Simple flow-injection system for the simultaneous determination of nitrite and nitrate in water samples

A novel spectrophotometric reaction system was developed for the determination of nitrite as well as nitrate in water samples, and was applied to a flow-injection analysis (FIA). The spectrophotometric flow-injection system coupled with a copperised cadmium reductor column was proposed. The detection was based on the nitrosation reaction between nitrite ion and phloroglucinol (1,3,5-trihydroxybenzene), a commercially available phenolic compound. Sample injected into a carrier stream was split into two streams at the Y-shaped connector. One of the streams merged directly and reacted with the reagent stream: nitrite ion in the samples was detected. The other stream was passed through the copperised cadmium reductor column, where the reduction of nitrate to nitrite occurred, and the sample zone was then mixed with the reagent stream and passed through the detector: the sum of nitrate and nitrite was detected. The optimised conditions allow a linear calibration range of 0.03-0.30 mug NO2--N ml(-1) and 0.10-1.00 mug NO3--N ml(-1). The detection limits for nitrite and nitrate, defined as three times the standard deviation of measured blanks are 2.9 ng NO2--N ml(-1) and 2.3 ng NO3--N ml(-1), respectively. Up to 20 samples can be analyzed per hour with a relative standard deviation of less than 1.5%. The proposed method could be applied successfully to the simultaneous determination of nitrite and nitrate in water samples.</p

Flow injection spectrophotometry coupled with a crushed barium sulfate reactor column for the determination of sulfate ion in water samples

A new type of a reactor column, a crushed BaSO4 reactor column used for the flow injection spectrophotometric determination of sulfate ion using the exchange reaction of sulfate ion and barium-dimethylsulfonazo III is proposed. The column is very simple and economical. It can be continuously used for 8 h before washing with water for repeated usage of at least 1 month. The procedure is sensitive. Application to various water samples was demonstrated. </p

Retention of Carbamate Pesticides by Different Surfactant-Modified Sorbents: a Comparative Study

Different surfactant-modified solid sorbents have been comparatively investigated for retention of carbamate pesticides in aqueous solution. Three modified-sorbents, including sodium dodecyl sulfate (SDS) treated alumina, cetyltrimethyl ammonium bromide (CTAB) coated silica and CTAB coated zeolite, were created using different surfactant concentrations. The studied carbamate pesticides including oxamyl, methomyl, aldicarb, carbofuran, carbaryl, isoprocarb, methiocarb, promecarb and carbosulfan were analyzed by HPLC/UV. Adsorption of all carbamate pesticides (concentration range between 0.5-5.0 mg L-1) onto surfactant-modified sorbents followed linear regressions with the correlation coefficients in the range of 0.857-0.995. CTAB-modified zeolite showed high uptake values for carbofuran, carbaryl, methiocarb and carbosulfan. SDS-modified alumina demonstrated high uptake values for carbaryl, isoprocarb, methiocarb, promecarb and carbosulfan. CTAB-modified silica gave high uptake values for methiocarb, promecarb and carbosulfan. Desorption of carbamate pesticides from surfactant-modified sorbents using methanol were better than that obtained from unmodified sorbents. The study clearly proved that the surfactant-modified sorbents are effective for carbamate pesticides extraction

Magnetic Stirring Assisted Demulsification Dispersive Liquid–Liquid Microextraction for Preconcentration of Polycyclic Aromatic Hydrocarbons in Grilled Pork Samples

A simple microextraction method, magnetic stirring assisted demulsification dispersive liquid&#8315;liquid microextraction, for preconcentration of five polycyclic aromatic hydrocarbons (fluorene, phenanthrene, anthracene, fluoranthrene, and pyrene) was investigated prior to analysis by high performance liquid chromatography. In this method, a mixture of extraction solvent and disperser solvent was rapidly injected into sample solution. The magnetic stirrer agitator aided the dispersion of the extraction solvent into the sample solution. After the formation of an emulsion, the demulsifier was added, resulting in the rapid separation of the mixture into two phases. No centrifugation step was required. Several parameters affecting the extraction efficiency of the proposed method were studied, including addition of salt, kind and volume of extraction solvent, volume of demulsifier solvent, and extraction times. Under the optimum conditions, high enrichment factor, low limit of detections (LODs) and good precision were gained. The proposed method was successfully applied to analysis of polycyclic aromatic hydrocarbon residues in grilled pork samples

Ultrasonically Modified Amended-Cloud Point Extraction for Simultaneous Pre-Concentration of Neonicotinoid Insecticide Residues

