Ionic liquid assisted extraction induced by emulsion breaking for extraction of trace metals in diesel, gasoline and kerosene prior to ICP-OES analysis
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ABSTRACT:
SUBMITTER: Mdluli N
PROVIDER: S-EPMC10912242 | biostudies-literature | 2024 Feb
REPOSITORIES: biostudies-literature
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Project description:The determination of trace rare-earth elements (REEs) can be used for the assessment of environmental pollution, and is of great significance to the study of toxicity and toxicology in animals and plants. N, N, N', N'-tetraoctyl diglycolamide (TODGA) is an environmental friendly extractant that is highly selective to REEs. In this study, an analytical method was developed for the simultaneous determination of 16 trace REEs in simulated water samples by inductively coupled plasma optical emission spectroscopy (ICP-OES). With this method, TODGA was used as the extractant to perform the liquid-liquid extraction (LLE) sample pretreatment procedure. All 16 REEs were extracted from a 3 M nitric acid medium into an organic phase by a 0.025 M TODGA petroleum ether solution. A 0.03 M ethylenediaminetetraacetic acid disodium salt (EDTA) solution was used for back-extraction to strip the REEs from the organic phase into the aqueous phase. The aqueous phase was concentrated using a vacuum rotary evaporator and the concentration of the 16 REEs was detected by ICP-OES. Under the optimum experimental conditions, the limits of detection (3σ, n = 7) for the REEs ranged from 0.0405 ng mL-1 (Nd) to 0.5038 ng mL-1 (Ho). The relative standard deviations (c = 100 ng mL-1, n = 7) were from 0.5% (Eu) to 4.0% (Tm) with a linear range of 4-1000 ng mL-1 (R2 > 0.999). The recoveries of 16 REEs ranged from 95% to 106%. The LLE-ICP-OES method established in this study has the advantages of simple operation, low detection limits, fast analysis speed and the ability to simultaneously determine 16 REEs, thereby acting as a viable alternative for the simultaneous detection of trace amounts of REEs in water samples.
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Project description:To overcome the corrosion of hydrofluoric acid on the ICP OES injection system in the acid dissolution system, this paper makes some improvements based on the traditional open digestion. The improved method does not require the complete removal of hydrofluoric acid. After appropriate digestion of the sample with a mixed acid, the solution can be transferred to a colorimetric tube containing ammonium hydroxide solution to give the final volume for analysis. In this paper, two-point standard curves are plotted using soil standards and process blanks, which is not only convenient but also overcomes the interference of the matrix effect. Through continuous experiments, the preferred ratio of mixed acid is 3 mL nitric acid + 5 mL hydrofluoric acid, and the concentration of ammonia solution is 0.5%. The spectral lines of the measured elements V (292.4), Cr (283.5), Co (228.6), Ni (231.6), Cu (324.7), Zn (213.8) and Pb (220.3) were determined. The method quantification limits of the seven measured elements V, Cr, Co, Ni, Cu, Zn and Pb were 0.909, 4.32, 0.269, 0.261, 0.968, 3.69 and 2.64 μg g-1, respectively, and the precision was 3.5%, 5.2%, 4.8%, 2.4%, 6.1% and 4.5%, respectively. After processing six national standard materials according to the experimental method, the measured values of each measured element were basically in agreement with the certified values, indicating that this method is fully feasible for the measurement of V, Cr, Co, Ni, Cu, Zn and Pb in soil. This method greatly improves the efficiency of pretreatment and is particularly suitable for analysing large batches of samples.
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Project description:This work describes a greener and cost-effective microwave-assisted hydrogen peroxide digestion (MA-HPD) with the addition of 1 mL of HNO3 (70% v/v) to enhance extraction of selected metals (Al, Ba, Cd, Co, Cr, Cu, Mg, Na, Ni, Pb, Sb, Ti and V) in crude-oil, diesel, gasoline and kerosene samples prior to inductively coupled plasma-optical emission spectroscopic (ICP-OES) analysis. The most influential parameters of the MA-HPD method were investigated by using multivariate optimization tools (two-level full factorial and central composite designs) and fuel oil certified reference material (NIST1634c). The optimum conditions were observed to be 245 ℃ microwave temperature, 25 min digestion time, 0.1 g sample mass and 5 M H2O2 were the optimum digestion conditions with accepted accuracy (104.8-117.7%) and precision (≤ 4.1%). In overall, the metals that reported high concentrations in the crude oil, diesel, gasoline, and kerosene samples were Na (51.94-58.86 mg/kg) and Mg (36.08-47.4 mg/kg), while Cu was the lowest (0.55-2.89 mg/kg). When comparing the obtained concentration levels with other literature reports, a conclusion can be drawn that South Africa is importing oils of reasonable quality.
