Simultaneous Atomic Absorption Research Articles

A simultaneous atomic absorption and emission spectrometer with dielectric barrier discharge for atomization and excitation

A DBD-AAS/AES simultaneous detection system by sharing a miniaturized multichannel CCD spectrometer.

Implementation of a spraying-assisted fine droplet formation-based simultaneous liquid-phase microextraction method for the determination of copper in clove extract samples

A simultaneous liquid-phase microextraction method was investigated as an alternative to the traditional dispersive liquid–liquid microextraction for the determination of copper. The potential of this approach is based on the simultaneous complexation and extraction process (SCE) using an innovative spraying apparatus forming finer droplets. Method optimization was performed after ensuring the complexation of copper with a novel ligand, namely 8-(1,3-dihydroxy-1-phenylpropan-2-ylimino)methyl)-7-hydroxy-4-phenyl-2H-chromen-2-one ligand with respect to the conventional FAAS system; the detection power of the new developed system (spraying-assisted fine droplet formation-based simultaneous liquid-phase microextraction-slotted quartz tube-flame atomic absorption spectrometry, SAFDF-SLPME-SQT-FAAS) was about 33.8. The quantification and detection values were calculated to be 8.7 and 2.6 µg L−1. Recovery studies were tested in clove extract samples. Obtained percent recoveries were between 96.0 and 103.3% highlighting the applicability and the accuracy of the developed method.

Simultaneous multi-element determination in electrothermal atomic-absorption spectrometry with electrothermal atomization

A discussion of the prospects for creating a multi-element atomic absorption (AA) spectrometer leads to the conclusion regarding the expediency of using spectral devices of relatively low resolution. Previous studies showed that the spectrometer with instrumental bandwidth 0.12 nm equipped with a CCD detector could provide the absorption measurements within a wavelength range of 200 – 400 nm using low-noise radiation sources, e.g., deuterium or low current xenon lamps. The rate of data acquisition was sufficient for vapour spectra monitoring during the pulse atomisation in graphite furnace atomizer. The loss in sensitivity due to low resolution is compensated by the possibility of direct determination of several elements in a single liquid or powder sample. Feasibility of multi-element simultaneous AA spectrometry depends on the efficiency of atomization technique and technology of data processing. The concurrent problems are discussed by the example of new calculation algorithm and its application to the analysis of multi-element nitrate and halogen containing reference materials. It is shown that linearization of the calibration curves for about 10 – 15 elements, which are not subject to chemical impacts, can be carried out automatically in a concentration range up to 4 – 5 orders of magnitude with 5 – 10 % deviation from the linearity at the ends of the interval. For the elements forming stable molecular compounds further improvement of the atomization technique is required.

Use of bone physicochemical characterization and biochemical analyses in an experimental model

Osteoporosis is a systemic skeletal disease characterized by a disorder between bone reabsorption and formation with increase in bone fragility. The aim of this study was to evaluate the bone mass loss using solid-state techniques and biochemical assays to characterized bone samples of ovariectomized rats (OVX) and control group (CTR). The in vivo assays were carried out using biochemical analyses and bone mineral density (BMD) measurements. After the animals were euthanized, the femurs were examined using simultaneous differential thermal analysis (DTA), thermogravimetry/derivative thermogravimetry (TG/DTG) and atomic absorption spectrometric. The microstructure was examined using scanning electron microscopy (SEM). OVX had statistically higher averages (p 0.05); however, OVX showed a significant weight gain (p < 0.0001) with a body mass increase of 30.23 ± 6.45 %. BMD results presented significant differences (p = 0.01985) between CTR and OVX. The total mass loss (TG) was 39.12 ± 0.45 % in OVX, while in CTR groups, it was the 32.45 ± 1.01 % (p = 0.0038). The results of the calcium amount in the bones of OVX (199.86 ± 8.08) were lower than the CTR (229.62 ± 10.02). SEM micrographs showed that OVX presented bone porosity, while CTR showed denser trabecular structure; this result corroborated with bone mass loss in OVX. The ovariectomy-induced bone loss in the rodent model can be evaluated using physical–chemical techniques based on thermal analysis, atomic absorption spectrometry and scanning electronic microscopy.

