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This paper presents results of speciation analysis of bottom sediments. In our examinations a five-step extraction procedure was applied. Direct analysis of sediments and analysis of extracts was carried out by X-ray fluorescence spectrometry with wavelength dispersion. Examinations were carried out with the use of lake sediments CRM.
The total content of chromium in natural waters does not generally exceed several mg/l. Thus, it is obvious that various forms of chromium will occur at the levels of tenths or hundredths of mg/l. Their determination requires the application of a sufficiently sensitive method, but an important role to play has its specificity in the case of chemical individuals or selectivity in regard to speciation of a group of compounds, e.g. valency states or organic chromium complexes. Generally, however, there is a lack of specific and selective methods, and the concentrations of various forms of the analyte occur often at the level of detection limits of even such sensitive techniques as atomic absorption spectrometry. This paper presents a review of currently available analytical possibilities of chromium speciation investigations in natural water samples. Analytical procedure schemes enabling "total speciation analysis" have been discussed in some detail. A large group of methods used in the speciation analysis of chromium(III) and chromium(VI), both in off-line and on-line mode, has also been discussed.
The study aimed at application of a high performance liquid chromatography (HPLC) with UV detector for selenium speciation in samples of mineral and well waters in Poland. Basic solutions 1000 μg/l SeO3 2- and SeO4 2- were prepared by dissolving 2.190 g of reagent Na2SeO3 and 2.393 g Na2SeO4 in 1000 ml of deionised water, respectively. Recent standards SeO3 2- and SeO4 2- (single or mixed) were prepared daily. Chromatographic separations were obtained on a column with reversed phase of C18, 250*4 mm, 5 μm ODS. As mobile phase mixture of 5 mmol/l phosphate tetrabutylammonium, 50/50 water/methanol at pH 3.4 was used. Flow rate of mobile phase was1 ml/min and detector was set on λ=210 nm. Injection volumes were 5 μl. The average concentration of Se(IV) was 4.10 μg/l and Se(VI) - 4.27 μg/l and Se(II) - 0.54 μg/l although the differences between water samples originating from various sources were relatively high. The developed method can be therefore recommended for determination of Se in samples of mineral water.
The purpose of this paper was to compare two methods of fractionation of reactive phosphorus forms (RP) in bottom sediments of polymictic water reservoirs located in rural areas. As a criterion for estimation, quantities RP extracted in analyzed fractions versus the general content of Al, Fe and Ca were used. The sediments were collected in springtime, from rural areas with different land use in the drainage basin (arable fields, uncultivated land, farmyards). The sediments were collected with a KC-Denmark core sampler for bottom sediments, which makes it possible to collect samples leaving the upper structure of 6 cm in thickness intact. After mineralization, each sample was analyzed for the general phosphorus content and a speciation analysis was performed by two methods. With the first method (M1), the RP bonded to Al (Al_RP), Fe (Fe_RP) and Ca (Ca_RP) was determined. The second method (M2) was applied to determine fractions of reactive phosphorus released from the sediments under reduced conditions, mainly from bonds with iron and manganese (BD_RP), adsorbed on aluminium oxides mainly AL2O3 and other surfaces (NaOH_RP) and apatite phosphorus and bonds with carbonates. In almost all the sediments, most RP was determined in the phosphorus fractions with Ca extracted with acid solution. For the fractions obtained via the M1 method, more of the general RP, as well as phosphorus bonded to calcium and iron was found than for fractions obtained with the M2 method, and the differences might be attributed to translocation of phosphorus from organic to inorganic compounds during fractioning. The fraction of reactive phosphorus determined with the M1 method is correlated more strongly with the general content of the metal in the sediments than reactive phosphorus fractions determined with the M2 method. The strong correlation between the content of iron and the fraction of BD_RP in mineral sediments shows that it can be an indicator of the sensitivity of sediment to changes in the redox potential.
