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1.
Pohl P  Prusisz B 《Talanta》2006,69(5):1227-1233
An analytical procedure was proposed to study the operational fractionation of Ca and Mg in bee honeys, fruit juices and tea infusions. The protocol devised was based on the solid phase extraction of distinct metal fractions on different sorbents, namely strong acidic cation exchanger Dowex 50Wx4, weak acidic cation exchanger Diaion WT01S and strong basic anion exchange resin Dowex 1x4. For the evaluation of the amounts of the metal fractions distinguished, a flame atomic absorption spectrometry was used off-line prior to the determination of Ca and Mg concentrations in the effluents obtained. It was established that Ca and Mg are mostly present in the analysed samples in the form of cationic species (96–100%). The accuracy of the entire fractionation scheme and sample preparation procedures involved was verified by the performance of the recovery tests.  相似文献   

2.
The physicochemical parameters (free acidity, moisture content, sucrose content, hydroxymethylfurfural, reducing sugars, electrical conductivity, diastase activity and water-insoluble content), elements (Cu, Fe, Zn, Mn, Cr, Co, Ni, Se, K, Na, Ca, Mg) and heavy metal/metalloid concentrations (Cd, Hg, Pb and As) of 84 honeys (linden, multifloral, honeydew and acacia) from Serbia, were analyzed using ICP-MS. Concerning the physicochemical parameters, all tested honeys were found to meet European Legislation (EC Directive 2001/110). Potassium was the major element, ranging between 943.9 ± 538.6 mg/kg and 2563 ± 1817 mg/kg. Statistical analysis showed significant differences in the concentrations of Zn, Mn, Co and Na between the honeys. Selenium and Hg levels were below the limits of detection. Positive correlations were found between electrical conductivity and most of the elements. The present study showed that Serbian honey examined were of good quality according to its physicochemical parameters and met safety criteria concerning the concentrations of Cd, Hg, Pb and As.  相似文献   

3.
The species patterns of nutrient and trace metals (K, Ca, Mg, Mn, Fe, Zn) obtained by extraction of plant roots have been determined as a function of extraction pH in the range 4-9. The extractable metal concentrations were subdivided into low-molecular-weight (<10 kDa) and high-molecular-weight (>10 kDa) metal species by TXRF analysis. Except for pH 9, the low-molecular-weight fraction is predominant. This fraction was further separated by HPLC with AAS detection. It was demonstrated that the nature of the metal species changes dramatically when the extraction pH is changed, especially in the range 9-7. Information about the chemical nature of chromatographically separated metal species is obtained by use of different electrochemical detectors (amperometric detection at a glassy carbon or copper electrode and pulsed amperometric detection) and diode-array UV detection.  相似文献   

4.
This research work aimed at studying the metal content of water and tilapia fish sample, Oreochromis spp., from a wastewater-fed pond around the University of Cape Coast community using instrumental neutron activation analysis. The metals studied were Al, As, Ca, Co, Cr, Cu, Fe, K, Mg, Mn, Na, V and Zn. In the water samples the order of elemental concentrations at sampling point 1, in ??g/g, was K (75.96?±?0.92), Na (18.52?±?0.35), Al (6.00?±?0.89), Mn (3.28?±?0.44), As (3.08?±?0.40), Mg (1.56?±?0.17), Ca (0.70?±?0.08), Cu (0.54?±?0.08) and V (0.04?±?0.01). Co, Cr, Fe and Zn were below detection limits of INAA. The order of elemental concentrations in the water at point 2 was as follows: Na (4.99?±?0.14), K (4.82?±?0.89), Mn (4.40?±?0.53), Mg (2.92?±?0.37), Al (1.98?±?0.21), As (0.69?±?0.10), Ca (0.24?±?0.07) and V (0.23?±?0.06) with Co, Cr, Cu, Fe and Zn falling below the detection limit of INAA. The concentrations recorded for Al, As, Cu and Mn in the water samples were all above WHO permissible limits. The mean levels of heavy metals in the soft tissue of tilapia was of the order: K?>?Mg?>?Fe?>?Ca?>?Na?>?Al?>?Mn?>?Zn?>?V?>?Cu?>?Cr?>?Co. Arsenic was below detection limit. The transfer factor values calculated for the metals Al, Ca, K, Mg, Mn, Na and V were all greater than one indicating movement of metals from the water column to the tilapia species. The hazard index (HI) calculated for Al, Fe, Mn and V suggested possible occurrence of adverse health effects (HI?>?1) where as the HI value obtained for Cr, Cu and Zn (i.e., HI?<?1) suggested unlikely adverse effects occurring.  相似文献   

