Determination of ultra-trace amounts of cadmium by ET-AAS after column preconcentration with a new sorbent of modified MWCNTs

The present research reports on the application of modified multiwalled carbon nanotubes as a new, easily prepared, and stable solid sorbent for the column preconcentration of ultra-trace amounts of cadmium in aqueous solution. Multiwalled carbon nanotubes were oxidized with concentrated HNO₃ and modified with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol and then were used as a solid phase for the column preconcentration of Cd(II). Elution was carried out with 0.5 mol?L^?1 HNO₃. The amount of eluted Cd(II) was measured using electrothermal atomic absorption spectrometry. Various parameters such as pH, sample and eluent flow rate, eluent concentration, breakthrough volume, and interference of a great number of anions and cations on the retention of analyte on sorbent were studied. Under the optimized conditions, the calibration graph was linear in the range of 0.67 ng?L^?1 to 5.0 μg?L^?1 and the detection limit (3S_b, n?=?7) was 0.14 ng?L^?1 in initial solution. A preconcentration factor of 300 and relative standard deviations of ±3.6 % for seven successive determinations of 3 ng of Cd(II) were achieved. The column preconcentration was successfully applied to the analysis of river water, waste water, and Persian Gulf water sample.     

FIA-coupled spectrophotometric method for determination of Cr (VI) traces in natural waters: application of in-line dissolution of 1,5-diphenylcarbazide after heat treatment and activated alumina as adsorbent for preconcentration

This work proposes the quantification of Cr (VI) ions in natural waters in trace level, using activated alumina (Al₂O₃) as preconcentration support, controlled in-line dissolution of the solidified chromophore diphenylcarbazide after heat treatment and spectrophotometric detection. The manifold ensures high sensitivity of analytical response, good repeatability, and stability. In this work, optimization of experimental conditions of a flow injection system was chosen as the parameters for greater sensitivity and better selectivity. The selected optimized conditions were 0.30 mol L^?1 for H₂SO₄ concentration, system flow rate as 0.40 mL min^?1, sample injection volume of 192.50 μL, 2 min for preconcentration time, and 0.10 mol L^?1 for eluent concentration. The analytical curves obtained for real sample analysis show linear range from 0.192 to 0.961 μM, linear correlation coefficient R?=?0.9997 and LOD?=?0.024 μM. The preconcentration factor of about four times was obtained through the passage of 800 μL of a standard solution containing 0.961 μM of Cr (VI) through mini-column of preconcentration followed by elution at 192.5 μL of NH₄OH 0.1 mol L^?1 solution. The solid chromogenic reagent presented high durability (weeks in daily use with mass of 0.0993 g) and good reproducibility in analytical signal. The reactivation of the mini-column of alumina should be executed after ten injections of eluent, using 800 μL of HCl 0.02 mol L^?1 solution in flow through the same. Each cycle of injection and elution of the sample takes about 5 min on the proposed terms. Despite the length of each cycle still be high, low concentrations can be detected using a technique of relatively low cost. This is due in part, the association dissolution of the chromogenic reagent directly in the line and the preconcentration step. Another important factor is the economy of reagent chromogenic, low generation of reject contributing to better quality of the environment, and the high potential for applications to work in field.     

Solid-phase extraction and separation procedure for trace aluminum in water samples and its determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS)

In the present study, a separation/preconcentration procedure for determination of aluminum in water samples has been developed by using a new atomic absorption spectrometer concept with a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator, and a charge-coupled device array detector. Sample solution pH, sample volume, flow rate of sample solution, volume, and concentration of eluent for solid-phase extraction of Al chelates with 4-[(dicyanomethyl)diazenyl] benzoic acid on polymeric resin (Duolite XAD-761) have been investigated. The adsorbed aluminum on resin was eluted with 5 mL of 2 mol L^-1 HNO₃ and its concentration was determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimal conditions, limit of detection obtained with HR-CS FAAS and Line Source FAAS (LS-FAAS) were 0.49 μg L^?1 and 3.91 μg L^?1, respectively. The accuracy of the procedure was confirmed by analyzing certified materials (NIST SRM 1643e, Trace elements in water) and spiked real samples. The developed procedure was successfully applied to water samples.     

