Source Flame Atomic Absorption Spectrometry Research Articles

The Influence of Copper and Zinc on Photosynthesis and Phenolic Levels in Basil (Ocimum basilicum L.), Borage (Borago officinalis L.), Common Nettle (Urtica dioica L.) and Peppermint (Mentha piperita L.).

This work is aimed at relationships which govern zinc and copper uptake by four popular medicinal herbs: basil (Ocimum basilicum L.), borage (Borago officinalis L.), common nettle (Urtica dioica L.) and peppermint (Mentha piperita L.). They are often grown in soils with significant copper or zinc levels. Herbs were cultivated by a pot method in controlled conditions. Manganese, iron, copper and zinc concentrations were determined by High-Resolution Continuum Source Flame Atomic Absorption Spectrometry. The efficiency of photosynthesis was estimated by measuring the chlorophyll content, water use efficiency, net photosynthesis, intercellular CO2, stomatal conductance, and transpiration rate. Phenolic compounds were determined by the Folin-Ciocalteu method. Analysis of variance showed that herbs grown in soil treated with copper exhibited a lower iron content in roots, while manganese behaved in the opposite way. The only exception was borage, where a decrease in the manganese content in roots was observed. Both copper and zinc supplementations increased the total content of phenolics, while the highest increases were observed for common nettle and basil. Peppermint and borage responded less to supplementation. In the majority of samples, zinc and copper did not significantly affect the photosynthesis. Herbal extracts from common nettle and basil had unique antioxidant properties and may be good free radical scavengers.

SEQUENTIAL DETERMINATION OF Zn, Fe, Mg, Ca, Na AND K IN SYNTHETIZED BABASSU FAME BY HIGH RESOLUTION CONTINUUM SOURCE FLAME ATOMIC ABSORPTION SPECTROMETRY

In this work, babassu FAME samples were synthesized by transesterification reaction under alkaline catalysis with sodium glyceroxide and by two steps process with KOH followed by H2SO4 as catalysts. A sequential multi-element method for determination of Zn, Fe, Mg, Ca, Na and K in synthesized babassu FAME by high resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) was developed. The proposed method is based on a microemulsion formation by mixing the babassu FAME samples with 1-propanol and aqueous phase. The mass proportion of the added components was evaluated through a ternary diagram. External and matrix-matching calibration techniques with inorganic and organic standard were investigated. In the five-level spike-recovery test, satisfactory results were obtained by performing the matrix-matching calibration along with inorganic standard solutions. By using the optimized conditions, limits of detection in the range of 0.002-0.12 mg kg-1 were obtained. Accuracy was attested by the agreement of the results obtained in the analysis of three certified reference materials. By applying the microemulsion system and HR-CS FAAS, the sequential determination of six elements was achieved. Therefore, the proposed method was a suitable alternative for metal determination in babassu FAME samples, with good sensitivities, accuracy, and a wide linear working range.

BaTiO3 is a novel adsorbent for solid-phase extraction of copper at trace levels in food and water samples before HR-CS-FAAS detection

A simple, precise, and rapid method for preconcentration and determination of copper in food and water samples, based on sonication/vortex-free solid phase extraction with high resolution-continuum source flame atomic absorption spectrometry has been developed. In this study, BaTiO3 was synthesized using a single-step hydrothermal method and used as an adsorbent. BaTiO3 was characterized by FT-IR, SEM-EDX, STEM, XRD, and BET methods. The significant feature of the adsorbent is its high surface-to-volume ratio (177.4 m²/g). Important parameters (pH, adsorbent amount, eluent type and volume, adsorption and desorption time, model solution volume, and matrix effects) were optimized. The linear working range (5 – 250 µg L-1) and the detection limit (1.6 µg L-1) were calculated. The presented method was validated with certified reference material and the addition-recovery tests. The application of the method was evaluated for the extraction and determination of Cu(II) in selected food and water samples and quantitative data were obtained.

Utilization of Extraction Procedures for Evaluating Environmental Risk from Waste Materials.

