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Inductively coupled plasma mass spectrometry (ICP-MS) offers excellent detection limits and isotopic analysis of Ni in aqueous standards, but is prone to interferences--mainly from Ca-containing polyatomics--when biological matrices are analyzed for Ni. We have used multivariate calibration with principal components analysis (PCA) to correct for mass overlaps in serum digests. The resulting detection limit for Ni is below 1 microgram/l and the within-run imprecision is 6% at 1.46 micrograms Ni/l. In urine, the higher Ca content renders routine application of PCA problematic. We evaluated several methods of pre-concentration, and have developed a method of Ca oxalate precipitation that allows direct analysis of Ni in the diluted supernatant. The stable isotope 62Ni and the radiosotope 63Ni were co-administered i.v. to rats and the serum and urinary clearances were determined by liquid scintillation counting and ICP-MS. Ni measurements by both methods were in excellent agreement, and serum clearance fit a double exponential decay consistent with the two-compartment model of Onkelinx et al. [24]. A human volunteer ingested 61Ni (20 micrograms Ni/kg body wt.) in water after an overnight fast. Identical serum levels, peaking near 35 micrograms/l at 2 h, were measured by electrothermal atomic absorption spectrometry and ICP-MS with PCA. Urinary excretion of 61Ni measured by ICP-MS demonstrated absorption of 30% of the administered dose. We conclude that Ni isotopes can be measured in body fluids by ICP-MS at levels that allow stable isotope tracer studies in humans.
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PMID:Isotope-specific analysis of Ni by ICP-MS: applications of stable isotope tracers to biokinetic studies. 802

Aluminium speciation was studied in forest soil extracts by size exclusion chromatography (SE) with UV and inductively coupled plasma-atomic emission spectrometric (ICP-AES) detection and cation exchange fast protein liquid chromatography (FPLC) with ETAAS detection. Size exclusion chromatography was performed on a Superdex HR75 10/30 column. Isocratic clution with 0.15 mol dm(-3) NaCl in TRIS-HCl buffer (pH = 5.5) was applied over 100 min at a flow rate of 0.35 cm(3) min(-1). The chromatographic run was followed at 278 nm and separated Al species also determined 'off line' in 0.875 cm3 fractions by ICP-AES. The analytical procedure enabled speciation of high molecular weight Al complexes. Cation exchange FPLC was performed on a Mono S HR 5/5 column. Aqueous 8 mol dm(-3) NH4NO3 linear gradient elution was applied over 10 min at a flow rate of 1 cm3 min(-1). Separated Al species were collected in 0.5 cm3 fractions and Al determined 'off line' by ETAAS. The analytical procedure enabled speciation of some positively charged monomeric Al species. Negatively charged species were eluted with the solvent front. The combination of the two analytical techniques was successfully employed in speciation of Al in forest soil extracts. Water was used as an extracting solution. It was found experimentally that 80-95% of Al in aqueous extracts of forest soils exists in monomeric Al forms. Water soluble Al (30-40%) is bound to high molecular weight complexes with humic substances. The remaining monomeric Al in the low molecular weight fraction exists as AIF2+, Al-oxalate and Al-citrate species.
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PMID:Speciation of aluminium in forest soil extracts by size exclusion chromatography with UV and ICP-AES detection and cation exchange fast protein liquid chromatography with ETAAS detection. 1100 89

A method to separate and quantify two inorganic arsenic species As(III) and As(V) and two organic arsenic species, monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA), by HPLC-ICP/MS has been developed. The separation of arsenic species was achieved on the anionic exchange column IonPac AS11 (Dionex) with NaOH as mobile phase. The technique was successfully applied to analyze extracts of two contaminated soils, sampled at a former tannery site (soil 1) and a former paint production site (soil 2). The soils were extracted at pH values similar to the natural environment. Extractions were performed at different pH values with 0.3 M ammonium oxalate (pH = 3), milli-Q water (pH = 5.8), 0.3 M sodium carbonate (pH = 8) and 0.3 M sodium bicarbonate (pH = 11). No organically bound arsenic was found in the extracts. As(V) was the major component. Only up to 0.04% of the total arsenic contained in soil 1 were mobilized. The highest amount of extracted arsenic was found at the highest pH. In the milli-Q water extract of soil 1 As(III) and As(V) were found. High amounts of As(V) were found in the extracts of soil 2. Up to 20% of the total arsenic bound to soil 2 constituents were released. The results show that the mobilization of arsenic depended on the pH value of the extraction solution and the kind of extracted soil. Dramatic consequences have to be expected for pH changes in the environment especially in cases where soils contain high amounts of mobile arsenic.
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PMID:Speciation of As(III), As(V), MMA and DMA in contaminated soil extracts by HPLC-ICP/MS. 1122 33