5.
In the present article, a method of operational fractionation of Mn and Zn in beer using flame atomic absorption spectrometry was developed. The proposed fractionation scheme was based on use of a hydrophobic adsorbing resin Amberlite XAD7 (first column, 2 g resin bed) connected in a series with a strong cation exchanger Dowex 50Wx4 (second column, 1 g resin bed). After passing the samples of beers through the columns, distinct groupings of Mn and Zn species retained on the sorbents, i.e., hydrophobic fraction of polyphenols bound metal species and cationic metal species fraction, respectively, were determined in respective eluates obtained after complete recovery of Mn and Zn species with 10 ml of 2.0 mol l−1 HNO3 (first column) and 10 ml of 4.0 mol l−1 HCl (second column). In addition, the effluents collected were analyzed prior to the evaluation of the third, residual fraction, presumably attributed to any hydrophilic anionic and inert metal species. The established fractionation patterns for Mn and Zn were discussed in reference to likely associations of metals with endogenous food bioligands and possible availability of the distinguished metal species classes. The quality of the results was proved by the recovery experiments.  相似文献   

6.
Honey is a sweet product made by bees using nectar from flowers. Concentrations of Ca, K, Mg, Fe, Zn, Mn, Cu, Pb and Cd were determined in 13 honey samples from the selected regions around the world. Levels of Ca, Mg, Cu, Fe, Zn and Mn were measured using flame atomic absorption spectrometry (FAAS). Potassium concentration was determined via flame photometry. Concentrations of Cd and Pb were determined using the electrothermal technique (ETAAS). It was estimated that the examined samples of honey from Greece, Turkey, Spain, Poland, Mexico, Argentina and Italy were of good quality in terms of metal concentrations (compliant with the norms referring to food products – WHO, Fifty-third Report of the joint FAO/WHO Expert Committee on Food Additives; Technical Report Series 776, Geneva), although the analysed samples were not free of heavy metals. The concentrations of the elements in the honey samples ranged from 2.38 to 9.31 μg · g?1 for Zn, from 3.86 to 35.10 μg · g?1 for Fe, from 0.19 to 21.64 μg · g?1 for Mn, from 49.53 to 1006.90 μg · g?1 for Ca, from 388.25 to 4761.50 μg · g?1 for K and from 0.20 to 1.53 μg · g?1 for Cu and regarding heavy metals from 0.11 to 2.78 μg · g?1 for Pb and from 0.02 to 0.44 μg · g?1 for Cd. According to these results it was found that the concentrations of heavy metals in the honey samples (except for alfalfa honey and eucalyptus honey from Italy) were under the acceptable limits for foods set out by the FAO/WHO. It was confirmed that the application of chemometric tools supports the extraction of significant information from analytical data, even though the availability of samples is not fully sufficient (this problem is often encountered in environmental analyses).  相似文献   

7.
In addition to color, ash and electrical conductivity (EC), the levels of 14 minerals were investigated in 23 varieties of honey from Saudi Arabia and six other countries. The quantities of the macrominerals obtained were as follows (in ppm): K (298.60–491.40), Mg (80.70–199.30), Ca (60.75–99.95), P (21.10–33.29), and Na (15.69–26.93). The quantities of trace minerals were as follows (in ppm): Fe (67.18–98.13), I (12.61–94.68), Mn (4.15–6.04), Zn (3.44–5.72), Li (1.15–4.26), Co (1.00–1.32), and Ni (0.15–0.67). The quantities of the heavy metals Pb and Cd were found to be 0.06–0.23 and 0.00–0.16, respectively. The values of the tested elements—color, ash and EC—varied among the tested honeys according to their botanical origin. Dark honeys, especially acacia honeys, had higher elemental content and EC values than lighter ones. Saudi and Yemeni seder honeys exhibited no distinctive characteristics in their tested parameters. The levels of heavy metals indicated that the tested honeys were safe for human consumption.  相似文献   

