Novel method for the determination of five carbamate pesticides in water samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography

A novel method for the determination of five carbamate pesticides （metolcarb, carbofuran, carbaryl, isoprocard and diethofencard） in water samples was developed by dispersive liquid-liquid microextraction （DLLME） coupled with high performance liquid chromatography-diode array detector （HPLC-DAD）. Some experimental parameters that influence the extraction efficiency were studied and optimized to obtain the best extraction results. Under the optimum conditions for the method, the calibration curve was linear in the concentration range from 5 to 1000 ng mL^-1 for all the five carbamate pesticides, with the correlation coefficients （r^2） varying from 0.9984 to 0.9994. Good enrichment factors were achieved ranging from 80 to 177- fold, depending on the compound. The limits of detection （LODs） （S/N = 3） were ranged from 0.1 to 0.5 ng mL^-1. The method has been successfully applied to the analysis of the pesticide residues in environmental water samples.

Application of Modified Silica Coated Magnetite Nanoparticles for Removal of Iodine from Water Samples

The adsorption of iodine onto silica coated magnetite nanoparticles(im-SCMNPs) that modified with imidazole was investigated for removal of high concentrations of iodine from wastewater. Modified silica magnetite nanoparticles showed high efficiency in removing iodine from wastewater samples. The optimum pH for iodine removal was 7.0-8.0. The adsorption capacity was evaluated using both the Langmuir and Freundlich adsorption isotherm models. The size of the produced magnetite nanoparticles was determined by X-ray diffraction analysis and scanning electron microscopy. Synthesized magnetite nanoparticles showed the high adsorption capacity and would be a good method to increase adsorption efficiency for the removal of iodine in a wastewater treatment process. The Langmuir adsorption capacity(qmax) was found to be 140.84 mg/g of the adsorbent.

Determination of triazine herbicide residues in water samples by on-line sweeping concentration in micellar electrokinetic chromatography

A new method for the determination of atrazine, simazine and prometryn in water samples by on-line sweeping concentration technique in micellar electrokinetic chromatography （MEKC） was developed. Various parameters affecting sample enrichment and separation efficiency were systematically studied. Compared with the conventional MEKC method, up to 60-200-fold improvement in concentration sensitivity was achieved in terms of peak height by using this sweeping injection technique. The compound strychnine was used as the internal standard for the improvement of the experimental reproducibility. The limits of detection （S/ N = 3：1） for atrazine, simazine and prometryn were 9, 10 and 0.5 ng mL-1, respectively. This method has been successfully applied to the analysis of atrazine, simazine and prometryn in lake, steam and ground water.

Cloud-point extraction and preconcentration of bisphenol A from water samples

A novel cloud-point extraction （CPE） was successfully used in preconcentration of biphenol A （BPA） from aqueous solutions. Majority of BPA is extracted into the surfactant-rich phase. The parameters affecting the CPE such as concentration of surfactant and electrolyte, equilibration temperature and time and pH of sample solution were investigated. The samples were analyzed by high-performance liquid chromatography with ultraviolet detection. Under the optimized conditions, preconcentration of 10 mL sample gives a preconcentration factor of 11. The limit of detection （LOD） and limit of quantification （LOQ） are 0.1 μg/L and 0.33 μg/L, respectively. The linear range of the proposed method is 0.2-20 μg/L with correlation coefficients greater than 0.998 7 and the spiking recove6es are 97.96%-100.42%. The interference factor was tested and the extraction mechanism was also investigated. Thus, the developed CPE has proven to be an efficient, green, rapid and inexpensive approach for extraction and preconcentration of BPA from water samples.