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Project description:We have compared the analytical results obtained by inductively coupled plasma optical emission spectroscopy (ICP-OES) and by scanning electron microscopy with an energy dispersive X-ray analytical system (SEM-EDX) in order to explore the mechanism of metal ions biosorption by biomass using two independent methods. The marine macroalga Enteromorpha sp. was enriched with Cu(II), Mn(II), Zn(II), and Co(II) ions via biosorption, and the biosorption capacity of alga determined from the solution and biomass composition before and after biosorption process was compared. The first technique was used to analyze the composition of the natural and metal-loaded biomass, and additionally the composition of the solution before and after biosorption. The second technique was used to obtain a picture of the surface of natural and metal ion-loaded macroalgae, to map the elements on the cell wall of dry biomass, and to determine their concentration before and after biosorption. ICP-OES showed a better precision and lower detection limit than EDX, but SEM-EDX gave more information regarding the sample composition of Enteromorpha sp. Both techniques confirmed that biosorption is a surface phenomenon, in which alkali and alkaline earth metal ions were exchanged by metal ions from aqueous solution.FigureThe advantages and disadvantages of ICP-OES and SEM-EDX techniques ELECTRONIC SUPPLEMENTARY MATERIAL: The online version of this article (doi:10.1007/s00604-010-0468-0) contains supplementary material, which is available to authorized users.
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Project description:Bredemeyera floribunda Willd (B. floribunda) is a medicinal plant used by the Brazilian rural population to treat snakebites, but there are no data on the elemental composition and stability of the emulsion of extract of this plant. In this article, we present for the first time data on contents obtained the roots of the medicinal plant B. floribunda by using inductively coupled plasma optical spectrometry (ICP OES), as well as the data on preliminary stability tests of emulsions formulated with aqueous extract of this plant. The first set of data shows a total of 13 elements (Al, Ca, Cr, Fe, K, Mg, Mn, Na, Ni, P, Cu, Se and Zn) detected in the roots of the plant. The second set of data shows that the extract data of the B. floribunda roots presented an emulsifying potential. In addition, the article provides information on the heating program for microwave oven digestion and ICP OES operating conditions. The data presented make way for nutritional and toxicological studies involving the roots of B. floribunda. The data on the cataloging of the plant can be found in the deposit nº 54366 of the Herbarium of the Federal University of Mato Grosso do Sul, available in www.splink.org.br/form?lang=pt&collectioncode=CGMS.
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Project description:Progress improving zinc nutrition globally is slowed by limited understanding of population zinc status. This challenge is compounded when small differences in measurement can bias the determination of zinc deficiency rates. Our objective was to evaluate zinc analytical accuracy and precision among different instrument types and sample matrices using a standardized method. Participating laboratories analyzed zinc content of plasma, serum, liver samples, and controls, using a standardized method based on current practice. Instrument calibration and drift were evaluated using a zinc standard. Accuracy was evaluated by percent error vs. reference, and precision by coefficient of variation (CV). Seven laboratories in 4 countries running 9 instruments completed the exercise: 4 atomic absorbance spectrometers (AAS), 1 inductively coupled plasma optical emission spectrometer (ICP-OES), and 4 ICP mass spectrometers (ICP-MS). Calibration differed between individual instruments up to 18.9% (p < 0.001). Geometric mean (95% CI) percent error was 3.5% (2.3%, 5.2%) and CV was 2.1% (1.7%, 2.5%) overall. There were no significant differences in percent error or CV among instrument types (p = 0.91, p = 0.15, respectively). Among sample matrices, serum and plasma zinc measures had the highest CV: 4.8% (3.0%, 7.7%) and 3.9% (2.9%, 5.4%), respectively (p < 0.05). When using standardized materials and methods, similar zinc concentration values, accuracy, and precision were achieved using AAS, ICP-OES, or ICP-MS. However, method development is needed for improvement in serum and plasma zinc measurement precision. Differences in calibration among instruments demonstrate a need for harmonization among laboratories.
