28 research outputs found

    Aqueous extraction of anions from coal and fly ash followed by ion-chromatographic determination

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    Three different techniques were applied for the aqueous extraction of anions from coal and fly ash: rotary mixer-and ultrasonic-assisted extraction with different duration time, and microwave-assisted extraction at different temperatures. Validation showed that the ion-chromatographic method was suitable for the analysis of anions in coal and fly ash extracts. The variations in the amounts of anions using different extraction times during rotary-assisted extraction were minimal for all investigated anions. The efficiency of ultrasound-assisted extraction of anions from coal depended on the sonication time and was highest at 30 min. The ultrasound-assisted extraction was less efficient for the extraction of anions from fly ash than rotary-assisted extraction. Increase of temperature in the microwave-assisted extraction had a positive effect on the amounts of all anions extracted from coal and sulphate from fly ash, while the amounts of fluoride and chloride in fly ash extracts decreased. The microwave-assisted extraction of coal at 150 degrees C was compared with standard ASTM methods, and results were in good agreement only for chloride. Changes in the pH value and conductivity during ultrasound-assisted extraction were measured in order to explain changes on the surface of coal particles in contact with water and different processes that occur under environmental conditions

    Comparison of sequential and single extraction in order to estimate the environmental impact of metals from fly ash

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    The aim of this paper is to simulate leaching of metals from fly ash in different environmental conditions using ultrasound and microwave-assisted extraction techniques. Single-agent extraction and sequential extraction procedures were used to determine the levels of different metals leaching. The concentration of metals (Al, Fe, Mn, Cd, Co, Cr, Ni, Pb, Cu, As and Be) in fly ash extracts were measured by inductively coupled plasma-atomic emission spectrometry. Single-agent extractions of metals were conducted at sonication times of 10, 20, 30, 40 and 50 min. Single-agent extraction with deionized water was also performed by exposing samples to microwave radiation at temperature of 50 degrees C. The sequential extraction was conducted according to the BCR procedure which was modified and applied to study the partitioning of metals in coal fly ash. The microwave-assisted sequential extraction was performed at different extraction temperatures: 50, 100 and 150 degrees C. The partitioning of metals between the individual fractions was investigated and discussed. The efficiency of the extraction process for each step was examined. In addition, the results of the microwave-assisted sequential extraction are compared to the results obtained by standard ASTM method. The mobility of most elements contained in the fly ash is markedly pH sensitive

    Investigation of different extraction procedures for the determination of major and trace elements in coal by ICP-AES and ion chromatography

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    This paper presents the extraction of major and trace elements from a coal sample, in deionized water, by using three different extraction techniques. Rotary mixing and ultrasonic extraction were examined for different extraction times, while the microwave-assisted extraction was performed at different temperatures. Metal concentrations (Na, K, Ca, Mg, Al, Fe, Mn, Be, Cd, Co, Cr, Hg, As, Ni, Se, Sb and Pb) in solution were determined employing inductively coupled plasma atomic emission spectrometry; whereas the results obtained for Na, K, Ca and Mg were compared employing ion chromatography. Comparing the rotary-and ultrasonic-assisted extractions, it was shown that the former technique was more efficient for the determination of Fe, Na and Pb, whereas the latter one proved more efficient for the determination of Co and Cr ions. Microwave-assisted extraction was shown to be the most efficient method for all the tested elements in coal. In addition, sequential extraction of the elements was realized using microwave digestion. The results of the sequential extraction experiments indicated associations of investigated elements with a mineral phase and organic matrix. Sequential extraction provided information on possible leaching of As, Cd, Co, Cr, Ni, Pb, Fe and Mn under environmental conditions

