通过考察电极长度及电极间距、检测管管径及材质、激励信号频率、电压和波形等参数对信噪比的影响,研制了一种适用于常规型离子色谱系统的电容耦合非接触式电导检测器(C^4D)。在抑制模式下,该检测器对常见无机阴离子(F^-、Cl^-、NO_2^-...通过考察电极长度及电极间距、检测管管径及材质、激励信号频率、电压和波形等参数对信噪比的影响,研制了一种适用于常规型离子色谱系统的电容耦合非接触式电导检测器(C^4D)。在抑制模式下,该检测器对常见无机阴离子(F^-、Cl^-、NO_2^-、Br^-、NO_3^-和SO_4^(2-))的检出限(信噪比=3)为0.02~0.08μmol/L;峰面积的相对标准偏差<1.8%(n=6);在0.1~10μm o l/L范围内上述6种无机阴离子线性关系良好,相关系数(R^2)>0.999。自制C4D的主要性能参数与商品化接触式电导检测器相当。该检测器具有结构简单、成本低廉、无电极污染等优点,有利于拓展离子色谱的应用范围。展开更多
By employing an electrical micro-titration system, in which a capacitively coupled contactless conductivity detector(C^4D) was used to monitor the reaction process in real time, herein a novel method for determining...By employing an electrical micro-titration system, in which a capacitively coupled contactless conductivity detector(C^4D) was used to monitor the reaction process in real time, herein a novel method for determining ciprofloxacin hydrochloride(CIPHCl) was developed for the first time. Mode 1: Standard CIPHCl solutions at different concentrations were loaded into reaction cells, respectively, and were titrated with standard Ag^+. Upon the titration, the formation of a precipitate alters the number of ions in the solution, raising the change of conductivity, which was monitored by a special C-4 D to construct a titration curve. The endpoint of the titration was located from the peak of the curve. Between the elapsed time and the initial concentration of titrand, a linear relationship was established over the range of2.0–8.0 mmol/L. Mode 2: Standard Fe^3+ took the place of Ag^+, and was used as titrant to recognize ciprofloxacin contributed to the formation of complexation, which also resulting a change of solution conductivity. Under optimized conditions, a working range of 1.0–5.0 mmol/L CIPHCl was found. Because the reaction solutions were isolated from the working electrodes, this pioneer work shows significant simplicity and cost-effectiveness, by eliminating the requirements for detector exchange/renewal between different measurements, and by involving no auxiliary chemicals. Both of the two approaches were applied successfully to determine CIPHCl in tablet samples. And the results were in good agreement with those obtained by reference method.展开更多
文摘通过考察电极长度及电极间距、检测管管径及材质、激励信号频率、电压和波形等参数对信噪比的影响,研制了一种适用于常规型离子色谱系统的电容耦合非接触式电导检测器(C^4D)。在抑制模式下,该检测器对常见无机阴离子(F^-、Cl^-、NO_2^-、Br^-、NO_3^-和SO_4^(2-))的检出限(信噪比=3)为0.02~0.08μmol/L;峰面积的相对标准偏差<1.8%(n=6);在0.1~10μm o l/L范围内上述6种无机阴离子线性关系良好,相关系数(R^2)>0.999。自制C4D的主要性能参数与商品化接触式电导检测器相当。该检测器具有结构简单、成本低廉、无电极污染等优点,有利于拓展离子色谱的应用范围。
基金financial support from Key R&D of Shandong Province (No. 2016GSF120008)Qingdao National Laboratory for Marine Science and Technology (No. 2015ASKJ02-05)
文摘By employing an electrical micro-titration system, in which a capacitively coupled contactless conductivity detector(C^4D) was used to monitor the reaction process in real time, herein a novel method for determining ciprofloxacin hydrochloride(CIPHCl) was developed for the first time. Mode 1: Standard CIPHCl solutions at different concentrations were loaded into reaction cells, respectively, and were titrated with standard Ag^+. Upon the titration, the formation of a precipitate alters the number of ions in the solution, raising the change of conductivity, which was monitored by a special C-4 D to construct a titration curve. The endpoint of the titration was located from the peak of the curve. Between the elapsed time and the initial concentration of titrand, a linear relationship was established over the range of2.0–8.0 mmol/L. Mode 2: Standard Fe^3+ took the place of Ag^+, and was used as titrant to recognize ciprofloxacin contributed to the formation of complexation, which also resulting a change of solution conductivity. Under optimized conditions, a working range of 1.0–5.0 mmol/L CIPHCl was found. Because the reaction solutions were isolated from the working electrodes, this pioneer work shows significant simplicity and cost-effectiveness, by eliminating the requirements for detector exchange/renewal between different measurements, and by involving no auxiliary chemicals. Both of the two approaches were applied successfully to determine CIPHCl in tablet samples. And the results were in good agreement with those obtained by reference method.