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By using an ICP optical emission spectrometer having two different observation modes, the authors compared the spectrochemical characteristics of various emission lines as viewed from the axial direction and the direction radial to the long axis of the plasma. The excitation temperature, the emission intensity, and the degree of ionization were investigated when iron and chromium were employed as the test sample and further potassium was added as an interfering element. These observations could lead to a similar conclusion that the emission intensities from the axial direction were more easily affected by the potassium addition. The reason for this effect is probably because the portion of the plasma observed from the axial direction includes the tail zone which is apart from the induction zone and thus has lower temperatures. On the other hand, in the radial observation, one can observe the emission intensities from a narrow portion of the plasma just above the load coil. The axial observation mode gave better analytical performance, including a lower detection limit as well as a better signal-to-background ratio, compared to the radial observation mode. However, interferences from co-existing elements should be noted if the axial observation is employed in practical applications.
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PMID:Comparative studies of spectrochemical characteristics between axial and radial observations in inductively coupled plasma optical emission spectrometry. 1651 16

Personal and area samples for airborne lead were taken at a lead mine concentrator mill, and at a lead-acid battery recycler. Lead is mined as its sulfidic ore, galena, which is often associated with zinc and silver. The ore typically is concentrated, and partially separated, on site by crushing and differential froth flotation of the ore minerals before being sent to a primary smelter. Besides lead, zinc and iron are also present in the airborne dusts, together with insignificant levels of copper and silver, and, in one area, manganese. The disposal of used lead-acid batteries presents environmental issues, and is also a waste of recoverable materials. Recycling operations allow for the recovery of lead, which can then be sold back to battery manufacturers to form a closed loop. At the recycling facility lead is the chief airborne metal, together with minor antimony and tin, but several other metals are generally present in much smaller quantities, including copper, chromium, manganese and cadmium. Samplers used in these studies included the closed-face 37 mm filter cassette (the current US standard method for lead sampling), the 37 mm GSP or "cone" sampler, the 25 mm Institute of Occupational Medicine (IOM) inhalable sampler, the 25 mm Button sampler, and the open-face 25 mm cassette. Mixed cellulose-ester filters were used in all samplers. The filters were analyzed after sampling for their content of the various metals, particularly lead, that could be analyzed by the specific portable X-ray fluorescence (XRF) analyzer under study, and then were extracted with acid and analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES). The 25 mm filters were analyzed using a single XRF reading, while three readings on different parts of the filter were taken from the 37 mm filters. For lead at the mine concentrate mill, all five samplers gave good correlations (r2 > 0.96) between the two analytical methods over the entire range of found lead mass, which encompassed the permissible exposure limit of 150 mg m(-3) enforced in the USA by the Mine Safety and Health Administration (MSHA). Linear regression on the results from most samplers gave almost 1 ratio 1 correlations without additional correction, indicating an absence of matrix effects from the presence of iron and zinc in the samples. An approximately 10% negative bias was found for the slope of the Button sampler regression, in line with other studies, but it did not significantly affect the accuracy as all XRF results from this sampler were within 20% of the corresponding ICP values. As in previous studies, the best results were obtained with the GSP sampler using the average of three readings, with all XRF results within 20% of the corresponding ICP values and a slope close to 1 (0.99). Greater than 95% of XRF results were within 20% of the corresponding ICP values for the closed-face 37 mm cassette using the OSHA algorithm, and the IOM sampler using a sample area of 3.46 cm2. As in previous studies, considerable material was found on the interior walls of all samplers that possess an internal surface for deposition, at approximately the same proportion for all samplers. At the lead-acid battery recycler all five samplers in their optimal configurations gave good correlations (r2 > 0.92) between the two analytical methods over the entire range of found lead mass, which included the permissible exposure limit enforced in the USA by the Occupational Safety and Health Administration (OSHA). Linear regression on the results from most samplers gave almost 1 ratio 1 correlations (except for the Button sampler), indicating an absence of matrix effects from the presence of the smaller quantities of the other metals in the samples. A negative bias was found for the slope of the button sampler regression, in line with other studies. Even though very high concentrations of lead were encountered (up to almost 6 mg m(-3)) no saturation of the detector was observed. Most samplers performed well, with >90% of XRF results within +/- 25% of the corresponding ICP results for the optimum configurations. The OSHA algorithm for the CFC worked best without including the back-up pad with the filter.
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PMID:A comparison of portable XRF and ICP-OES analysis for lead on air filter samples from a lead ore concentrator mill and a lead-acid battery recycler. 1652 23

