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() Amperometric i-t response of h-CrSe modified SPCE for addition of different concentration of 4-NP into the constantly stirred pH 7. Inset is calibration plot for current response vs. [4-NP], and an enlarged view of amperometric response of h-CrSe modified SPCE for addition of 0.05 µM (a), 0.1 µM (b), 0.2 µM (c), 0.7 µM (d), 1.5 µM (e), 2.5 µM (f), 4 µM (g) and 5.7 µM (h) 4-NP at the working potential of −0.73 V. () Amperometric response of h-CrSe modified SPCE for addition of 10 µM 4-NP and 500 µM additions of dihydroxybenzene isomers and metal ions at pH 7 with the working potential of −0.73 V. () At similar conditions, amperometric response of h-CrSe modified SPCE for addition of 10 µM of 4-NP and 500 µM additions of phenolic and nitro compounds.

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The selectivity of the h-Cr 2 Se 3 modified SPCE towards detection of 4-NP was investigated by amperometric method. Figure shows the amperometric response of h-Cr 2 Se 3 modified SPCE for the addition of 10 µM of 4-NP and 500 µM additions of catechol, resorcinol, hydroquinone, Mn 2+ , Cu 2+ , Ni 2+ , Pb 2+ , Cl , Br , SO 4 2− and Zn 2+ at pH 7 with an applied potential of –0.74 V. A well-defined and sharp amperometric response was observed for the addition of 4-NP. The previously discussed electroactive interferences did not show any response on h-Cr 2 Se 3 modified SPCE. Accordingly, the results clearly reveal that h-Cr 2 Se 3 modified SPCE is highly selective for detection of 4-NP in the presence of phenolic compounds and metal ions. We have also tested the selectivity of the sensor in the presence of electrochemically reducible compounds such as 4-acetamidophenol, 4-aminophenol, 4-nitrobenzoic acid, 4-nitrobenzyl alcohol and H 2 O 2 . The selectivity studies were performed in the presence of 50-fold additions of the aforementioned electrochemically reducible compounds by amperometry and the results are shown in Fig.. It can be seen that the Cr 2 Se 3 modified SPCE shows a stable amperometric response for the addition of 10 µM of 4-NP and 500 µM additions of electrochemically reducible compounds did not result in any measureable response. Hence, the modified sensor can be used for the selective detection of 4-NP in the presence of electrochemically reducible compounds and metal ions.

Stability, repeatability, and reproducibility are critical to utilization of the sensor in real time applications. Fig. shows the operational stability of h-Cr 2 Se 3 modified SPCE for the addition of 10 µM of 4-NP into the constantly stirred electrolyte at pH 7, and the background current response up to 1200 s. The amperometric profile of h-Cr 2 Se 3 modified SPCE clearly shows that the sensor retains 97.3% of its initial current response after 1200 s. This result demonstrates high operational stability of the h-Cr 2 Se 3 modified SPCE in the detection of 4-NP. To evaluate the repeatability of the sensor, a single h-Cr 2 Se 3 modified SPCE was used in five set of pH 7 containing 476 µM of 4-NP by CV. In the same manner, five independently prepared h-Cr 2 Se 3 modified SPCEs were used for the detection of single sample containing 476 µM of 4-NP. Other experimental condtions are similar to Fig.. The h-Cr 2 Se 3 modified SPCEs demonstrate a relative standard deviation (RSD) of approximately 2.2%, and show appropriate repeatability in the detection of 4-NP. In addition, the RSD about 2.1% was observed for five independently prepared h-Cr 2 Se 3 modified SPCEs towards detection of 4-NP. The result also demonstrates good reproducibility of the sensor matrix.

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