全氟辛酸 (PFOA) 是最常見的全氟和多氟烷基化合物之一，由於其廣泛使用和環境持久性，使其在多種環境基質中均可檢測到。然而，研究顯示PFOA 與多種疾病密切相關，促使了相關嚴格法規的建立以及多種整治策略的發展。本研究主要探討現地整治策略，選用磁鐵礦 (Fe3O4) 催化過氧化氫 (H2O2) 降解 PFOA，此為一種在溫和條件下具潛力的現地修復方法。為解決異相催化反應速率較慢的問題，本研究添加了五種螯合劑 (CAs) 為增強反應之策略，探討其對 Fe3O4-H2O2 反應機制的影響。
根據中央合成設計實驗的結果，隨著 H2O2 濃度上升( 0 增加到 2 M)，Fe3O4-H2O2 反應中的 PFOA 降解量隨之增加。相反，Fe3O4 則需保持在 3 至 5.5 g/L 的特定濃度範圍內才能達到最佳的 PFOA 降解效果，然而，即使在最佳條件下 ([H2O2] = 2 M, [Fe3O4] =3-5.5 g/L, [PFOA] = 100 μg/L)，反應 48 小時後僅約降解15%的PFOA。而添加螯合劑之反應，於H2O2濃度1 M及Fe3O4濃度5 g/L的條件下反應48小時降解100 g/L PFOA的效果依次為：抗壞血酸 (81.2%) > 草酸 (77.2%) >> 檸檬酸 (27.3%) > 磷酸乙酸 (23.4%) > N-甲基亞胺二乙酸 (12.1%) > 無螯合劑添加 (8.6%)，顯示添加螯合劑能有效增強 Fe3O4-H2O2 反應降解 PFOA。
本研究篩選出抗壞血酸 (AA) 和草酸 (OX) 為兩種最有效促進反應的螯合劑，以監測反應中總溶解Fe與Fe2+及H2O2濃度隨時間之變化深入研究其增強反應的機制。結果發現，抗壞血酸能有效地將 Fe3+ (或≡Fe(III)) 還原為 Fe2+ (或≡Fe(II))，從而加速初始反應速率，在初始階段所觀察到的速率常數 (kobs,0-10 min) 從 0.0077 min-1 增加至 0.0304 min-1，而草酸則藉由快速溶解 Fe3O4，並與 Fe2+ 形成錯合物，加速 H2O2 的利用，進而顯著加速 PFOA 的降解反應，觀察到的速率常數 (kobs,0-2 min 和 kobs,2-10 min) 分別為 0.4392 min-1 和 0.0189 min-1。然而，在反應大約 10-20 分鐘後，由於抗壞血酸已被氧化，其氧化產物已無還原能力但仍能進一步溶解 Fe3O4幫助反應進行，因此Fe3O4-H2O2-AA 反應仍維持較高的反應性 (kobs,10-180 min = 0.0050 min-1)，反之在 Fe3O4-H2O2-OX 反應中則因形成 Fe3+-OX 錯合物而導致後續反應幾乎停止 (kobs,10-180 min = 0.0009 min-1)。此外經由添加第三丁醇以及對苯醌等自由基抑制劑之實驗，本研究確認超氧化物自由基為反應系統中降解 PFOA 的主要活性物種。本研究之研究結果顯示在 Fe3O4 催化的 H2O2 反應中加入螯合劑，特別是抗壞血酸和草酸，具顯著提升 PFOA 降解效率之潛力，實驗結果將可應用於受全氟化物污染場址之現地復育。

Perfluorooctanoic acid (PFOA) is one of the most well-known per- and polyfluoroalkyl substances (PFAS). It is widely used and persistent, making it ubiquitous in the environment. However, PFOA has been linked to several health issues, which prompted strict regulations and the development of various remediation strategies. This study focused on the in-situ remediation strategy, which uses the magnetite (Fe3O4)-catalyzed H2O2 reaction, a promising in-situ remediation process under mild conditions, to degrade PFOA. In addition, to address the typically slow reaction rate of using heterogeneous catalysts, five chelating agents (CAs) were added to the reaction to be an enhancement strategy and investigate their mechanism, which affects the Fe3O4-H2O2 reaction.
According to the central composite design result, PFOA degradation in the Fe3O4-H2O2 reaction increased with the concentrations of H2O2 increasing from 0 to 2 M. Conversely, Fe3O4 needed to be maintained within a specific range of 3 to 5.5 g/L for optimal performance. However, even under optimal conditions ([H2O2] = 2 M, [Fe3O4] =3-5.5 g/L, [PFOA] = 100μg/L), only 15% of PFOA was degraded after 48 hours. In contrast, the addition of chelating agents significantly enhanced PFOA degradation (100 μg/L PFOA under the conditions of 1 M H2O2 and 5 g/L Fe3O4 after 48 hours). The enhancement order was as follows: ascorbic acid (81.2%) > oxalic acid (77.2%) >> citric acid (27.3%) > phosphonoacetic acid (23.4%) > N-Methyliminodiacetic acid (12.1%) > no CA addition (8.6%). The values in parentheses represent the percentage of PFOA degradation and demonstrate that chelating agents can effectively enhance the Fe3O4-H2O2 reaction for PFOA degradation.
Ascorbic acid (AA) and oxalic acid (OX) have been shown to be the two most effective CAs for promoting the reaction. To investigate the mechanism of their role in the reaction, the changes in total dissolved Fe, Fe2+, and H2O2 concentration were monitored over time. Results show that AA effectively reduces Fe3+ (or ≡Fe(III)) to Fe2+ (or ≡Fe(II)), thereby accelerating the initial reaction rate. The kobs,0-10 min increases from 0.0077 to 0.0304 min-1 at the initial stage. In contrast, OX facilitates the rapid dissolution of Fe3O4, forming a complex with Fe2+ that improves H2O2 utilization and significantly accelerates the reaction at the initial stage. The observed kobs,0-2min, and kobs,2-10min are 0.4392 and 0.0189 min-1, respectively. After approximately 10-20 minutes, the oxidized product of AA, despite losing its reducing capacity, continued to dissolve Fe3O4. This maintains higher reactivity in the Fe3O4-H2O2-AA reaction (kobs,10-180 min = 0.0050 min-1). In contrast, the Fe3O4-H2O2-OX reaction almost stopped (kobs,10-180min = 0.0009 min-1) due to Fe3+-OX complex formation. Moreover, quenching experiments with tert-butyl alcohol and p-benzoquinone identified superoxide radicals as the primary reactive species responsible for PFOA degradation in the reaction system. This study underscores the significant potential of incorporating CAs, particularly AA and OX, to enhance the PFOA degradation efficiency of the Fe3O4-catalyzed H2O2 reaction, providing a promising approach for in-situ remediation of persistent contaminants like PFOA.

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