- Sediment is an important repository and sink for sulfur (S) gen within these sediments [13]. The method has become [1]. The biogeochemical cycles of S in sediments were highly especially attractive for the speciation of S in sediments and complex, because the aquatic ecosystems have anaerobic other environmental samples, most prominently at the S K- zones which strongly affect the chemical forms of S [2, 3]. In edge [10, 12, 14, 15]. the previous studies, the wet-chemical speciation method was In previous investigations, XANES spectroscopy has been generally used to analyze the S speciation in sediments and applied to the analysis of the chemical form and oxidation revealitsgeochemicalprocessesintheaquaticecosystems[4– state of S in soil and marine sediments [10, 12, 16], providing 9]. In fact and often neglected, S in natural samples existed in information about the deposition and diagenesis of organic a large variety of organic and inorganic forms with different matter and S mineralogy. However, there have been relatively electronic oxidation states, ranging from −2 (inorganic sul- few studies of S XANES spectroscopy in sediments of the fide) to +6 (sulfate) [10]. This made traditional wet-chemical terrestrial aquatic ecosystems [17]. Particularly, comparative S speciation complicated [11]. Therefore, sensitive analytical studies of the oxidation states of sedimentary S in different methods are needed to analyze and monitor many functions types of lakes from distinct geological background areas and transformations of S species in biochemical reactions are scarce. In this study, we used the K-edge XANES to and in our environment [12]. X-ray absorption near edge determine S speciation in the sediments collected from structure (XANES) spectroscopy affords the opportunity to Taihu Lake (Eastern China), Qinghai Lake (Western China), 2 Journal of Chemistry QH N (km) 060 TH 40∘ (km) Beijing 030 Qinghai Lake DC (km) ∘ 30 Taihu Lake 020 CH (km) Caohai Lake 05 Hongfeng Lake Dianchi Lake (km) 20∘ 0 1000 HF (km) ∘ ∘ ∘ ∘ 010 90 E 100 110 120 Figure 1: Location of the studied lakes. Hongfeng Lake (Southwest China), Caohai Lake (Southwest 30 cm length and 6 cm diameter Plexiglas cylinder tube was China), and Dianchi Lake (Southwest China). The object employed to obtain the sediment cores. The core samples is to understand the S speciation and its transformation in were sliced with intervals of 2 cm, with the exception of the sediments of the terrestrial aquatic ecosystems. core from Qinghai Lake sectioned at 1 cm intervals. Sedi- ments were handled under protective nitrogen atmospheres 2. Materials and Methods (purity 99.9%, Guiyang Shenjian Gas Co., Ltd.). All samples were put in sealed plastic bag and immediately transferred ∘ 2.1. Area Description. In this study, five lakes were chosen to laboratory in iceboxes (<4 C) and freeze-dried. After that, based on economic and geographic status in the Yangtze the samples were frozen with liquid nitrogen. Before XANES River region, Southwest Plateau, and Qinghai-Tibet Plateau, analysis, dry samples were ground and sieved with a standard China (Figure 1). Geographic and limnological features for 100-mesh sieve. thefiveselectedlakesareshowninTable1[18,22].Taihu Lake is the third largest freshwater lake in China located 2.3. Sulfur K-Edge XANES. The sulfur K-edge XANES spec- at the downstream of the Changjiang River. More than 200 tra were recorded at 4B7A beamline (medium X-ray beam- brooks, canals, and rivers discharge industrial wastewater, line 2100–6000 eV) using synchrotron radiation from Beijing mostly from nearby cities, into the lake. Many effluents