Band 12, Heft 6

Riboflavin (RF) is a light sensitive compound and is known to form a number of photoproducts. These photoproducts possess the same nucleus and may interfere in the analysis of RF by UV and visible spectrometry. Therefore, it is necessary to apply the methods of multicomponent spectrometric analysis to quantify the vitamin and its photoproducts accurately. Such methods are useful in the study of the kinetics of photodegradation reactions of RF to obtain accurate and reliable results. Any interference in these methods due to linear or nonlinear irrelevant absorption of the minor unknown products can be accounted for by the application of appropriate correction procedures prior to kinetic treatment. Various factors affecting the accuracy, precision and selectivity of these analytical procedures are also discussed. This review highlights the principles and applications of multicomponent spectrometric methods and their application to the simultaneous determination of RF and its major photoproducts in degraded solutions to evaluate the kinetics of degradation.

Eordaia basin located in northwest of Greece, comprises an area which is characterized by intense energy related activities, including coal burning at four power plants and the associated mining operations. Air samples of inhalable (PM10) and respirable particles (PM2.5) were collected in cold and warm periods in 2010 at an urban background site of Kozani, the major city and capital of the region which is located close to the power plants. Particulate matter concentration, particle-bound polycyclic aromatic hydrocarbons and anionic species concentrations were determined using gravimetric, GC-MS in SIM mode and Ion Chromatography analysis, respectively. For the cold period, the mean PM10 and PM2.5 mass concentration was found to be 19.62 and 14.68 µg m−3, respectively. Correspondingly, for the warm period, the mean PM10 and PM2.5 values were 35.29 and 25.75 µg m−3, respectively. In general, the results indicated that the major sources of air pollution in Kozani are traffic, combustion from agricultural activities and lignite power plants emissions, contributing by different percentages to each particle fraction.

A new heterometallic compound, [CoCl(NH3)5][KCr(C2O4)3]·0.5H2O (1), has been synthesized and characterized by elemental analysis, IR and electronic spectra, thermal analysis, variable temperature magnetic susceptibility measurements, and single crystal X-ray diffraction. Compound 1 consists of two-dimensional [{KCr(C2O4)3}n]2n− layers, [CoCl(NH3)5]2+ ions and water molecules. Within the 2-D layer, three different types of oxalate coordination modes are present. Each K cation is coordinated by eight oxygen atoms from oxalate groups and also weakly interacts with the ninth oxygen atom. The extensive network of hydrogen bond is formed between the [KCr(C2O4)3]2− layer and the [CoCl(NH3)5]2+ ions. These interactions involve all hydrogen atoms of ammonia ligads and water molecule.

Ultraviolet (UV) photolysis of sixteen pharmaceutical compounds (PhCs) in mixed solutions with four types of water and two sets of UV radiation was investigated. UVC (254 nm) photolysis was ineffective at eliminating a large number of PhCs while a big number of them were refractory. However, vacuum UV (VUV: 185 nm + 254 nm) photolysis in the same experimental conditions eliminated the PhCs almost completely. The eliminations in ultrapure water (UPW), tap water (TW) and Neya River water (NRW) and their organic/inorganic contents were inversely correlated, which was more evident in VUV photolysis. Natural organic matter (NOM) in NRW did not have an impact in indirect photolysis, but effluent organic matter (EfOM) in secondary-treated effluent (NWTPE) enhanced indirect photolysis, which was more evident in VUV photolysis underlining the point that radiation wavelength/intensity can be a limiting factor in organic-rich waters. Moreover, VUV photolysis was far superior (90% mineralization) to UVC photolysis (10% mineralization) for PhCs mineralization. The greatly enhanced elimination and mineralization efficiencies observed for VUV photolysis were attributed to accelerated direct photolysis with 185 nm wavelength and indirect photolysis involving ·OH. The results demonstrated efficacy of VUV photolysis in wastewater treatment and its potential use as a tertiary treatment.

The thermal decomposition of five double-base propellants modified with RDX was studied by dynamic pressure thermal analysis to determine the effect of RDX content (20–60 wt.%) on performance. All have good stability. Both stability and activation energy increase as RDX increases from 20% to 50% then decrease; 50% RDX performs best. The decomposition mechanism is affected by RDX content and temperature. Increasing temperature induces autocatalysis and accelerates decomposition.

Production of new catalysts requires effective analytical quality control. The study of trace element composition of heterogeneous catalysts, based on C+PdO, using atomic emission spectrometry (AES) was carried out. A new method for the direct solid-state analysis by means of AES with direct current arc discharge was developed. On the basis of the qualitative analysis of elements, Al, Fe, Ni, Si and Ti have been identified, and for these elements, the quantitative method of determination has been developed. Optimization of excitation parameters and validation of the analytical method are presented. Calibration samples of the following composition were prepared: graphite powder (as a matrix), 3% of PdO and increasing contents of determined element oxides (spectrally pure). Calibrations were calculated by means of the least squares method. Working range for element impurities was from 1% to 0.0003%, and the limits of quantification — LOQ, (10-σ criterion) varied in the range from 0.002% (Ti) to 0.0038% (Si). For the control of active component, palladium was calibrated (working range — 0.01%–10.00%; LOQ −0.027%). The developed method can be used, also, for the elemental determinations of the other carbon based catalysts with the different active components (of platinum group elements).

