離子層析／化學放光偵測法對鐵物種之同時分析

Simultaneous Determination of Iron Species by Ion Chromatography with Chemiluminescence Detection

簡郁苓(Yu-Ling Jian)

指導教授 ： 葉華光

中原大學/理學院/化學系/碩士(2009年)

https://doi.org/10.6840/cycu200900098

摘要

化學放光偵測法結合流動注射（flow injection analysis, FIA）或液相層析（liquid chromatography, LC）法已被廣泛地使用在分析化學及生化樣品的檢測中。自1928年Albrecht就觀察到魯米諾（luminol）在鹼性介質中化學放光行為，此反應大部分應用在過氧化氫、氧化劑和金屬離子的偵測中。本研究以魯米諾-過氧化氫為反應基礎，利用二價鐵及三價鐵可催化此化學放光反應的特性，作為此反應的催化劑來偵測水體中二價鐵及三價鐵的含量。
本研究主要是利用離子層析法結合化學放光法，進行二價鐵及三價鐵在水中檢測分析。使用Dionex CS5A離子層析管柱先將二價以及三價鐵分離，藉由催化劑（二價鐵及三價鐵）催化放光試劑（luminol）的反應而產生化學放光，再由化學放光偵測器（Soma S-3400）來偵測。
二價鐵以及三價鐵檢量線製備結果均在7.5至1000 μg/L的範圍內線性效果良好，二價鐵方法偵測極限為7 μg/L，三價鐵方法偵測極限為3 μg/L。
本研究檢測的真實樣品為放流水、地下水及飲用水，上機前只需將真實樣品以Nylon 0.45 μm filter過濾，並用鹽酸調pH至小於2，二價鐵及三價鐵在地下水及飲用水中就能有好的添加回收率，介於90至100 %之間。放流水的實際樣品中則含有二價鐵和三價鐵分別為8 μg/L和45 μg/L，而添加回收率介於80至90 %之間。

本實驗研究主要利用離子層析／化學放光系統同時偵測二價鐵以及三價鐵，與其他檢測方法相比較，有較高的靈敏度，分析時間較短，並且無須太繁瑣的前處理過程，可降低樣品污染的機率。

關鍵字

化學放光 ； 鐵 ； 離子層析

並列摘要

Iron is an important element in the environment and it has essential roles in biological systems as a trace element. Iron is present as bivalent and trivalent states in natural waters. Changes between these two forms of iron are important in various biological and geochemical processes. Today, the accelerated pace of development, rapid industrialization, and higher population density have increased demand for iron, thus resulting in iron pollution, particularly in natural waters, to worsen over the years. The pollution of iron arises mainly from mineral separation, smelting, iron-smelting, etch cleaning, and electroplating.

Measurement of iron content is very important in evaluating the quality of natural waters. It is well known that excessive intake of iron influences human health, thus a simple and rapid method is required for iron detection. Chemiluminescence (CL) methods are a means of enabling the rapid, simple, and economical detection of various substances. Numerous analytical techniques have been employed in the determination of heavy and transition metals, but ion chromatography (IC) seems to be one of the most effective and simple techniques to determine both anionic and cationic species owing to its high sensitivity, rapidity, selectivity, and simplicity coupled with the possible advantage of simultaneous determination .

The goal of this research is to develop a rapid, accurate, sensitive, selective, and economic method for iron speciation in aqueous samples by simultaneous analysis of divalent and trivalent iron ions with Ion Chromatography- Chemiluminescence Detection (IC-CLD). The experimental show that IC-CLD with a luminol/hydrogen peroxide luminescent system is an viable technique for the simultaneous detection of Fe(II) and Fe(III) species, with detection limits as low as 6 ppb and 3 ppb, respectively. This method has high selectivity and requires little sample preparation, short analysis time, and inexpensive instrumentation to achieve low-level detection and speciation of iron.

並列關鍵字

chemiluminescence ； ion chromatography ； iron

參考文獻

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