A flow-through hyphenated analytical method has been tested that enables not only the accelerated and efficient fractionation of trace elements (TE) species in environmental solids to be achieved but allows real-time studies on the leaching process to be made. Rotating coiled columns (RCC), earlier used mainly in countercurrent chromatography, have been successfully applied to the dynamic fractionation of heavy metals in soil, sediment, and sludge samples. A ground solid sample (about 0.5 g) was retained in a PTFE rotating column as the stationary phase whereas different aqueous eluents, chosen according to recent data on the selectivity of leachants, were continuously pumped through. Elements were determined in the effluent on-line by inductively coupled plasma atomic emission spectrometry (ICP-AES). Since the flow rates used in the RCC are in good agreement with those needed for cross-flow nebulization in the ICP-AES spectrometer, both devices were coupled directly without any additional interface systems. Simultaneous investigation of the elution profiles of trace and major elements has made it possible to study the elements association in separated fractions and hence to prove the efficacy of extractants and their selectivity toward targeted mineralogical phases of samples. The close association of heavy metals with Mn oxides in the sediment and sludge samples was confirmed. The time-resolved dissolution of different organic complexes of metals was observed for the sediment sample. It was found that in sediment and sludge samples the dynamics of iron release under the action of Tamm's reagent is somewhat different from that of aluminium. In addition, the proposed method can also be applied to develop effective leaching schemes and in the analysis of environmental solids for risk assessment of their contaminants addressed to water quality and bioavailability.
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PMID:A hyphenated flow-through analytical system for the study of the mobility and fractionation of trace and major elements in environmental solid samples. 1656 67

Purple acid phosphatases (PAPs) from sweet potato (sp) have been classified on the basis of their primary structure and the dinuclear metal center into isoforms spPAP1 [Fe(III)-Zn(II)] and spPAP2 [Fe(III)-Mn(II)]; for spPAP3 only the cDNA is known. With the aim of unraveling the character of the dinuclear metal center we report here the characterization of this isoform at the protein level. We cloned spPAP3 cDNA in a baculovirus and overexpressed this enzyme in Sf9 insect cells. Preparation of recombinant spPAP3 in two steps afforded pure enzyme with yields of 4.5 mg.L(-1) culture medium. This enzyme is a dimeric, disulfide-linked PAP of 110 kDa, similar to known PAP isoforms from higher plants. Enzymatic studies and spectroscopic properties (max. absorption at 550-565 nm) indicated a diiron enzyme; quantitative and semiquantitative metal analysis using ICP-OES and TOF-SIMS, respectively, revealed the presence of only iron in purified spPAP3. Metal replacement in the second metal-binding site upon preparation of the semiapo-enzyme with Fe(II), Zn(II), or Mn(II) showed highest activities with Fe(II). The data show that recombinant spPAP3 has a diiron metal center. Site-directed mutagenesis was conducted to check catalytic efficiency at the atomic level. Tyr291 at the substrate-binding site in spPAP3 was mutated to His and Ala, the respective residues found in spPAP1 and spPAP2. Kinetic analysis showed that conversion of Tyr291 to His further optimized the performance of this protein as a diiron enzyme, whereas the Ala mutation weakened the catalytic efficiency regardless of the metal present in the second binding site.
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PMID:Recombinant purple acid phosphatase isoform 3 from sweet potato is an enzyme with a diiron metal center. 1662 2

