Pervaporation-flow injection analysis of phenol after on-line derivatisation to phenyl acetate
Pervaporation-flow injection analysis of phenol after on-line derivatisation to phenyl acetate
复制标题
在线衍生化为乙酸苯酯后苯酚的渗透汽化流注射分析
DOI：
10.1016/s0003-2670(03)00393-3
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发表时间：
2003
期刊：
影响因子：
--
通讯作者：
S. Kolev
中科院分区：
文献类型：
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作者：
S. Satienperakul;S. Sheikheldin;T. J. Cardwell;R. Cattrall;M. D. L. Castro;I. McKelvie;S. Kolev
建立了在线衍生化反渗透流动注射法（rPFI）测定水中痕量苯酚的方法。在线rPFI衍生化是通过将乙酸酐直接注入标准或样品苯酚溶液的供体流中进行的，该供体流已与上游的碱性浓氯化钠流合并。反应混合物通过混合室生成乙酸苯酯，然后将其输送到渗透蒸发装置。经蒸发进入渗透蒸发装置顶空后，乙酸苯酯通过疏水膜扩散到受体室的静态碱性溶液中，并在此被捕获15min。乙酸苯酯转化为酚酸盐离子，然后输送到电化学检测器，在+0.62V（相对于Ag/AgCl）的玻璃碳电极上进行安培分析。校正图在50-1000μgl−1范围内呈线性，样品通量为4h−1。n=6时（1000μgl−1）的检出限为25μgl−1，相对标准偏差为4.85%。将该方法应用于多个样品的分析，并与标准4-氨基安替比林（4-AAP）法和反相高效液相色谱法进行了比较。
A reverse pervaporation-flow injection (rPFI) method coupled with on-line derivatisation was developed for the determination of trace phenol in aqueous samples. On-line rPFI derivatisation was performed by direct injection of acetic anhydride into a donor stream of standard or sample phenol solution, which had been merged upstream with an alkaline concentrated sodium chloride stream. The reaction mixture was passed through a mixing chamber to generate phenyl acetate, which was then transported to the pervaporation unit. After evaporation into the headspace of the pervaporation unit, phenyl acetate diffused through a hydrophobic membrane into a static alkaline solution in the acceptor chamber where it was trapped for 15min. Phenyl acetate was converted to phenolate ions and then transported to an electrochemical detector where it was analysed amperometrically at a glassy carbon electrode at +0.62V (versus Ag/AgCl). The calibration plot was linear over the range of 50–1000μgl−1with a sample throughput of 4h−1. The detection limit was determined to be 25μgl−1and 4.85% R.S.D. for n=6 (at 1000μgl−1). This new method was applied to the analysis of several samples and the data compared with those obtained by the standard 4-aminoantipyrine (4-AAP) method and reversed-phase HPLC.