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和所代表的不同情況下的土壤污染的土壤樣品上 取樣 。 然后 從 BCR 過程中獲得的數(shù)據(jù)進(jìn)行比較 得出結(jié)果。 Materials and methods Materials Sixtynine percent HNO3, Aristar174。 (BDH), 40% HF Aristar174。 (BDH), 70% HClO4 RPE (FLUKA) and ultrapure water ( MΩcm?1 at 25176。C) obtained from a MilliQ Element System (Millipore, France) were used for samples and calibrating solution preparation and dilution. For leaching experiments, a buffer solution was prepared with 141g of trisodium citrate Na3C6H5O .2HO RPE (CARLO ERBA REAGENTI) and 19 g of hydroxylamm monium hydrochloride RPE (CARLO ERBA REAGENTI) dissolved in 1 L water and the pH adjusted to with NH3 Aristar174。 (BDH). Acetic acid CH3COOH (. BAKER), hydroxylammmonium hydrochloride RPE (CARLO ERBA REAGENTI), 30% hydrogen peroxide H2O2 ―suprapure‖(Merck) and amm onium ac eta te CH3COONH4 (RUDI PONT) were prepared according to the BCR procedure (Rauret et al. 2021). For titration analysis ≈?5 M dithizone (1,5diphenylthiocarbazone C13H12N4S (FLUKA)) was prepared daily by dissolving the appropriate amount of the corresponding chemical in Toluene ( BAKER). Single element ICPMS Aristar174。, (BDH) standard solutions of 1,000 mgL?1 in nitric acid were used for the preparation of calibrating solutions. Rhodium ICPMS standard solution Aristar174。 (BDH) was used as the internal standard to correct matrix interferences in ICPMS analysis. Polypropylene Falcon Tubes (Blue Max?) were used during sampling handling, and filter membranes ( Mil lex174。HV, Millipore174。) and syringes BD Plastipack? were used for leaching experiments. All labware used in the experiments was soaked in diluted nitric acid overnight and then rinsed with double deionised water. All the experiments were performed in triplicate,and the mean values were considered. A blank procedure was always evaluated.。 材料和方法 ; 材料 :69%的 HNO3, Aristar 174。 BDH, 40 高頻 Aristar 174。 BDH、 70 HClO4 視網(wǎng)膜色素上皮 FLUKA 和純水 182 MΩcm?1,從 法國 專家 MilliQ 元系統(tǒng)微孔,獲得的 25 176。 c 條件下將樣品 用和校準(zhǔn)溶液制備及稀釋。 浸出實(shí)驗(yàn),緩沖溶液準(zhǔn)備以 141 g 鈉枸櫞酸鹽 視網(wǎng)膜色素上皮卡羅和 19 g 視網(wǎng)膜色素上皮卡羅 鹽酸中的溶解 1 L 水中和 ph 值調(diào)整為 NH3 Aristar 174。 BDH。 醋酸 CH3COOH ,hydroxylammmonium 鹽酸 視網(wǎng)膜色素上皮卡羅 ERBA REAGENTI, 30 過氧化氫 H2O2suprapure默克和銨醋酸 CH3COONH4 RUDI 蓬當(dāng)時準(zhǔn)備根據(jù) BCR 過程 Rauret et al., 2021年。 滴定分析 ≈?5 M 雙硫腙為 1, 5diphenylthiocarbazone C13H12N4S FLUKA 份由每天適當(dāng)數(shù)額的甲苯 貝克在相應(yīng)的化學(xué)溶解。 電感耦合等離子體質(zhì)譜 Aristar 174。, BDH 標(biāo)準(zhǔn)溶液中硝酸 1000 mgL?1 的單個元素用于校準(zhǔn)解決方案的研制。 銠 等離子體質(zhì)譜標(biāo)準(zhǔn)解決方案 Aristar 174。 BDH 用于內(nèi)部標(biāo)準(zhǔn)作為更正電感耦合等離子體 質(zhì)譜分析中的矩陣干擾。 用聚丙烯獵鷹管藍(lán)色最大 ? 中采樣處理與濾膜 密 lex 174。 高壓、 微孔 174。 和注射器屋宇署 Plastipack ? 用于浸出實(shí)驗(yàn)。 在實(shí)驗(yàn)中使用的所有 labware 泡稀硝酸在一夜之間,然后用雙 deionised 水沖洗。 一式三份,進(jìn)行的一切實(shí)驗(yàn)和被認(rèn)為是平均的值。 一個空的過程始終計算。 Instrumentation A microwave system (Milestone 1200 Mega, Italy) was used for sample digestion. All the measurements of trace elements concentrations were made using a Perkin Elmer ICPMS Elan 6100 equipped with a crossflow nebuliser and a Perkin Elmer ICPOES 2021 DV equipped with Scotttype spray chamber.。 