Flow injection online spectrophotometric determination of uranium after preconcentration on XAD-4 resin impregnated with nalidixic acid

In this work, spectrophotometer was used as a detector for the determination of uranium from water, biological, and ore samples with a flow injection system coupled with solid phase extraction. In order to promote the online preconcentration of uranium, a minicolumn packed with XAD-4 resin impregnated with nalidixic acid was utilized. The system operation was based on U(VI) ion retention at pH 6 in the minicolumn at flow rate of 15.2 mL min^?1. The uranium complex was removed from the resin by 0.1 mol dm^?3 HCl at flow rate of 3.2 mL min^?1 and was mixed with arsenazo III solution (0.05 % solution in 0.1 mol dm^?3 HCl, 3.2 mL min^?1) and driven to flow through cell of spectrophotometer where its absorbance was measured at 651 nm. The influence of chemical (pH and HCl (as eluent and reagent medium) concentration) and flow (sample and eluent flow rate and preconcentration time) parameters that could affect the performance of the system as well as the possible interferents was investigated. At the optimum conditions for 60 s preconcentration time (15.2 mL of sample volume), the method presented a detection limit of 1.1 μg L^?1, a relative standard deviation (RSD) of 0.8 % at 100 μg L^?1, enrichment factor of 30, and a sample throughput of 42 h^?1, whereas for 300 s of the preconcentration time (76 mL of sample volume), a detection limit of 0.22 μg L^?1, a RSD of 1.32 % at 10 μg L^?1, enrichment factor of 150, and a sampling frequency of 11 h^?1 were reported.     

The use of silica gel modified with allyl 6-methyl-4-phenyl-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate for selective separation and preconcentration of lead in environmental samples

The aim of the present work is the assessment of a new sorbent, prepared using silica gel coated with a pyrimidine derivative (allyl 6-methyl-4-phenyl-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate), for extraction and preconcentration trace amount of lead from different samples prior to determination by flame atomic absorption spectrometry. Common coexisting ions did not interfere with the separation and determination of lead at pH?6, so that lead ion completely adsorbed on the column. The limit of detection based on three times the standard deviation of the blank was found to be 0.53 ng?mL^?1 in original solution. Obtained sorption capacity for 1 g sorbent was 5.0 mg Pb. The linearity was maintained in the concentration range of 0.1–30.0 ng?mL^?1 for the concentrated solution. Eight replicate determinations of 2.0 μg?mL^?1 of lead in the final solution gave relative standard deviation of ±2.6 %. The proposed method was successfully applied to the determination trace amounts of lead in the environmental samples such as carrot, rice, zardchoobe, and real water samples.     

Preconcentration of metal ions through chelation on a synthesized resin containing O, O donor atoms for quantitative analysis of environmental and biological samples

Nascent Amberlite XAD-4 has been used as the polymeric support for the synthesis of a stable extractor of metal ions, by incorporating phthalic acid through azo bridging. Elemental analyses and infra-red spectral and thermal studies were carried out for its characterization. The water regain value and hydrogen ion capacity were found to be 12.50 and 5.75 mmol g^?1, respectively. The optimum pH range for the maximum sorption of Ni(II), Mn(II), Cu(II), Zn(II), Cd(II), Cr(III), and Co(II) was observed at pH 5.5–8.0 with the corresponding half-loading time (t _1/2) of 9, 5, 9, 9, 3, 9, and 5 min, respectively. The preconcentration factor for Ni(II), Mn(II), Cu(II), Zn(II), Cd(II), Cr(III), and Co(II) are 190, 190, 190, 180, 180, 160, and 160, with the corresponding limit of preconcentration in the range of 5.25–6.25 μg L^?1. The detection limits, for flame atomic absorption spectrophotometry, were found to be 0.62, 0.60, 0.65, 0.75, 0.72, 0.84, and 0.85 μg L^?1, respectively. Method has been successfully applied to the analysis of water samples, multivitamin formulations, infant food substitutes, hydrogenated oil, and fishes.     