Novel Gas-tight Multi-sampler for Discrete Deep-sea Water

The issues of how to quickly collect seawater samples and of how to make sure that those samples truly reflect the in-situ information on gas composition and concentration have therefore become a hot but difficult topic in the field of ocean technology.Most conventional seawater samplers only focus on collecting seawater itself,but take little consideration on gas preservation.A set of new oceanographic tools are presented for ocean resource exploration such as hydrothermal sulfide and gas hydrate,and for investigations on the processes and mechanisms of marine physical,chemical and biological evolutions.A gas-tight deep-sea water sampling system（GTWSS） is designed for the collection of deep-sea geochemical samples.This set of tools mainly consists of a conductivity temperature depth profiler（CTD）,release devices and gas-tight deep-sea water samplers（GTWS）.The GTWS is able to hold the gases in deep-sea water samples tightly,providing in-situ information on gas contents in the seawater samples and can be deployed on a routine wire-deployed CTD sampler for multi-layer discrete sampling of gas-tight seawater.Sea trials are performed successfully in 2008 and 2009,on a research vessel named HaiYang Si Hao in South China Sea,with the deepest trial depth 3 930 m.GTWSS is capable of quickly sampling 12 discrete gas-tight seawater samples（8.3 L per sample） during its single deployment.The head space method is employed to separate the gases from the seawater samples immediately after recovery of the seawater samples on the vessel.Field geochemical analysis is carried out by gaseous hydrocarbon sensors and an infrared gas analyzer.Results show that the concentrations of CH4 and CO2 in the seawater sampled by GTWSS are higher than those sampled by general non-gas-tight water samplers,thus confirming the gas tightness of GTWSS.Seawater samples can be collected quickly by using GTWSS,and GTWSS can keep the samples＇ integrity quite well.

Rapid determination of atrazine in environmental water samples by a novel liquid phase microextraction

A novel method was described for the rapid determination of atrazine using dispersive liquid phase microextraction in combination with high performance liquid chromatography （HPLC）. Possible impact parameters such as sample pH, extraction and disperser solvents, salting-out effect, and extraction time were investigated. The experimental results indicated that proposed method possessed an excellent analytical performance, The linear range, detection limit, and precision （R.S.D.） were 0.1- 50 ng mL- 1 （R2 = 0.9955）, 0.601 ng mL- 1 and 6,4%, respectively. The proposed method was validated with the real water samples, and the spiked recoveries were in the range of 69.9-89.8%, respectively. These results indicated that the established method with high enrichment factor, short extraction time was an excellent alternative for the routine analysis of atrazine in environmental samples. 2007 Qing Xiang Zhou. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.

Determination of Cobalt in Food, Environmental and Water Samples with Preconcentration by Dispersive Liquid-Liquid Microextraction

A new method for the determination of cobalt was developed by dispersive liquid-liquid microextraction preconcentra-tion and flame atomic absorption spectrometry. In the proposed approach, 1,5-bis(di-2-pyridyl) methylene thiocarbohydrazide (DPTH) was used as a chelating agent, and chloroform and ethanol were selected as extraction and dispersive solvents. Some factors influencing the extraction efficiency of cobalt and its subsequent determination, including extraction and dispersive solvent type and volume, pH of sample solution, concentration of the chelating agent, and extraction time, were studied and optimized. Under the optimum conditions, a preconcentration factor of 8 was reached. The detection limit for cobalt was 12.4 ng?mL–1, and the relative standard deviation (RSD) was 3.42% (n = 7, c = 100 ng?mL–1). The method was successfully applied to the determination of cobalt in food, environmental and water samples.

Scanning electron microscopy coupled with energydispersive X-ray spectrometry for quick detection of sulfuroxidizing bacteria in environmental water samples

Detection of sulfur-oxidizing bacteria has largely been dependent on targeted gene sequencing technology or traditional cell cultivation, which usually takes from days to months to carry out. This clearly does not meet the requirements of analysis for time-sensitive samples and/or complicated environmental samples. Since energy-dispersive X-ray spectrometry(EDS) can be used to simultaneously detect multiple elements in a sample, including sulfur, with minimal sample treatment, this technology was applied to detect sulfur-oxidizing bacteria using their high sulfur content within the cell. This article describes the application of scanning electron microscopy imaging coupled with EDS mapping for quick detection of sulfur oxidizers in contaminated environmental water samples, with minimal sample handling. Scanning electron microscopy imaging revealed the existence of dense granules within the bacterial cells, while EDS identified large amounts of sulfur within them. EDS mapping localized the sulfur to these granules. Subsequent 16S rRNA gene sequencing showed that the bacteria detected in our samples belonged to the genus Chromatium, which are sulfur oxidizers. Thus, EDS mapping made it possible to identify sulfur oxidizers in environmental samples based on localized sulfur within their cells, within a short time(within 24 h of sampling). This technique has wide ranging applications for detection of sulfur bacteria in environmental water samples.

Rapid Sample Product Trial Manufacture Technique for Developing Water Meter New Products

This paper advances the viewpoints and methods of the rapid sample product trial manufacture technique for developing water meter new products by CAD and simulation, computer virtual assembling and optimizing, rapid machining process and measurement etc. as the design and sample product trial manufacture process of water meter new products are long in product development period, and low in product development efficiency in the present time.

