本文選題：沉積物 + 硫��； 參考：《華東師范大學(xué)》2016年碩士論文

【摘要】：沉積物作為物質(zhì)遷移轉(zhuǎn)化的蓄積庫,記錄了成巖作用時(shí)硫的生物地球化學(xué)過程,包括硫酸鹽還原和硫化物形成等信息。研究沉積物中硫循環(huán),可為全球碳和鐵循環(huán)、古氣候變化以及地質(zhì)歷史演化等提供重要的資源。本論文詳細(xì)討論了沉積物樣品中主要基體組分對(duì)硫測(cè)定的影響,并比較了不同的定量校正方法消除基體效應(yīng)的效果,建立了簡(jiǎn)便有效的沉積物樣品前處理技術(shù)和準(zhǔn)確快速的測(cè)定方法。利用搭建的熱蒸餾裝置,建立了一套連續(xù)提取沉積物中可溶性硫和可交換態(tài)硫(H2O-S+A-S)、酸揮發(fā)性硫(AVS)、鹽酸溶解性硫(HCl-S)、元素硫(S0)、黃鐵礦硫(Spy)、有機(jī)硫(Sorg)六種形態(tài)的分離方法：應(yīng)用建立的連續(xù)提取技術(shù),研究了東海內(nèi)陸架區(qū)沉積物中各形態(tài)硫和硫同位素比值的分布特征。主要研究結(jié)果如下：1. 在中分辨率模式下,采用雙聚焦電感耦合等離子體質(zhì)譜儀結(jié)合微波消解技術(shù),建立了準(zhǔn)確測(cè)定沉積物中硫含量的分析方法。針對(duì)基體組份對(duì)硫測(cè)定的影響,以Rh做內(nèi)標(biāo),比較了常規(guī)標(biāo)準(zhǔn)曲線法(SCM)和標(biāo)準(zhǔn)加入法(SAM)對(duì)基體效應(yīng)的校正效果。結(jié)果顯示,SCM法無法消除基體組分對(duì)硫測(cè)定的影響,而SAM法能有效消除基體效應(yīng),但樣品分析通量低�；诖�,又進(jìn)一步創(chuàng)新性提出了標(biāo)準(zhǔn)加入校正曲線法(SACM),且當(dāng)實(shí)際樣品與SACM標(biāo)準(zhǔn)系列溶液中的基體濃度匹配在士50%范圍內(nèi)時(shí),可簡(jiǎn)單有效地消除同類沉積物樣品的基體效應(yīng)。2. 采用搭建的裝置,分別對(duì)H2O-S+A-S、AVS、HCl-S.S0、Spy、Sorg提取時(shí)提取劑的濃度和用量、提取溫度與時(shí)間等參數(shù)進(jìn)行了系統(tǒng)優(yōu)化,建立了連續(xù)提取沉積物中硫形態(tài)的分析技術(shù)。選用表層沉積物樣品進(jìn)行多次重復(fù)提取實(shí)驗(yàn),方法的全程平均回收率為94.1±2.3%,準(zhǔn)確度較優(yōu)。3. 將建立的連續(xù)提取沉積物中硫形態(tài)方法應(yīng)用于東海內(nèi)陸架區(qū)A和B站位的柱狀沉積物樣品分析,探討了沉積物樣品中硫形態(tài)及硫同位素比值的分布特征。結(jié)果表明：H2O-S+A-S和Spy是A、B站位沉積物中硫形態(tài)的主要存在形式,分別占總硫比重的83.6%和90.0%,兩站位中AVS和S0的含量總體比重低于2.0%；A、B站位沉積物樣品中SEM(同步浸提的酸溶性金屬)/AVS比值均1, SEM-AVS差值均在0-5范圍內(nèi),表明兩站位沉積物樣品存在一定的毒性效應(yīng)。兩站位AVS/Spy比值均小于0.3,表明AVS能有效地轉(zhuǎn)化成Spy；B站位δ34SH2O-S+A-S(‰)變化范圍為12.13‰～18.92‰,δ34SHCl-S(‰)變化范圍為2.41‰～16.439‰,而δ34SAVS(‰)、δ34SS0 (‰）、δ34Spy(‰)、δ34Sorg(‰)比值均為負(fù)值,變化范圍為-13.09‰～-46.51‰,且δ34SAVS(‰)和δ34Ss0(‰)變化趨勢(shì)(先不斷增大后保持穩(wěn)定)與δ34Spy(‰)較為一致,Spy的形成與AVS和S0具有較好的相關(guān)性。
[Abstract]:As a reservoir of material migration and transformation, sediments record the biogeochemical processes of sulfur during diagenesis, including sulfate reduction and sulphide formation. The study of sulfur cycle in sediments can provide important resources for the global carbon and iron cycle, paleoclimate change and geological history evolution. In this paper, the effects of the main matrix components in sediment samples on the determination of sulfur are discussed in detail, and the effectiveness of different quantitative correction methods in eliminating the matrix effect is compared. A simple and effective pretreatment technique and an accurate and rapid method for the determination of sediment samples were established. Using the built thermal distillation unit, A set of methods for the continuous extraction of six forms of soluble sulfur and exchangeable sulfur H _ 2O -S _ (A-S), acid volatile sulfur (AVS), hydrochloric acid dissolved sulfur (HCl-S), elemental sulfur (S _ 0), pyrite sulfur (Spyn), organic sulfur (Sorg) have been established. The distribution characteristics of sulfur