This paper presents results of speciation analysis of soils coming from Silesia. In examinations a five-step extraction procedure has been applied. Direct analysis of sediments and analysis of extracts was carried out by the X-ray fluorescence spectrometry with wavelength dispersion. Examinations were carried out with the use of soil CRM S-1.
Owing to its biological properties the microelement selenium has attracted enormous interest. It has been established that selenium stimulates the human immune system and has anti-carcinogenic effect. The main sources of selenium are high-protein foodstuffs of plant and animal origin, as well as high-protein dairy products. The aim of this study was to detect selenium content in confectionery products using speciation analysis in order to determine inorganic forms of selenium such as Se2- SeO32- and SeO42- anions. The hydride generation method combined with the atomic absorption spectroscopy was used for the final determination of selenium forms. The determination of selenium was conducted using aqueous extraction and digestion of samples with concentrated acids. The speciation determination of selenium was conducted in ten confectionery products. The correlation between the total content of selenium and its individual forms (-II), (IV),(VI) of different oxidation degree was also examined. It was shown that there was no correlation between the total selenium and inorganic forms of selenium. That means that speciation analysis is the only correct analysis of selenium content in foods.
This paper presents the results of speciation analysis of aluminium in the River Silnica. The concentration of individual aluminium forms has been correlated with the select physical and chemical parameters of water.
The total concentration of zinc, iron, nitrogen and phosphorus, as well as their water and acetic acid extractable forms - nitrate nitrogen, ammonium nitrogen and phosphate phosphorus - were determined in st. John's wort herb (Hypericumperforatum L.) yarrow herb (Achillea millefolium L.), nettle leaves (Urtica dioica L .) and birch leaves (Betula pendula Roth.), collected from four natural locations in northern Poland. The content of total Zn and Fe was determined by FAAS, whereas of total N, total P and their extractable forms by UV/Vis spectrophotometry. The obtained results showed that particular plant species differed significantly in the contents of Zn, Fe, P and P-P04. The area of harvest didn't have major effects on the concentration of analyzed elements in the studied plant species. Significantly, 13 inter-element correlations were obtained for the studied elements, mainly between iron and nitrogen, iron and phosphorus, phospho­rus and nitrogen and among their water-extractable forms, indicating their involvment in metabolism of medicinal plants. Nutritional and toxicological aspects of the analyzed plants used commonly as folk medi­cines in Poland were evaluated by comparison of the obtained results with the WHO/FAO norms.
W niniejszej pracy podjęto badania w kierunku szerszego monitoringu związków krzemu w wybranych produktach spożywczych dostępnych w Polsce. Opracowano schemat analizy specjacyjnej, według którego analizowano krzem w połączeniach organicznych i nieorganicznych. Uzyskane wyniki potwierdziły specjacyjny charakter proponowanej metody oraz wykazały jej przydatność do analizy ilościowej związków krzemu w próbach żywności.
Bottom deposits of selected rivers in the Świętokrzyskie Region of Poland flowing through areas of various geological characteristics and land development were analyzed for the presence of cadmium, zinc and lead. Microwave-assisted 3-stage sequential extraction recommended by the European Union (EU) was applied for that purpose as well as a 5-stage extraction proposed by Tessier et al. Residues after sequential extraction were mineralized in concentrated nitric acid in order to check if applied sequential extraction procedures allowed extraction of total amounts of metals from bottom deposits. Metal contents were determined with F-AAS technique in particular extracts.
Oznaczono formy żelaza i cynku w glebach nawadnianych ściekami komunalnymi na polach irygowanych Wrocław — Osobowice metodą ekstrakcji sekwencyjnej według Zeiena i Bruemmera. Stwierdzono, że żelazo występuje głównie w krystalicznych formach tlenków i wodorotlenków oraz w połączeniach organicznych. Cynk związany jest w tlenkach żelaza i połączeniach organicznych, ale nawet do 47% całkowitej zawartości stanowią formy mobilne w środowisku glebowym.
