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The literature about direct solid sample analysis of the past 10-15 years using electrothermal atomic absorption spectrometry has been reviewed. It was found that in the vast majority of publications aqueous standards were reported as having been used for calibration after careful program optimization. This means the frequently expressed claim that certified reference materials with a matrix composition and analyte content close to that of the sample have to be used for calibration in solid sample analysis is not confirmed in the more recent literature. There are obviously limitations, and there are examples in the literature where even calibration with certified reference materials did not lead to accurate results. In these cases the problem is typically associated with spectral interferences that cannot be corrected properly by the systems available for conventional line source atomic absorption spectrometry, including Zeeman-effect background correction. Using high-resolution continuum source atomic absorption spectrometry, spectral interferences become visible owing to the display of the spectral environment at both sides of the analytical line at high resolution, which makes program optimization straightforward. Any spectrally continuous background absorption is eliminated automatically, and even rapidly changing background absorption does not cause any artifacts, as measurement and correction of background absorption are truly simultaneous. Any kind of fine-structured background can be eliminated by “subtracting” reference spectra using a least-squares algorithm. Aqueous standards are used for calibration in all published applications of high-resolution continuum source atomic absorption spectrometry to direct solid sample analysis.

The contents of lead, cadmium, chromium, copper, and nickel were determined in 25 tea samples from China, including green, yellow, white, oolong, black, Pu'er, and jasmine tea products, using high-resolution continuum source graphite furnace atomic absorption spectrometry. The methods used for sample preparation, digestion, and quantificational analysis were established, generating satisfactory analytical precisions (represented by relative standard deviations ranging from 0.6% to 2.5%) and recoveries (98.91–101.32%). The lead contents in tea leaves were 0.48–10.57 mg/kg, and 80% of these values were below the maximum values stated by the guidelines in China. The contents of cadmium and chromium ranged from 0.01 mg/kg to 0.39 mg/kg and from 0.27 mg/kg to 2.45 mg/kg, respectively, remaining in compliance with the limits stipulated by China's Ministry of Agriculture. The copper contents were 7.73–63.71 mg/kg; only 64% of these values complied with the standards stipulated by the Ministry of Agriculture. The nickel contents ranged from 2.70 mg/kg to 13.41 mg/kg. Consequently, more attention must be paid to the risks of heavy metal contamination in tea. The quantitative method established in this work lays a foundation for preventing heavy metal toxicity in human from drinking tea and will help establish regulations to control the contents of heavy metals in tea.

In this study, a simple and rapid sample preparation method named liquid-nitrogen-induced homogeneous liquid–liquid microextraction has been developed for the extraction and pre-concentration of Co(II) and Ni(II) ions before their analysis by flame atomic absorption spectrometry. For this purpose, first, acetonitrile containing 8-hydroxyquinoline is added into a sample solution and the mixture is vortexed. As a result, a homogeneous solution is formed. Subsequently, the solution is cooled using liquid nitrogen for a few seconds. By this process, due to difference in the freezing point of acetonitrile and water, the homogeneous state is broken and the analytes (as oxinate complexes) are extracted into liquid acetonitrile phase collected on top of the frozen aqueous phase. The linear dynamic ranges obtained for Ni(II) and Co(II) were 1.0–30 and 0.50–20 μg L−1, respectively. The obtained limits of detection were 0.36 and 0.20 μg L−1 for Ni(II) and Co(II), respectively.

The therapeutic dose of lithium (Li) compounds, which are widely used for the treatment of psychiatric and hematologic disorders, is close to its toxic level; therefore, drug monitoring protocols are mandatory. Herein, we propose a fast, simple, and low-cost analytical procedure for the traceable determination of Li concentration in human serum, based on the monitoring of the Li isotope dilution through the partially resolved isotope shift in its electronic transition around 670.80 nm using a commercially available high-resolution continuum source graphite furnace atomic absorption spectrometer. With this technique, serum samples only require acidic digestion before analysis. The procedure requires three measurements—an enriched 6Li spike, a mixture of a certified standard solution and spike, and a mixture of the sample and spike with a nominal 7Li/6Li ratio of 0.82. Lanthanum has been used as an internal spectral standard for wavelength correction. The spectra are described as the linear superposition of the contributions of the respective isotopes, each consisting of a spin-orbit doublet, which can be expressed as Gaussian components with constant spectral position and width and different relative intensity, reflecting the isotope ratio in the sample. Both the spectral constants and the correlation between isotope ratio and relative band intensity have been experimentally obtained using commercially available materials enriched with Li isotopes. The Li characteristic mass (mc) obtained corresponds to 0.6 pg. The procedure has been validated using five human serum certified reference materials. The results are metrologically comparable and compatible to the certified values. The measurement uncertainties are comparable to those obtained by the more complex and expensive technique, isotope dilution mass spectrometry.

In this study, a preconcentration strategy based on Ni(OH) 2 nanoflowers (NFs) was developed for the extraction/separation of bismuth ions from environmental water samples before the determination by flame atomic absorption spectrometry (FAAS). The homogeneous coprecipitation method was employed for the synthesis of the flower-shaped Ni(OH) 2 and used as an adsorbent for the preconcentration of bismuth. The extraction variables were determined by a univariate optimization strategy to obtain maximum extraction performance. The optimal parameters of the method were as follows: 15 min mechanical shaking at 120 rpm, pH 6.0 buffer solution (1.0 mL), 20 mg of sorbent, and 250 µL of 6.0 M nitric acid for the elution. Under the optimized instrumental and extraction conditions, LOD (limit of detection), LOQ (limit of quantitation), and linear dynamic range were determined as 2.8 µg/L, 9.4 µg/L, and 0.010–0.30 mg/L, respectively. The enhancement factor of the sorbent-based method was calculated as 139.1-folds by comparing the slopes of calibration plots obtained from FAAS and the preconcentration method. To assess the feasibility and reliability of the developed method, tap water and spring water samples were analyzed under optimized conditions. The satisfactory %recoveries were obtained close to 100% using the direct comparison method. The obtained results show that the presented method is a promising candidate for efficient extraction and trace determination of bismuth in several sample mediums.