Rapid spectrophotometric determination of trace amounts of palladium in water samples after dispersive liquid–liquid microextraction

A simple, rapid, and efficient dispersive liquid–liquid microextraction method, followed by UV–Vis spectrophotometry was developed for the preconcentration and determination of Pd ions in water samples. Pd ions react with α-furildioxime (chelating agent) to form a hydrophobic complex. Various parameters were altered to study and optimize their effects on the extraction efficiency, such as pH, ligand concentration, the type and volume of extraction and dispersive solvents, extraction time, and salt concentration. Under optimized conditions, the method exhibited an enrichment factor (C _org/C _aq) of 25 and recovery more than 98 % within a very short extraction time. The linearity of the method ranged from 10 to 200 μg?L^?1. The limit of detection was 1.1 μg?L^?1. The relative standard deviation for the concentration of 100 μg?L^?1 of Pd was 2.3 % (n?=?10). Finally, the developed method was successfully applied to the extraction and determination of Pd in tap, river, mineral, and sea water samples.     

Coupling of solvent-based de-emulsification dispersive liquid–liquid microextraction with high performance liquid chromatography for simultaneous simple and rapid trace monitoring of 2,4-dichlorophenoxyacetic acid and 2-methyl-4-chlorophenoxyacetic acid

A simple, rapid, and efficient sample pretreatment technique, based on solvent-based de-emulsification dispersive liquid–liquid microextraction (SD-DLLME), followed by high performance liquid chromatography (HPLC) has been developed for simultaneous preconcentration and trace detection of 2,4-dichlorophenoxyacetic acid (2,4-D) and 2-methyl-4-chlorophenoxyacetic acid (MCPA) in water and urine samples. Some parameters such as acidity of solution, the amount of salt, type, and volume of extraction solvents, type of disperser/de-emulsifier solvent, and its volume were investigated and optimized. Under optimum extraction conditions, the limits of detections (LODs) of this method for MCPA and 2,4-D were 0.2 and 0.6 μg L^?1 (based on 3S_b/m) in water and 0.4 and 1.6 μg L^?1 in urine, respectively. Furthermore, dynamic linear range of this method for MCPA and 2,4-D was 1–300 and 2–400 μg L^?1, repectively. Finally, the applicability of the proposed method was evaluated by extraction and determination of the herbicides in urine and different water samples.     

Monitoring of trace amounts of heavy metals in different food and water samples by flame atomic absorption spectrophotometer after preconcentration by amine-functionalized graphene nanosheet

We are introducing graphene oxide modified with amine groups as a new solid phase for extraction of heavy metal ions including cadmium(II), copper(II), nickel(II), zinc(II), and lead(II). Effects of pH value, flow rates, type, concentration, and volume of the eluent, breakthrough volume, and the effect of potentially interfering ions were studied. Under optimized conditions, the extraction efficiency is >97 %, the limit of detections are 0.03, 0.05, 0.2, 0.1, and 1 μg L^?1 for the ions of cadmium, copper, nickel, zinc, and lead, respectively, and the adsorption capacities for these ions are 178, 142, 110, 125, and 210 mg g^?1. The amino-functionalized graphene oxide was characterized by thermogravimetric analysis, transmission electron microscopy, scanning electron microscopy, and Fourier transform infrared spectrometry. The proposed method was successfully applied in the analysis of environmental water and food samples. Good spiked recoveries over the range of 95.8–100.0 % were obtained. This work not only proposes a useful method for sample preconcentration but also reveals the great potential of modified graphene as an excellent sorbent material in analytical processes.     

Assessment of the labile fractions of copper and zinc in marinas and port areas in Southern Brazil