An effective pre-concentration method, namely amended-cloud point extraction (CPE), has been developed for the extraction and pre-concentration of neonicotinoid insecticide residues. The studied analytes including clothianidin, imidacloprid, acetamiprid, thiamethoxam and thiacloprid were chosen as a model compound. The amended-CPE procedure included two cloud point processes. Triton&trade; X-114 was used to extract neonicotinoid residues into the surfactant-rich phase and then the analytes were transferred into an alkaline solution with the help of ultrasound energy. The extracts were then analyzed by high-performance liquid chromatography (HPLC) coupled with a monolithic column. Several factors influencing the extraction efficiency were studied such as kind and concentration of surfactant, type and content of salts, kind and concentration of back extraction agent, and incubation temperature and time. Enrichment factors (EFs) were found in the range of 20&ndash;333 folds. The limits of detection of the studied neonicotinoids were in the range of 0.0003&ndash;0.002 &micro;g mL&minus;1 which are below the maximum residue limits (MRLs) established by the European Union (EU). Good repeatability was obtained with relative standard deviations lower than 1.92% and 4.54% for retention time (tR) and peak area, respectively. The developed extraction method was successfully applied for the analysis of water samples. No detectable residues of neonicotinoids in the studied samples were found

In-Situ Formation of Modified Nickel&ndash;Zinc-Layered Double Hydroxide Followed by HPLC Determination of Neonicotinoid Insecticide Residues

A single-step preconcentration procedure using the in-situ formation of modified nickel&ndash;zinc-layered double hydroxides (LDHs) prior to high-performance liquid chromatography (HPLC) is investigated for the determination of neonicotinoid insecticide residues in honey samples. The LDHs could be prepared by the sequential addition of sodium hydroxide, sodium dodecyl sulfate, nickel nitrate 6-hydrate and zinc nitrate 6-hydrate, which were added to the sample solution. The co-precipitate phase and phase separation were obtained by centrifugation, and then the precipitate phase was dissolved in formic acid (concentrate) prior to HPLC analysis. Various analytical parameters affecting extraction efficiency were studied, and the characterization of the LDHs phase was performed using Fourier-transformed infrared spectroscopy and scanning electron microscopy. Under optimum conditions, the limit of detection of the studied neonicotinoids, in real samples, were 30 &mu;g L&minus;1, for all analytes, lower than the maximum residue limits established by the European Union (EU). The developed method provided high enrichment, by a factor of 35. The proposed method was utilized to determine the target insecticides in honey samples, and acceptable recoveries were obtained

Selective Uptake and Bioaccumulation of Antidepressants in Fish from Effluent-Impacted Niagara River

The continuous release of pharmaceuticals and personal care products (PPCPs) into freshwater systems impacts the health of aquatic organisms. This study evaluates the concentrations and bioaccumulation of PPCPs and the selective uptake of antidepressants in fish from the Niagara River, which connects two of the North American Great lakes (Erie and Ontario). The Niagara River receives PPCPs from different wastewater treatment plants (WWTPs) situated along the river and Lake Erie. Of the 22 targeted PPCPs, 11 were found at part-per-billion levels in WWTP effluents and at part-per-trillion levels in river water samples. The major pollutants observed were the antidepressants (citalopram, paroxetine, sertraline, venlafaxine, and bupropion, and their metabolites norfluoxetine and norsertraline) and the antihistamine diphenhydramine. These PPCPs accumulate in various fish organs, with norsertraline exhibiting the highest bioaccumulation factor (up to about 3000) in the liver of rudd (<i>Scardinius erythrophthalmus</i>), which is an invasive species to the Great Lakes. The antidepressants were selectively taken up by various fish species at different trophic levels, and were further metabolized once inside the organism. The highest bioaccumulation was found in the brain, followed by liver, muscle, and gonads, and can be attributed to direct exposure to WWTP effluent

A sensitive nonenzymatic hydrogen peroxide sensor using cadmium oxide nanoparticles/multiwall carbon nanotube modified glassy carbon electrode

A simple sensing scheme for hydrogen peroxide has been described by electrochemical deposition of cadmium oxide (CdO) nanoparticles with 3c50 nm in diameter on a glassy carbon (GC) electrode modified with multiwall carbon nanotubes (MWCNT). The CdO/MWCNT modified sensor, with a surface coverage of 1.13 7 10 128 mol/cm2, displayed high synergistic electrocatalytic activity for H2O2. The sensor was capable of reducing H2O2 at 121.2 V vs. Ag/AgCl (H2O2 + 2H+ + 2e 12 \u2192 2H2O) in a broad pH range. At the optimal pH 7, the sensor exhibited a detection limit of 0.1 \u3bcM, broad linearity from 0.5 to 200 \u3bcM, good reproducibility (RSD of 5.9%), and long-term stability. Uric acid, ascorbic acid and dopamine up to 100 \u3bcM provoked no signal response, attesting selectivity of the CdO/MWCNT modified electrode for hydrogen peroxide.Peer reviewed: YesNRC publication: Ye