Several procedures for extracting content from different waste materials types were investigated, with the aim of evaluating their environmental impact. The waste materials consisted of wastes from bauxite ore processing by means of the Bayer process (red mud, Ajka, Hungary), bauxite ore using the sintering process followed by the Bayer process (brown-red mud, Žiar nad Hronom, Banská Bystrica region, Slovakia) and sulphide ores (metal-rich post-flotation tailing, Lintich, Slovakia). The extraction procedures were carried out with the aim of isolating "mobilizable" fractions using 0.05 M ethylenediaminetetraacetic acid (EDTA) and 0.43 M acetic acid (AA) (representing environmental risk during changes in normal environmental conditions) and "maximum potentially mobilizable" fractions using 2 M HNO3 (representing the total environmental risk). The content of chosen toxic heavy metals (THMs) (Cd, Cr, Cu, Pb, Ni, Zn) and Fe, Mn as metals creating Fe/Mn oxides in the extracts and solutions after microwave digestion was determined using high-resolution continuum source flame atomic absorption spectrometry (HR CS FAAS). On the basis of the results obtained in this study, it is possible to state that different origin of waste materials is reflected in different mobility of toxic heavy metals into the surrounding environment. From the point of view of toxic heavy metals mobility, disposal site of wastes after bauxite processing are much less of a threat to the environment than disposal site of flotation sludge after processing sulphide ores. The single extraction of 0.43 M AA is more effective than the extraction of 0.05 M EDTA for the purposes of determining the content of metals in the mobilizable fraction of tailing waste materials. The mobility of the studied toxic heavy metals in the Lintich tailing decreases in the direction from the lagoon to the dam, which may indicate the fact that the dam serves to a certain extent to inhibit the mobility of metals into the surrounding ecosystem.

Closed-Vessel Conductively Heated Digestion of Dry Dog Food for Spectrometric Determination of Essential Nutrients

The closed-vessel conductively heated digestion system (CHDS) was evaluated to digest dry dog foods for further determination of K, Na, Cu, Fe, Mn, and Zn by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). The CHDS method was optimized using a fractional factorial design with five variables (HNO3 concentration, H2O2 volume, temperature, holding time, and pre-digestion time) at two levels. The accuracy of the CHDS procedure was checked by the analysis of reference materials from the National Institute of Standards and Technology (NIST SRM 1577b Bovine Liver and 2976 Mussel Tissue) and Brazilian Agricultural Research Corporation (Embrapa MR-E1002A Fish Food). Also, the digestion efficiencies were calculated from residual carbon contents (RCCs). The RCC and blank values in the CHDS digested samples were consistently low, which is suitable for determinations using ICP OES and ICP-MS techniques. For comparison, all samples were also digested by microwave-assisted digestion in closed vessels (MW-AD). Results for Na, K, Cu, Fe, Mn, and Zn determined in sample digests obtained by CHDS were not statistically different at a 95% confidence level from those observed for MW-AD. Limits of quantification (LOQ) calculated from digests in CHDS and MW-AD were comparable, and the values provided adequate limits for elemental determinations in dog foods. Data from mineral composition and moisture were employed in a clustering analysis (HCA) and the discrimination of the samples among different manufacturers and food for dogs at different life stages was possible.

Magnetic Adsorbent Decorated with Poly(N-Isopropylacrylamide) (PNIPAM) Brushes for the Vortex-Assisted Solid Phase Extraction (VASPE) of Lead in Water, Cigarettes and Soil with High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS) Detection

