Determination of Uranium in Carbonate Solutions by Extraction onto a Chemically Modified Surface

1977 ◽  
Vol 21 ◽  
pp. 59-69
Author(s):  
Bruce B. Jablonski ◽  
Donald E. Leyden

Silica gel treated with a commercial silylation reagent (Dow-Corning Z-6020) has been found to extract uranium from carbonate solutions. The materials used are simple to prepare and once the uranium is extracted, x-ray fluorescence may be employed to determine the uranium directly on the solid. A dependence of the extraction upon carbonate concentration is observed. A lower limit of detection of 2.46 μg of 0.12 ppm uranium from a 20 ml sample is obtained.

1994 ◽  
Vol 48 (2) ◽  
pp. 236-240 ◽  
Author(s):  
Régina Zamojska ◽  
Jeff Sharman ◽  
Yvon Cote ◽  
Carmel Jolicoeur

Energy-dispersive x-ray spectrometric methods have been developed for the determination of chlorine in asbestos (chrysotile) fibers. Chlorine, which is a minor constituent, is determined by a standard addition method from the ground fiber and by a standardless method in six different fibers. The lower limit of detection for a qualitative analysis and the lower limit of determination for a quantitative analysis of chlorine in the asbestos matrix are 40 ppm and 120 ppm, respectively. The water-soluble and acid-soluble chlorine have also been determined by ion-exchange chromatography and by a colorimetric method. The agreement of the three different methods is very good in all cases.


1992 ◽  
Vol 36 ◽  
pp. 73-80
Author(s):  
Bruno A.R. Vrebos ◽  
Gjalt T.J. Kuipéres

Accurate analysis of the light elements has been, from the early applications of X-ray fluorescence spectrometry a struggle compared to the determination of heavy elements in the same matrices. In contrast, there has been virtually no upper limit to the atomic number of the element that could be determined. The lower limit, however, has been continuously adjusted downward through the years. Clearly, the sensitivity as well as the lower limit of detection for the heavy elements have also been improved, but the effect is Jess striking than the advances made in the region of tight element performance. This paper deals specifically with wavelength dispersive sequential x-ray fluorescence spectrometry, although some of the observations made are equally applicable to energy dispersive spectrometry.


1985 ◽  
Vol 29 ◽  
pp. 503-509
Author(s):  
Ya-Wen Liu ◽  
A.R. Harding ◽  
D.E. Leyden

AbstractTrace elements in oil may be determined by adsorption of the oil sample onto maguesium oxide followed by thermal degradation of the organic material. The resulting powder is easily pressed into a pellet suitable for X-ray spectrometric analysis. The lower limit of detection depends upon the trace impurities in the MgO and is a few parts per million for most elements determined.


2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
D. R. do Carmo ◽  
S. Gabriel ◽  
D. R. Silvestrini ◽  
U. O. Bicalho ◽  
L. R. Cumba

Poly(propylene)imine hexadecylamine dendrimer (DAB-Am-16) was anchored on the surface of 3-chloropropylsilyl silica gel and subsequently interacted with copper nitroprusside. The composite was characterized by infrared (FTIR), energy dispersive X-ray (EDX), and cyclic voltammetry. The above techniques confirmed the successful anchoring of the dendrimer on the silica gel modified surface and its interaction with copper nitroprusside. The cyclic voltammogram of CuNPSD was found to exhibit two redox couples with (Eθ′)1= 0.30 V and (Eθ′)2= 0.78 V versus Ag/AgCl ( mol L−1;  mV s−1) attributed to the redox processes and , respectively. The CuNPSD-modified graphite paste electrode was found to show a linear response of to  mol L−1for nitrite determination with a detection limit (DL) of  mol L−1and an amperometric sensitivity of 25.0 mA/mol L−1. The CuNPSD-modified graphite paste electrode was found to show a good electrochemical stability and an excellent response to the electrocatalytic oxidation of sodium nitrite.


1999 ◽  
Vol 23 (9) ◽  
pp. 578-579
Author(s):  
Rainer Schobert ◽  
Hermann Pfab ◽  
Jutta Böhmer ◽  
Frank Hampel ◽  
Andreas Werner

Racemates of (η3-allyl)tricarbonyliron lactone complex Fe(CO)3{η1:η3-C(O)XCH2CHCMeCH2} 1a (X = O) and (η3-allyl)tricarbonyliron lactam complex 2a (X = NMe) are resolved on a preparative scale by HPLC on cellulose tris(3,5-dimethylphenyl)carbamate/silica gel RP-8 and the absolute configuration of (-)-2a is determined by X-ray crystal structure analysis.


Nanomaterials ◽  
2020 ◽  
Vol 10 (3) ◽  
pp. 537 ◽  
Author(s):  
Chrys. O. Chikere ◽  
Nadimul Haque Faisal ◽  
Paul Kong-Thoo-Lin ◽  
Carlos Fernandez

Amorphous zirconium oxide nanoparticles (ZrO2) have been used for the first time, to modify carbon paste electrode (CPE) and used as a sensor for the electrochemical determination of gallic acid (GA). The voltammetric results of the ZrO2 nanoparticles-modified CPE showed efficient electrochemical oxidation of gallic acid, with a significantly enhanced peak current from 261 µA ± 3 to about 451 µA ± 1. The modified surface of the electrode and the synthesised zirconia nanoparticles were characterised by scanning electrode microscopy (SEM), Energy-dispersive x-ray spectroscopy (EDXA), X-ray powdered diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR). Meanwhile, the electrochemical behaviour of GA on the surface of the modified electrode was studied using differential pulse voltammetry (DPV), showing a sensitivity of the electrode for GA determination, within a concentration range of 1 × 10−6 mol L−1 to 1 × 10−3 mol L−1 with a correlation coefficient of R2 of 0.9945 and a limit of detection of 1.24 × 10−7 mol L−1 (S/N = 3). The proposed ZrO2 nanoparticles modified CPE was successfully used for the determination of GA in red and white wine, with concentrations of 0.103 mmol L−1 and 0.049 mmol L−1 respectively.


2007 ◽  
Vol 90 (3) ◽  
pp. 720-724
Author(s):  
Sevgi Tatar Ulu

Abstract A sensitive and selective high-performance liquid chromatographic method has been developed for the determination of tianeptine (Tia) in tablets. The method is based on derivatization of Tia with 4-chloro-7-nitrobenzofurazan (NBD-Cl). A mobile phase consisting of acetonitrile10 mM orthophosphoric acid (pH 2.5; 77 + 23) was used at a flow rate of 1 mL/min on a C18 column. The Tia-NBD derivative was monitored using a fluorescence detector, with emission set at 520 nm and excitation at 458 nm. Gabapentin was selected as an internal standard. Linear calibration graphs were obtained in the concentration range of 45300 ng/mL. The lower limit of detection (LOD) was 10 ng/mL at a signal-to-noise ratio of 4. The lower limit of quantitation (LOQ) was 45 ng/mL. The relative standard values for intra- and interday precision were <0.46 and <0.57%, respectively. The recovery of the drug samples ranged between 98.89 and 99.85%. No chromatographic interference from the tablet excipients was found. The proposed method was validated in terms of precision, robustness, recovery, LOD, and LOQ. All the validation parameters were within the acceptance range. The proposed method was applied for the determination of Tia in commercially available tablets. The results were compared with those obtained by an ultraviolet spectrophotometric method using t- and F-tests.


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