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研究生： 林柏宇
Lin, Bo-Yu
論文名稱： 利用無機沈澱溫控實驗探討碳酸鈣中穩定同位素及微量元素的分佈特性
Distribution of stable isotope and trace element in inorganic calcium carbonate: Laboratory temperature controlled experiment
指導教授： 游鎮烽
You, Chen-Feng
學位類別： 碩士
Master
系所名稱： 理學院 - 地球科學系
Department of Earth Sciences
論文出版年： 2006
畢業學年度： 94
語文別： 中文
論文頁數： 99
中文關鍵詞： 同位素 、硼同位素 、方解石 、穩定同位素 、溫度 、代用指標 、微量元素 、無機沈澱 、碳酸鈣
外文關鍵詞： calcium carbonate, calcite, isotope, proxy, stable isotope
相關次數： 點閱：173  下載：2 
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    • 摘要
    本研究系統性控制八個溫度（5 - 40℃），固定溶液離子濃度和pH值，利用固定流速導入法固定碳酸鈣生長速率無機沈澱生成碳酸鈣。以拉曼光譜儀及掃瞄式電子顯微鏡確定礦物相為方解石，以高精度質譜術分析碳酸鈣內的微量元素Li、B、Mg、Sr、Ba和U濃度及B、O和C同位素，加以探討溫度與微量元素濃度及穩定同位素之關係，以期瞭解在無機作用下微量元素與穩定同位素對於溫度分化的關係，找出古溫度合適代用指標。
    結果顯示本研究無機沈澱方解石Li/Ca接近實際鈣化情形，溫度方程式：D(Li/Ca)=0.0068e-0.0337T；B/Ca有潛力成為古溫度的代用指標，溫度方程式：D（B/Ca）=0.0088e-0.0395T；Mg/Ca絕對值較自然界高許多，顯示自然界Mg/Ca比值除受控於溫度外，仍有其他因子影響，溫度方程式：D（Mg/Ca）=0.0115e0.0366T；Sr/Ca方解石與霰石回歸線明顯區別，顯示進入碳酸鈣行為受礦物相影響大，溫度方程式：D（Sr/Ca）=0.2676e-0.0318T；Ba/Ca與無機沈澱霰石雖趨勢相同但絕對值有所差異，溫度方程式：D（Ba/Ca）=0.7296e-0.0490T；δ18O與溫度呈負相關且與理論計算方解石值相符，證實此無機沈澱方法，氧同位素可達平衡，溫度方程式δ18OPDB（‰）= -0.23 T（℃） - 3.19。U/Ca比值和δ13C與溫度無關。過去研究認為碳酸鈣中硼同位素受溫度影響不大，但本研究中碳酸鈣硼同位素隨溫度變化在5 - 40℃ 變化~17 ‰ （δ11B = -9.43 ~ -28.43 ‰），且與溫度有良好相關性δ11B（‰） = 0.52T（℃） - 30.10，欲使用硼同位素作為環境指標，需謹慎考慮溫度效應影響。

    Abstract
    Understanding the real correlation between incorporation of trace metals into carbonate and temperature is the most important issue for the applications of paleoceanographic and paleoclimatic researches. In this study, calcium carbonates were inorganically precipitated under eight well-controlled temperatures ranged from 5 to 40°C. Concentrations of trace elements and pH values in parent solution were maintained in order to obtain a constant precipitation rate. All of the inorganic precipitations were identified to be pure calcite crystals by using Raman spectrometry and SEM techniques. Distribution coefficients (D) for trace elements (Li, B, Mg, Sr, Ba, and U) and stable isotopes (B, C and O) were then calculated based on high precision measurements on trace elements (HR-ICP-MS) and stable isotopes (TIMS and IRMS) both in calcites and parent solutions.
    Preliminary results showed that DLi/Ca is close to the biogenic carbonates (DLi/Ca = 0.0068e-0.0337T), suggesting that it can faithfully record the ambient seawater Li concentration during calcification of calcite. However, DMg/Ca, DSr/Ca and DB/Ca can be discriminated from those in natural system (DMg/Ca = 0.0115e0.0366T, and DSr/Ca = 0.2676e-0.0318T, DB/Ca = 0.0088e-0.0395T), but are highly correlated to temperature effect, indicating that other factors possibly exert an influence on the co-precipitations of Mg, Sr and B in calcite. Furthermore, incorporation of Sr into calcite seems to be affected by mineral structure based on a significant discrepancy between the previous works on aragonite and the present study on calcite. Of special interest is that DBa/Ca follows the thermodynamic substitution (DBa/Ca = 0.7296e-0.0490T), suggesting Ba/Ca may at least in part be influenced by changes in temperature. Therefore, care should be taken about temperature effect on Ba/Ca record in carbonates (e.g., coral Ba/Ca as a proxy for sediment flux and/or regional upwelling).
