本研究使用APDC-MIBK和Aliquat 336-MIBK二種不同萃取系統，來濃縮海水中的Cr(VI)。本研究探討不同pH值、螯合劑添加量、螯合反應時間和萃取時間對萃取效率之影響，由此得到最佳萃取條件及萃取效果。並以GFAAS偵測其吸收值，進而利用此最佳條件來偵測海水中的Cr(VI)。
在APDC-MIBK系統中，找到最佳萃取條件為，每400 mL樣品，調整至pH 3.0，添加4％APDC 4 mL，螯合反應時間為60分鐘，20 mL MIBK振盪萃取後靜置時間為5分鐘。在海水樣品測定之添加回收率在68％~123％之間，偵測極限為0.2 ppb。
對於Aliquat 336-MIBK系統而言，最佳萃取條件為每400 mL樣品，調整至pH 2.0，添加4 mL 5％Aliquat 336，加入20 mL MIBK萃取振盪時間為2分鐘，萃取靜置時間為5分鐘。海水樣品之添加回收率在80％~120％之間，偵測極限為0.1 ppb。
研究結果顯示APDC對於低濃度Cr(VI)的螯合萃取相當不穩定。其優點為可同時萃取不同金屬，但相對而言，水樣中同時含高濃度其他可被萃取之金屬時，會增加其干擾。而Aliquat 336在酸性pH下與Cr(VI)螯合效果較APDC穩定，對於海水中Cr(VI)的分析，是一個非常可行之萃取方法。

In this research, in order to set up the ultimate approaches to determine the content of chromium(Ⅵ) in seawater, different pH values, the amount of chelating agent, chelating time and extraction time were investigated in two different solvent extraction systems, APDC-MIBK and Aliquat 336-MIBK.
In APDC-MIBK system, the ultimate extracting condition is that 400 mL sample is adjusted to pH 3.0, added 4 % APDC 4 mL to chelate chromium(Ⅵ) for 60 minutes, and added 20 mL MIBK to partiton into two fractions for 5 minutes. The recovery in APDC-MIBK system is 68 %~ 123 %. The method detection limit is 0.2 ppb.
In Aliquat 336-MIBK system, the ultimate extracting condition is that 400 mL sample is adjusted to pH 2.0, added 5 % Aliquat 336 4 mL to chelate chromium(Ⅵ), added 20 mL MIBK to be shaken for 2 minutes, and partitoned into two fractions for 5 minutes. The recovery in Aliquat 336-MIBK system is 80 %~ 120 %. The method detection limit is 0.1ppb.
Although in APDC-MIBK system assorted metals can be extracted at same time, it is steadier in Aliquat 336-MIBK system than APDC-MIBK system. Therefore, it is a feasible extraction method to adopt Aliquat 336-MIBK system to determine the content of chromium(Ⅵ) in seawater.

目 錄

中文摘要 …………………………………………………………….. I
英文摘要 …………………………………………………………….. II
目錄 ………………………………………………………………….. III
圖目錄 ……………………………………………………………….. V
表目錄 ……………………………………………………………….. VI


壹、緒論 ……………………………………………………………. 1
一、鉻之簡介 ……………………………………………………… 1
二、鉻之工業用途及污染 ………………………………………... 6
三、鉻之毒性 ……………………………………………………… 9
四、海水中重金屬的分析方法 …………………………………… 10
五、石墨爐式原子吸收光譜儀分析之原理與應用 ……………… 14
六、研究目的 ……………………………………………………… 20
貳、實驗材料與方法 ……………………………………………….. 21
一、儀器與設備 ……………………………………………………. 21
二、藥品 …………………………………………………………… 22
三、試劑 …………………………………………………………… 24
四、器皿之清洗 …………………………………………………… 26
五、實驗方法 ……………………………………………………… 27
參、結果與討論 ……………………………………………………. 37
一、APDC-MIBK萃取系統 ……………………………………… 37
二、Aliquat 336-MIBK萃取系統 ………………………………… 48
三、偵測極限 ……………………………………………………… 56
四、海水樣品測定 ………………………………………………… 56
肆、結論 ……………………………………………………………. 61
伍、參考文獻 ………………………………………………………. 63
圖 目 錄

圖1-1 Cr(III)化合物形成與pH之關係 …………………………….. 3
圖1-2 Cr(VI)化合物形成與pH之關係 …………………………….. 3
圖1-3 海水中鉻的循環過程 ……………………………………........ 5
圖1-4 石墨爐裝置之構造圖 ………………………………………….. 16
圖2-1 APDC-MIBK萃取步驟流程圖 ………………………………. 30
圖2-2 Aliquat 336-MIBK萃取步驟流程圖 …………………………. 33
圖2-3 海水中MIBK溶解度與溫度的關係圖 ……………………… 34
圖3-1 pH值對APDC-MIBK萃取系統之影響 …………………….. 39
圖3-2 2％APDC添加量對APDC-MIBK萃取系統之影響 ……….. 41
圖3-3 4％APDC添加量對APDC-MIBK萃取系統之影響 ………... 42
圖3-4 APDC螯合時間對APDC-MIBK萃取系統之影響 ………… 43
圖3-5 MIBK萃取靜置時間對APDC-MIBK萃取系統之影響 …… 44
圖3-6 試劑水以APDC-MIBK萃取之檢量線 ………………………. 46
圖3-7 人工海水以APDC-MIBK萃取之檢量線 …………………… 47
圖3-8 pH值對Aliquat 336-MIBK萃取系統之影響 ………………. 49
圖3-9 振盪時間對Aliquat 336-MIBK萃取系統之影響 ………....... 51
圖3-10 Aliquat 336添加量對Aliquat 336-MIBK萃取系統之影響 …. 52
圖3-11 萃取靜置時間對Aliquat 336-MIBK萃取系統之影響 ……… 53
圖3-12 人工海水以Aliquat 336-MIBK萃取之檢量線 ……………… 55
圖3-13 海水樣品以APDC-MIBK萃取法測定之檢量線 …………… 59
圖3-14 海水樣品以Aliquat 336-MIBK萃取法測定之檢量線 ……… 60
表 目 錄

表3-1 試劑水以APDC-MIBK萃取之添加回收率 ……………… 46
表3-2 人工海水以APDC-MIBK萃取之添加回收率 …………… 47
表3-3 人工海水以Aliquat 336-MIBK萃取之添加回收率 ……... 55
表3-4 測點基本水文資料 ………………………………………... 58
表3-5 以APDC-MIBK萃取法測定之樣品 …………………….. 59
表3-6 以Aliquat 336-MIBK萃取法測定之樣品 ……………….. 60

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