Carbon quantum dots (CQDs) were synthesized via a hydrothermal method, in which extracellular polymeric substance (EPS) from anaerobic ammonium oxidation (anammox) granular sludge was used as a carbon precursor, while citric acid and ethylenediamine were applied as auxiliary carbon source and passivation agent, respectively. The synthesized CQDs, with orderly spherical shape and mean size of 7.15 nm, emitted blue fluorescent light under UV radiation of 365 nm. The CQDs had a high fluorescence yield (40.84%), with good water solubility and excellent spectroscopic properties. In addition, the CQDs exhibited selective, sensitive and distinctive fluorescence quenching behaviors for Cr(VI) and Mn(VII) in a PBS buffer solution (NaH2PO4–Na2HPO4) of pH 7, with a detection limit of 5.8 nM for Cr(VI) and 2.3 nM for Mn(VII). Owing to the nitrogen components from the EPS of anammox granules, the CQDs were well nitrogen-doped, promoting electron-transfer and leading to reduction between the CQDs and Mn(VII)/Cr(VI). These results indicate that CQD-based chemical sensing is a simple and efficient means for the fluorescence detection of Mn(VII) and Cr(VI).
Zou Deqing,Qing Ye,Li Yingtang,Liu Mosheng,Yang Yaling
A highly sensitive method for the determination of manganese (VII), chromium (VI) and nickel (II) in medicinal herb samples is proposed. The method is based on analytes reacted with ammonium pyrrolidinedithiocarbamate (APDC) to give hydrophobic chelates (M–APDC), which were separated and enriched by cloud-point extraction (CPE) with non-ionic surfactant Tergitol TMN-6 as extractant. The surfactant-rich phase containing the chelates is determined with a high-performance liquid chromatography system. To achieve the best CPE method, the Box–Behnken design was used to study the concentration of Tergitol TMN-6, equilibrium temperature, equilibrium time as well as their interaction. What followed was the individual research for the pH of the sample solutions and the concentration of APDC. What is more, in the given optimized experimental conditions, calibration plots were found to be linear in the range of 0.0200–0.500 mg/L for Mn (VII) and Cr (VI), meanwhile 0.0500–1.00 mg/L for Ni (II), the linear correlation coefficients were between 0.996 and 0.999, the recoveries ranged from 91.8 to 97.8 % and the relative standard deviations were between 1.09 and 2.30 % ( n = 3). The limits of detection were 0.164 μg/L for Mn (VII), 0.562 μg/L for Cr (VI) and 5.12 μg/L for Ni (II), respectively. The proposed method was applied to determine manganese (VII), chromium (VI) and nickel (II) in medicinal herb samples with satisfactory results.
危险品化学品经营许可证（带存储）