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.     

Determination of trace amounts of zirconium in real samples after microwave digestion and ternary complex dispersive liquid–liquid microextraction

In this study, a ternary Zr(IV) system with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) and fluoride was chosen on the basis of dispersive liquid–liquid microextraction method. Zirconium was extracted into the fine droplets of dichlorobenzene as extracting solvent. These drops dispersed as a cloud in the aqueous sample with the help of ultrasonic waves, and the procedure was done. Finally, atomic absorption spectrometry was applied for the determination of zirconium. The effects of different factors that influence complex formation and extraction, such as pH, amounts of complexing agents, type and volume of the extracting solvent, as well as sonication and centrifuging time, were optimized. Under optimum conditions, the calibration curve was linear in the range of 150.0–800.0 ng mL^?1 with a limit of detection of 44.0 ng mL^?1. Relative standard deviation was calculated to be 4.1 % (n?=?7, c?=?400.0 ng mL^?1). The enrichment factor was 80. The proposed method was successfully used to determine the zirconium in several water, wastewater, and soil samples.     

Assessment of liquid disposal originated by uranium enrichment at Aramar Experimental Center São Paulo--Brazil

This work presents a liquid disposal monitoring originated from uranium enrichment process at Aramar Experimental Center from 1990 to 1998. Assessment of uranium, fluorides, ammoniacal nitrogen, chemical oxygen demand, and pH measurements were made in water samples and compared with results achieved in other countries, as North America and India. The liquid disposal evaluation, generated by uranium enrichment process, showed low levels, considering most parameters established by Federal and State Legislation, aiming environmental pollution control. However, uranium levels were above the limits established by Conselho Nacional do Meio Ambiente, Environment Protection Agency and mainly by the World Health Organization.     

Estimation of chlorpyriphos and cypermethrin residues in chilli (Capsicum annuum L.) by gas–liquid chromatography

Dissipation of chlorpyriphos and cypermethrin in chilli was studied following three applications of a combination formulation of Nurelle-D 505 (chlorpyriphos 50 %?+?cypermethrin 5 %) at 1 and 2 L?ha^?1 at an interval of 15 days. Residues of chlorpyriphos and cypermethrin in chilli were estimated by gas–liquid chromatography and confirmed by gas chromatography–mass spectrometry. Half-life periods for chlorpyriphos were found to be 4.43 and 2.01 days, whereas for cypermethrin these values were observed to be 2.51 and 2.64 days at single and double the application rates, respectively. Residues of chlorpyriphos dissipated to more than 80 % after 10 days at both the dosages. However, residues of cypermethrin dissipated to the extent of more than 70 % in 7 days. Soil samples collected after 15 days of the last application did not show the presence of chlorpyriphos and cypermethrin at their respective determination limit of 0.01 mg?kg^?1. The use of chlorpyriphos and cypermethrin mixture at the recommended dosage does not seem to pose any hazards to the consumers, and a waiting period of 1 day is suggested to reduce the risk before consumption of green chilli.     

Optimization and determination of Cd (II) in different environmental water samples with dispersive liquid�Cliquid microextraction preconcentration combined with inductively coupled plasma optical emission spectrometry

Dispersive liquid?Cliquid microextraction followed by inductively coupled plasma-optical emission spectrometry has been investigated for determination of Cd(II) ions in water samples. Ammonium pyrrolidine dithiocarbamate was used as chelating agent. Several factors influencing the microextraction efficiency of Cd (II) ions such as extracting and dispersing solvent type and their volumes, pH, sample volume, and salting effect were optimized. The optimization was performed both via one variable at a time, and central composite design methods and the optimum conditions were selected. Both optimization methods showed nearly the same results: sample size 5 mL; dispersive solvent ethanol; dispersive solvent volume 2 mL; extracting solvent chloroform; extracting solvent volume 200  $\upmu $ L; pH and salt amount do not affect significantly the microextraction efficiency. The limits of detection and quantification were 0.8 and 2.5 ng L^???1, respectively. The relative standard deviation for five replicate measurements of 0.50 mg L^???1 of Cd (II) was 4.4%. The recoveries for the spiked real samples from tap, mineral, river, dam, and sea waters samples ranged from 92.2% to 104.5%.     

Community air monitoring for pesticides—part 2: multiresidue determination of pesticides in air by gas chromatography,gas chromatography–mass spectrometry,and liquid chromatography–mass spectrometry

Two multiresidue methods were developed to determine pesticides in air collected in California. Pesticides were trapped using XAD-4 resin and extracted with ethyl acetate. Based on an analytical method from the University of California Davis Trace Analytical Laboratory, pesticides were detected by analyzing the extract by gas chromatography–mass spectrometry (GC-MS) to determine chlorothalonil, chlorthal-dimethyl, cycloate, dicloran, dicofol, EPTC, ethalfluralin, iprodione, mefenoxam, metolachlor, PCNB, permethrin, pronamide, simazine, trifluralin, and vinclozolin. A GC with a flame photometric detector was used to determine chlorpyrifos, chlorpyrifos oxon, diazinon, diazinon oxon, dimethoate, dimethoate oxon, fonophos, fonophos oxon, malathion, malathion oxon, naled, and oxydemeton. Trapping efficiencies ranged from 78 to 92 % for low level (0.5 μg) and 37–104 % for high level (50 and 100 μg) recoveries. Little to no degradation of compounds occurred over 31 days; recoveries ranged from 78 to 113 %. In the California Department of Food and Agriculture (CDFA) method, pesticides were detected by analyzing the extract by GC-MS to determine chlorothalonil, chlorpyrifos, cypermethrin, dichlorvos, dicofol, endosulfan 1, endosulfan sulfate, oxyfluorfen, permethrin, propargite, and trifluralin. A liquid chromatograph coupled to a MS was used to determine azinphos-methyl, chloropyrifos oxon, DEF, diazinon, diazinon oxon, dimethoate, dimethoate oxon, diuron, EPTC, malathion, malathion oxon, metolachlor, molinate, norflurazon, oryzalin, phosmet, propanil, simazine and thiobencarb. Trapping efficiencies for compounds determined by the CDFA method ranged from 10 to 113, 22 to 114, and 56 to 132 % for 10, 5, and 2 μg spikes, respectively. Storage tests yielded 70–170 % recovery for up to 28 days. These multiresidue methods represent flexible, sensitive, accurate, and cost-effective ways to determine residues of various pesticides in ambient air.