The dissolved labile and labile particulate fractions (LPF) of Cu and Zn were analyzed during different seasons and salinity conditions in estuarine waters of marina, port, and shipyard areas in the southern region of the Patos Lagoon (RS, Brazil). The dissolved labile concentration was determined using the diffusive gradients in thin films technique (DGT). DGT devices were deployed in seven locations of the estuary for 72 h and the physicochemical parameters were also measured. The LPF of Cu and Zn was determined by daily filtering of water samples. Seasonal variation of DGT–Cu concentrations was only significant (p?<?0.05) at one shipyard area, while DGT–Zn was significant (p?<?0.05) in every locations. The LPF of Cu and Zn concentrations demonstrated seasonal and spatial variability in all locations, mainly at shipyard areas during high salinity conditions. In general, except the control location, the sampling locations showed mean variations of 0.11–0.45 μg?L^?1 for DGT–Cu, 0.89–9.96 μg?L^?1 for DGT–Zn, 0.65–3.69 μg?g^?1 for LPF–Cu, and 1.35–10.87 μg?g^?1 for LPF–Zn. Shipyard areas demonstrated the most expressive values of labile Cu and Zn in both fractions. Strong relationship between DGT–Zn and LPF–Zn was found suggesting that the DGT–Zn fraction originates from the suspended particulate matter. Water salinity and suspended particulate matter content indicated their importance for the control of the labile concentrations of Cu and Zn in the water column. These parameters must be taken into consideration for comparison among labile metals in estuaries.     

Application of zirconium–iridium permanent modifier for the simultaneous determination of lead, cadmium, arsenic, and nickel in atmospheric particulate matter by multi-element electrothermal atomic absorption spectrometry

A novel and robust method for the simultaneous determination of lead, cadmium, arsenic, and nickel in atmospheric particulate matter by multi-element electrothermal atomic absorption spectrometry was developed, using zirconium–iridium coating as permanent modifier (140 μg Zr and 4 μg Ir). After 300 atomization cycles, it was necessary to add 2 μg of Ir. Due to the varying concentrations of Pb in atmospheric particulate matter, lead was monitored at two wavelengths, at the less sensitive line of 261.4 nm for high concentration samples (>20 μg?L^?1) or at 283.3 nm for the low concentration samples. Matrix-matched calibration had to be performed for quantitative recoveries (96–102 %). Following this approach, the four elements were determined in atmospheric particulate matter samples from an industrial area near the city of Athens in two different time periods (cold–warm) with limits of detection of 5.5 ng?m^?3 for Pb at 261.4 nm and 0.29 ng?m^?3 at 283.3 nm, 0.019 ng?m^?3 for Cd, 0.14 ng?m^?3 for As, and 0.22 ng?m^?3 for Ni. Lead, Cd, and As levels were very low, whereas Ni content was at comparable levels with other areas worldwide.     

Hazard assessment of metals in invasive fish species of the Yamuna River,India in relation to bioaccumulation factor and exposure concentration for human health implications

Monitoring of heavy metals was conducted in the Yamuna River considering bioaccumulation factor, exposure concentration, and human health implications which showed contamination levels of copper (Cu), lead (Pb), nickel (Ni), and chromium (Cr) and their dispersion patterns along the river. Largest concentration of Pb in river water was 392 μg L^?1; Cu was 392 μg L^?1 at the extreme downstream, Allahabad and Ni was 146 μg L^?1 at midstream, Agra. Largest concentration of Cu was 617 μg kg^?1, Ni 1,621 μg kg^?1 at midstream while Pb was 1,214 μg kg^?1 at Allahabad in surface sediment. The bioconcentration of Cu, Pb, Ni, and Cr was observed where the largest accumulation of Pb was 2.29 μg kg^?1 in Oreochromis niloticus and 1.55 μg kg^?1 in Cyprinus carpio invaded at Allahabad while largest concentration of Ni was 174 μg kg^?1 in O. niloticus and 124 μg kg^?1 in C. carpio in the midstream of the river. The calculated values of hazard index (HI) for Pb was found more than one which indicated human health concern. Carcinogenic risk value for Ni was again high i.e., 17.02?×?10^?4 which was larger than all other metals studied. The results of this study indicated bioconcentration in fish due to their exposures to heavy metals from different routes which had human health risk implications. Thus, regular environmental monitoring of heavy metal contamination in fish is advocated for assessing food safety since health risk may be associated with the consumption of fish contaminated through exposure to a degraded environment.     