Here is reported the synthesis of a magnetic phosphorus-containing adsorbent decorated with poly(N-isopropylacrylamide) (PNIPAM) brushes via surface-initiated atom transfer radical polymerization (SI-ATRP) and its application for vortex assisted solid phase extraction of lead in water, cigarettes and soil. The adsorbent was characterized using Fourier-transform infrared spectroscopy (FT-IR) and energy dispersive x-ray (EDX) spectroscopy. A high-resolution continuum source flame atomic absorption spectrometer (HR-CS FAAS) was used for the quantification of lead. All factors affecting the extraction efficiency including the solution pH, adsorbent dose, sample volume, vortex time, and elution protocols were optimized. The limits of detection (LOD) and quantification (LOQ) were determined to be 0.05 µg L−1 and 0.18 µg L−1, respectively. The preconcentration and enhancement factors were 20 and 18. Validation was performed using TMDA 64.3 fortified water and INCT-OBTL-5 tobacco leaves certified reference materials with satisfactory recoveries. The method was shown to be sensitive, efficient and reproducible.

The principle of pooled calibrations delivers full correspondence between uncertainties of measurements of Na, Mg and Ni when determined using HR-CS FAAS

Methods for determination of elements in various types of samples are generally considered to be very precise and highly accurate. For reliable analysis of elements Na, Mg and Ni in food samples is it worthwhile to perform an extensive method validation of high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) according to the principle of pooled calibrations (PoPC). Under routine laboratory conditions of analysis, elevated levels of relative uncertainty of measurement reaching values of more than 50% were detected, which jeopardized the validity of results, even when the measurements in the present study were performed with samples of tap water and borehole water. Comparison of relative uncertainties with corresponding literature results indicates that sample-signal differences may be due to detector noise rather than specimen variations.

Closed-Vessel Conductively Heated Digestion System for the Elemental Analysis of Agricultural Materials by High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS)

Novel applications of the closed-vessel conductively heated digestion system (CHDS) are proposed to digest biomass, biochar, oyster shell flour, bone meal and swine manure for the determination of Ca, K, Mg, Na, Cu, Fe, Mn, and Zn by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). The performance of the digestion method using 14 and 7 mol L−1 HNO3 was checked by analyzing soil, rock, and plant certified reference materials (CRMs). For comparative purposes, all samples were analyzed after microwave-assisted digestion (MW-AD). Results obtained for most analytes by the closed-vessel conductively heated digestion system (CHDS) were in agreement with certified values and those attained by the comparative digestion method. The use of 7 mol L−1 HNO3 furnished lower blanks for most analytes and was effective to prepare challenging samples as biomass, biochar, shell and bone meal, swine manure, plants, soil, phosphate rock, and may be a good alternative for elemental determinations using most analytical techniques that rely on solution-based sample introduction systems. The detection limits (dry basis, mg kg−1) for Ca, Cu, Fe, K, Mg, Mn, Na, and Zn were 3, 0.4, 4, 4, 0.7, 0.4, 3, and 2, respectively. The mean relative standard deviations were close to 4.9% for closed-vessel conductively heated digestion (CHDS) and 5.9% for microwave-assisted digestion (MW-AD).

Magnetic solid‐phase extraction of nickel(II) as the 2‐(5‐bromo‐2‐pyridilazo)‐5‐(diethylamino)phenol chelate on magnetite@methacrylic ester copolymer prior to high‐resolution–continuum source flame atomic absorption spectrometric detection

A Fe3O4@ Diaion HP‐2MG resin was used for separation-preconcentration and determination of trace Ni(II) as the 2‐(5‐bromo‐2‐pyridilazo)‐5‐(diethylamino)phenol (PADAP) chelate. Nickel determination was performed by high‐resolution–continuum source flame atomic absorption spectrometry (HR-CS FAAS). Among the parameters affecting the recoveries of Ni(II) on the Fe3O4@ Diaion HP-2MG, the pH, resin mass, and sample volume were optimized. The influence of matrix ions upon the analyte recovery was evaluated and the tolerance limit was determined for common ions. The Fe3O4@ Diaion HP-2MG resin was used 15 times without any degradation in performance. The limit of detection, the limit of quantification, and preconcentration factor were 15.0 µg L−1, 49.0 µg L−1, and 100 respectively. The accuracy of the developed method was validated by the analyzing certified reference materials (NIST 1573a tomato leaves and TMDA-64.3 fortified water). The developed procedure was applied to natural water and food samples.