    On the other hand, according to previous study on biogenic carbonate, temperature fractionation of boron isotope could be negligible while calcifying. Unexpectedly, there reveals a good relationship between boron isotopic composition and temperature (δ11B (‰) = 0.52T (℃) - 30.10). Furthermore, a range of approximately 17‰ (δ11B = -9.43 ~ -28.43 ‰) variation in δ11B is consistent with published inorganic precipitation experiments. More investigations are still required to further confirm the potential contribution of temperature on calcitic δ11B.

    目錄 摘要…………………………………………………………………Ⅰ Abstract…………………………………………………………….Ⅱ 誌謝…………………………………………………………………Ⅲ 章節目錄……………………………………………………………Ⅳ 表目錄………………………………………………………………Ⅶ 圖目錄………………………………………………………………Ⅷ <章節目錄> 第一章 前言…………………………………………………………1 1.1 研究背景 …………………………………………………1 1.2 研究目的、動機 …………………………………………1 1.3 前人研究 …………………………………………………2 1.3.1 分配係數與同位素分化係數 ……………………2 1.3.2 無機沈澱實驗方法 ………………………………3 1.3.3 微量元素和同位素代用指標（proxy）………… 5 第二章 原理 ………………………………………………………12 2.1 碳酸鈣……………………………………………………12 2.2 沈澱原理…………………………………………………12 2.3 影響沈澱機制……………………………………………13 2.4 影響微量元素分化機制…………………………………14 2.5 影響同位素的分化機制…………………………………15 2.5.1 硼同位素…………………………………………15 2.5.2 氧同位素…………………………………………16 2.5.3 碳同位素 …………………………………………17 2.6 分析原理 …………………………………………………17 2.6.1 拉曼光譜儀（Raman spectrometer）………… 17 2.6.2 掃瞄式電子顯微鏡（SEM） ……………………18 2.6.3 感應耦合電漿質譜儀（ICP-MS）……………… 19 2.6.4 熱游離源質譜儀（TIMS） ………………………21 第三章 步驟與方法…………………………………………………22 3.1 樣品生成 …………………………………………………22 3.2 實驗狀態控制及校正 3.2.1 晶種 ……………………………………………… 23 3.2.2 生長速率 ………………………………………… 24 3.2.3 溫度…………………………………………………24 3.2.4 pH值…………………………………………………27 3.2.5 溶液濃度……………………………………………27 3.3 清洗及取樣…………………………………………………28 3.4 實驗環境及器皿清洗………………………………………28 3.5 分析…………………………………………………………28 3.5.1 拉曼光譜儀（Raman spectrometer）……………28 3.5.2 掃瞄式電子顯微鏡（SEM）……………………… 31 3.5.3 感應耦合電漿質譜儀（ICP-MS）…………………31 3.5.4 熱游離質譜儀（TIMS）……………………………32 3.5.5 氣體比值型質譜儀（IRMS）………………………34 3.5.6 氣相比值質譜儀…………………………………… 34 第四章 結果與討論 ………………………………………………… 36 4.1 拉曼光譜儀分析結果……………………………………… 36 4.2 掃瞄式電子顯微鏡結果……………………………………40 4.3 碳酸鈣微量元素與溫度關係………………………………44 4.3.1 Li/Ca比值……………………………………………47 4.3.2 B/Ca比值……………………………………………50 4.3.3 Mg/Ca比值 ……………………………………… 52 4.3.4 Sr/Ca比值 ………………………………………… 55 4.3.5 Ba/Ca比值 …………………………………………58 4.3.6 U/Ca比值……………………………………………60 4.3.7 微量元素量測結果與理論計算討論………………61 4.4 無機沈澱碳酸鈣硼同位素與溫度關係 ………………… 68 4.4.1 溫度對硼同位素影響………………………………68 4.4.2 pH值對硼同位素影響………………………………69 