Application of cold-induced aggregation microextraction as a fast,simple, and organic solvent-free method for the separation and preconcentration of Se(IV) in rice and various water samples

The developed method is based on cold-induced aggregation microextraction of Se(IV) using the 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid as an extractant followed by spectrophotometry determination. The extraction of Se(IV) was performed in the presence of dithizone as the complexing agent. In this method, a very small amount of 1-butyl-3-methylimidazolium hexafluorophosphate was added to the sample solution containing Se-dithizone complex. Then, the solution was kept in a thermostated bath at 50 °C for 4 min. Subsequently, the solution was cooled in an ice bath and a cloudy solution was formed. After centrifuging, the extractant phase was analyzed using a spectrophotometric detection method. Some important parameters that might affect the extraction efficiency were optimized (HCl, 0.6 mol L^?1; dithizone, 4.0?×?10^?6 mol L^?1; ionic liquid, 100 μL). Under the optimum conditions, good linear relationship, sensitivity, and reproducibility were obtained. The limit of detection (LOD) (3S_b/m) was 1.5 μg L^?1, and the relative standard deviation (RSD) was 1.2 % for 30 μg L^?1 of Se(IV). The linear range was obtained in the range of 5–60 μg L^?1. It was satisfactory to analyze rice and various water samples.     

Assessment of cylindrospermopsin toxin in an arid Saudi lake containing dense cyanobacterial bloom

This study reports the presence of the cyanobacterial toxin cylindrospermopisn (CYN) and its producer Cylindrospermopsis raciborskii for the first time in Saudi freshwater sources. C. raciborskii was found in Gazan Dam Lake water with two morphotypes (coiled and straight). The appearance and cell density of this species was significantly positively related to high temperature and high ammonium concentrations, and negatively with nitrate and phosphate concentrations in the lake. Intracellular concentrations of CYN (4–173 μg L^?1) were associated with C. raciborskii rather than other cyanobacteria with a maximal value obtained in June 2011, coinciding with the highest bloom of this species (19?×?10⁷ trichome L^?1). CYN cell quotas (0.6–14.6 pg cell^?1) varied significantly along the study period and correlated with most environmental factors. The results of ELISA and liquid chromatography-mass spectrometry proved that the CYN production by strains of this species was isolated from this lake during the present study, with an amount reaching 568 μg g^?1. Extracellular CYN was also detected in cell-free lake water at concentrations 0.03–23.3 μg L^?1, exceeding the drinking water guideline value of 1 μg L^?1 during the Apr–Jul period. As this lake is an important source for drinking and irrigation waters, CYN monitoring should be included in the environmental and health risk assessment plans of these water bodies.     

UV/H2O2 oxidation of arsenic and terbuthylazine in drinking water

Arsenic is a widespread contaminant in the environment. The intake of water containing high concentrations of arsenic could have serious impact on human health, such as skin and lung cancer. In the European Union, thus, also in Italy, the arsenic limit in drinking water is 10 μg L^?1. Several water remediation treatment technologies are available for arsenic removal. For some processes, the removal efficiencies can be improved after an oxidation step. Most full-scale applications are based on conventional oxidation processes for chemical micropollutant removal. However, if water contains arsenic and refractory organic contaminants, the advanced oxidation processes could be considered. The aim of this work was to investigate the effectiveness of ultraviolet (UV) radiation alone and in combination with hydrogen peroxide for the oxidation of arsenic and terbuthylazine (TBA). The experimental tests were performed in groundwater at the laboratory scale (0.1 mg L^?1 As(III) and 10 μg L^?1 TBA). Hydrogen peroxide alone (15 mg L^?1) was ineffective on both arsenic and TBA oxidation; the 253.7-nm radiation alone did not oxidize arsenic(III), but photolyzed efficiently TBA (52 % removal yield at a UV dose of 1,200 mJ cm^?2). The UV/H₂O₂ advanced oxidation (UV dose 600–2,000 mJ cm^?2, 5–15 mg L^?1 H₂O₂) was the most effective process for the oxidation of both arsenic and TBA, with observed oxidation efficiencies of 85 and 94 %, respectively, with 5 mg L^?1 H₂O₂ and a UV dose of 2,000 mJ cm^?2.     