8.
The possible adverse effect of competitive binding on DGT (diffusive gradients in thin films) measurements of metals in marine situations was investigated. Of the divalent transition metals, manganese binds most weakly to Chelex resin and is most likely to be affected by competition. In media resembling seawater, the Chelex within DGT devices becomes saturated with Ca and Mg within 2 h, and at pH 5–6 the sensitivity of the DGT measurement for Mn is substantially reduced, due to the appreciable concentration of Mn in contact with the resin. For media resembling freshwater DGT gives a near theoretical response for Mn. Iron was shown to be capable of displacing Mn and to a more limited extent Cd from the resin when its capacity for Fe is approached. Vertical profiles of Mn in a mesocosm sediment, obtained by deploying DGT for different times, could be explained by this displacement effect. The problem only occurs when Fe concentrations are exceptionally high and can be avoided by using short deployment times, typically less than 12 h. Whilst most trace metals can be simply measured by deploying DGT in marine systems, for Mn consideration should be given to possible effects associated with the capacity of the Chelex binding layer being approached by accumulation of the other cations present.  相似文献   

9.
《Analytical letters》2012,45(9):1615-1622
Abstract

A simple and rapid method for the simultaneous determination of seven trace elements in biodiesel by axial and radial view Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES) is proposed, in which the sample is emulsified with Triton X-100 and water, and in which yttrium is employed as an internal standard. The better obtained quantification limits (10 s) were by axial view, 0.165, 0.099, 0.033, 0.007, 0.016, 0.132, 0.660 µg g?1 for Ca, Cu, Fe, Mg, Mn, Na, and P, respectively, based on a sample mass of 1.0 g diluted to a final mass of 10 g in the analytical solution. Calibration was carried out with aqueous standards, thus avoiding the use of frequently instable organic standards. Elemental recoveries were in the range of 90 to 109% for all seven analytes studied, and also the precision of the method was satisfactory (RSD < 8%).  相似文献   

10.
The distribution patterns and the organ-specific accumulation trends of 10 trace metals (iron, manganese, zinc, copper, chromium, nickel, cobalt, lead, cadmium and silver) and 4 major elements (sodium, potassium, calcium and magnesium) in 10 different tissues (heart, muscle, kidney, stomach, intestine, liver, gill, gonads, white skin and dark skin) of a benthic fish species (Solea senegalensis) from a densely populated coastal area affected by anthropogenic activities, the Bay of Cadiz (SW Spain), have been investigated. High variability of metal concentrations among tissues were found for Ca, Fe, Zn, Cu, Pb and Ag. Factor analysis was applied to study this variability. Five principal components were found explaining the 92.95% of the total variance and similarities in behavioural patterns of bioaccumulation were described. They associated Mg, Cr, Ni and Mn to intestine and stomach tissues (PC1), Ag, Cu and Cd to liver (PC2), Zn, K and Co to gonads (PC3), Na, Fe and Pb to gill, heart and kidney tissues (PC4) and Ca, Pb and Mn to gill and dark skin (PC5). The metallic concentration in the sediment and water was also studied. The pollution in this area was found moderate with outstanding values of Zn, Cu and Pb (average values of 139, 50.4 and 75.6?mg?kg?1, respectively) in sediment and dissolved Cu (average value of 2.5?µg?L?1). Metal bioconcentration trends followed the order Zn?>?Cu?>?Cd?>?Pb for dissolved metals in seawater, Cu?>?Zn?>?Cd?>?Pb?≈?Mn?>?Fe?≈?Ni?≈?Co for metals associated to particulate matter and Zn?≈?Cu?>?Cd?>?Mn?>?Co?≈?Fe?>?Ni?≈?Pb?>?Cr for metals in the sediment. Higher values were found for copper in liver, zinc in gonads and lead in gill, showing the relationship between biotic and abiotic environment. In addition, Cd bioconcentration factors were found high in liver and gill showing the sensitivity of sole to this metal even at low concentrations.  相似文献   

11.

