Qingxiang Zhou

Trace determination of organophosphorus pesticides in environmental samples by temperature-controlled ionic liquid dispersive liquid-phase microextraction

This paper described a new approach for the determination of organophosphorus pesticides by temperature-controlled ionic liquid dispersive liquid-phase microextraction prior to high-performance liquid chromatography with ultraviolet detection. Methylparathion and phoxim, two of the typical organophosphorus pesticides, were used as the model analytes for the investigation of the development and application of the new microextraction method. 1-Hexyl-3-methylimidazolium hexafluorophosphate [C6MIM][PF6] was used as the extraction solvent and the factors affecting the extraction efficiency such as the volume of [C6MIM][PF6], pH of working solutions, extraction time, centrifuging time, dissoluble temperature and salt effect were optimized. Under the optimal extraction conditions, methylparathion and phoxim exhibited good linear relationship in the concentration range of 1-100 ng mL(-1). The detection limits were 0.17 ng mL(-1) and 0.29 ng mL(-1), respectively. Precisions of proposed method (RSDs, n=6) were 2.5% and 2.7%, respectively. This proposed method was successfully applied in the analysis of four real environmental water samples and good spiked recoveries over the range of 88.2-103.6% were obtained. These results indicated that temperature-controlled ionic liquid dispersive liquid-phase microextraction had excellent application prospect in environmental field.

Determination of atrazine and simazine in environmental water samples using multiwalled carbon nanotubes as the adsorbents for preconcentration prior to high performance liquid chromatography with diode array detector

Multiwalled carbon nanotubes, a new nanoscale material, has been gained many interests for use in various fields, and has exhibited exceptional merit as SPE absorbents for enrichment of environmental pollutants. This paper focused on the enriching power of atrazine and simazine, two important widely used triazine herbicides and described a novel and sensitive method for determination of these two herbicides based on SPE using multiwalled carbon nanotubes as solid phase absorbents followed by high performance liquid chromatography with diode array detector. Factors that maybe affect the enrichment efficiency of multiwalled carbon nanotubes such as the volume of eluent, sample flow rate, sample pH, and volume of the water samples were optimized. Under the optimal procedures, multiwalled carbon nanotubes as the absorbents have obtained excellent enrichment efficiency for atrazine and simazine. The detection limits of the atrazine and simazine were 33 and 9ngl(-1), respectively. The spiked recoveries of the two analytes were over the range of 82.6-103.7% in most cases. Good analytical performance was achieved from real-world water samples such as river water, reservoir water, tap water and wastewater after primary pretreatment with proposed method. All these experimental results indicated that the developed method could be used as an alternative for the routine analysis of atrazine and simazine in many real water samples.

Ultrasound-assisted ionic liquid dispersive liquid-phase micro-extraction: a novel approach for the sensitive determination of aromatic amines in water samples.

Ultrasound-assisted ionic liquid dispersive liquid-phase micro-extraction was developed for the determination of four aromatic amines such as 2,4-dichloroaniline, 1-naphthylamine, 6-chloroanline and N,N-dimethylaniline. High-performance liquid chromatography coupled with UV detector was used for the determination of aromatic amines. In the novel procedure, 1-hexyl-3-methylimidazolium hexafluorophosphate [C(6)MIM] [PF(6)] was dispersed into the aqueous sample solution as fine droplets by ultrasonication, and which promoted the analytes more easily migrate into the ionic liquid phase. Variable affecting such as the volume of [C(6)MIM] [PF(6)], sample pH, ultrasonication time, extraction time, centrifuging time have been investigated in detail. The proposed method has been found to have excellent detection sensitivity with limits of detection (LOD, S/N=3) in the range of 0.17-0.49mugL(-1) and precisions in the range of 2.0-6.1% (RSDs, n=6). This method has been also successfully applied to analyze the real water samples and good spiked recoveries over the range of 92.2-119.3% were obtained.

Temperature-controlled ionic liquid-liquid-phase microextraction for the pre-concentration of lead from environmental samples prior to flame atomic absorption spectrometry.

Hydrophobic ionic liquid could be dispersed into infinite droplets under driving of high temperature, and then they can aggregate as big droplets at low temperature. Based on this phenomenon a new liquid-phase microextraction for the pre-concentration of lead was developed. In this experiment, lead was transferred into its complex using dithizone as chelating agent, and then entered into the infinite ionic liquid drops at high temperature. After cooled with ice-water bath and centrifuged, lead complex was enriched in the ionic liquid droplets. Important parameters affected the extraction efficiency had been investigated including the pH of working solution, amount of chelating agent, volume of ionic liquid, extraction time, centrifugation time, and temperature, etc. The results showed that the usually coexisting ions containing in water samples had no obvious negative effect on the recovery of lead. The experimental results indicated that the proposed method had a good linearity (R=0.9951) from 10 ng mL(-1) to 200 ng mL(-1). The precision was 4.4% (RSD, n=6) and the detection limit was 9.5 ng mL(-1). This novel method was validated by determination of lead in four real environmental samples for the applicability and the results showed that the proposed method was excellent for the future use and the recoveries were in the range of 94.8-104.1%.

Preconcentration of nickel and cadmium by TiO2 nanotubes as solid-phase extraction adsorbents coupled with flame atomic absorption spectrometry

TiO(2) nanotubes, a new nanomaterial, are often used in the photocatalysis. Due to its relatively large specific surface areas it should have a higher enrichment capacity. However, very few applications in the enrichment of pollutants were found. This paper described a new procedure to investigate the trapping power of TiO(2) nanotubes with cadmium and nickel in water samples as the model analytes and flame atomic absorption spectrometry for the analysis. The possible parameters influencing the enrichment were optimized. Under the optimal SPE conditions, the method detection limits and precisions (R.S.D., n=6) were 0.25 ngmL(-1) and 2.2% for cadmium, 1 ngmL(-1) and 2.6% for nickel, respectively. The established method has been successfully applied to analyze four realworld water samples, and satisfactory results were obtained. The spiked recoveries were in the range of 90.2-99.2% for them. All these indicated that TiO(2) nanotubes had great potential in environmental field.