This paper deals with the principles for processing the analytical information obtained by speciation analytics. Main speciation analytics trends have been discussed, including integration of the analytical methods, sample preparation techniques, and hyphenated techniques. The importance of speciation analytics in deriving standards from the overall factors has been demonstrated.
Opracowano metodę specjacyjnego oznaczania nieorganicznych form selenu (-II), (IV), (VI) oraz całkowitej zawartości selenu w próbkach produktów spożywczych uwzględniając ich złożoną matrycę. Wykorzystano do oznaczeń końcowych technikę generowania wodorków w połączeniu z metodą atomowej spektroskopii absorpcyjnej HG-AAS. Oznaczenie selenu opiera się na połączeniu ekstrakcji wodnej próbki z roztwarzaniem próbki stężonymi kwasami. Oznaczenie specjacyjne selenu wykonano w pięciu grupach produktów spożywczych: kaszach, ziołach, sokach owocowych, odżywkach dla niemowląt oraz w wybranych pokarmach stanowiących potencjalne naturalne źródła selenu.
Celem pracy była ocena zawartości ogólnej miedzi oraz we frakcjach wydzielonych z gleb, położonych na stoku morenowym Wysoczyzny Siedleckiej. Sekwencyjne frakcjonowanie przeprowadzono metodą Zeiena i Brümmera. Analiza specjacyjna wykazała, iż metal ten był związany z różnymi częściami fazy stałej gleby. Największy procentowy udział miedzi stwierdzono we frakcji rezydualnej (F7), w poziomach skały macierzystej, a najmniejszy we frakcji łatwo rozpuszczalnej (F1) i wymiennej (F2). W badanych glebach, w transekcie A i B zanotowano istotne związki korelacyjne między udziałem miedzi w wydzielonych frakcjach, a jej zawartością ogólną, zawartością węgla związków organicznych a frakcją organiczną (F4), pojemnością sorpcyjną CEC oraz frakcją iłową gleby (< 0,002 mm).
Organometallic compounds are widely used in almost all sectors of industry. As a result of emissions from natural and anthropogenic sources they are released to the environment, where they undergo a variety of conversions and interactions. Some organometallic compounds exhibit high toxicity. Organometallic compounds of mercury, tin, lead, selenium and arsenic are among the most common and hazardous compounds. Based on literature dealing with the occurrence and methods of determination of selected organometallic compounds of mercury, tin, lead, selenium and arsenic, we describe their sources, uses and the mechanism of toxicity. Fundamental problems associated with speciation analysis are discussed and the basic steps of analytical procedure used for the determination of organometallic compounds of Hg, Sn, Pb, Se, and As in soil and bottom sediments, including sample collection, preservation, storage, extraction, separation and determination, are characterized.
W pracy oznaczono całkowitą zawartość żelaza oraz jego formy przyswajalne przez organizm człowieka, stosując model ekstrakcji prostej gorącą wodą redestylowaną. Materiał poddany analizie specjacyjnej stanowiło 37 próbek liści, korzeni, kłączy oraz owoców i nasion pochodzących z różnych zakładów zielarskich w Polsce. Analizowane surowce roślinne zmineralizowano w systemie mikrofalowym, a następnie oznaczono zawartość żelaza całkowitego metodą FAAS. Oznaczając Fe(Il) w ekstraktach wodnych użyto metody spektrofotometrycznej z o-fenantroliną, a w przypadku Fe(III) posłużono się metodą opierającą się na ekstrakcji połączenia tej formy żelaza z KNCS ketonem metyloizobutylowym (MJBK), a następnie pomiarze spektrofotometrycznym. Uzyskane wyniki wskazują na zróżnicowanie badanego materiału pod względem całkowitej zawartości żelaza, a także na znikomy, rzędu kilku procent udział form tego pierwiastka ulegających ekstrakcji wodą w jego całkowitej puli w roślinnych surowcach leczniczych.
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