Background

The characterization of three types of Marche (Italy) honeys (Acacia, Multifloral, Honeydew) was carried out on the basis of the their quality parameters (pH, sugar content, humidity) and mineral content (Na, K, Ca, Mg, Cu, Fe, and Mn). Pattern recognition methods such as principal components analysis (PCA) and linear discriminant analysis (LDA) were performed in order to classify honey samples whose botanical origins were different, and identify the most discriminant parameters. Lastly, using ANOVA and correlations for all parameters, significant differences between diverse types of honey were examined.

Results

Most of the samples' water content showed good maturity (98%) whilst pH values were in the range 3.50 – 4.21 confirming the good quality of the honeys analysed. Potassium was quantitatively the most relevant mineral (mean = 643 ppm), accounting for 79% of the total mineral content. The Ca, Na and Mg contents account for 14, 3 and 3% of the total mineral content respectively, while other minerals (Cu, Mn, Fe) were present at very low levels. PCA explained 75% or more of the variance with the first two PC variables. The variables with higher discrimination power according to the multivariate statistical procedure were Mg and pH. On the other hand, all samples of acacia and honeydew, and more than 90% of samples of multifloral type have been correctly classified using the LDA. ANOVA shows significant differences between diverse floral origins for all variables except sugar, moisture and Fe.

Conclusion

In general, the analytical results obtained for the Marche honeys indicate the products' high quality. The determination of physicochemical parameters and mineral content in combination with modern statistical techniques can be a useful tool for honey classification.  相似文献   

12.
Duolite GT-73 resin was used for the preconcentration of Hg(II) from hydrochloric acid media as well as separation of the analyte from diversity of the co-existing metal ions (Al, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Ni, Pb and Zn) in off-line column operation. Due to the high affinity of the resin to the transition metals, Hg was adsorbed alongside with the foreign metals investigated. A complete release of the concomitant metals from the resin without the desorption of Hg was carried out using solutions of HCl and HNO3. A quantitative recovery of Hg was obtained by digestion of the resin using a H2SO4 and H2O2 mixture in an open-vessel system. An enrichment factor of 40 was achieved. The devised procedure was applied for the determination of Hg(II) in tap-water samples.  相似文献   

13.
Measurements of the major cations Ca and Mg by the technique of diffusive gradients in thin films (DGTs) were systematically evaluated. The concentration in solution was calculated using Fick’s first law of diffusion from the directly measured flux to the DGT device. A selective cation exchange resin (Bio-Rad Chelex®100), which has been used extensively with DGT for trace metals, such as Cd2+, Cu2+ and Ni2+, was used for this work.

Elution of Ca and Mg from the resin with 1 M HNO3 was very reproducible. Measurements of Ca and Mg concentrations in synthetic solutions agreed well with the theoretical predictions. The negative response on uptake caused by lowered pH was investigated. Uptake was found to decline below pH 5. The capacity of the DGT device for Ca and Mg was also investigated to establish maximum deployment times for given concentrations.

Experiments with filtered and modified lake water show that DGT can be used to measure Ca and Mg when trace metals are present in the solution. An in situ deployment of DGT combined with an ultrafiltration study suggest that the Mg concentration measured by DGT is similar to the concentration found in the fraction <1 kDa.  相似文献   


