Authors:Bernd Spangenberg, Klemens Lorenz, and Steffen Nasterlack
In-situ densitometry for qualitative or quantitative purposes is a key step in thin-layer chromatography. It offers a simple way of quantifying by measuring the optical density of the separated spots directly on the plate. A new TLC scanner has been developed which is able to measure TLC plates or HPTLC plates, at different wavelengths simultaneously, without destroying the plate surface. The system enables absorbance and fluorescence measurements in one run. Fluorescence measurements are possible without filters or other adjustments.The measurement of fluorescence from a TLC plate is a versatile means of making TLC analysis more sensitive. Fluorescence measurements with the new scanner are possible without filters or special lamps. Improvement of the signal-to-noise ratio is achieved by wavelength bundling. During plate scanning the scattered light and the fluorescence are both emitted from the surface of the TLC plate and this emitted light provides the desired spectral information from substances on the TLC plate. The measurement of fluorescence spectra and absorbance spectra directly from a TLC plate is based on differential measurement of light emerging from sample-free and sample-containing zones.The literature recommends dipping TLC plates in viscous liquids to enhance fluorescence. Measurement of the fluorescence and absorbance spectra of pyrene spots reveals the mechanism of enhancement of plate dipping in viscous liquids — blocked contact of the fluorescent molecules with the stationary phase or other sample molecules is responsible for the enhanced fluorescence at lower concentrations.In conclusion, dipping in TLC analysis is no miracle. It is based on similar mechanisms observable in liquids. The measured TLC spectra are also very similar to liquid spectra and this makes TLC spectroscopy an important tool in separation analysis.
Authors:Ceren Kütahyali, Joaquin Cobos, and Vincenzo Rondinella
Results from tests aimed at optimizing an instrumental procedure for the direct and fast determination of uranium in solution
by laser fluorescence are presented. A comparison of sample fluorescence measured using different fluorescence enhancing reagents
was performed: sodium pyrophosphate, orthophosphoric acid, sulphuric acid and a commercially available fluorescence enhancer
were tested for the determination of uranium. From the experimental results, 0.01 M Na4P2O7·10H2O showed the best performance. Effects of reagent pH, different matrices, different concentrations of dissolved Th, and sample
volume were investigated. Applications of the improved procedure for the determination of uranium in samples arising from
UO2-based high level nuclear waste dissolution studies are described.
Authors:S. Ganesh, Fahmida Khan, M. Ahmed, P. Velavendan, N. Pandey, U. Mudali, and S. Pandey
A simple and rapid, laser fluorimetric method for the determination of uranium concentration in raffinate stream of Purex
process during reprocessing of spent nuclear fuel has been developed. It works on the principle of detection of fluorescence
of uranyl complex formed by using fluorescence enhancing reagent like sodium pyrophosphate. The uranium concentration was
determined in the range of 0–40 ppb and detection limit of 0.2 ppb. The optimum time discrimination is obtained when the uranyl
ion is complexed with sodium pyrophosphate. Need of preconcentration step or separation of uranium from interfering elements
is not an essential step.
A simple and rapid laser fluorometric determination of trace and ultra trace level of uranium in a wide variety of low uranium
content materials like soil, basic and ultra basic rocks, plant ash, coal fly ash and red mud samples is described. Interference
studies of some common major, minor and trace elements likely to be present in different, geological materials on uranium
fluorescence are studied using different fluorescence enhancing reagents like sodium pyrophosphate, orthophosphoric acid,
penta sodium tri-polyphosphate and sodium hexametaphosphate. The accurate determination of very low uranium content samples
which are rich in iron, manganese and calcium, is possible only after the selective separation of uranium. Conditions suitable
for the quantitative single step extraction of 25 ng to 20 μg uranium with tri-n-octylphosphine oxide and single step quantitative
stripping with dilute neutral sodium pyrophosphate, which also acts as fluorescence enhancing reagent is studied. The aqueous
strip is used for the direct laser fluorometric measurement without any further pretreatment. The procedure is applied for
the determination of uranium in soil, basalt, plant ash, coal fly ash and red mud samples. The accuracy of the proposed method
is checked by analyzing certain standard reference materials as well as synthetic sample with known quantity of uranium. The
accuracy and reproducibility of the method are fairly good with RSD ranging from 3 to 5% depend upon the concentration of
Authors:R. Radhamani, P. Mahanta, P. Murugesan, and G. Chakrapani
A simple, rapid, effective and eco-friendly decomposition method is developed for the determination of uranium (U) by laser
induced fluorimetry (LIF). The salts of sodium di-hydrogen phosphate (NaH2PO4) and di-sodium hydrogen phosphate (Na2HPO4) were used in the ratio of 1:1 (phosphate flux) for the decomposition and dissolution of refractory, non silicate minerals
like ilmenite, rutile, columbite, tantalite, and xenotime. The effect of associated matrix elements (Ti, Fe, Nb, Ta, Mn and
Y present in the sample) on quenching of uranyl fluorescence was studied. The flux used for the sample decomposition has several
advantages. In the reported sample decomposition methods, α-hydroxy acids are used as complexing agents to prevent hydrolysis
and to get clear and stable solution. This solution can not be directly used for U determination by LIF as α-hydroxy acids
quench uranyl fluorescence, hence separation is required. In the present method no such separation is required. The flux itself
acts as fluorescence enhancing reagent and buffer (maintaining the optimum pH of 7.1 ± 0.1). The fused melt of the flux mixture,
when disintegrated in water, gives clear and stable solution and has high tolerance for most of inorganic quenchers compared
to reported phosphate buffers. Also just by dilution (due to high sensitivity of LIF), the concentration of quenchers could
be brought down well within the tolerance limit. The accuracy and precision of the method was evaluated by analyzing Certified
Reference Materials (IGS-33 and IGS-34 of Institute of Geological Sciences, UK) and Synthetic Minerals. The accuracy of the
data is further evaluated by comparing with standard decomposition methods. The results are well within the experimental error.
The RSD of the method is ±10% (n = 6) at 10 ppm level for Ilmenite and for other minerals the RSD of the method is ±5% (n = 6) at 50 ppm level. The method is being routinely applied to various refractory samples received from Rare Metal and Rare
Earth Investigations for determination of uranium by laser fluorimetry.
-guanidine-based multisignaling sensor molecule that displays redox-ratiometric behavior or fluorescenceenhancement in the presence of anions and cations . Org Lett . 8 : 2107 – 2110 10.1021/ol060495i .