The development and validation of a reliable analytical procedure for the determination of selected metals (Cd, Cr, Cu, Pb, Zn and Mn) in sediments accumulated in the Utrata River (Poland) is described. The aqua regia extraction followed by inductively coupled plasma optical emission spectrometry (ICP-OES) was used for this purpose. The optimized analytical procedure was validated, and adequate quality control actions were implemented in order to provide reliable data. The precision under’ within-laboratory’ reproducibility conditions was estimated from duplicate analysis. Certified reference material (CRM) was used in order to evaluate the accuracy of the results regarding the sewage sludge amended soil CRM 143R. The detection limits for all elements of interest were well-below their content in the investigated sediment samples. The obtained reliable data could be used for assessment of the relationship between human economic activity in the past and the geochemical features of the sediments.

In this study, antioxidant properties of commercial green teas and dietary supplements containing Camellia sinensis extracts were evaluated. Extracts were examined using two antioxidant assays (DPPH· radical method and ABTS·+ cation radical method). A Folin-Ciocalteu assay was used to evaluate the total polyphenol content in the extracts. In order to compare and characterize the investigated Camellia sinensis extracts, chemometric techniques based on fingerprint chromatograms, antioxidant activity and total polyphenol content were applied. Application of chemometric methods allowed for reduction of multidimensionality of the data set and grouped the samples into differentiable clusters. The relationship between the antioxidant activity and total polyphenol content was also assessed. The results indicated that extracts with the higher polyphenolic content exhibited the stronger antiradical activity against both DPPH· radicals and ABTS·+ cation radicals. The multivariate calibration technique (such as a tree regression algorithm) can be a useful tool for rapid determining the antioxidant activity of a herbal product based on its fingerprint chromatogram

In this paper, an electrochemical application of bismuth film modified glassy carbon electrode for azo-colorants determination was investigated. Bismuth-film electrode (BiFE) was prepared by ex-situ depositing of bismuth onto glassy carbon electrode. The plating potential was −0.78 V (vs. SCE) in a solution of 0.15 mg mL−1 Bi(III) and 0.05 mg mL−1 KBr for 180 s. In the next step, a thin film of chitosan was deposited on the surface of bismuth modified glassy carbon electrode, thus the bismuth-chitosan thin film modified glassy carbon electrode (Bi-CHIT/GCE) was fabricated and compared with bare GCE and bismuth modified GCE. Azo-colorants such as Sunset Yellow and Carmoisine were determined on these electrodes by differential pulse voltammetry. Due to overlapping peaks of Sunset Yellow and Carmoisine, simultaneous determination of them is not possible, so net analyte signal standard addition method (NASSAM) was used for this determination. The results showed that coated chitosan can enhance the bismuth film sensitivity, improve the mechanical stability without caused contamination of surface electrode. The Bi-CHIT/GC electrode behaved linearly to Sunset Yellow and Carmoisine in the concentration range of 5×10−6 to 2.38×10−4 M and 1×10−6 to 0.41×10−4 M with a detection limit of 10 µM (4.52 µg mL−1) and 10 µM (5.47 µg mL−1), respectively

The research reported here concerns the synthesis, characterization and potential applications of silica/lignosulfonate hybrid materials. Three types of silica were used (Aerosil®200, Syloid®244 and hydrated silica), along with magnesium lignosulfonate. The effectiveness of the hybrid material synthesis methodology was confirmed indirectly, using Fourier transform infrared spectroscopy, elemental and colorimetric analysis. Dispersive-morphological analysis indicates that the products with the best properties were obtained using 10 parts by weight of magnesium lignosulfonate per 100 parts of Syloid®244 silica. The relatively high thermal stability recorded for the majority of the synthesized products indicates the potential use of this kind of a material as a polymer filler. Results indicating the high electrokinetic stability of the materials are also of great importance. Additionally, the very good porous structure properties indicate the potential use of silica/lignosulfonate systems as biosorbents of hazardous metal ions and harmful organic compounds.

Six samples of propolis were analyzed in the paper: a sample from Brazil, Estonia, China and three samples from different locations of Uruguay. Static headspace technique coupled with gas chromatography-mass spectrometry analysis has been applied for the determination of the characteristic volatile profile with the aim to differentiate the propolis from different regions. Monoterpenes (α- and β-pinenes) were predominant in all samples, except the sample from China. This sample separated itself by the alcohols 3-methyl-3-buten-1-ol and 3-methyl-2-buten-1-ol, (40.33% and 11.57%, respectively) and ester 4-penten-1-yl acetate (9.04%). α-Pinene and β-pinene composed 64.59–77.56% of volatiles in Brazilian and Uruguayan propolis, and 29.43% in Estonian propolis. Brazilian propolis was distinguished by a high amount of β-methyl crotonaldehyde (10.11%), one of Uruguayan samples 3- by limonene (15.58%), and the Estonian sample — by eucalyptol (25.95%). Statistical investigation of the samples was made applying principal component, hierarchical cluster and K-Means cluster analyses. Various data pre-processing techniques were proposed and used to study and obtain the important volatile compounds contributed to the differentiation of the propolis samples from different regions to separate clusters.