    Ispitivanje adsorpcije fenola na makroporoznim polimernim adsorbensima

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    This work reports results on phenol adsorption from aqueous solution by porous copolymers based on glycidyl methacrylate: two samples of macroporous crosslinked poly(glycidyl methacrylate-co-ethylene glycol dimethacrylate), were synthetized by suspension copolymerisation with ethylene glycol dimethacrylate. In addition, the two copolymer samples were functionalized with ethylene diamine. The amounts of adsorbed phenol were presented in the form of adsorptions isotherms, which were interpreted using Langmuir, Freundlich and Sips' equations. The first was found to express high level of agreement with experimental data. Phenol adsorption indicate the homogeneous distribution of active sites present on the investigated polymers. It was found that adsorption of phenol on copolymers is fast and depends on the presence of amino groups and on the pore size. From the obtained results, it was possible to distinguish macroporous polymer as a material which possesses the capacity for adsorption of phenol comparable to that of activated carbon.Ovaj rad se bavi proučavanjem adsorpcije fenola iz vodenih rastvora na kopolimerima različitih poroznih karakteristika i polarnosti. KoriŔćeni adsorbensi se baziraju na glicidil metakrilatu: dva uzorka makroporoznog poli(glicidil metakrilat-co-etilen glikol dimethakrilat) su sintetisani suspenzionom kopolimerizacijom sa etilen glikol dimetakrilatom. Dodatno, dva kopolimera su funkcionalizovani sa etilen diaminom. Količina adsorbovanog fenola je predstavljena u vidu adsorpcionih izotermi, koje su interpretirane koriŔćenjem Langmuir-ove, Freundlich-ove i Sips-ove jednačine: prva od ovih daje visok nivo slaganja sa eksperimentalnim podacima. Adsorpcija fenola ukazuje na homogenu raspodelu aktivnih mesta prisutnih u ispitivanim polimernim sistemima. Rezultati dobijeni u ovom istraživanju pokazuju da adsorpcija fenola na ispitivanim kopolimerima zavisi od prisustva amino grupa i od veličine pora. Adsorpcija fenola iz vodenih rastvora je brza u slučaju svih koriŔćenih adsorbenasa. Na osnovu dobivenih rezultata, može se zaključiti da su makroporozni polimeri materijali čije je adsorpcioni kapacitet za fenol uporediv sa onim koji ima aktivni ugalj

    Primena klasičnih i instrumentalnih metoda analize u kontroli kvaliteta piva

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    In order to control the quality of beer and raw materials for production of beer in Belgrade Beer Industry (BIP), water is analyzed (city, technological and demineralized water). Measurements of pH values indicated the increased pH values in the sample of technological water, which had no impact on wort hopping, since the tested samples of wort, young beer and final product had a pH value within the expected range. After processing city water, a sample of technological water was found with increased carbonate hardness, which is caused by the increased content of sodium hydrogen carbonate. Analysing the titration alkalinity, titration acidity and buffering power, it was found that the alkalinity was decreasing which is in accordance with the determination of pH values of wort and beer samples (young beer and final product). Analyzing the content of anions and cations in the examined water samples, it has been shown that the concentration of these examinated anions (Cl-, NO3-, SO42- and PO43-) and cations (NH4+, Na+, K+, Ca2+, Mg2+) are within the limits prescribed by the Regulations on hygienic safety of drinking water, and thus by the Regulations of quality and other requirements for beer. The contents of anions in wort and beer samples (young beer and final product) were determined by ion chromatography method. The contents of sulphate and nitrate ions were within the recommended limits. The concentration of chloride ions was above 150 mg/dm3, which may have an impact on the sensory properties of beer, while changes in the content of phosphate ions were insignificant.U cilju kontrole kvaliteta piva i sirovina za proizvodnju piva u Beogradskoj industriji piva (BIP) analizirana je voda (gradska, tehnoloÅ”ka i demineralizovana). Merenja pH vrednosti ukazala su na povećanu vrednost pH u uzorku tehnoloÅ”ke vode, ali to nije imalo uticaja na ukomljavanje slada poÅ”to su ispitivani uzorci sladovine, kao i uzorci mladog piva i gotovog proizvoda imali vrednost pH u očekivanom opsegu. Obradom gradske vode dobio se uzorak tehnoloÅ”ke vode sa povećanom karbonatnom tvrdoćom, koja je prouzrokovana povećanim sadržajem natrijum-hidrogenkarbonata. Analizom titracionog alkaliteta, titracionog aciditeta, i moći puferovanja, utvrđeno je da se alkalitet smanjuje Å”to je u saglasnosti i sa određivanjem pH vrednosti uzoraka sladovine i piva (mladog i gotovog proizvoda). Analiza sadržaja anjona i katjona u ispitivanim uzorcima vode, pokazala je da je koncentracija ispitivanih anjona (Cl-, NO3-, SO42- i PO43-) i katjona (NH4+, Na+, K+, Ca2+, Mg2+) u granicama propisanim Pravilnikom o higijenskoj ispravnosti vode za piće, a time i sa Pravilnikom o kvalitetu i drugim zahtevima za pivo. Sadržaj anjona u uzorcima sladovine i piva (mladog i gotovog proizvoda) određen je metodom jonske hromatografije. Sadržaj sulfat- i nitrat-jona je bio u preporučenim granicama. Koncentracija hlorid-jona je bila iznad 150 mg/dm3, Å”to može imati uticaja na senzorne karakteristike piva, dok je promena sadržaja fosfat-jona bila neznatna