4.4.3 與前人文獻比較……………………………………72 4.5 無機沈澱碳酸鈣氧同位素與溫度關係……………………75 4.6 無機沈澱碳酸鈣碳同位素與溫度關係……………………81 第五章 結論………………………………………………………… 83 第六章 參考文獻…………………………………………………… 85 <表目錄> 表1-1、生物性碳酸鈣環境記錄代用指標，以珊瑚為例……………11 表4-1、水溶液及各種礦物25℃時形成的反應焓及熵………………45 表4-2、微量元素進入碳酸鈣時反應式25℃時的反應焓……………46 表4-3、40℃與5℃時的Kd比值計算結果…………………………… 62 表4-4、無機沈澱方解石中各微量元素相對於鈣之分配係數……… 63 表4-5、溫度回歸方程式與前人文獻比較…………………………… 64 表4-6、實際量測分配係數與理論計算之比較………………………65 表4-7、氧同位素分化係數換成103lnα與溫度（凱氏溫度）倒數（103/T）相比較 ………………………………………………………78 表4-8、碳酸鹽沈澱樣品中δ11B、δ13C和δ18O同位素值………………82 <圖目錄> 圖1-1、固定流速導入法…………………………………………………5 圖3-1、實驗流程圖…………………………………………………… 22 圖3-2、實驗裝置圖…………………………………………………… 25 圖3-3、無機沈澱水浴溫度控制……………………………………… 26 圖3-4、無機沈澱裝置照片…………………………………………… 26 圖3-6、拉曼儀器圖（正面）………………………………………… 29 圖3-7、雷射光射出之情形……………………………………………30 圖3-8、拉曼儀器圖（反面）…………………………………………30 圖3-9、感應耦合電漿質譜儀為Finnigan Element 2…………………32 圖3-10、固態熱離子源質譜儀TIMS（Triton TI） ………………… 33 圖3-11、氣體比值型質譜儀IRMS …………………………………… 34 圖3-12、中研院地球所氣相比值質譜儀VG SIRA-10 ……………… 35 圖4-1、標準方解石拉曼光譜…………………………………………37 圖4-2、標準霰石拉曼光譜……………………………………………37 圖4-3、不同溫度下方解石拉曼光譜…………………………………38 圖4-4、無機沈澱中方解石與霰石之拉曼光譜比較…………………39 圖4-5、方解石常見晶體………………………………………………40 圖4-6、掃瞄式電子顯微鏡拍攝之SEI影像 ………………………… 41 圖4-7、掃瞄式電子顯微鏡拍攝之SEI影像 ………………………… 41 圖4-8、掃瞄式電子顯微鏡拍攝之SEI影像 ………………………… 42 圖4-9、掃瞄式電子顯微鏡拍攝之SEI影像 ………………………… 42 圖4-10、掃瞄式電子顯微鏡拍攝之SEI影像…………………………43 圖4-11、掃瞄式電子顯微鏡拍攝之SEI影像…………………………43 圖4-12、無機沈澱方解石中D（Li/Ca）比值與溫度關係………………47 圖4-13、本研究無機沈澱方解石D（Li/Ca）與溫度關係和前人文獻比較 ………………………………………………………… 49 圖4-14、無機沈澱方解石中D（B/Ca）比值與溫度關係………………50 圖4-15、本研究無機沈澱方解石D（B/Ca）與溫度關係和前人文獻比較 ………………………………………………………… 51 圖4-16、無機沈澱方解石中D（Mg/Ca）值與溫度關係 ……………… 52 圖4-17、本研究無機沈澱方解石D（Mg/Ca）與溫度關係和前人文獻比較……………………………………………………………53 圖4-18、無機沈澱方解石中D（Sr/Ca）比值與溫度關係………………55 圖4-19、本研究無機沈澱方解石D（Sr/Ca）與溫度關係和前人文獻比較 …………………………………………………………56 圖4-20、無機沈澱方解石中D（Ba/Ca）值與溫度關係…………………58 圖4-21、本研究無機沈澱方解石D（Ba/Ca）與溫度關係和前人文獻比較……………………………………………………………59 圖4-22、無機沈澱方解石中D(U/Ca)值與溫度關係 ………………… 60 圖4-23、本研究中硼同位素隨溫度變化情形 ………………………69 圖4-24、水體中兩種型態的硼濃度相對含量 ……………………… 71 圖4-25、11B易形成B(OH)3結構而10B則相對偏好形成B(OH)4-結構硼同位素比值也會隨著pH值的改變而有變化 …………… 71 圖4-26、本研究不同溫度碳酸鈣相對於母液標準化後分化情形與自然界生物性碳酸鈣和海水分化之硼同位素值比較，與水體pH值作圖………………………………………………………73 圖4-27、本研究溫度（℃）與方解石中氧同位素δ18O（‰）作圖……………………………………………………………76 圖4-28、碳酸鈣-水體氧同位素分化係數換成103lnα與溫度（凱氏溫度）倒數（103/T）與前人文獻比較………………………… 79 圖4-29、本研究碳同位素隨溫度變化可看見本無機沈澱中碳同位素與溫度變化無關 …………………………………………… 81

    第六章 參考文獻
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