Determination of trace europium based on new fluorimetric system of europium(III) with thenoyltrifluoroacetone and N,N'-dinaphthyl-N,N'-diphenyl-3,6-dioxaoctanediamide.
In the present paper, N,N'-dinaphthyl-N,N'-diphenyl-3,6-dioxaoctanediamide acts as a specific reagent for enhancing the fluorescence intensity of Eu(III) complex with thenoyl trifluoroacetone (TTA), the spectrofluorimetric determination of trace amounts of Eu(III) based on the above system was carried out and its luminescence mechanism was studied. The excitation and emission wavelengths are 343.6 and 613.3 nm, respectively. The fluorescence intensities vary linearly with the concentration of europium(III) in the range 3.647x10(-3)-3.039 mug ml(-1) for the original fluorescence with a detection limit down to 2.279x10(-4) mug ml(-1) and the standard deviation is 0.063 mug ml(-1) for 10 times measurements, and in the range 7.598x10(-4)-0.0243 mug ml(-1) (SD=0.035 for 15 times measurements), 0.06078-0.6100 mug ml(-1) (SD=0.52 for 10 times measurements) for the first derivative fluorescence signal with a detection limit down to 8.566x10(-5) mug ml(-1). The interferences of other rare earths and some of inorganic ions are described. This method is a direct, rapid, selective and sensitive analytical method for the determination of trivalent europium in rare earth ore samples and high purity of rare earth oxides.
The application of trimesic acid to the determination of terbium by spectrofluorimetry.
A sensitive, direct spectrofluorimetric method for the trace determination of terbium with use of trimesic acid (TMA) has been developed. The reaction conditions for the fluorescence system of terbium with TMA were studied. The terbium ion can form a stable binary chelate with TMA, having a ratio of 1:1 in the pH range 3.5-6.5. The maximum excitation and emission wavelengths are 260 nm and 545 nm for the terbium chelate, respectively. The reaction is instantaneous and the fluorescence intensity of the terbium chelate remains stable from 0.25 to 4 h. Under the optimal experimental conditions the fluorescence intensity is a linear function of concentration in the range 0.0248-6.35 mug ml(-1) of terbium. The relative standard deviation is still within +/-4% in the presence of one-thousandfold amounts of the other lanthanide ions, and common foreign ions hardly interfere in the determination. The method can be employed for the determination of trace amounts of terbium in rare earth ores or oxides because of its high sensitivity and selectivity with good reproducibility and accuracy.
HPLC determination of chlorhexidine gluconate and p-chloroaniline in topical ointment.
A novel fast isocratic reversed-phase HPLC method for simultaneous determination of chlorhexidine and its degradation product p-chloroaniline was developed. Zorbax SB Phenyl column (75 mm x 4.6 mm, 3.5 microm) was used for the separation. Mobile phase composed of acetonitrile and buffer solution of 0.08 M sodium phosphate monobasic containing 5 ml of triethylamine (0.5%) and adjust with 85% phosphoric acid to pH 3.0 in ratio 35:65 (v/v) pumped isocratically at flow rate 0.6 ml min(-1) was used. UV detection was performed at 239 nm, the total analysis time was about 10 min. The method is suitable for practical routine analysis of topical ointment in the quality control laboratory.