Multi-Element Determination of Cu, Mn, and Se using Electrothermal Atomic Absorption Spectrometry

Simultaneous multi-element graphite furnace atomic absorption spectrometer (SIMAA 6000) is used to get a new multi-element determinations methodology for Cu, Mn, and Se. Firstly, the optimum conditions for single-element mode are determined (which include: pyrolysis and atomization temperatures). Secondly, the optimum conditions for multi-element mode are also determined. The conditions in the two modes have been compared in terms of the characteristic masses, detection limits and pyrolysis and atomization temperatures. The effect of the matrix on the determination has been studied using urine standard sample from Seronorm (LOT 0511545). The accuracy of the developing methods has been confirmed by analysis different biological reference materials. Simultaneous multi-element GF-AAS offers a rapid, low cost and sensitive method for the analysis of trace elements.

Atomic absorption analysis of solid river suspended matter and sorption concentrates

A direct simultaneous atomic absorption method for the determination of trace heavy metals (Cd, Pb, Tl, and Hg) in solid sea and river suspended matter and sorption concentrates has been suggested (without chemical preparation of the samples). Two stages of the preliminary fractional evaporation of the solid samples (at temperatures of 700–1000°C and 1500–2000°C) were used. The simultaneous atomization of both condensates was carried out in electrothermal atomizers including two evaporation zones. The approaches proposed make it possible to determine the volatile Hg and the less volatile Cd, Pb, and Tl at the level of the background concentration.

준 실시간 측정시스템을 이용한 미세입자 원소성분 배출특성 조사

Fine particulate matter was collected as a slurry using the Semicontinuous Elements in Aerosol Sampler with time resolution of 30-min between May 23 and 27, 2002 at the Sydney Supersite, Florida, USA. Concentrations of 11 elements, i.e., Al, As, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Se, and Zn, in the collected slurry samples were determined off-line by simultaneous multi-element graphite furnace atomic absorption spectrometry. Temporal profiles of and elemental concentrations combined with meteorological parameters such as wind direction and wind speed indicate that some transient events in their concentrations are highly correlated with the periods when the plume from an animal feed supplement processing facility influenced the Sydney sampling site. The peaking concentrations of the elemental species during the transient events varied clearly as the plume intensity varied, but the relative concentrations for As, Cr, Pb, and Zn with respect to Cd showed almost consistent values. During the transient events, metal concentrations increased by factors of >10~100 due to the influence of consistent plumes from an individual stationary source. Also the multi-variate air dispersion receptor model, which was previously developed by Park et al. (2005), was applied to ambient and 8 elements (Al, As, Cd, Cr, Cu, Fe, Pb, and Zn) measurements between 20:00 May 23 and 09:30 May 24 when winds blew from between 70 and , in which animal feed processing plant is situated, to determine emission and ambient source contributions rates of and elements from one animal feed processing plant. Agreement between observed and predicted concentrations was excellent (R of 0.99; and their ratio, ) when one emission source was used in the model. Average ratios of observed and predicted concentrations for As, Cd, Cr, Pb, and Zn varied from for Pb to for Cd.

Simultaneous Determination of Aluminum, Cadmium and Lead in Whole Blood by Simultaneous Atomic Absorption Spectrometry with Oxygen Charring

AbstractA method for the simultaneous determination of aluminum (Al), cadmium (Cd) and lead (Pb) in whole blood has been developed by using simultaneous atomic absorption spectrometry (SIMAAS) with oxygen charring. The optimized conditions for the simultaneous determination of Al, Cd and Pb were obtained in the presence of palladium (Pd) as the chemical modifier, using 600 °C and 2400 °C as the pyrolysis and the atomization temperature, respectively. The whole blood samples were diluted 1+5 (v/v) directly with 0.1% (v/v) Triton X‐100. Oxygen was employed to eliminate the interference of carbonaceous residues in the charring step before pyrolysis. The calibration curves were carried out with aqueous standard solutions and the linear ranges were 0–40 ng mL−1, 0–4 ng mL−1 and 0–40 ng mL−1 for Al, Cd and Pb, respectively. The detection limits were 0.96 ng mL−1 (19.2 pg) for Al, 0.03 ng mL−1 (0.6 pg) for Cd and 0.60 ng mL−1 (12.0 pg) for Pb. The spiked recoveries of Al, Cd and Pb in whole blood were 98.0%, 100.0% and 101.7%, respectively. The accuracy of the proposed method was evaluated with the analysis of a whole blood certified reference material (Seronorm, level 2). The found concentrations were in agreement with the recommended values. The proposed method has been successfully applied to the simultaneous determination of Al, Cd and Pb in whole blood of healthy volunteers before and after eating barbecued foods.