Food fortification is an interesting strategy to treat and prevent iron anemia. This study aims to quantify the iron in yoghurt, with gelatin and sugar and without, prepared in iron and glass containers. Sensorial test was use to evaluate the acceptance and preference of the both products. The yoghurt was prepared in containers of iron and glass with UHT milk, powder milk and natural industrialized yoghurt. After fermentation, half of the product received addition of sugar and strawberry flavor gelatin. The collected samples get the total iron quantified by ICP OES. Sensorial analysis involving 105 consumers was use to determine the acceptance and preference of the products. 0,018 and 0,882mg of iron per 100g added in the natural yoghurt prepared in the glass and in the iron pots, respectively. The yoghurt with gelatin presented 0,037 and 1,302mg of iron per 100g when prepared in the glass and in the iron pots, respectively. The preference was low for the yoghurt prepared in the iron pot (29,5%), but when added strawberry gelatin it was about 51,5%. The yoghurt prepared in iron pots, is easily home made and adds important amount of iron. Add gelatin and sugar can favored its consumption.
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PMID:[Iron concentration and acceptation of yoghurt prepared in casting iron pots (iron migration and acceptation of yogurt)]. 1664 Feb

Flow field flow fractionation (FIFFF), inductively coupled plasma-mass spectroscopy (ICP-MS), and transmission electron microscopy (TEM) coupled to X-ray energy dispersive spectrometry (X-EDS) are used in series for the first time to characterize colloids. Results demonstrate the utility of FIFFF-ICP-MS-TEM/X-EDS to relate physical properties (size) of colloids to their chemical properties (chemical composition, surface chemical composition, and colloids-trace elements association). Results suggest that the major part of natural organic matter (NOM) is concentrated in the fraction < 0.01 microm (C2). Aluminum, iron, and manganese are the main colloidal components in the fraction 0.01-0.45 microm (C1). Aluminum occurs as aluminum oxides or aluminosilicates in the whole size range, while iron and manganese occur as individual oxyhydroxides in the size range < 0.20 microm. Within the C2 fraction, Al, Mn, Cu, and Ni elements are complexed to NOM (e.g., humic substances). Iron is complexed to NOM in some samples and probably free in other samples. Lead is totally free in all samples. Within the C1 fraction, Cu and Pb are mostly associated to Fe and Mn oxyhydroxides. Consequently, NOM with Fe and Mn oxyhydroxides are the main colloidal carriers of trace elements in the Loire watershed system.
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PMID:Size-based speciation of natural colloidal particles by flow field flow fractionation, inductively coupled plasma-mass spectroscopy, and transmission electron microscopy/X-ray energy dispersive spectroscopy: colloids-trace element interaction. 1664 47

The Qaraaoun Reservoir (impoundment of the River Litani) is the only artificial surface water body in the country, Lebanon. Earlier study on the water quality of the Qaraaoun Reservoir identified three water quality zoning with a central distinct zone suitable for multipurpose water usage. The objective of this study was to extend the earlier work by considering the total metal content of reservoir bed sediments and hence to evaluate factors that control metal deposition or capture. Water samples were collected from 15 sampling sites and sediment samples were simultaneously collected from 9 sites. Water parameters analyzed were pH, Eh, DO and temperature. Sediment samples were dried and sieved and sediment < 75 microm was retained for analysis. Sediments were subjected to a stepwise heating process with aqua regia to extract the metals, and their content in sediments determined by ICP-MS. The sediment data revealed higher metal contents where the river entered the reservoir which matched higher concentrations of water parameters at the influx site. Regression analysis of total metals in sediments with distance from the river Litani influx point to the dam revealed a log trend for Fe, Cr and Ni, whereas, the concentrations of Cu, Zn, Cd, Pb were better described by a polynomial regression. Three sediment zones were identified: entrance, oxidation (central) and reducing (near dam) zones. Sediment contents of Zn, Cu and Pb correlated with organic content, whereas sediment Cr and Ni were associated with iron. It was concluded that sediments act as a sink for metals and the deposition of metals is primarily related to sediment organic content and the level of dissolved oxygen in water.
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PMID:Variation of metals in bed sediments of Qaraaoun Reservoir, Lebanon. 1664 37

