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以静电纺丝法自制的尼龙6纳米纤维膜为吸附材料,建立了快速测定水体痕量多环芳烃(PAHs)的固相表面荧光光谱法(SSF)。将直径为5 cm的尼龙6纳米纤维膜作为滤膜用于抽滤菲、芘、荧蒽的水溶液,将膜自然晾干后置于可变角粉末样品池上,利用荧光分光光度计测量膜表面PAHs的三维固相表面荧光光谱特征,确定最佳激发发射波长,考察荧光强度随溶液初始质量浓度的线性变化关系。结果表明,菲、芘、荧蒽的最大激发发射荧光中心分别位于Ex/Em=255nm/368 nm、Ex/Em=340 nm/376 nm和Ex/Em=290 nm/437 nm处。当抽滤水样体积为500 m L时,菲、芘、荧蒽荧光强度与初始质量浓度之间的标准曲线分别为y=9432.4x+261.1,线性范围为5~500ng/m L;y=753480x+805.51,线性范围为0.2~10 ng/m L;y=9946.06x+603.48,线性范围为10~400 ng/m L,检出限分别为0.973 ng/m L、0.016 2 ng/m L和0.089 6 ng/m L。当质量浓度分别为100 ng/m L、10ng/m L和50 ng/m L时,7次测量的相对标准偏差(RSD)分别为7.1%、2.6%和5.1%,平均值相对误差分别为1%、2%和-0.2%。自来水低中高3个质量浓度的平均加标回收率分别为87.2%~98.2%、101%~120%、85.8%~92.3%。本方法具有简便、经济、灵敏度高等优点,适合于水体痕量PAHs的快速测定。
A solid-phase surface fluorescence spectrometry (SSF) method was developed for the rapid determination of trace polycyclic aromatic hydrocarbons (PAHs) in water using nylon 6 nanofiber membranes made by electrospinning as adsorbent. A nylon 6 nanofiber membrane with a diameter of 5 cm was used as a membrane filter for the filtration of aqueous solutions of phenanthrene, pyrene and fluoranthene. The membrane was naturally dried and placed on a sample cell of variable angle powder. The surface of the membrane was measured with a fluorescence spectrophotometer PAHs three-dimensional solid surface fluorescence spectra to determine the best excitation emission wavelength, the fluorescence intensity with the solution of the initial concentration of linear changes in the relationship. The results showed that the maximum excitation emission centers of phenanthrene, pyrene and fluoranthene lie at Ex / Em = 255 nm / 368 nm, Ex / Em = 340 nm / 376 nm and Ex / Em = 290 nm / 437 nm, respectively. When the water sample volume was 500 m L, the standard curves of fluorescence intensity, initial concentration of phenanthrene, pyrene and fluoranthene were y = 9432.4x + 261.1 and linear range was 5 ~ 500ng / m L, respectively; y = The linear range was from 0.2 to 10 ng / mL and the linear range was from 10 to 400 ng / mL with the detection limits of 0.973 ng / mL and 0.016 2 ng / mL, respectively And 0.089 6 ng / m L. The relative standard deviations (RSDs) of 7 measurements were 7.1%, 2.6% and 5.1% when the concentrations were 100 ng / m L, 10 ng / m L and 50 ng / m L, respectively. The average relative errors were 1%, 2% and -0.2%. The average spiked recoveries of low, middle and high quality tap water were 87.2% ~ 98.2%, 101% ~ 120%, 85.8% ~ 92.3% respectively. The method is simple, economical and has the advantages of high sensitivity and is suitable for the rapid determination of trace PAHs in water.