Determination of Diethyldithiocarbamate in the Solid Phase of a Fibrous Cation Exchanger in the Cu-Form Using Diffuse Reflectance Spectroscopy

2020 ◽  
Vol 75 (6) ◽  
pp. 759-763
Author(s):  
V. P. Dedkova ◽  
O. P. Shvoeva ◽  
A. A. Grechnikov
Author(s):  
I. I. Kuzmin ◽  
T. Kh. Chyong ◽  
Ya. I. Simakina ◽  
A. V. Mikhailova ◽  
Yu. I. Fabelinsky

A method for copper(II) determination based on copper(II) ions interaction with the organic reagent picramine-ε, concentrating the formed complex on a solid-phase matrix and recording diffuse reflectance spectroscopy spectra by a portable combined LED miniphotometer was developed. Poly-ε-caproamide membranes were investigated as solid-phase matrixes. It was found that the diffuse reflectance coefficient of the studied membranes in the visible spectrum region does not depend on wavelength. So, the signal from membranes does not distort the results of the analysis. Factors controlling the process of sorption of the copper(II) complex with picramine-ε were studied. It was shown that the poly-ε-caproamide membranes are effective sorbents which provide the possibility of concentrating the analyte at a level higher than 105. The dependences of analytical signal on the acidity of the solution, the time of keeping the complex in the solution and the initial volume of the solution passed through the membrane were studied. Based on the obtained data, the optimal conditions of the analysis were found. Calibration dependence of the analytical signal on the concentration of copper(II) in model solutions was estimated. The method was tested for the determination of copper(II) ions in white wine. The method of additives was used for the analysis. It was found that the concentration of copper(II) ions in “Vagrus” wine is 0.0016 mkg/ml.


2019 ◽  
Vol 9 (22) ◽  
pp. 4933 ◽  
Author(s):  
Sergej Bock ◽  
Christian Kijatkin ◽  
Dirk Berben ◽  
Mirco Imlau

This paper addresses the challenging task of optical characterization of pure, dielectric (nano-)powders with the aim to provide an end-to-end instruction from appropriate sample preparation up to the determination of material remission and absorption spectra. We succeeded in establishing an innovative preparation procedure to reproducibly obtain powder pellet samples with an ideal Lambertian scattering behavior. As a result, a procedure based on diffuse reflectance spectroscopy was developed that allows for (i) performing reproducible and artifact-free, high-quality measurements as well as (ii) a thorough optical analysis using Monte Carlo and Mie scattering simulations yielding the absorption spectrum in the visible spectral range. The procedure is valid for the particular case of powders that can be compressed into thick, non-translucent pellets and neither requires embedding of the dielectric (nano-)powders within an appropriate host matrix for measurements nor the use of integrating spheres. The reduced spectroscopic procedure minimizes the large number of sources for errors, enables an in-depth understanding of non-avoidable artifacts and is of particular advantage in the field of material sciences, i.e., for getting first insights to the optical features of a newly synthesized, pure dielectric powder, but also as an inline inspection tool for massively parallelised material characterization.


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