Assessment of physico-chemical qualities and heavy metal concentrations of Umgeni and Umdloti Rivers in Durban,South Africa

We assessed the effects of seasonal dynamics on the physico-chemical qualities and heavy metals concentrations of the Umgeni and Umdloti Rivers in Durban, South Africa. Water samples were taken from nine different sampling points and analysed for the following parameters; temperature, pH, turbidity, electrical conductivity (EC), biological oxygen demand (BOD₅), chemical oxygen demand (COD), phosphate (PO₄ ^2?), nitrate (NO₃ ^2?), ammonium (NH₄ ⁺), sulphate (SO₄ ^2?), lead (Pb²⁺), mercury (Hg²⁺), cadmium (Cd²⁺), aluminium (Al³⁺), and copper (Cu²⁺) using standard methods. The data showed variations it terms of the seasonal fluctuations and sampling regime as follows: temperature 12–26.5 °C; pH 5.96–8.45; turbidity 0.53–18.8 NTU; EC 15.8–5180 mS m^?1; BOD₅ 0.60–7.32 mg L^?1; COD 10.5–72.9 mg L^?1; PO₄ ^2??<?500–2,460 μg L^?1; NO₃ ^2? <0.05–4.21 mg L^?1; NH₄ ⁺?<?0.5–1.22 mg L^?1; SO₄ ^2? 3.90–2,762 mg L^?1; Pb²⁺ 0.023–0.135 mg L^?1; Hg²⁺ 0.0122–0.1231 mg L^?1 Cd²⁺ 0.068–0.416 mg L^?1; Al³⁺ 0.037–1.875 mg L^?1, and Cu²⁺0.006–0.144 mg L^?1. The concentrations of most of the investigated parameters exceeded the recommended limit of the South African Guidelines and World Health Organization tolerance limits for freshwater quality. We conclude that these water bodies are potentially hazardous to public health and this highlights the need for implementation of improved management strategies of these river catchments for continued sustainability.     

Metal pollution and ecological risk assessment in marine sediments of Karachi Coast, Pakistan

Concentrations of 12 metals (Fe, Mn, Cr, Mo, Ni, Pb, Se, Sr, U, V, Zn, and Zr) in surface sediments of Karachi Coast, Pakistan were determined to evaluate their distribution and pollution assessment. The measured metals in the sediments were found to be in the range of Fe, 0.84–6.96 %; Mn, 300–1,300 μg/g; Cr, 12.0–319.84 μg/g; Mo, 0.49–2.03 μg/g; Ni, 1.53–58.86 μg/g; Pb, 9.0–49.46 μg/g; Se, 0.25–.86 μg/g; Sr, 192–1185 μg/g; U, 0.19–1.66 μg/g; V, 15.80–118.20 μg/g; Zn, 15.60–666.28 μg/g; and Zr, 44.02–175.26 μg/g. The mean contents of the metal studied were: Fe, 3.07 %, Mn, 0.05 %; Cr, 96.75 μg/g; Mo, 1.34 μg/g; Ni, 31.39 μg/g; Pb, 23.24 μg/g; Se, 0.61 μg/g; Sr, 374.83 μg/g; U, 0.64 μg/g; V, 61.75 μg/g; Zn, 204.75 μg/g; and Zr:76.27 μg/g, and arrangement of the metals from higher to lower mean content in this area is: Fe?>?Zn?>?Mn?>?Sr?>?Zn?>?Cr?>?Zr?>?V?>?Ni?>?Pb?>?Mo?>?U?>?Se. There is no significant correlation among most of these metals, indicating different anthropogenic and natural sources. To assess ecotoxic potential of marine sediments, Numerical Sediment Quality Guidelines were also applied. The concentration of Pb in all the sediments except one was lower than the threshold effect concentration (TECs) showing that there are no harmful effects to marine life from Pb. On the other hand, the concentrations of Cr, Ni, and Zn exceeded TEC in three stations, indicating their potential risk. The degree of pollution in sediments for metals was assessed by calculating enrichment factor (EF) and pollution load index (PLI). The results indicated that sediments of Layari River Mouth Area, Fish Harbour, and KPT Boat Building Area are highly enriched with Cr and Zn (EF?>?5). Sediments of Layari River Outfall Zone were moderately enriched with Ni and Pb (EF?>?2). The pollution load index was found in the range of 0.98 to 1.34. Lower values of PLI (≤1) at most of sampling locations imply no appreciable input from anthropogenic sources. However, relatively higher PLI values (>1) at Layari River Mouth Area, Fish Harbour, and KPT Boat Building Area are attributed to increased human activity in the area.     