Ti3AlC2 max phase- graphene oxide (GO) nanocomposite for selective solid phase microextraction of palladium in environmental samples and medical appliances prior to its detection with high-resolution continuum source flame atomic absorption spectrometry (HR-CS-FAAS)

Palladium is an important metal as it has a wide range of applications in different fields but can cause cancer in human beings. Therefore, precise quantification of palladium is important. For this purpose, new material Ti3AlC2 max phase having unique properties like high stability, thermal conductivity and environmental friendly has been synthesized. To increase its surface area of Ti3AlC2 max phase, graphene oxide (GO) has been incorporated to form Ti3AlC2 max phase GO nanocomposite. Ti3AlC2 max phase GO nanocomposite was used as solid phase extracting material for microextraction and preconcentration of Pd(II) in environmental samples and medical appliances. Characterization of the adsorbent was achieved by using fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM), X-ray diffraction (XRD), energy dispersive X-ray (EDX) and surface area analyzer (SAA). All the parameters that influence the extraction efficiency of the adsorbent like solution pH, amount of adsorbent, volume of sample, vortex time, desorption condition and interferences effect were determined and optimized. The limit of detection (0.327 µg/L) and limit of quantification (1.09 µg/L) show that the method is highly sensitive. The relative standard deviation was calculated as 5.48 % for five repeated measurements, which shows that the developed method is reproducible. The method is highly efficient with large values of preconcentration factor (20) and enhancement factors (20). The method was validated by applying the method to real water samples, soil samples and medical appliances with satisfied recovery results (94–106 %).

Ag modified ZnO nanoflowers for the dispersive micro-solid-phase extraction of lead(II) from food and water samples prior to its detection with high-resolution continuum source flame atomic absorption spectrometry

Ag modified ZnO nanoflowers were synthesized by using hydrothermal method and used as dispersive micro-solid phase extractant for separation and preconcentration prior to its flame atomic absorption spectrometric detection. The Ag modified ZnO nanoflowers has been characterized by FT-IR, XRD, FESEM, EDX and BET. The factors effecting extraction efficiency like pH, Adsorbent dose, sample volume, eluent concentration, eluent volume was optimized. Matrix effects were also studied. The limit of detection and preconcentration factor (PF) were calculated as 8.52 μg L−1, and 100, respectively. The presented dispersive micro-solid phase extraction technique was validated using GBW07424 (GSS-10) soil and GBW07425 (GSS-11) soil certificated reference materials (CRMs) with satisfactory recovery results. The presented dispersive micro-solid-phase extraction (d-μSPE) procedure was successfully applied to food and water samples.

Metal decorated silica-based core-shell magnetic nanocomposite for the solid-phase microextraction of cadmium(II) with determination by high-resolution continuum source flame atomic absorption spectrometry

The present study describes a facile and environmentally friendly hydrothermal method for the fabrication of metal decorated silica-based core-shell magnetic nanocomposite M@Si-MNCs, applied as a sustainable coating material for the solid-phase microextraction of toxic cadmium ions. M@Si-MNCs were characterized by scanning electron microscopy, X-ray-diffraction, Fourier transform infrared spectroscopy and Brunauer–Emmett–Teller analyzer. Relevant parameters have been studied to obtain maximum recovery, including pH, adsorbent dosage, model solution volume, - adsorption and desorption time, and matrix effects. The developed method obtained excellent linearity from 50 to 500 µg/L with a limit of detection of 1.2 µg/L and a limit of quantification of 4.1 µg/L. The new method was applied for separation, preconcentration and determination of cadmium in environmental and tobacco samples.