Optimization of the direct simultaneous atomic absorption determinations of several elements in marine or riverine particulate matter

A highly sensitive procedure is proposed for direct simultaneous atomic absorption determinations of three elements (Ag, Cd, and Pb or Cd, Pb, and Tl) in marine and riverine particulate matter. To decrease the influence of nonselective interference and matrix effects and to improve the detection limits of the elements, the course of the analysis included a preliminary stage of fractional evaporation of the sample (a graphite rod with a diaphragm as the evaporator) and condensation of the elements (a graphite rod as the collector). The condensate atomization proceeded in a rod-cell electrothermal graphite atomizer with independent heating of the zones of evaporation and atomization.

Cobalt as internal standard for arsenic and selenium determination in urine by simultaneous atomic absorption spectrometry

The effectiveness of internal standardization for simultaneous atomic absorption spectrometry (SIMAAS) was investigated for As and Se determination in urine. Co and Sn were selected as internal standard (IS) candidates based on the evaluation of some physico-chemical parameters related to the atomization. Correlation graphs, plotted from the normalized absorbance signals ( n = 20) of internal standard (axis y) versus analyte (axis x), precision, and accuracy of the analytical results were the supportive parameters to choose Co as the most appropriate IS. The urine samples were diluted 1 + 2 to 1.0% (v/v) HNO 3 + 80 μg L −1 Co 2+. The mixture 20 μg Pd + 3 μg Mg was used as chemical modifier and the optimized temperatures for pyrolysis and atomization steps were 1400 and 2300 °C, respectively. The characteristic masses for As (47 ± 1 pg) and Se (72 ± 2 pg) were estimated from the analytical curves. The detection limits ( n = 20, 3 δ) were 1.8 ± 0.1 and 2.6 ± 0.1 μg L −1 for As and Se, respectively. The reliability of the entire procedure was checked with the analysis of certified reference material from Sero AS(Seronorm™ Trace Elements in Urine). The obtained results showed the matrix interference disallowed the instrument calibration with aqueous standards. The best analytical condition was achieved when matrix-matched standards were used in combination with Co as IS, which improved the recoveries obtained for As. Under this experimental condition, eight urine samples were analysed and spiked with 10 and 25 μg L −1 As and Se. The mean recoveries were 96 ± 6% (10 μg L −1 As), 95 ± 6% (25 μg L −1 As), 101 ± 7% (10 μg L −1 Se), and 97 ± 4% (25 μg L −1 Se).

Simultaneous Atomic Absorption Spectrometry for Cadmium and Lead Determination in Wastewater. A Laboratory Exercise

Atomic absorption spectrometry is revisited to present the most updated instrumentation, which allows multi-element determinations. Simultaneous atomic absorption spectrometry (SIMAAS) with electrothermal atomization is introduced to undergraduate students through a problem-based instructional laboratory. An environmental problem of water polluted with cadmium and lead in trace quantities is presented to the students, who were asked to analyze wastewater samples from potential contaminating industries. The proposed experiment is divided into two parts: the first part is devoted to optimization of instrumental parameters, and the second part is the application of the optimized conditions to execute the simultaneous determination of cadmium and lead. Each part can be carried out during a 3 or 4-hour laboratory class.

Elemental Analysis of Sub-Hourly Ambient Aerosol Collections

Simultaneous multielement graphite furnace atomic absorption spectrometry was used to determine Al, As, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Sb, Se, and Zn in ambient air sampled at 170 L·min−1 for 30 min and collected as a slurry after dynamic preconcentration. In PM20 samples collected at College Park, MD, results were > 2σ above system blank in > 95% of samples for Al, Cd, Cu, Cr, Fe, Mn, Pb, and Zn, and > 2σ above system blank in > 80% of samples for As, Ni, and Se. Analyses of slurries of NIST SRM 1648, Urban Particulate Matter, were typically within 10% of expected values for all elements except Al, Cr, and Fe, elements for which deviations were mostly due to difficulties in transferring large particles. This problem will be reduced for urban fine particulate matter samples (PM2.5). Trends in the concentrations of elemental source markers were readily correlated with wind direction and other meteorological factors to identify the influences of local industrial emissions, including motor vehicle traffic, coal...