Dissipation kinetics and assessment of processing factor for chlorpyrifos and lambda-cyhalothrin in cardamom

The dissipation kinetics and method for estimation of residues of chlorpyrifos and lambda-cyhalothrin in cardamom were studied and developed. The limit of detection and limit of quantitation arrived for the compounds were 0.01 and 0.025 μg?g^?1, respectively. Gas chromatographic response of chlorpyrifos and lambda-cyhalothrin residues was linear in the range of 0.01–0.50 μg?g^?1 and the mean recovery obtained was 97.3 % for chlorpyrifos and 98.9 % for lambda-cyhalothrin with satisfactory relative standard deviation values. The mean initial residues of chlorpyrifos applied at a concentration of 0.05 % in cardamom was 2.5 μg?g^?1 and the residue was 8.1 μg?g^?1 after processing, with a processing factor of 3.24, while lambda-cyhalothrin when applied at 0.0025 % resulted in initial residues of 1.63 μg?g^?1 that magnified to 4.86 μg?g^?1 on curing, with a processing factor of 2.98. The half-life of chlorpyrifos was in the range of 5.1–5.24 days while that of lambda-cyhalothrin was in the range of 4.40–4.55 days. The processing factor arrived at in the above experiment lead to the conclusion that the residues of chlorpyrifos got magnified to 3.24–3.68 times and that of lambda-cyhalothrin got magnified to 2.98–3.46 times of initial residues, consequent to loss of weight due to dehydration during curing.     

Synthesis,characterization, and systematic studies of a novel aluminum selective chelating resin

A procedure is detailed for the selective analysis of trace aluminum by flame atomic absorption spectrophotometer coupled with off-line column separation and preconcentration. Chelating resin was synthesized by covalent functionalization of Amberlite XAD-16 by 2-(2-hydroxyphenyl) benzoxazole. The modified resin was characterized using FT-IR spectroscopy, energy dispersive x-ray analysis, elemental analysis, thermogravimetric analysis/differential thermal analysis, and minimum energy run. The optimum sorption was at pH 9?±?0.1 with corresponding t _1/2 of only 7 min. Many competitive anions and cations studied did not interfere at all in the selective determination of Al(III), at the optimized conditions. The resin shows maximum sorption capacity of 21.58 mg g^?1 and can be regenerated up to 75 cycles without any discernible capacity loss. The Langmuir isotherm model provides the better correlation of the experimental data (r ²?=?0.999) in comparison to Freundlich isotherm model, while the Scatchard analysis revealed homogeneous binding sites in the chelating resin. Analytical figures of merit were evaluated by accuracy (standard reference materials and recovery experiment), precision (RSD <5 %), and detection limit (2.8 μg L^?1). The applicability was demonstrated by analysis of trace aluminum in biological, environmental, and food samples.     

Simultaneous quantification of Bi(III) and U(VI) in environmental water samples with a complicated matrix containing organic compounds

Trace amounts of bismuth(III) and uranium(VI) can be simultaneously determined in a single scan by adsorptive cathodic stripping voltammetry in the presence of cupferron as a complexing agent. Optimal conditions were found to be: 0.1 mol?L^?1 acetate buffer (pH 5.3), 5?×?10^?5?mol?L^?1 cupferron, accumulation potential of ?0.25 V, and accumulation time of 30 s. The linear range of Bi(III) and U(VI) was observed over the concentration range from 2?×?10^?9 to 2?×?10^?7?mol?L^?1 and from 1?×?10^?8 to 5?×?10^?7?mol?L^?1, respectively. The influence of the main components of real water samples such as foreign ions and organic substances (surface active substances, humic substances) was precisely investigated. The method was applied to the simultaneous measurements of bismuth and uranium in natural water samples.