State Key Laboratory of Marine Environmental Science, Environmental Science Research Center, Xiamen University, Xiamen 361005, China.
Talanta. 2012 May 15;93:86-93. doi: 10.1016/j.talanta.2012.01.050. Epub 2012 Feb 2.
A method for determining iron in seawater had been developed by coupling reverse flow injection analysis (rFIA) and catalytic spectrophotometric detection with N,N-dimethyl-p-phenylenediamine dihydrochloride (DPD). With a seawater sample or a standard solution as the carrier, the mixture of DPD and buffer was injected into the carrier stream quantitatively and discretely. After mixing with H(2)O(2), the DPD was oxidized to form two pink semiquinone derivatives that were monitored at 514 nm wavelength with a reference at 700 nm. The method detection limit was 0.40 nmol L(-1), lower than half of that of normal flow injection analysis (nFIA) method. The sample throughput was 10h(-1) with triplicate determination, compared with 4h(-1) for nFIA-DPD method. The analysis results of the certified seawaters CASS-4 (12.33 ± 0.18 nmol L(-1)) and NASS-5 (3.47 ± 0.23 nmol L(-1)) well agreed with the certified values (12.77 ± 1.04 and 3.71 ± 0.63 nmol L(-1), respectively). The typical precision of the method for a 2.97 nmol L(-1) iron sample was 4.49% (n=8). Interferences from copper and salinity were investigated. An instrument was assembled based on the proposed method and applied successfully to analyze total dissolvable iron (TDFe) in surface seawater samples collected from the Pearl River Estuary, the results of which revealed non-conservative behavior of TDFe during the estuarine mixing. Results for these samples with both rFIA-DPD and nFIA-DPD methods showed good agreement with each other. The proposed method was superior to the currently used nFIA-DPD method, particularly when it is adapted for field and in situ deployment, due to its lower reagent consumption, higher sample throughput and keeping the manifold tubing clean.
一种利用反相流动注射分析(rFIA)与 N,N-二甲基对苯二胺二盐酸盐(DPD)催化分光光度检测相结合的方法被用于测定海水中的铁。将海水样品或标准溶液作为载流,将 DPD 和缓冲液的混合物定量、离散地注入载流中。与 H(2)O(2)混合后,DPD 被氧化为两种粉红色半醌亚胺衍生物,在 514nm 波长处用 700nm 处的参比进行监测。该方法的检出限为 0.40nmol L(-1),低于常规流动注射分析(nFIA)法的一半。与 nFIA-DPD 法的 4h(-1)相比,该方法的样品通量为 10h(-1),可进行三次重复测定。对经过认证的海水 CASS-4(12.33±0.18nmol L(-1))和 NASS-5(3.47±0.23nmol L(-1))的分析结果与认证值(分别为 12.77±1.04 和 3.71±0.63nmol L(-1))吻合良好。对 2.97nmol L(-1)铁标准样品的典型精密度为 4.49%(n=8)。考察了铜和盐度的干扰。根据提出的方法组装了一种仪器,并成功地用于分析珠江口采集的表层海水中的总可溶解铁(TDFe),结果表明 TDFe 在河口混合过程中表现出非保守行为。rFIA-DPD 和 nFIA-DPD 两种方法对这些样品的分析结果相互吻合良好。与目前使用的 nFIA-DPD 方法相比,该方法具有试剂消耗低、样品通量高、歧管管清洁等优点,特别适用于野外和原位应用。