    Određivanje katjona i metala u pivu i sirovinama za proizvodnju piva metodama jonske hromatografije (IC) i atomske apsorpcione spektrofotometrije (AAS)

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    In order to control the quality of beer and raw materials for beer production, methods as ion chromatography (IC) and atomic absorption spectrophotometry (AAS) were applied. Water was analyzed as a raw material for beer production (urban, technological and demineralized water). Measurements of pH values indicated the increased pH values in the sample of tehnological water, but it had no impact on wort hopping, since the tested samples of wort, young beer and final product had a pH value in the expected range. Analyzing the content of anions and cations in the examinated water samples, it is shown that the concentration of these examinated anions (Cl- , NO3-, SO42- and PO43-) and cations (NH4+, Na+, K+, Ca2+, Mg2+), as and microelements (Fe, Cu i Zn) are within the limits prescribed by the Regulations on hygienic safety of drinking water and the Regulations of quality and other requirements for beer. Investigating contents of anions in samples of wort and beer (young beer and final product) showed that the contents of SO42- and NO3- ions were within recommended limits and the concentration of Cl- ions was above 150 mg/dm3, which may have an impact on sensory characteristics of beer, while changes in the content of PO43- ions were insignificant. Since AAS method is a standard method for analyzing content of alkaline and alkaline earth metals, the results obtained by this method in beer samples are taken as a referent results and according to them an analyse was performed and results obtained by IC method were compared. Results of the determination of Na, Ca and Mg in examinated water samples have shown variations, but both methods have shown the increased content of Na in demineralized water. The contents of alkaline and alkaline earth metals in wort and beer (young beer and final product) have shown that the results obtained by these two methods were in agreement.U cilju kontrole kvaliteta piva i sirovina za proizvodnju piva u Beogradskoj industriji piva (BIP) primenjene su metode jonske hromatografije (IC) i atomske apsorpcione spektrofotometrije (AAS). Od sirovina za proizvodnju piva analizirana je voda (gradska, tehnoloÅ”ka i demineralizovana). Merenja pH vrednosti ukazala su na povećanu pH vrednost u uzorku tehnoloÅ”ke vode, ali to nije imalo uticaj na ukomljavanje slada poÅ”to su ispitivani uzorci sladovine, kao i uzorci mladog piva i gotovog proizvoda imali pH vrednost u očekivanom opsegu. Analiza sadržaja anjona i katjona u ispitivanim uzorcima vode, pokazala je da je koncentracija ispitivanih anjona (Cl-, NO3 -, SO4 2- i PO4 3-) i katjona (NH4 +, Na+, K+, Ca2+, Mg2+), kao i mikroelemenata (Fe, Cu i Zn) u granicama propisanim Pravilnikom o higijenskoj ispravnosti vode za piće i Pravilnikom o kvalitetu i drugim zahtevima za pivo. Ispitivanje sadržaja anjona u uzorcima sladovine i piva (mladog i gotovog proizvoda) pokazalo je da je sadržaj SO4 2-- i NO3 --jona bio u preporučenim granicama, koncentracija Cl-- jona bila je iznad 150 mg/dm3, Å”to može imati uticaj na senzorne karakteristike piva, dok je promena sadržaja PO4 3--jona bila neznatna. PoÅ”to je AAS standardna metoda za analizu sadržaja alkalnih i zemnoalkalnih metala, rezultati dobijeni ovom metodom u uzorcima piva uzeti su kao referentni i prema njima je izvrÅ”ena analiza i upoređivanje rezultata dobijenih metodom IC. Rezultati određivanja Na, Ca i Mg u ispitivanim uzorcima vode, pokazala su odstupanja, ali su obe metode ukazale na povećan sadržaj natrijuma u demineralizovanoj vodi. Sadržaj alkalnih i zemnoalkalnih metala u uzorcima sladovine i piva (mladog i gotovog proizvoda) ukazao je da su rezultati dobijeni ovim dvema metodama bili u saglasnosti

