Yolcu Şükran Melda, Fırat Merve, Chormey Dotse Selali, Büyükpınar Çağdaş, Turak Fatma, Bakırdere Sezgin
Department of Chemistry, Yıldız Technical University, 34349, Istanbul, Turkey.
Bull Environ Contam Toxicol. 2018 May;100(5):715-719. doi: 10.1007/s00128-018-2283-y. Epub 2018 Feb 6.
In this study, dispersive liquid-liquid microextraction was systematically optimized for the preconcentration of nickel after forming a complex with diphenylcarbazone. The measurement output of the flame atomic absorption spectrometer was further enhanced by fitting a custom-cut slotted quartz tube to the flame burner head. The extraction method increased the amount of nickel reaching the flame and the slotted quartz tube increased the residence time of nickel atoms in the flame to record higher absorbance. Two methods combined to give about 90 fold enhancement in sensitivity over the conventional flame atomic absorption spectrometry. The optimized method was applicable over a wide linear concentration range, and it gave a detection limit of 2.1 µg L. Low relative standard deviations at the lowest concentration in the linear calibration plot indicated high precision for both extraction process and instrumental measurements. A coal fly ash standard reference material (SRM 1633c) was used to determine the accuracy of the method, and experimented results were compatible with the certified value. Spiked recovery tests were also used to validate the applicability of the method.
在本研究中，对分散液液微萃取进行了系统优化，用于在与二苯卡巴腙形成络合物后对镍进行预富集。通过在火焰燃烧器头部安装定制切割的开槽石英管，进一步提高了火焰原子吸收光谱仪的测量输出。萃取方法增加了进入火焰的镍的量，而开槽石英管增加了镍原子在火焰中的停留时间，以记录更高的吸光度。两种方法相结合，灵敏度比传统火焰原子吸收光谱法提高了约90倍。优化后的方法适用于较宽的线性浓度范围，检测限为2.1μg/L。线性校准曲线最低浓度下的低相对标准偏差表明萃取过程和仪器测量都具有高精度。使用煤飞灰标准参考物质（SRM 1633c）来确定该方法的准确性，实验结果与认证值相符。加标回收试验也用于验证该方法的适用性。