The distribution of aqueous Tl(I)/Tl(III) as a function of light exposure and solution properties was studied by quantifying the oxidation states after separation with ion chromatography and on-line detection with ICP-MS. Ultraviolet irradiation of aqueous solutions containing 1 microg l(-1) Tl(III) and in equilibrium with the atmosphere increases the reduction rate. In systems with photoreduction of Fe(III)(aq) a quantitative oxidation of Tl(I)(aq) was observed, notably at low pH. The process is reversible, as indicated by formation of Tl(I) when the irradiated systems were kept in the dark. In systems with colloidal silica-stabilised ferrihydrite, UV irradiation also leads to oxidation of Tl(I)(aq), but not quantitatively. It is suggested that adsorption of thallium to the ferrihydrite determines the rate of oxidation. Detectable, but not quantitative, oxidation of Tl(I)(aq) took place when natural water samples with 1 microg l(-1) Tl(I)(aq) were exposed to either sunlight or UV-light. For these samples, the reduction was not quantitative when they were kept in the dark for 24 h. The results suggest that the light dependent iron cycle in fresh water systems strongly influences the redox state of thallium.
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PMID:The effect of light and iron(II)/iron(III) on the distribution of Tl(I)/Tl(III) in fresh water systems. 1676 31

We assessed the use of anodic stripping voltammetry (ASV) for in-situ determinations of both total concentration and speciation of dissolved heavy metals (Cd, Cu, Pb and Zn) in acid mine drainage (AMD). In the Kwangyang Au-Ag mine area of South Korea, different sites with varying water chemistry within an AMD were studied with a field portable anodic stripping voltammeter. Anodic stripping voltammetry after wet oxidation (acidification) was very sensitive enough to determine total concentration of dissolved Cd because Cd was dominantly present as 'labile' species, whilst the technique was not so effective for determining total Cu especially in the downstream sites from the retention pond, due to its complexation with organic matter. For dissolved Pb, the concentrations determined by ASV after wet oxidation generally agreed with those by ICP-AES. In the downstream samples (pH>5), however, ASV data after wet oxidation were lower than ICP-AES data because a significant fraction of dissolved Pb was present in those samples as 'inert' species associated with colloidal iron oxide particles. The determination of total dissolved Zn by ASV after wet oxidation appeared to be unsatisfactory for the samples with high Cu content, possibly due to the interference by the formation of Zn-Cu intermetallic compounds on the mercury coated electrode. In AMD samples with high dissolved iron, use of ultraviolet irradiation was not effective for determining total concentrations because humate destruction by UV irradiation possibly resulted in the removal of a part of dissolved heavy metals from waters through the precipitation of iron hydroxides.
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PMID:In-situ electrochemical measurements of total concentration and speciation of heavy metals in acid mine drainage (AMD): assessment of the use of anodic stripping voltammetry. 1676 66

Efficiencies of He/NH3 and He/H2 collision gases were compared in a conventional type of hexapole cell of an inductively coupled plasma mass spectrometer (ICP-MS). The optimum conditions [hexapole and quadrupole bias voltage (V(H) and V(Q)) and collision/reaction gas flow rates] were tested for vanadium determination (51V) in chloride matrices. When the He/H2 mixture was used, the optimum values of V(H) and V(Q) were -10.0 and -8.0 V, respectively. This set-up corresponds to the kinetic energy discrimination effect. When the He/NH3 mixture was used, the optimum values of V(H) and V(Q) were +10.0 and -7.0 V, respectively. Positive V(H) values correspond to the ion kinetic energy effect, which allows the reactivity of the ions entering the collision/reaction cell with the reaction gas to be controlled. The obtained results showed that the He/H2 mixture is not optimal for V determination in samples containing chlorides due to the insufficient suppression of the polyatomic interference of 35Cl16O+. Data obtained from vanadium determination using the He/NH3 mixture were consistent for all selected Cl- concentrations, and the results were acceptable. The detection limit was comparable with detection limits obtained from ICP-MS equipped with a dynamic reaction cell. Analyses of elements forming interfering molecules, e.g., iron (56Fe), arsenic (75As) and selenium (80Se), were in good agreement with the certified values for both studied collision/reaction gas mixtures.
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PMID:Vanadium determination in chloride matrices using ICP-MS: finding the optimum collision/reaction cell parameters for suppressing polyatomic interferences. 1679 79


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