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Project description:Very little is known about how the elemental composition (ionome) of an insect cuticle varies as a result of different colouration. Using inductively-coupled plasma optical emission spectrometry (ICP-OES), we established ionomic profiles in microsamples of two adjacent regions of an insect cuticle with a contrasting colour pattern, namely, the black and orange regions of the elytra of the aposematic burying beetle Nicrophorus vespillo. The analysis revealed 53 elements (ranging in atomic weight from Na to Bi) occurring above the detection limit. The frequency of detectability of individual elements varied strongly, and only ten elements (Ba, Cu, Fe, K, Mg, Mn, P, Rb, Sb and Zn) were present in concentrations exceeding the detection limit in all the samples. The sum of concentrations of all elements in the orange regions of the elytra was 9% lower than in the black ones. The opposite distribution was displayed by the rare earth elements (REEs), the sum of which was 17% lower in the black elytral regions than in the orange ones. The concentrations of six elements were significantly higher in the black than in the orange regions: Al (by 97%), Cu (41%), Mn (14%), Na (46%), Se (97%) and W (47%). The concentrations of essential elements measured in both the black and orange regions exhibited very considerable variance: Ca (σ2 = 1834; 1882, respectively), K (145; 82) P (97; 76), Na (84; 53), Mg (24; 26) and Ba (9; 13). This, in part, could be attributed to individual differences, e.g. those resulting from the consumption of animal carcasses of different quality/chemical composition, but interference between elements and the consequent lowering of measurement quality are also possible. We highlight the fact that deeper insight into the basic relationship between insect colouration and variation in elemental composition requires micro-sampling of the homogeneous layers of an exoskeleton.
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Project description:This work reports the preparation of a novel Cu(II)-ion imprinted polymer using 2-thiozylmethacrylamide (TMA) for on-line preconcentration of Cu(II) prior to its determination by inductively coupled optical emission spectroscopy (ICP-OES). Cu(II)-TMA monomer (complex) was synthesized and copolymerized via bulk polymerization method in the presence of ethyleneglycoldimethacrylate cross-linker. The resulting polymer was washed with 5% (v/v) HNO3 to remove Cu(II) ions and then with water until a neutral pH. The ion imprinted polymer was characterized by FT-IR and scanning electron microscopy. The experimental conditions were optimized for on-line preconcentration of Cu(II) using a minicolumn of ion imprinted polymer (IIP). Quantitative retention was achieved between pH 5.0 and 6.0, whereas the recoveries for the non-imprinted polymer (NIP) were about 61%. The IIP showed about 30 times higher selectivity to Cu(II) in comparison to NIP. The IIP also exhibited excellent selectivity for Cu(II) against the competing transition and heavy metal ions, including Cd, Co, Cr, Fe, Mn, Ni, Pb and Zn. Computational calculations revealed that the selectivity of IIP was mediated by the stability of Cu(II)-TMA complex which was far more stable than those of Co(II), Ni(II) and Zn(II) that have similar charge and ionic radii to Cu(II). A volume of 10 mL sample solution was loaded onto the column at 4.0 mL min-1 by using a sequential injection system (FIALab 3200) followed by elution with 1.0 mL of 2% (v/v) HNO3. The relative standard deviation (RSD) and limit of detection (LOD, 3s) of the method were 3.2% and 0.4 μg L-1, respectively. The method was successfully applied to determination of Cu(II) in fish otoliths (CRM 22), bone ash (SRM 1400) and coastal seawater and estuarine water samples.
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Project description:Minerals are inorganic compounds that are essential to the support of a variety of biological functions. Understanding the range and variability of the content of these minerals in biological samples can provide insight into the relationships between mineral content and the health of individuals. In particular, abnormal mineral content may serve as an indicator of illness. The development of robust, reliable analytical methods for the determination of the mineral content of biological samples is essential to developing biological models for understanding the relationship between minerals and illnesses. This paper describes a method for the analysis of the mineral content of small volumes of serum and whole blood samples from healthy individuals. Interday and intraday precision for the mineral content of the blood (250 ?L) and serum (250 ?L) samples was measured for eight essential minerals--sodium (Na), calcium (Ca), magnesium (Mg), potassium (K), iron (Fe), zinc (Zn), copper (Cu), and selenium (Se)--by plasma spectrometric methods and ranged from 0.635 to 10.1% relative standard deviation (RSD) for serum and 0.348-5.98% for whole blood. A comparison of the determined ranges for ten serum samples and six whole blood samples provided good agreement with literature reference ranges. The results demonstrate that the digestion and analysis methods can be used to reliably measure the content of these minerals and potentially of other minerals.
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Project description:A high-resolution analysis of the distribution of major and trace elements across the Cretaceous/Paleogene boundary (KPgB) in the distal section of Agost (SE Spain) was performed. The KPgB sediments were drilled to recover a 22 cm-long core; the lower 5 cm corresponding to the uppermost Maastrichtian and the upper 17 cm to the lowermost Danian. The unconsolidated sediments were resin-embedded under O2-free conditions, cut and polished. Laser Ablation-Inductivity Coupled Plasma-Mass Spectrometry (LA-ICP-MS) analyses were conducted at 10 µm increments and a laser-beam of 80 µm. Discrete samples were taken immediately prior to the resin-embedding and analyzed by Inductivity Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). Results obtained by both analytical methods (LA-ICP-MS and ICP-OES) are presented. (Further interpretations and discussion are included in Sosa-Montes de Oca et al., 2018 [6]).
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