W+Rh as permanent chemical modifier in simultaneous atomic absorption spectrometry: interference studies on As, Cd, Pb and Se determination

A systematic study of Na+, K+, Ca2+, Mg2+, Cl-, NO3-, SO42- and PO43- interference on the simultaneous atomization of As, Cd, Pb and Se was carried out using an electrothermal atomic absorption spectrometer. The mixture 250 mg W + 250 mg Rh was thermally deposited on the graphite tube platform and used as permanent chemical modifier. The compromised heating program adjustments (Tp = 650&ordmC and Ta = 2200&ordmC) diminished the thermal decomposition and volatilization efficiency of the interfering species during the pyrolysis step. The Cl- and SO42- anions caused the most severe interference, while NO3- only affected the analytes' atomization when high amounts (> 27 mg) were used. The anion PO43- produced a strong negative interference on the Se absorbance signals. The presence of Na+, K+, Ca2+ and Mg2+ prejudiced mainly Cd, and the interference effects of Cl- salts were more pronounced than NO3- salts.

Silver as internal standard for simultaneous determination of Cd and Pb in whole blood by electrothermal atomic absorption spectrometry

The use of internal standardization for simultaneous atomic absorption spectrometry (SIMAAS) was investigated for Cd and Pb determination in whole blood. The comparison of thermochemical and physico-chemical parameters allowed the selection of Ag, Bi, and Tl as internal standard candidates. Correlation graphs, plotted from the normalized absorbance signals (n = 20) of internal standard (axis y) versus analyte (axis x), precision and accuracy were used to select Ag as the most appropriate internal standard. Blood samples were diluted (1 + 9) with 0.11% (m/v) Triton X-100 + 1.1% (v/v) HNO3 + 0.28% (m/v) NH4H2PO4 + 10 µg L−1 Ag+. Pyrolysis and atomization temperatures for the optimized heating program were 550 and 1700 °C, respectively. Characteristic masses based on integrated absorbance were 1.68 ± 0.01 pg for Cd and 30.3 ± 0.1 pg for Pb. The detection limits (DL) were 0.095 ± 0.001 µg L−1 and 0.86 ± 0.01 µg L−1 for Cd and Pb, respectively. The mean RSD for all determinations was the same for Cd (13 ± 9%) with or without Ag as internal standard (IS). On the other hand, the use of Ag as IS improved the RSD for Pb from 3.6 ± 4.0% to 2.2 ± 2.0%. An effective contribution of the internal standard Ag was verified in the recoveries of spiked samples (0.5 µg L−1 Cd2+ and 5.0 µg L−1 Pb2+). The mean recoveries were 81 ± 8% and 91 ± 4% for Cd, and 80 ± 11% and 93 ± 6% for Pb without and with IS correction, respectively. This is the first application of IS for a simultaneous determination by SIMAAS.

Simultaneous determination of manganese and selenium in serum by electrothermal atomic absorption spectrometry

A method for determination of manganese and selenium in serum by simultaneous atomic absorption spectrometry (SIMAAS) is proposed. The samples (30 μl) were diluted (1+3) to 1.0% v/v HNO 3+0.10% w/v Triton X-100 directly in the autosampler cups. A total of 20 μg Pd+10 μg Mg(NO 3) 2 was used as chemical modifier. The pyrolysis and atomization temperatures for the simultaneous heating program were 1200 and 2300 °C, respectively. The addition of an oxidant mixture (15% w/w H 2O 2+1.0% v/v HNO 3) and the inclusion of a low temperature pyrolysis step (400 °C) attenuated the build-up of carbonaceous residues onto the integrated platform. An aliquot of 15 μl of the reference or sample solution was introduced into the graphite tube and heated at 80 °C; subsequently, 10 μl of oxidant mixture+10 μl of chemical modifier was introduced over that aliquot and the remaining heating program steps were executed. This strategy allowed at least 250 heating cycles for each THGA tube without analytical signal deterioration. The characteristic masses for manganese (6 pg) and selenium (46 pg) were estimated from the analytical curves. The detection limits were 6.5 pg ( n=20, 3 δ) for manganese and 50 pg ( n=20, 3 δ) for selenium. The reliability of the entire procedure was checked with the analysis of serum from Seronorm™ Trace Elements in Serum (Sero AS) and by addition and recovery tests (97±9% for manganese and 96±7% for selenium) using five serum samples.