Passive Samplers Deployment in the Ayapel Swamp for Monitoring Temporal Dynamics of Mercury in the Water Column

Passive sampling is a simple and efficacious sampling technique that guarantees a safe collection and transportation of samples to the analysis site, and obtaining results with more temporal resolution. As a case of study, passive samplers were deployed in the Ayapel Swamp, Colombia, located in the influence zone of open pit gold mines. Mercury, iron and manganese were sampled at two different depths by the Chemcatcher? passive sampler and regular grab sampling. Additionally, dissolved oxygen, oxidation-reduction potential, pH and water temperature were measured. The results showed that depth and time did not have a significant influence (ANOVA, confidence level of 95%) on mercury concentration on both passive samplers and grab sampling. However, concentration of Fe and Hg in passive samplers had a high positive correlation, but it may be because depth increase during sampling period caused the dilution of both analytes. In conclusion, passive samplers proved to be a valuable tool for understanding the response of mercury to the Ayapel Swamp dynamics.

Effects of Conservation Methods of Water Samples on Determination of Total Phosphorus

Effects of conservation methods of water samples on determination of total phosphorus were analyzed from aspects of methods of adding conserving agent, SS concentration, natural sedimentation time, conservation temperature and time. The results showed that SS concentration in water and natural sedimentation time had the greatest impact on the determination of total phosphorus, while the influence of methods of adding conserving agent, conservation temperature and time was relatively smaller. TP concentration in water samples conserved irregularly was higher than the standard value due to the existence of SS and microorganisms in water, and the deviation became larger with the increase of SS concentration in water. In addition, quality control measures and matters needing attention during the conservation process of water samples were put forward to improve the accuracy of TP concentration.

Rapid Determination of Three Kinds of Microcystins in Environmental Water Samples by Disk SPE-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

A method of rapidly detecting three kinds of microcystins( MCs) in environmental water samples by using disk SPE- ultra high performance liquid chromatography- tandem mass spectrometry( UPLC- MS / MS) was established. Firstly,environmental water samples were extracted by disk SPE column( C_(18)),and three kinds of MCs were separated by Waters BEH C_(18) chromatographic column with acetonitrile- 0. 2% formic acid solution as the mobile phase. After the gradient elution separation,the external standard method was used for quantitative and qualitative analysis under MRM of UPLC- MS / MS. The results showed that the three kinds of MCs in the range of 0. 05- 10 μg / L showed good linear relation,and the correlation coefficients were higher than 0. 999 4,while the method detection limit was 0. 04 ng / L. Under 0. 1,1,and 5 μg / L standard addition for the same environmental sample,the average recovery was 82. 8%- 108. 8%,and the relative standard deviation of determination results was2. 1%- 10. 1%( n = 6). This method is rapid,sensitive and accurate,so it can be effectively applied in the monitoring of MCs in environmental water samples.

The Effect of Measuring Magnetic Susceptibility of Water Samples by Starting with Isothermal Remanent Magnetization (IRM) before Anhysteretic Remanent Magnetization (ARM)

Estimating magnetic properties of water samples by first measuring the Anhysteretic Remanent Magnetization (ARM) before Isothermal Remanent Magnetization (IRM) is induced has been costly due to the discard of samples measured by staring with the latter before the former. However, no clear understanding exists on the effect of measuring magnetic properties values by first inducing IRM before ARM. This study explored the effect of measuring concentration related parameters (χlf, χfd and χARM), a mineral related parameter (S-300) and grain size parameters (χfd% and χARM/SIRM ratio) fromwater samples by starting with IRM before ARM. Forty three surface water samples were collected from the estuarine of Yangtze River (China) with the aim of measuring magnetic characteristics by starting with IRM before ARM. The results indicated that, measuring magnetic properties by either starting with ARM or IRM led to similar values for χlf, χfd, χfd%, χARM, S-300 and χARM/SIRM ratio (p > 0.05). These results imply that, measuring concentrationrelated parameters does not necessarily require measuring ARM first and then IRM. Researchers can start by measuring any parameter between ARM and IRM without affecting the final results of the water samples, but with proper demagnetization when started with IRM.

Experiment Study of Reverse Demulsifier on Simulated Water Sample Treatment at Different Oscillation Time and Different Concentrations of Drugging

In recent years, the water content of oilfield production fluid is high and there is a large amount of oily sewage. In order to improve the capability of sewage treatment, usually using demulsifier for oily sewage processing. This article uses simulated water sample to test the treatment effect of the optimized reverse demulsifier at different oscillation time. As the increase of action time and oscillation, the average size of droplets increases and the amount of the droplets under 1 μm decreases.