and sulfur isotopic ratios in sediments of continental shelf in the East China Sea are studied. The main results are as follows: 1. An accurate analytical method for the determination of sulfur in sediments was established by using a dual-focus inductively coupled plasma mass spectrometer and microwave digestion technique in the medium resolution mode. In view of the effect of matrix composition on the determination of sulfur, the correction effect of conventional standard curve method (SCM) and standard addition method (SAM) on the matrix effect was compared with Rh as internal standard. The results showed that the effect of matrix composition on sulfur determination could not be eliminated by SAM method, while the matrix effect could be effectively eliminated by SAM method, but the sample analysis flux was low. Based on this, the standard addition correction curve method is further innovated, and the matrix effect of similar sediment samples can be eliminated simply and effectively when the actual sample is matched with the matrix concentration of SACM standard series solution in the range of 50%. The concentration and dosage of the extractant, the extraction temperature and the time were optimized by using the set up apparatus, and the analytical technique of sulfur form in the continuous extraction of sediment was established by using the set up apparatus. The parameters such as the concentration and dosage of the extractant, the extraction temperature and the time of the extraction of H2O-S A-SV AVSU HCl-S.S0S0Sorg were systematically optimized. Surface sediment samples were selected for repeated extraction experiments. The average recovery of the method was 94.1 鹵2.3, and the accuracy was better. 3. The method of continuous extraction of sulfur forms in sediments was applied to the analysis of columnar sediment samples at stations A and B in the continental shelf of the East China Sea. The distribution characteristics of sulfur forms and sulfur isotope ratios in sediment samples were discussed. The results showed that the main forms of sulfur forms in the sediments of the Agna B station were H _ 2O -S A-S and Spy. The total specific gravity of AVS and S0 in the two stations was lower than that in the sediment samples at the station 2.0 and the ratio of acid-soluble metal / / AVS was 1, and the difference of SEM-AVS was in the range of 0-5, respectively, which accounted for 83.6% and 90.0% of the total sulfur specific gravity, respectively, and the total specific gravity of AVS and S0 in the two stations were lower than those in the sediment samples at the station 2.0. The results indicate that the two station sediment samples have some toxic effects. The ratio of AVS/Spy in the two stations was less than 0.3, which indicated that the range of 未 34SH2O-S A-S (鈥，

本文編號(hào)：1790408