Minimalism approach for determination of Cu, Fe and Zn in serum by simultaneous electrothermal atomic absorption spectrometry

Copper, iron and zinc were determined in serum by simultaneous atomic absorption spectrometry (SIMAAS). The minimalism approach was adopted throughout this analytical method, to reduce time, costs, sample, reagent, energy requirements, and residue production. Samples were 80-fold diluted with 0.01% (w/v) Triton X-100+1% (v/v) HNO 3 directly in the autosampler cups. Three strategies were implemented to match the final diluted analyte concentrations with the SIMAAS linear concentration ranges: a reduced 5 μl aliquot of analytical reference or diluted sample solution was introduced into the preheated graphite tube at 100 °C; a super-estimated pyrolysis temperature was chosen for selective zinc volatilization; and a mini argon flow of 50 ml min −1 was used during the atomization step. The pyrolysis and atomization temperatures for the simultaneous heating program were 700 and 2300 °C, respectively. The characteristic masses for copper (26 pg), iron (16 pg), and zinc (2.7 pg) were estimated from the analytical graphs. The detection limits ( n=20, 3 σ) were 4.0, 2.2, and 0.4 μg l −1 for copper, iron and zinc, respectively. The reliability of the entire procedure was checked with the analysis of Seronorm™ trace elements in serum (Sero AS). Serum samples of five volunteers were analyzed and the recovery tests for additions of 2.0, 2.0 and 1.0 mg l −1 were 100±4, 99±6, and 95±5% for copper, iron and zinc, respectively.

Multielement electrothermal atomic absorption spectrometry: a study on direct and simultaneous determination of chromium and manganese in urine.

A study was carried out on the direct determination of Cr and Mn in urine using simultaneous atomic absorption spectrometry (SIMAAS). The heating program conditions, the absorbance signal profiles, the influence of different chemical modifiers, and the urine sample volume delivery into the tube were optimized to perform the calibration with aqueous solutions. Among several chemical modifiers tested, the best recovery and repeatability results were obtained for 3 microg Mg(NO3)2. On using this modifier, the pyrolysis and atomization temperatures for simultaneous determination of Cr and Mn were 1,300 degrees C and 2,500 degrees C, respectively. Urine samples were diluted (1+1) with 2.0% (v/v) HNO3 + 0.05% (w/v) Triton X-100 prepared in high purity water. A 20-microL aliquot of analytical solution and 10 microL of chemical modifier solution were delivered to the graphite tube. The characteristic masses were 7.8 pg for Cr (RSD=4.0%) and 4.6 pg for Mn (RSD=2.6%). The limits of detection were 0.08 microg L(-1) (n=20, 3s) for Cr and 0.16 microg L(-1) (n=20, 3s) for Mn. Recovery studies for 1.0 or 2.5 microg L(-1) of Cr and Mn added to different urine samples showed acceptable results for Cr (100%, RSD=14%) and Mn (88%, RSD=5.6%).

Possibilities for the simultaneous preconcentration and flame atomic absorption spectrometric determination of Cr(III) and Cr(VI) using a C18 column and sorption loop

The sorption loop as a preconcentration unit used so far in the low-pressure flow injection (FI) system was combined with the hydraulic high-pressure nebulizer (HHPN) and a high-pressure liquid chromatographic (HPLC) column. Thus, the sorption preconcentration of Cr(VI) can be coupled to a powerful sample introduction method or preconcentration techniques of Cr(III). The subsequent determination of the Cr(VI) content of the samples was carried out by flame atomic absorption (FAAS).

Multivariate data analysis of trace element content in animal organs measured by simultaneous atomic absorption spectrometry

The simultaneous determination of trace elements in animal organs offers improved possibilities to characterize the geographical origin of the animal by analyzing its pollution characteristics. Pb, Cd, Ni (GF-AAS) and Cu, Zn, Fe, Mn (F-AAS) in kidneys and livers of cows from different sites have been measured using simultaneous AAS. The correct allocation of cows to specific regions shows that multivariate data analysis provides efficient tools for the geographical classification. The consideration of absorbance rather than concentration as the data input simplified the analytical procedures by omitting the calibration step.

Frequency-modulated simultaneous Atomic Absorption Spectrometry (FremsAAS): Determination of As, Se and Sb.

The evaluation of accuracy and efficiency of the frequency-modulated simultaneous Atomic Absorption Spectrometry (FremsAAS) has been extended to an arrangement with EDL as light sources. Fundamental calibrations have been worked out for As, Se and Sb using a graphite furnace as well as hydride generation in combination with a heated quartz tube as atomization unit. The characteristic data are in good agreement with results obtained by conventional single-channel AAS instruments. Determinations in three standard reference materials with different complex matrices resulted in complete agreement with the certified values.