The use of electrothermal vaporizer coupled to the inductively coupled plasma mass spectrometry for the determination of arsenic, selenium and transition metals in biological samples treated with formic acid.

A fast method for the determination of As, Co, Cu, Fe, Mn, Ni, Se and V in biological samples by ETV-ICP-MS, after a simple sample treatment with formic acid, is proposed. Approximately 75 mg of each sample is mixed with 5 mL of formic acid, kept at 90°C for 1 h and then diluted with nitric acid aqueous solution to a 5% (v/v) formic acid and 1% (v/v) nitric acid final concentrations. A palladium solution was used as a chemical modifier.

Biochemical biomarkers and metals in Perna perna mussels from mariculture zones of Santa Catarina, Brazil.

The activity of cholinesterase (ChE), glutathione-S transferase (GST), glutathione reductase (GR), glucose-6-phosphate dehydrogenase (G6PDH) and catalase (CAT) was evaluated in the gill and digestive glands of the Perna perna mussel transplanted to three non-contaminated mariculture zones under the influence of distinct physical-chemical characteristics. Differences among sites for ChE, GST and CAT activities in gill, as well as ChE, GST and G6PDH activity in digestive gland of mussels, were found and possibly related to differences in physicochemical characteristics of the sites and/or biological status of the mussels. Mussels that were transplanted to another, more urbanized site (Ponta do Lessa) with similar physicochemical characteristics to one of the farming sites (Sambaqui), was also chosen to evaluate biomarker responses to pollution.

Ambient mass spectrometric detection of organometallic compounds using direct analysis in real time.

The present work describes the mass spectrometric detection of organometallic compounds following their atmospheric pressure ionization using a commercial direct analysis in real time (DART) ion source. Several organometallic compounds of As, Fe, Hg, Pb, Se, and Sn were examined, and their corresponding mass spectra as well as induced fragmentation patterns were recorded. Gas phase sampling of the pure organometallic compounds or their solutions prepared in toluene generated temporally stable signals.

Determination of Co, Cu, Fe, Mn, Ni and V in diesel and biodiesel samples by ETV-ICP-MST.

This work presents the determination of Co, Cu, Fe, Mn, Ni and V in diesel and biodiesel samples by ETV-ICP MS using emulsion sample preparation. The emulsion composition was: 1.0 g of the diesel or biodiesel sample, 2.

The development of a method for the determination of trace elements in fuel alcohol by ETV-ICP-MS using isotope dilution calibration.

A method for the determination of Ag, Cd, Cu, Pb and Tl in fuel alcohol by isotope dilution electrothermal vaporization inductively coupled plasma mass spectrometry (ID ETV-ICP-MS) is proposed. The analytes were separated in two groups: Ag and Cu were determined without modifier and Cd, Pb and Tl with the use of Pd as chemical modifier. The employed ETV operational conditions were pyrolysis temperature of 800 degrees C for Cd, Pb and Tl and of 900 degrees C for Ag and Cu and vaporization temperature of 2400 degrees C for both groups.

Determination of Cd in biological samples by flame AAS following on-line preconcentration by complexation with O,O-diethyldithiophosphate and solid phase extraction with Amberlite XAD-4.

A method for the on-line preconcentration of Cd based on its complex formation with the ammonium salt of O,O-diethylditiophosphate (DDTP) and using the Amberlite XAD-4 resin as a solid support in a column is proposed. Cadmium was detected by flame atomic absorption spectrometry. Different conditions, such as complexing agent concentration, preconcentration time, solutions flow rates and nature and concentration of the eluent were optimized.

Determination of cadmium in biological samples solubilized with tetramethylammonium hydroxide by electrothermal atomic absorption spectrometry, using ruthenium as permanent modifier.

The feasibility of Ru as a permanent modifier for the determination of Cd in biological samples treated with tetramethylammonium hydroxide (TMAH) by ET AAS was investigated. The tube treatment with Ru was carried out only once and lasted for about 300 atomization cycles. The pyrolysis and atomization temperatures, 750 degrees C and 1300 degrees C, respectively, were chosen from the temperature curves.

Simultaneous determination of Cd, Cu, Mn, Ni, Pb and Zn in nail samples by inductively coupled plasma mass spectrometry (ICP-MS) after tetramethylammonium hydroxide solubilization at room temperature: comparison with ETAAS.

A simple method is described for the determination of Cd, Cu, Mn, Ni, Pb and Zn in nails by using inductively coupled plasma mass spectrometry (ICP-MS) or electrothermal atomic absorption spectrometry (ETAAS). Prior to analysis, 10-20 mg of nail samples were accurately weighed into (15 mL) conical tubes. Then, 1 mL of 25% (w/v) tetramethylammonium hydroxide (TMAH) solution was added to the samples, incubated at room temperature overnight and then further diluted to 10 mL with 1% (v/v) HNO(3).