con- Synchrotron Radiation Facility, the Institute of High Energy tain pesticides, toxic chemicals, or heavy metals. Southwest Physics, the Chinese Academy of Sciences. The samples were Plateau China is the largest karst area in China. According pressedintothinfilmsbeforeanalysis.Thestorageringwas to previous lake chemistry surveys [23], one slightly polluted operated at the energy of 2.5 GeV with Si (111) double crystals. lake (Caohai Lake) and two heavily polluted lakes (Dianchi Spectra were scanned at step widths of 0.3 eV in the region and Hongfeng Lakes) were selected in this area. Qinghai Lake, between 2420 and 2520 eV, with fluorescence mode using a closed-basin lake, is the largest inland saline lake in China. a fluorescent ion chamber Si (Li) detector (PGT LS30135). The amount of evaporation (∼1400 mm/year) is in excess of Additional filters were placed between the sample and the themeanannualprecipitation(∼400 mm/year), resulting in detector to reduce the fluorescence signal derived from Si in the development of a saline lake. the samples. Fe monosulfide (FeS), pyrite (FeS2), R-SH, RSOR , 2.2. Sampling Procedures. Sediment core samples were Na2SO3,NaRSO3,andNa2SO4 were chosen as the standard obtained from the five lakes in September 2013, nearly in compounds. Electronic oxidation states, white-line energies, the centre of the lakes. A plastic static gravity corer with and intensities of reference S compounds were shown in Journal of Chemistry 3 Table 1: Geographic and limnological features of the studied lakes [18–21]. Parameters Eastern China Southwestern China Western China Taihu Lake Hongfeng Lake Dianchi Lake Caohai Lake Qinghai Lake ∘ ∘ ∘ ∘ ∘ ∘ ∘ ∘ 30 05 –32 08 N, 26 25 –34 N, 24 40 –25 02 N, 26 49 –53 N, 36 32 –37 15 N, Positions ∘ ∘ ∘ ∘ ∘ ∘ ∘ ∘ 119 08 –121 55 E 106 20 –28 E 102 36 – 47 E 104 12 –18 E 99 36 –100 47 E 2 Surface area (km ) 2338 56 306 20 4583 Elevation (m) 51235188621713196 Maximum depth (m) 2.6 45.0 8.0 2.5 32.8 Water pH 8.36 8.40 7.37 8.78 9.35 DO (mg/L) 10.1 8.8 8.9 9.4 ND Salinity (g/L) <1.0 <1.0 <1.0 <1.0 12.5 Sulfate (mg/L) 100 80 60 40 2500 Sediment Organic matter (%) 6.5 5.4 6.5 ND 2.4 TN (%) ND 0.31 0.33 1.38 0.50 TP (%) 0.08 0.16 0.15 0.07 ND Fe (%) 2.65 5.98 ND ND 2.50 Warm, Warm, Warm, Climate type Warm, humid Cool, semiarid semihumid semihumid semihumid Deposition rate (cm/yr) ND 0.16 0.20 0.25 0.10 Table 2. The X-ray energy was calibrated with reference Table 2: Electronic oxidation states, white-line energies, and inten- to the spectrum of the highest resonance energy peak of sities of reference S compounds. Na2SO4 at 2480.4 eV. For all edge-normalized spectra, the Electronic White-line White-line contribution of different S species to total S was calculated Compound oxidation state energy (eV) intensity using the software package ATHENA (Ravel and Newville, − 2005). Linear combination fitting (LCF) was carried out in FeS 22472.21.17 − the energy range 2466–2487 eV using the ATHENA [10]. FeS2 12472.81.33 RSH +0.5 2473.4 1.58 2.4. Analysis of the Total Sulfur. Total S contents were RSOR +2 2476.2 1.81 measured with an elemental analyzer (vario MACRO cube, Na2SO3 +3.68 2478.4 2.03 Elementar, Germany), with an experimental error of 0.5%. NaRSO3 +5 2481.2 2.33 Two certified reference materials (RTS-2 and KZK-1, State Na2SO4 +6 2482.6 2.54 Key Laboratory of Environmental Geochemistry, Institute ofGeochemistry,CAS)wereusedascalibrationstandard. Concentrations of total S in sediments of the five studied lakes relatively high proportion of in the oxidation state of S in were shown in Table 3.
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