    Ambient air particles: The use of ion chromatography and multivariate techniques in the analysis of water-soluble substances

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    Seventeen water-soluble substances (of sodium, ammonium, potassium, magnesium, calcium, formate, methanesulfonate, glyoxylate, chloride, nitrite, nitrate, glutarate, succinate, malate, malonate, sulfate and oxalate) in 94 samples of particle matter in the ambient air, collected over ten months, in a suburb of Belgrade (Serbia), were determined by ion chromatography. To apportion the sources of the air pollution, the log-transformed data were processed by applying multivariate techniques. Principal component and factor analysis identified three main factors controlling the data variability: stationary combustion processes with the highest loadings of oxalate, malonate and malate; landfill emission and secondary inorganic aerosol characterized by high levels of ammonium, nitrate and sulfate; a contribution of mineral dust composed of magnesium, calcium and chloride. The hierarchical cluster analysis pointed out a differentiation of the samples into five groups belonging to different variables inputs. For the classification of ambient air samples using nine selected ions, the recognition ability of linear discriminant analysis, k-nearest neighbors, and soft independent modeling of class analogy were 87.0, 94.6, and 97.8 %, respectively. Time-series analysis showed that the traffic emission is more pronounced in winter in contrast to the mineral dust influence, while the effect of waste combustion exhibits no trend

    Indirect determination of lutetium by differential pulse anodic stripping voltammetry at a hanging mercury drop electrode

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    Lutetium has been determined by differential pulse anodic stripping voltammetry in an acidic solution containing Zn-EDTA. Lutetium (III) ions liberated zinc (II), which was preconcentrated on a hanging mercury drop electrode and stripped anodically, resulting in peak current linearly dependent on lutetium (III) concentration. Less than 0.4 ng mL(-1) lutetium could be detected after a 2 min deposition

    The dominant contribution on wet deposition of water-soluble main ions in the South-Eastern Adriatic region

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    The results of content of water-soluble ions measured in 604 samples of precipitation collected in South-Eastern Adriatic region during 6 years have been analyzed. The HYSPLIT model was used to study the air mass paths. Although the ion concentrations of investigated ions in precipitation of air masses from the continental parts of Europe were significant, the total wet deposition is dominated by precipitation coming over the Mediterranean Sea. The sea salt components are significantly correlated. The correlations between Ca2+ and Mg2+, Ca2+ and SO4 (2-) and Ca2+ and K+ indicate the main terrigeneous ions

    Physicochemical analysis and phenolic profile of polyfloral and honeydew honey from Montenegro

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    The research subject of this paper was a detail physicochemical analysis of 28 honey samples from the northern part of Montenegro. The honey from Montenegro has not been previously studied in such detail. Differentiation between samples, such as honeydew honey and polyfloral honey, was based on electrical conductivity, which was higher than 0.8 mS cm-1 for honeydew honey, as was expected. Other investigated physicochemical parameters (water content, free acids, diastase activity, hydroxymethylfurfural (HMF) content and sugar content) have shown great similarity for all honey samples. The main interest of this study was the identification and quantification of phenolic compounds using ultra-high performance liquid chromatography (UHPLC) with mass spectrometry detection. The results show that honey samples are very rich in phenolic compounds, especially quercetin. Among the 31 quantified phenolic compounds, the most dominant were phenolic acids. The highlight was based on p-hydroxybenzoic acid, p-coumaric acid, caffeic acid and ferulic acid. Considering polyphenolic compounds and sugar content, a high nutritional value can be observed in all samples, with an emphasis on polyfloral honeys, as was confirmed with principal component analysis (PCA). In addition, all honey samples were tested for total phenolic content (TPC) and radical scavenging activity (RSA). The results indicate the higher antioxidant ability of honeys from Montenegro in comparison to some honey samples from other countries in the region.Supplementary material: [http://cherry.chem.bg.ac.rs/handle/123456789/3828
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