14.
Rosa AH  Rocha JC  Burba P 《Talanta》2002,58(5):969-978
The binding and availability of metals (Al, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Zn) in therapeutically applied peat (Grosses Gifhorner Moor, Sassenburg/North Germany) was characterized by means of a versatile extraction approach. Aqueous extracts of peat were obtained by a standardized batch equilibrium procedure using high-purity water (pH 4.5 and 5.0), 0.01 mol l(-1) calcium chloride solution, 0.01 mol l(-1) ethylenediaminetetraacetic acid (EDTA) and 0.01 mol l(-1) diethylenetriamine pentaacetic acid (DTPA) solution as metal extractants. In addition, the availability of peat-bound metal species was kinetically studied by collecting aliquots of extracts after different periods of extraction time (5, 10, 15, 30, 60 and 120 min). Metal determinations were performed by atomic spectrometry methods (AAS, ICP-OES) and dissolved organic matter (DOM) was characterized by UV/Vis measurements at 254 and 436 nm, respectively. Of the extractants studied Ca, Mg and Mn were the most available metals, in contrast to peat-bound Fe and Al. The relative standard deviation s(r) of the developed extraction procedures was mostly in the range of 4 to 20%, depending on the metal and its concentration in peat. A pH increase favored the extraction of metals and DOM from peat revealing complex extraction kinetics. Moreover, a competitive exchange between peat-bound metal species and added Cu(II) ions showed that >100 mg of Cu(II) per 50 g wet peat was necessary to exchange the maximum of bound metals (e.g. 21.8% of Al, 3.9% of Fe, 79.0% of Mn, 81.9% of Sr, related to their total content).  相似文献   

15.
A flow-injection system is developed for Cu, Mn and Zn partitioning in seawater by flame atomic absorption spectrometry. The first approach is where the trace metal species are fractionated in situ, but analysis is performed by using a flow injection manifold in the laboratory. This operational mode is used for the determination of the dissolved labile metallic fraction and is based on the elution of this fraction from a minicolumn packed with a chelating resin containing iminodiacetic acid groups (Serdolit Chelite Che) loaded in situ with the sample. The second is used for the determination of total dissolved concentrations of trace metals. This last mode is based on the retention/preconcentration of total dissolved metals on the chelating resin after on-line sonolysis of seawater samples acidified with diluted nitric acid to breakdown the metal-organic matter complexes. The figures of merit for Cu, Mn and Zn determinations in both fractions are given and the obtained values are discussed. The fractionation scheme is applied to the analysis of coastal seawater samples collected in Galicia (Northwest, Spain). The results of fractionation showed that Mn and Zn are mainly in the labile fraction, while Cu was mainly present in the organic fraction.  相似文献   

16.
Atmospheric bulk deposition of major and trace elements was measured at Venice from November 1995 to October 1997. Collection was carried out using polyethylene bulk passive samplers, samples being collected bi-weekly. In order to highlight the contribution of the atmosphere to water chemistry and particle budgets in the Lagoon of Venice, the geochemical composition (Si, Al, Ca, Mg, K, Na, Mn, Cr, Zn, Pb, Cd, Cu, As) of dissolved and insoluble bulk fractions was determined by AAS + ICP mass spectrometry. Great sample variability was found, with almost two orders of magnitude between maximum and minimum values for several metals. All fluxes in 1995/96 were 30% lower than in 1996/97, ranging from -3% (Ca) to -57% (Li), except for Zn, Cd and As. On the contrary, the solubility of all elements decreased during 1996/97. Partitioning between soluble and insoluble phases shows that Al, Cr, Fe and Si are mainly in the insoluble form, whereas for As, Ca, Cu, Mg, Na, Ni, K, Pb and Zn the dissolved fraction represents 50-90% of total input. The amount of particle load affects partitioning between dissolved and particulate, especially for Al and Pb. Seasonal variability was evident. The lowest pH values (approximately 5.2) were recorded in winter, causing an increase of solubility for all metals except for As, which showed the highest solubility in summer.  相似文献   