DETERMINATION OF ANTIMONY IN WATER SAMPLES BY FLOW-INJECTION HYDRIDE GENERATION ATOMIC ABSORPTION SPECTROMETRY WITH ON-LINE ION-EXCHANGE COLUMN PRECONCENTRATION

On-line ion-exchange separation and preconcentration were combined with flow-injection hydride generation atomic absorption spectrometry (HGAAS) to determine ultra-trace amounts of antimony in water samples. Antimony(Ⅲ) was preconcentrated on a micro-column packed with CPG-8Q chelating ion-exchanger using time-based sample loading and eluted by 4 mol l^(-1) HCl directly into the hydride generation AAS system. A detection limit (3σ) of 0.0015μg l^(-1) Sb(Ⅲ) was obtained on the basis of a 20 fold enrichment and with a sampling frequency of 60h^(-1). The precision was 1.0% r.s.d.(n=11) at the 0.5μg l^(-1) Sb(Ⅲ) level. Recoveries for the analysis of antimony in tap water, snow water and sea water samples were in the range 97-102%.

Determination of Organochlorine and Synthetic Pyrethroid Pesticide Residues in Water Samples Collected from Different Locations of Bangladesh

The present study was aimed to validate an analytical method for the quantification of 19 organochlorine and 2 synthetic pyrethroid pesticide residues in water samples using modified quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction and Gas Chromatography coupled with Electron Capture Detector (ECD). The selected pesticide residues were determined by in-house validated method. The analytical method was validated by evaluating the accuracy, precision, linearity, limit of detection (LOD) and limit of quantification (LOQ). The average recoveries of the selected pesticides ranged from 78% to 117% with RSDr ≤ 12% in two fortification levels of 0.02 and 0.1 mg/L. The linearity was ≥0.995 for all of the selected pesticides. The LOD ranged from 0.003 to 0.006 mg/L and the LOQ was 0.02 mg/L for all the selected analytes. This method was applied satisfactorily for the residue analysis of 108 water samples collected from nine districts of Bangladesh. Among the analyzed samples, only 4 had cypermethrin residues (0.026 mg/L, 0.034 mg/L, 0.045 mg/L and 0.05 mg/L). The level of detected cypermethrin residues were above the WHO recommended guide line values of water quality.

Effect of Sample Disturbance on Unconfined Compression Strength of Natural Marine Clays

Quantitatively correcting the unconfined compressive strength for sample disturbance is an important research project in the practice of ocean engineering and geotechnical engineering. In this study, the specimens of undisturbed natural marine clay obtained from the same depth at the same site were deliberately disturbed to different levels. Then, the specimens with different extents of sample disturbance were trimmed for both oedometer tests and unconfined compression tests. The degree of sample disturbance SD is obtained from the oedometer test data. The relationship between the unconfined compressive strength q u and SD is studied for investigating the effect of sample disturbance on q u. It is found that the value of q u decreases linearly with the increase in SD. Then, a simple method of correcting q u for sample disturbance is proposed. Its validity is also verified through analysis of the existing published data.

Preconcentration of Cadmium in Environmental Samples by Cloud Point Extraction and Determination by FAAS

Cloud point extraction (CPE) has been used for the preconcentration of cadmium, after the formation of a complex with 1, 5-bis(di-2-pyridylmethylene) thiocarbonohydrazide (DPTH), and further determination by flame atomic absorption spectrometry (FAAS) using Triton X-114 as surfactant. The main factors affecting the CPE, such as concentration of Triton X-114 and DPTH, pH, equilibration temperature and incubation time, were optimized for the best extract efficiency. Under the optimum conditions i.e., pH 5.4, [DPTH] = 6x10-3%, [Triton X-114] = 0.25% (v/v), an enhancement factor of 10.5 fold was reached. The lower limit of detection (LOD) obtained under the optimal conditions was 0.95 μg L?1. The precision for 8 replicate deter- minations at 20 and 100 μgL?1 Cd were 2.4 % and 2 % relative standard deviation (R.S.D.). The calibration graph using the preconcentration method was linear with a correlation coefficient of 0,998 at levels close to the detection limit up to at least 200 μgL?1. The method was successfully applied to the determination of cadmium in water, environmental and food samples and in a BCR-176 standard reference material.