Soils are biogeochemical systems under continual modification by biological and chemical processes. Trace element solid-solution partitioning is thus influenced by long-term changes to these solid phases. We study Pb, Cd, Zn, and Cu solution speciation and solid-phase dynamics in two soils of volcanic origin (Te Akatea and Egmont, high in noncrystalline aluminosilicates), an oxisol from Brazil (Oxisol, high in oxides of Al and Fe), and several sludge-treated soils (labeled NYS soils, high in organic materials). Total soluble (by ICP) and labile (by ASV) concentrations of Pb, Cd, Zn, and Cu were determined after incubation of the soils for about 1.5 yr at room (23 degrees C) and elevated (70 degrees C) temperatures. Changes occurring to the solid phases were monitored by FTIR and extraction with oxalate and pyrophosphate. It is shown that induced hydrolysis or decomposition of organic materials in soils results in increases in both labile and total soluble concentrations of Pb, Cd, Cu, and Zn in solution. Labile and total soluble concentrations of Cu and Zn increase concomitantly with dissolved organic carbon (DOC); the nonlabile soluble fraction also increases with increasing DOC. Similarly, the concentration of Cd and Pb in solution increases with increasing DOC; however, most soluble Cd and Pb is asv-labile. Only in the Egmont soil (mineralogy dominated by proto-imogolite allophane) was reduced Pb solubility observed after prolonged equilibration and heating. Lead solubility increased after partial crystallization of amorphous minerals in the Te Akatea and the Oxisol. Thus, for most of the metal-soil systems studied, prolonged thermal treatment at 70 degrees C increased total soluble and asv-labile metals, suggesting that aging effects on metals in contaminated soils could release metals to labile forms in some cases.
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PMID:Thermally induced changes in metal solubility of contaminated soils is linked to mineral recrystallization and organic matter transformations. 1135 34

For selective dissolution of Mn oxides as components of soil (easily reducible oxides) 0.05 mol L(-1) and 0.1 mol L(-1) NH2OH.HCl acidified to pH 2 and for dissolution of Fe oxides (crystalline form of the oxides) 0.25 mol L(-1) NH2OH.HCl in 25% acetic acid, 0.2 mol L(-1) oxalate buffer and 0.1 mol L(-1) ascorbic acid in oxalate buffer were tested. Dissolved elements were determined by ICP-MS and ICP-OES. The studies indicate that the use of 0.05 mol L(-1) NH2OH.HCl in nitric acid solution (pH 2) and 0.1 mol L(-1) ascorbic acid in 0.2 mol L(-1) oxalate buffer led to selective leaching of trace metals bound by Mn and Fe oxide phases in soil. Comparison of different extraction schemes indicates that the trace elements investigated are mainly bound to minerals consisting of crystalline Fe oxides and insoluble minerals (under the extraction conditions used). The studies also indicate that Mn oxides and organic matter retain a major mobile fraction of the elements investigated in the soil.
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PMID:Selective leaching of elements associated with Mn-Fe oxides in forest soil, and comparison of two sequential extraction methods. 1168 55

Three different azodyes were used as target molecules to test the efficiency of the photodegradation process catalysed by titanium dioxide under UV irradiation. A comparison of different catalytic systems was performed using the catalyst both free in solution (system I) and immobilised in a polymeric membrane (system II). Iron oxalate and a conducting polymer (polyaniline, PA) were added to the I and II systems respectively to check an eventual synergetic effect. The research evolved through three different steps involving each one the use of a different analytical method. Shortly, the UV spectrophotometry were preliminarily used to monitor the bleaching process and allowed to choose the best catalytic system, HPLC and GC/MS were used to monitor the appearance and disappearance of the photodegradation intermediates and, lastly, the effective mineralisation was tested by an indirect ICP (Inductively Coupled Plasma) determination of the produced carbon dioxide.
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PMID:Photodegradation of azodyes: comparison of different catalytic systems and control of the effective mineralisation. 1550 16

A sensitive and efficient flow-injection (FI) preconcentration and matrix-separation technique coupled to sector field ICP-mass spectrometry (SF-ICP-MS) has been developed and validated for simultaneous determination of ultra-low levels of uranium (U) and thorium (Th) in human urine. The method is based on selective retention of U and Th from a urine matrix, after microwave digestion, on an extraction chromatographic TRU resin, as an alternative to U/TEVA resin, and their subsequent elution with ammonium oxalate. Using a 10 mL sample, the limits of detection achieved for 238U and 232Th were 0.02 and 0.03 ng L(-1), respectively. The accuracy of the method was checked by spike-recovery measurements. Levels of U and Th in human urine were found to be in the ranges 1.86-5.50 and 0.176-2.35 ng L(-1), respectively, well in agreement with levels considered normal for non-occupationally exposed persons. The precision obtained for five replicate measurements of a urine sample was 2 and 3% for U and Th, respectively. The method also enables on-line measurements of the 235U/238U isotope ratios in urine. Precision of 0.82-1.04% (RSD) was obtained for 235U/238U at low ng L(-1) levels, using the FI transient signal approach.
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PMID:Flow-injection technique for determination of uranium and thorium isotopes in urine by inductively coupled plasma mass spectrometry. 1582 19