17.
An ICP-OES procedure was developed for fast and accurate determination of various crustal (Al, Ca, Fe, Mg, Si) and trace elements (Ba, Cu, Mn, Na, K, Sr, Ti, Zn) in airborne particulate matter. The method is based on a preliminary treatment of the aerosol samples with a mixture of nitric acid and hydrogen peroxide at elevated temperature leading to a mineralization of the organic sampling substrate, dissolution of soluble material and homogeneous suspension of the remaining non-soluble fraction. After dilution the derived slurry solutions were measured using ICP-OES. The reproducibility of analysis given as the relative standard deviation (% RSD) varied between 3.2 and 6.8% for bulk constituents such as Al, Ca, Fe, Mg and Si whereas values ranging from 3.5 to 9.1% were obtained for trace metals present with distinctly lower abundance in PM10 (e.g. Ba, Cu, Mn, Sr, Zn). The limits of detection (LOD) calculated as three times the standard deviation (3σ) of the signal derived from filter blank samples ranged from approximately 1?ng?m?3 (Sr) to 71?ng?m?3(Ca). The developed procedure was evaluated by comparing the obtained results with the findings derived for the same set of aerosol samples analyzed using a microwave procedure for sample dissolution with subsequent ICP-OES analysis. Finally the developed procedure was applied for the analysis of crustal and trace elements in PM10 samples collected at an urban site (Getreidemarkt, Vienna) and a rural site (Hartberg, Styria), in Austria. The concentrations of the investigated crustal elements varied between some hundred ng?m?3 and few µg?m?3 with highest concentrations for Fe and Si, distinctly reduced concentrations ranging from some ng?m?3 (Sr) to more than hundred ng?m?3 (K) were found for trace elements. Observed PM10 concentrations were found to be in accordance to literature findings from urban sites in central Europe.  相似文献   

18.
P. Pohl  B. Prusisz 《Talanta》2007,71(1):411-418
A simple and versatile protocol, based on use of solid phase extraction on strong ion exchangers and off-line detection by flame atomic absorption spectrometry, was devised to fractionate iron and zinc in common dietary food and beverages products, i.e., bee honeys, fruit juices and tea infusions. In the procedure proposed, cation exchanger Dowex 50Wx4 and anion exchanger Dowex 1x4 were used separately for distinguishing broadly meant the cationic metal fraction and the fraction of stable anionic metal complexes, respectively, after retention of metal species and their exhaustive elution by means of a 4.0 mol l−1 HCl solution. The third fraction, referred to the residual metal species, was retrieved by difference between total soluble metal contents and sum of metal quantities in separated cationic and anionic fractions. The fractionation pattern observed for both metals was described and discussed.  相似文献   

19.
The chromatographic separation of Mg, Ca, Sr, Ba, Fe(II, III) and Mn(II) by elution with ammonium sulphate solution from Dowex 50–X10 was studied. The optimum conditions for the separation of the alkaline earths from each other were established. The method was applied for the separation of Mg, Ca and Sr in salt waters; Mg and Ca were determined by EDTA titration and Sr spectrographically, the coefficient of variation being 1.9% for Mg and 1.4% for Ca.  相似文献   

20.
Humic-rich hydrocolloids and their metal loading in selected German bog-waters have been characterized by a novel on-site approach. By use of an on-line multistage ultrafiltration (MST-UF) unit equipped with conventional polyethersulfone (PES)-based flat membranes (nominal cut-off 0.45, 0.22, and 0.1 microm, or 100, 50, 10, 5, 3 kDa) the hydrocolloids could be fractionated on-site in both sub-particulate and macromolecular size ranges. Characterization (dissolved organic carbon (DOC), metals) of the colloid fractions obtained this way was performed off-site by use of conventional instrumental methods (carbon analyzer, AAS, ICP-OES, and TXRF (total reflection X-ray fluorescence)). Major DOC fractions of the hydrocolloids studied were found to be in the size range <5 kDa. The assessed metals (Al, Cu, Fe, Mn, Pb, and Zn) were, however, predominantly enriched in the macromolecular and sub-particulate range, depending on the metal and the sample, respectively. In addition, metal species bound to these hydrocolloids were kinetically characterized on-site by use of competitive ligand (EDTA (ethylenediaminetetraacetate)) and metal (Cu(II)) exchange; the EDTA complexes formed and the metal ions exchanged were separated by means of a small time-controlled tangential-flow UF unit (cut-off 1 kDa). Bound metal fractions, in particular Al and Fe, reacted only slowly (500 to 1000 min) with EDTA; the conditional availability was 60-99%, depending on the hydrocolloid. In contrast, the Cu(II) exchange of colloid-bound metal species approached equilibrium within 5-10 min, with characteristic exchange constants, Kex, of the order of 0.01 to 90 for the metals (Fe相似文献   

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