Single drop micro-extraction with O,O-diethyl dithiophosphate for the determination of lead by electrothermal atomic absorption spectrometry.

Lead was extracted as the O,O-diethyldithiophosphate (DDTP) complex from aqueous solution into a drop of CHCl(3) immersed in the solution. Unlike previously reported procedures using single drop micro-extraction (SDME) for the extraction of inorganic analytes, the complexation reaction was conducted in the aqueous phase, as the ammonium salt of DDTP is soluble in water. The concentration of DDTP was optimized as 0.

Simultaneous on-line pre-concentration and determination of trace metals in environmental samples by flow injection combined with inductively coupled plasma mass spectrometry using silica gel modified with niobium(V) oxide.

This work presents the development of an on-line pre-concentration system for simultaneous determination of Cd, Cu, Ni, V, Zn, Co and Pb in aqueous environmental samples and detection by inductively coupled plasma mass spectrometry. The system is based on cationic retention of the analytes onto a mini-column filled with silica gel modified with niobium(V) oxide. The effects of chemicals and flow variables have been investigated.

Determination of mercury in biological samples by cold vapor atomic absorption spectrometry following cloud point extraction with salt-induced phase separation.

Method development for the pre-concentration of mercury in human hair, dogfish liver and dogfish muscle samples using cloud-point extraction and cold vapor atomic absorption spectrometry is demonstrated. Before the extraction, the samples were submitted to microwave-assisted digestion in a mixture of H(2)O(2) and HNO(3). Cloud point extraction was carried out using 0.

Determination of total mercury and methylmercury in biological samples by photochemical vapor generation.

Cold vapor atomic absorption spectrometry (CV-AAS) based on photochemical reduction by exposure to UV radiation is described for the determination of methylmercury and total mercury in biological samples. Two approaches were investigated: (a) tissues were digested in either formic acid or tetramethylammonium hydroxide (TMAH), and total mercury was determined following reduction of both species by exposure of the solution to UV irradiation; (b) tissues were solubilized in TMAH, diluted to a final concentration of 0.125% m/v TMAH by addition of 10% v/v acetic acid and CH(3)Hg(+) was selectively quantitated, or the initial digests were diluted to 0.

Determination of lead in sediments and sewage sludge by on-line hydride-generation axial-view inductively-coupled plasma optical-emission spectrometry using slurry sampling.

Among the "traditional" hydride-forming elements, lead is probably the most difficult, and its determination in this form has rarely been reported in the literature. In this paper a simple and rapid method, axial-view inductively-coupled plasma optical-emission spectrometry using on-line hydride generation (HG-ICP-OES) from samples prepared as slurry, is proposed for determination of lead in environmental samples. The samples (20-50 mg, particle size View Article and Find Full Text PDF

Contrasting effects of age on the plasma/whole blood lead ratio in men and women with a history of lead exposure.

We examined the effect of age and sex on the relationship between the concentrations of Pb in blood (Pb-B) and in plasma (Pb-P) in an adult population with a history of lead exposure. Pb-P was determined by inductively coupled plasma mass spectrometry (ICP-MS) and Pb-B by graphite furnace atomic absorption spectrometry (GF AAS). We studied 154 adults (56 men and 98 women) from 18 to 60-year old.

Direct determination of selenium in urine samples by electrothermal atomic absorption spectrometry using a Zr plus Rh-treated graphite tube and co-injection of Rh as chemical modifier.

Different chemical modifiers for use with electrothermal atomic absorption spectrometry (ET AAS) were investigated in relation to determining the selenium in human urine samples. The samples were diluted in a solution containing 1% v/v HNO3 and 0.02% m/v cetyltrimethylammonium chloride (CTAC).

Determination of cadmium in coal using solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry.

This work describes the development of a method to determine cadmium in coal, in which iridium is used as a permanent chemical modifier and calibration is performed against aqueous standards by high-resolution continuum source atomic absorption spectrometry (HR-CS AAS). This new instrumental concept makes the whole spectral environment in the vicinity of the analytical line accessible, providing a lot more data than just the change in absorbance over time available from conventional instruments. The application of Ir (400 microg) as a permanent chemical modifier, thermally deposited on the pyrolytic graphite platform surface, allowed pyrolysis temperatures of 700 degrees C to be used, which was sufficiently high to significantly reduce the continuous background that occurred before the analyte signal at pyrolysis temperatures <700 degrees C.

Slurry sampling of sediments and coals for the determination of Sn by HG-GF AAS with retention in the graphite tube treated with Th or W as permanent modifiers.

A method for the determination of Sn in slurry samples of sediment and coal by hydride generation graphite furnace electrothermal atomic absorption spectrometry (HG-GF AAS) is proposed. The slurries were prepared by mixing the ground sample (particle size < or =50 microm) with 2.0 mol L(-1) HCl for the sediment samples or with 2.