使用配備橫流 nebuliser 的珀金埃爾默電感耦合等離子體質(zhì)譜大 6100 和斯科特 ICP OES 2021 DV型 噴水室配備的珀金埃爾默 來測量所有 微量元素濃度的所有測量都了 ,從而用 儀器儀表微波系統(tǒng)里程碑 來消解 。 Sample description and preparation The proposed screen ing method has been developed and applied on soil samples collected from rural, urban and mining areas, representing different situation of contamination: LIS samples were collected in a rural area 200 km SouthEast from Rome (Italy)。 CAR 36 and PIN31 urban samples were collected in traffic areas of Rome, and BL0102 sample was collected from horizons of selected soil profiles in the Baccu Locci stream catchment near Muravera (Southeastern Sardinia— Italy), characterised by sulphide deposit exploited since ancient times, while EP3 and P5C19 samples came from an abandoned Sb mine in an area with abundant sulphide mineralization resulting from hydrothermal activities (Manciano Tuscany). Soil samples were airdried at 40176。C and sieved at 2 mm before their use in the experiments. 樣品 說明和建議的屏幕方法已開發(fā)和應(yīng)用于 從農(nóng)村、 城市和采礦領(lǐng)域代表不同的污染情況收集的 土壤樣品的制備 : LIS 樣本 是 從羅馬農(nóng)村地區(qū)東南 200公里 收集 來的 ; 在收集了CAR 36及 PIN31樣本 在羅馬的交通區(qū)收集 ,并 BL0102 示例所選的土壤剖面中 是在 附近 Muravera Baccu Locci 的視野流流域 收集來的 以自古以來的硫化物礦床特征 的土壤 , 而EP3 和 P5C19 的的樣品是 來自一個被遺棄的銻礦山地區(qū)豐富硫化礦熱液活動而引致的 。 土壤樣品在 40 176。 C會 風(fēng)干 , 而且在試驗(yàn)之前應(yīng)篩選出直徑 2mm之內(nèi)。 Determination of total content The elemental position of the soil samples was determined by analyzing several samples after digestion in microwave system with HNO3, HClO4 and HF (as determined by Brunori et al. 2021). This analytical procedure was considered reliable, having been widely experienced in the past in the work of several interparison exercises on the same types of matrices for other trace elements. The analytical performance of the laboratory was evaluated by analysing 10 different aliquots of till 1 (soil) certified reference material (CRM) to ensure adequate quality assurance. Results of HM total content in the studied soils are reported in Table 1. 總濃度的測定: 土壤樣品的元素組成 的測定時 通過分析 一些被以 HNO HClO4 和 HF高頻微波系統(tǒng) 處理后的出來的 。此分析過程被認(rèn)為是可靠的而過去 被廣泛的應(yīng)用在 通過 網(wǎng)絡(luò)用 相同方法追蹤其他 內(nèi)在有某一定聯(lián)系的 元素 。 該實(shí)驗(yàn)室的性能 分析 是對 10份 不同組分的試樣進(jìn)行分析直到有一份 CRM可以確保 質(zhì)量保證的土壤 。表 1是 HM研究土壤中的總含量的 報告 結(jié)果。 EP3 Mine 24 177。 1 664 177。 30 177。 1,010 177。 9 BL0102 Mine 30 177。 1 142 177。 10 177。 152 177。 2 P5C19 Mine 146 177。 11 1,560 177。 64 177。 404 177。 5 LIS 1 Rural 32 177。 1 56 177。 2 177。 162 177。 2 LIS 2 Rural 31 177。 1 54 177。 2 177。 145 177。 1 CAR 36 Urban 139 177。 15 1,026 177。 40 177。 301 177。 6 PIN 31 Urban 58 177。 3 400 177。 50 177。 291 177。 4 y = – R2 = 792 R2 = 792= 098x – 005 M++ Titred 181。mol Sequential extraction The BCR threestep sequential procedure (Rauret et al. 2021) was applied to different soils. The residues from step 3 were treated by the procedure used for determination of the total trace element content of the soil