Fabrication and characterization of MgCo2O4 for solid phase extraction of Pb(II) from environmental samples and its detection with high-resolution continuum source flame atomic absorption spectrometry (HR-CS-FAAS)

Magnesium cobaltite (MgCo2O4) nanosorbent was prepared by hydrothermal synthesis method. It has been characterized by various techniques such as FTIR, XRD and SEM. Enrichment and separation of Pb(II) by using MgCo2O4 on solid phase extraction was investigated. The effects of parameters such as pH of the solutions, amount of adsorbent, vortex time, sample volume, eluent concentration and matrix ions were investigated for optimum recovery of analyte ions. The enrichment factor was 125. The limit of detection (LOD) and limit of quantification (LOQ) under optimal conditions for Pb(II) were determined as 0.39 µg L-1 and 1.30 µg L-1, respectively. The validity of the developed SPE method was obtained by the analysis of certified reference material TMDA-64.3 and IC-INCT-OBTL-5 (Oriental Basma Tobacco Leaves), and when the obtained results were compared with the certified values, acceptable values ​​were obtained. The SPE method under optimized parameters conditions was applied to determination of lead(II) in water and food samples.

Extraction Induced by Emulsion Breaking for Ca, Fe, Mg, and Zn Determination in Edible Oils Using High-Resolution Continuous Source Flame Atomic Absorption Spectrometry

Extraction Induced by Emulsion Breaking for Ca, Fe, Mg, and Zn Determination in Edible Oils Using High-Resolution Continuous Source Flame Atomic Absorption Spectrometry

Spectrophotometric Determination of Fe(II) and Fe(III) Using 5-(4-Ethylphenyl azo ) 2-Hydroxybenzaldehyde Oxime Reagent

Spectrophotometric Determination of Fe(II) and Fe(III) Using 5-(4-Ethylphenyl azo ) 2-Hydroxybenzaldehyde Oxime Reagent

Fast sequential multi element analysis of lead and cadmium in canned food samples using effervescent tablet-assisted switchable solvent based liquid phase microextraction (EA-SS-LPME) coupled with high-resolution continuum source flame atomic absorption spectrometry (HR-CS-FAAS)

An effervescent tablet-assisted switchable solvent based liquid phase microextraction (EA-SS-LPME) was developed for multi-element determination of Pb and Cd in various samples using high-resolution continuum source flame atomic absorption spectrometry (HR-CS-FAAS). The effervescent tablets were used for improving the extraction efficiency. Triethylamine as a hydrophobic solvent was switched to protonated triethylamine carbonate by CO2 and used to extract dithizone complexes from samples. Calibration linearities were obtained from 0.06 to 10.0 mg L−1 (Pb) and 0.02 to 1.50 mg L−1 (Cd). LODs of the proposed method were 0.0195 (Pb) and 0.0068 (Cd). LOQs were 0.0649 mg L−1 (Pb) and 0.0228 mg L−1 (Cd) with %RSDs of 1.25%–1.69% (Pb) and 1.07%–1.64% (Cd). The proposed method was applied for the determination of Pb and Cd in water and canned food samples. The spiked recoveries were 82.3–119.0% (Pb) and 81.7–120.0% (Cd). In addition, the PF was 3.3, with EF at 1.4 (Pb) and 2.6 (Cd) obtained after extraction for under 8 min.

Multi-Element Determination of Trace Elements in B7-diesel Oil by High-Resolution Continuum Source Flame Atomic Absorption Spectrometry

In this work, a method for sequential multi-element determination of Cu, Fe, Ni, Pb, Zn, Al, Cr and Sn in B7-diesel oil samples by high-resolution continuum source flame atomic absorption spectrometry (HR-CS F AAS) was proposed. The sample preparation was based on formation of microemulsion (ME), which was investigated through a three-phase diagram. The ME composition adopted was B7-diesel oil (3.3 g), aqueous phase containing nitric acid (1.4 mol L-1, 300 μL) and n-propanol (up to 10 mL). The use of surfactant Triton X-100 in the formation of ME was also evaluated. Limits of detection in the range of 0.01 – 0.4 mg kg-1 were obtained. Spike-recovery tests were accomplished and the results varied between 93 and 124%. The accuracy of the proposed method was confirmed by the analysis of certified reference material (CRM) NIST SRM 1084a (Wear-Metals in Lubricating Oil); there was no statistical difference between the obtained results and the certified values (at 95% confidence level). Twelve B7-diesel oil samples were analyzed and Cu, Fe and Cr were found in three samples. The proposed method was simple, fast and accurate. The sequential multi-element determination of trace elements presented advantages as low costs and reduction in analysis time, being appropriate for routine analysis.