In this work, a dispersive solid-phase extraction method based on Ni(OH) 2 nanoflowers (Ni(OH) 2 -NFs-DSPE) was developed to separate and preconcentrate copper ions from tap water samples for determination by flame atomic absorption spectrometry (FAAS). Ni(OH) 2 -NFs was synthesized using a homogeneous precipitation technique and used as sorbent for copper preconcentration. X-ray diffraction, scanning electron microscopy, and Fourier-transform infrared spectroscopy were used to characterize the synthesized sorbent. All experimental variables were carefully optimized to achieve a high enhancement factor of 107.5-folds with respect to the detection sensitivity of the conventional FAAS. The proposed method’s analytical parameters including LOD, LOQ, and linear range were determined as 1.33 μg/L, 4.42 μg/L, and 3.0–40 μg/L, respectively. To assess the applicability and reliability of the developed method, optimal conditions were applied to tap water samples and satisfactory percent recoveries (94–103%) were obtained for the samples spiked at 20 and 30 μg/L. This validated the accuracy and feasibility of the developed method to real samples. The developed method can be described as a simple, efficient, and rapid analytical approach for the accurate determination of trace copper ions in water samples.

A solid-phase microextraction (SPME) method had been applied to speciate chromium in natural and wastewater samples. MWCNTs@CuAl2O4@SiO2 nanocomposite was synthesized by sol–gel and calcination methods and then characterized using SEM, FTIR, and XRD techniques. MWCNTs@CuAl2O4@SiO2 was used to extract Cr(VI) as pyrrolidine dithiocarbamate chelates. Some analytical parameters involving pH, ligand (APDC) and adsorbent amounts, sample initial and final volume, and the effects of matrices were tested and optimized. For the oxidation of Cr(III) to Cr(VI), potassium permanganate was used, and after that, the presented method was applied to determine the total chromium levels. The calculations were carried out to obtain Cr(III) concentration by finding differences between total chromium and Cr(VI) concentrations. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 6.2 µg L−1 and 20.8 µg L−1, respectively. The proposed method was successfully applied for chromium speciation in wastewater samples.

The widely consumed vegetables, khat, lettuce, and Swiss chard, in Hirna town, West Hararghe, Ethiopia, are extensively cultivated through irrigation with an effluent-impacted river that flows through the town which denotes that monitoring the safety of the vegetables is crucial. Herein, the contents of Pb, Zn, Cu, Cr, and Cd in vegetables, water, and soils were determined by flame atomic absorption spectrometry after a wet digestion procedure based on a mixture of HNO 3 and HClO 4 at 200 °C. pH and electrical conductivity of the water and soil, and health risks associated with vegetable consumption were determined. The pH of the water (6.64) and soil (6.67) was slightly acidic, and electrical conductivity values were 0.416 and 0.024 mS/cm, respectively, indicating both are in good condition. The metal concentrations were in the range of ND–3.12, 3.43–9.22, and 0.15–10.6 mg/L in the water, soil, and vegetables, respectively, and the contents followed a trend of Cu > Zn > Cr > Pb > Cd. The irrigation water contained all metals above the guidelines except Cd, and the soil contained safe levels except Cd which is above the guideline. The obtained metal levels in the vegetables were below the safe limits. Estimated daily intakes and the total target cancer risks were below the guidelines, and the target hazard quotient and the hazard index were below 1 indicating that the vegetables are safe for consumption. In general, the obtained results suggest that the vegetables are safe for consumption. However, continuous monitoring and policy development are required to mitigate contamination of the river.

In this study, detection sensitivity of the conventional flame atomic absorption spectrophotometer (FAAS) for the determination of manganese (Mn 2+ ) was enhanced by employing a preconcentration method from wastewater samples. Flower-shaped Ni(OH) 2 nanomaterials were synthesized and used as sorbent material in preconcentration procedure. With the aim of attaining optimum experimental conditions, effective parameters of extraction method were optimized and these included pH of buffer solution, desorption solvent concentration and volume, mixing type and period, nanoflower amount, and sample volume. The detection limit of the optimized method was determined to be 2.2 μg L −1 , and this correlated to about 41-fold enhancement in detection power relative to direct FAAS measurement. Domestic wastewater was used to test the feasibility of the proposed method to real samples by performing spike recovery experiments. The wastewater sample was spiked at four different concentrations of manganese, and the percent recoveries determined were in the range of 95–120%.

Mercury (Hg) and its compounds are much concerned for their high toxicity and wide presence in the environment. Since the toxicity of Hg is species dependent, various methods have been developed for the speciation analysis of Hg. This review focus on the determination and speciation analysis of Hg chemical species in water, sediment, and soil samples. Recent developments on sample pre-treatment and extraction/pre-concentration, separation, and quantification of Hg chemical species, and associated analytical challenges have been reviewed and briefly discussed based on recent reports.