Simultaneous determination of nickel, cobalt and mercury ions in water samples by solid phase extraction using multiwalled carbon nanotubes as adsorbent after chelating with sodium diethyldithiocarbamate prior to high performance liquid chromatography.

Multiwalled carbon nanotubes (MWNTs) have been widely used for the enrichment of trace important pollutants in environment because of its large specific surface area, high extraction efficiency, and easy operation. In this study, a solid phase extraction method was established to determine nickel (Ni(2+)), cobalt (Co(2+)) and mercury (Hg(2+)) ions using MWNTs as the adsorbent and sodium diethyldithiocarbamate (DDTC) as the chelating agent. The final analysis was performed on a high performance liquid chromatography (HPLC). The factors that may influence the extraction efficiency were optimized in detail including the type and volume of elution solvent, sample pH, volume of chelating agent solution, and volume of sample solution, etc. The experimental results indicated that good linear relationship between peak area and the concentration of the ions was achieved in the range of 0.1-100μgL(-1), 0.1-50μgL(-1), and 2.7-300μgL(-1) for Ni(2+), Co(2+), and Hg(2+), respectively. The precision was determined by calculating the relative standard deviation (R.S.D.) values that were in the range of 6.2-11.7% under the optimal conditions. The detection limits of Ni(2+), Co(2+), and Hg(2+) were in the range of 0.04-0.9μgL(-1) (S/N=3). The presented method was applied for the determination of the metal ions mentioned above in real water samples, and satisfied results were achieved. All these indicated that proposed method will be a good alternative tool for monitoring the target ions in environmental samples in the future.

Trace determination of dichlorodiphenyltrichloroethane and its main metabolites in environmental water samples with dispersive liquid–liquid microextraction in combination with high performance liquid chromatography and ultraviolet detector

Dichlorodiphenyltrichloroethane,1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane (DDT) and its main metabolites have been paid much more attention, and present paper describes a new process for the rapid determination of such pollutants in environmental water samples based on dispersive liquid-liquid microextraction (DLLME) and high performance liquid chromatography with ultraviolet detector, which has merits such as high enrichment factor and sensitivity, low cost and easy to operate. Significant parameters such as extraction solvent and dispersive solvent type and volume, pH, extraction time and centrifuging time, which would have important impact on the enrichment of target pollutants, have been investigated in detail. The results exhibited that excellent performance could be achieved with carbon tetrachloride and acetonitrile as the extraction solvent and dispersive solvent, respectively. Under the optimal conditions, excellent linear relationship was gained in the range of 1.0-5 microg L(-1), and detection limits were in the range of 0.32-0.51 microg L(-1). The precisions of the proposed method were in the range of 2.80-7.50% (RSD). The proposed method was validated with real water samples, and the results indicated the spiked recoveries were in the range of 85.58-119.6% and the established method was very good and competitive in the determination of DDT and its metabolites.

Temperature‐controlled ionic liquid‐dispersive liquid‐phase microextraction for preconcentration of chlorotoluron, diethofencarb and chlorbenzuron in water samples

This article describes a new, rapid and sensitive method for the determination of chlorotoluron, diethofencarb and chlorbenzuron from water samples with temperature-controlled ionic liquid-dispersive liquid-phase microextraction. In the preconcentration procedure, ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate [C(6)MIM] [PF(6)] was employed as the extraction solvent. The parameters, such as volume of [C(6)MIM] [PF(6)], sample pH, extraction time, centrifuging time, temperature and salting-out effect, were investigated in detail. Under the optimal extraction conditions, it has been found that three analytes had excellent LODs (S/N=3) in the range of 0.04-0.43 microg/L. The RSDs (n=6) were in the range of 1.3-4.7%. The proposed method was evaluated with lake water, tap water and melted snow water samples. The experimental results indicated that the proposed method had excellent prospect and would be widely used in the future.

Investigation of the applicability of highly ordered TiO2 nanotube array for enrichment and determination of polychlorinated biphenyls at trace level in environmental water samples

Present study investigated the applicability of ordered TiO(2) nanotube arrays for the enrichment and determination of polychlorinated biphenyls (PCBs) in water samples. A new and reliable method was developed for the preconcentration and determination of PCBs by micro-solid phase equilibrium extraction in combination with gas chromatography and electron capture detection (GC-ECD), which exploited the special physical and chemical properties of ordered TiO(2) nanotube arrays. The experimental results indicated that low LODs were easily achieved in the range of 0.02-0.10 μg L(-1) for PCB-28, PCB-52, PCB-101, PCB-153, PCB-138, and PCB-180. The proposed method was validated with several real water samples, and good spiked recoveries have been obtained in the range of 95.8-110.5%. The experimental results demonstrated that TiO(2) nanotube arrays could be reused for over 200 times without the lost of the extraction efficiency. All these showed that TiO(2) nanotube arrays would be very useful in the enrichment and determination of trace pollutants.

Application of multiwalled carbon nanotubes treated by potassium permanganate for determination of trace cadmium prior to flame atomic absorption spectrometry

In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes (MWCNTs) and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry. The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing. Parameters influencing the recoveries of target analytes were optimized. Under optimal conditions, the target analyte exhibited a good linearity (R2=0.9992) over the concentration range 0.5-50 ng/ml. The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%, respectively. The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%. All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.