Simultaneous determination of Fe and Zn in dried blood spot by HR-CS GF AAS using solid sampling

Dried Blood Spot (DBS) was evaluated as a solid sampling (SS) strategy for the simultaneous determination of Fe and Zn in blood samples by Solid Sampling High-Resolution Continuum Source Graphite Furnace Atomic Absorption Spectrometry (SS HR-CS GF AAS). The alternative lines of Fe and Zn at 307.572 and 307.589 nm, respectively, were evaluated. A good correlation between the area of DBS (in mm2) and volume of blood (in µL) was observed up to 200 µL of blood. A 3.4 mm diameter paper disk, equivalent 3.86 ± 0.13 µL, was punched from the DBS and employed for blood analysis. Random sampling through the area of the paper circle produced by 50 μL blood samples showed no chromatographic effects. The upside of the solid sampling 'boat type' graphite platform was coated with a W-based film. This coating allowed around 350 firings. The use of 3 µL of 15% v/v H2O2 solution as chemical modifier improved both the thermal stability and peak profile of Zn for aqueous medium (standard solution deposited onto Whatman paper), possibly because of the weakening of Zn-paper interactions or even by the formation of thermally more stable Zn oxides. Solid standards used for calibration in the 0.1–3.0 µg Fe and 5.0–50.0 ng Zn ranges were prepared with Whatman 903® paper discs impregnated with standard solutions of the analytes. Results for Fe and Zn determined by the proposed SS HR-CS GF AAS method were in agreement at a 95% confidence level (paired t-test) with those obtained by the comparative method (except for one sample) based on microwave-assisted acid digestion of blood and High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS F AAS). The limits of quantification were 10.2 mg/L (0.04 µg) for Fe and 1.2 mg/L (4.6 ng) for Zn. The relative standard deviation was < 10% (n = 12) for a sample containing 516 mg/L Fe and 8.7 mg/L Zn, and the sample throughput was equivalent to ca. 90 s per measurement.

Development of an Iron Internal Standard Method Using a Molecular Beam of Phosphorus Oxide for Determination of Nickel in Steel Samples by Continuous Source Flame Atomic Absorption Spectrometry

Development of an Iron Internal Standard Method Using a Molecular Beam of Phosphorus Oxide for Determination of Nickel in Steel Samples by Continuous Source Flame Atomic Absorption Spectrometry

Development of New Canned Chub Mackerel Products Incorporating Edible Seaweeds-Influence on the Minerals and Trace Elements Composition.

This study aimed to develop new canned chub mackerel products incorporating edible seaweeds (Ascophyllum nodosum, Fucus spiralis, Saccorhiza polyschides, Chondrus crispus, Porphyra sp. and Ulva sp.) harvested in the Portuguese North-Central coast, with simultaneous sensory improvement and minerals enrichment. Two processes were compared, namely the addition of seaweeds in i) the canning step and ii) in the brining step (as the replacement for salt). The concentrations of four macrominerals (Na, K, Ca and Mg), chloride, and twelve trace elements (Co, Cu, Fe, I, Li, Mn, Mo, Rb, Se, Sr, V and Zn) were determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS-FAAS) and inductively coupled plasma mass spectrometry (ICP-MS), respectively. Results showed that canned chub mackerel incorporating C. crispus and F. spiralis was found to be the preferred sensory option, also exhibiting contents enriched with Cl, Co, Cu, Fe, I, Li, Mg, Mn, Mo, Na, Rb, Se, and Sr. This effect was more pronounced when both seaweed species were added to replace the salt added in the brining step.