Variability of trace element distribution in Noccaea spp., Arabidopsis spp., and Thlaspi arvense leaves: the role of plant species and element accumulation ability.

Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) was applied for the determination of Cd and Zn distributions within the leaves of Cd- and Zn-hyperaccumulating plants, Noccaea caerulescens, N. praecox, and Arabidopsis halleri, in contrast to nonaccumulator species, Thlaspi arvense and A. thaliana. The elemental mapping of the selected leaf area was accomplished via line scans with a 110-µm-diameter laser beam at a 37-µm s-1 scan speed and repetition rate of 10 Hz. The lines were spaced 180 µm apart and ablated at an energy density of 2 J cm-2. The elemental imaging clearly confirmed that Cd was predominantly distributed within the parenchyma of the T. arvense, whereas in the Noccaea spp. and A. halleri, the highest intensity Cd signal was observed in the veins of the leaves. For Zn, higher intensities were observed in the veins for all the plant species except for A. thaliana. Close relationships between Zn and Ca were identified for the Noccaea spp. leaves. These relationships were not confirmed for A. halleri. Significant correlations were also proved between the Cd and Zn distribution in A. halleri, but not for the Noccaea spp. For both T. arvense and A. thaliana, no relevant significant relationship for the interpretation of the results was observed. Thus, the LA-ICP-MS imaging is proved as a relevant technique for the description and understanding of the elements in hyperaccumulating or highly accumulating plant species, although its sensitivity for the natural element contents in nonaccumulator plant species is still insufficient.

Contribution to vapor generation-inductively coupled plasma spectrometric techniques for determination of sulfide in water samples.

Vapor generation-inductively coupled plasma-optical emission spectrometry was used for the determination of sulfide in water samples preserved by the addition of a zinc acetate and sodium hydroxide solution. Hydrogen sulfide and acid-volatile sulfides were transformed, by acidification, to a gaseous phase in a vapor generator and subsequently detected by inductively coupled plasma optical emission spectrometry. Compounds interfering with iodometric titration and spectrophotometric determination were examined as potential chemical interferents. The proposed method provides results comparable to iodometric titration in the tested concentration range 0.06-22.0 mg L(-1). Limit of detection for the determination of hydrogen sulfide by this method is 0.03 mg L(-1).

Determination of free and total sulfur dioxide in wine samples by vapour-generation inductively coupled plasma-optical-emission spectrometry.

Sulfur dioxide (SO(2)) is used as a preservative and stabilizer in wine production to prevent undesired biochemical processes in the must and the final product. The concentration of SO(2) is restricted by national regulations. There are two main forms of SO(2) in wine-free (inorganic forms) and bound (fixed to organic compounds, e.g. aldehydes). Iodometric titration is commonly employed for determination of SO(2) concentration (either by direct titration or after pre-separation by distillation); other techniques are also used. In this work inductively coupled plasma-optical-emission spectrometry with vapour generation was used for determination of free and total SO(2) in wine. Gaseous SO(2) is released from the sample by addition of acid and swept into the ICP by an argon stream. The intensity of the sulfur atomic emission lines is measured in the vacuum UV region. Determination of total SO(2) is performed after hydrolysis of bound forms with sodium hydroxide (NaOH). Concentrations of acid for vapour generation and NaOH for hydrolysis were optimised. The method was used for determination of free and total SO(2) in red and white wine samples and results were compared with those from iodometric titration.

Direct solid analysis of powdered tungsten carbide hardmetal precursors by laser-induced argon spark ablation with inductively coupled plasma atomic emission spectrometry.

The potential of the laser-induced argon spark atomizer (LINA-Spark atomizer) coupled with ICP-AES as a convenient device for direct analysis of WC/Co powdered precursors of sintered hardmetals was studied. The samples were presented for the ablation as pressed pellets prepared by mixing with powdered silver binder containing GeO2 as internal standard. The pellets were ablated with the aid of a Q-switched Nd:YAG laser (1064 nm) focused 16 mm behind the target surface with a resulting estimated power density of 5 GW cm(-2). Laser ablation ICP-AES signals were studied as a function of ablation time, and the duration of time prior to measurement (pre-ablation time) which was necessary to obtain reliable results was about 40 s. Linear calibration plots were obtained up to 10% (m/m) Ti, 9% Ta and 3.5% Nb both without internal standardization and by using germanium as an added internal standard or tungsten as a contained internal standard. The relative uncertainty at the centroid of the calibration line was in the range from +/- 6% to +/- 11% for Nb, Ta and Ti both with and without internal standardisation by Ge. A higher spread of points about the regression was observed for cobalt for which the relative uncertainty at the centroid was in the range from +/- 9% to +/- 14%. Repeatability of results was improved by the use of both Ge and W internal standards. The lowest determinable quantities calculated for calibration plots were 0.060% Co, 0.010% Nb, 0.16% Ta and 0.030% Ti with internal standardization by Ge. The LA-ICP-AES analyses of real samples led to good agreement with the results obtained by solution-based ICP determination with a relative bias not exceeding 10%. The elimination of the dissolution procedure of powdered tungsten (Nb, Ta, Ti) carbide is the principal advantage of the developed LA-ICP-AES method.

Determination of selenium in blood serum by inductively coupled plasma atomic emission spectrometry with pneumatic nebulization.

The possibility of determining selenium in blood serum using inductively coupled plasma emission spectrometry with conventional pneumatic nebulization was studied. A high-resolution spectrometer (SBW=6 pm) with laterally viewed ICP was employed. Analysis with conventional pneumatic nebulization could overcome laborious and demanding digestion, which is necessary for hydride generation. A pressure digestion with nitric acid at 160 degrees C was sufficient to decrease the carbon content in the serum sample to 5%-10% of its original value. Spectral interference of the CN band was observed and mathematically corrected. It was found that the carbon-induced selenium line emission enhancement occurred even under ICP optimized conditions. A method of determination was developed and applied to the analysis of blood serum. True limit of detection in real samples is 0.01-0.02 mg/L and the limit of quantification (RSD 10%) is 0.03-0.07 mg/L using Se I 196.090 nm line at an integration time of 10-2 s. The method was tested by analysis of porcine blood serum and the serum reference material Seronorm MI 0181.