An analytical procedure for precisely determining the stoichiometry of Na(x)CoO(2)-type superconductor material is presented. Sodium and cobalt contents, ranging between 3.5 and 11 mg L(-1) and 18 and 32 mg L(-1), respectively, were measured simultaneously using CID-ICP-OES. Sodium was found to significantly lower the emission intensity of cobalt, so the addition of 6.4 g L(-1) of the ionization buffer LiCl was required to compensate for this effect. The recoveries and precisions of the measurements were significantly increased by internal standardization using yttrium: Co(II) emission intensities at 230.786 nm, 237.862 nm, and 238.346 nm can be corrected using Y ion emission intensities, as can the atomic emissions of Co at 345.351 nm and Na at 589.592 nm. The cobalt contents of three real superconductor samples were independently verified by complexometric titration using EDTA. The valence state of cobalt was determined with a relative uncertainty of ~0.5% by redox titration using sodium oxalate as reductive agent and Ce(SO(4))(2) solution. The final stoichiometries of the superconductor samples can be calculated using the Na and Co contents, and the Co valence state. Conclusions about the quality of the prepared samples in terms of phase purity and presence of side products are drawn.
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PMID:Method for precisely analyzing the stoichiometry of Na(x)CoO2-type superconductor material. 1613 4

Aluminium (Al) in the blood is bound to transferrin (Tf), a glycoprotein of about 80kDa that is characterized by its need for a synergistic anion. In this focused review, the binding affinity of Al to Tf is surveyed in the context of our recent studies using on-line high-performance liquid chromatography/high-resolution inductively coupled plasma mass spectrometry (HPLC/HR-ICP-MS). Al in human serum without any in vitro Al-spikes was present in a form bound to the N-lobe site of Tf. The influences of sialic acid in the carbohydrate chain of human serum Tf (hTf) were studied using asialo-hTf, obtained by treatment with sialidase. The binding affinity of Fe was similar between asialo-hTf and native-hTf, while that of Al for asialo-hTf was larger than that for native-hTf, especially in the presence of oxalate, a synergistic anion. The above findings are discussed in relation to diseases in which the serum concentrations of carbohydrate-deficient Tf and oxalate are augmented.
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PMID:Binding affinity of aluminium to human serum transferrin and effects of carbohydrate chain modification as studied by HPLC/high-resolution ICP-MS--speciation of aluminium in human serum. 1613 93

Calcium oxalate supersaturation of the blood is associated with deposition of crystals in various tissues. We measured the serum levels of oxalate, citrate, calcium, and magnesium to estimate their saturation in 112 hemodialysis patients without primary hyperoxaluria and two boys with primary hyperoxaluria. Serum levels of oxalate and citrate were determined by high-performance capillary electrophoresis, while calcium and magnesium were measured by ICP spectroscopy. The serum levels of oxalate, citrate, calcium, and magnesium were 44.9+/-16.5, 138.1+/-54.9 micromol/l, 2.30+/-0.28, and 1.07+/-0.18 mmol/l, respectively, while the levels in patients with primary hyperoxaluria were 83.9+/-34.3, 197.9+/-63.5 micromol/l, 2.53+/-0.15, and 1.14+/-0.34 mmol/l, respectively. Serum calcium oxalate saturation (SS), as calculated by the Equil program, was significantly correlated with the serum oxalate level. Most patients showed metastable supersaturation (1<SS<8.9), which was associated with a serum oxalate level of more than 30 micromol/l. Serum saturation exceeded the formation product (SS=8.9) in some specimens from patients with type 1 primary hyperoxaluria. The serum calcium oxalate saturation [SS(CaOx)] showed a significant positive correlation with the levels of oxalate [Ox], calcium [Ca], and citrate [Cit]: [SS(CaOx)]=-0.3562+34.634[Ox]+0.394[Ca]-0.483[Mg]+0.101[Cit], (all mmol/l, r=0.9848, P<0.01). This formula is useful for estimating the saturation. In conclusion, the serum oxalate level is a good indicator of calcium oxalate saturation and should be monitored accurately while keeping it lower in dialysis patients.
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PMID:Calcium oxalate saturation in dialysis patients with and without primary hyperoxaluria. 1643 91


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