Determination of organophosphorus pesticides and related compounds in water samples by membrane extraction and gas chromatography

A membrane extraction-gas chromatography method was developed fordetermination of organophosphorus pesticides and related compounds including methamidophos, DDVP, dimethoate, methyl parathion, parathion, thiophosphoric acid trimethyl ester, and thiophosphoramidic acid dimethyl ester in water samples. In thismethod, surface-modified acetic cellulose membranes were used to extract the target analytes in water samples, the extracted analytes were back-extracted into a small amount of methanol, andgas chromatography with pulsed flame photometric detector (GC-PFPD) was used to determine the concentrations of targetanalytes in the extracts. The recoveries obtained for thetarget analytes spiked into the water samples ranged from 66to 94%. The method detection limit for each target analyte was 0.05 g L^-1. The method developed in this study had shown the advantages of being cheap, simple, fast, and reliable. It had been used successfully to determine the concentrations of target analytes in river water samples.     

A novel environmental indicator for monitoring of pesticides

The identification of an indicator for monitoring pesticides is a very effective analytical approach because it allows one to schedule and simplify the analytical routine. In this study, a new indicator has been designed, which has to be able to define a scale of priorities in the pesticides monitoring. A starting equation was developed involving the escaping tendency of a given substance from a phase (based on the Mackay model I level). The reliability of the indicator was tested by application to a model system, consisting of a defined and limited area, choosing water as matrix over a period of 6 years. A group of marker compounds was also defined to implement the predictive efficacy of the indicator. The results obtained by modeling were compared to those obtained by experimentation of the same model system. The indicator was subsequently and appropriately modified creating a new equation, including a kinetic factor, which considers the environmental degradation processes. The effect of the rectified indicator was consistent with the sales data list of compounds, when applied to the markers. The indicator developed in this study, tested as a model on specific area-phase-period (Province of Siena, water phase, 2000?C2006), is applicable to any other area-phase-period, adjusting the partition value of the Mackay model for the case under study.     

磁性分散固相萃取气相色谱法测定地表水中有机磷化合物

应用磁性分散固相萃取技术对环境水体中有机磷化合物进行萃取测定,并对萃取剂的用量、萃取时间、解吸溶剂、盐度等实验影响因素进行了优化。在优化条件下,有机磷的回收率为80.1%~93.1%,相对标准偏差为4.6%~5.9%,检出限为0.000 2~0.000 4 mg/L。与传统的液液萃取及固相萃取相比,该磁性分散固相萃取方法操作更为简单、迅速,有机溶剂消耗量很少,方法环保。能很好的满足环境水体中有机磷化合物的测定。     

The first monoclonal antibody-based,matrix-resistant immunoassay for the carbamate herbicide asulam,in water

To date, no ligand binding assay has been described for the carbamate herbicide asulam, although a variety of physical methods, dependent on pre-concentration of water samples, have been documented for its assessment. However, asulam is increasingly used in sensitive agricultural areas, and statutory regulations concerning its monitoring will undoubtedly become more stringent. Antibodies are optimal partners in ligand binding assays, but it is commonly understood by immunological researchers that where no antibody reactive with a particular antigen has yet been described, the immunogenicity of the antigen may be particularly restricted. By the expedient of employing a specialised approach to final immunisation with an asulam-protein conjugate, prior to the immortalisation of a specific anti-asulam antibody-producing cell, we have succeeded in generating a monoclonal antibody reactive specifically with asulam that can be configured in a convenient immunoassay. This antibody may be used flexibly in a number of ways: small sample volumes of 10 microl can be assessed to sensitivities of 4.35 x 10(-7) M (10 microg L(-1)) while avoiding discrepancies contributed by the assay matrix; this antibody-based assay can also be formatted to deliver sensitivities at levels stipulated by regulatory authorities (e.g., 4.35 x 10(-9) M or 0.1 microg L(-1)) directly from a water sample, without prior pre-concentration.     

Synthetic musks in environmental samples: indicator compounds with relevant properties for environmental monitoring

Synthetic musks (nitro and polycyclic musks) are a group of chemicals offering a wide range of important properties for environmental monitoring programs. They are produced as odorous chemicals and added to a wide variety of perfumes, toiletry products and other household products. As such, they are directly applied in cosmetic products or in washed textiles to the human body in considerable concentrations and accumulate owing to dermal resorption. In addition, synthetic musks also enter the environment via waste water treatment. Several polycyclic musks are chiral. By using chiral gas chromatographic methods, it is possible to determine the enantiomeric ratio and assess their bioavailability. Although an comprehensive quality assurance program must be followed during the analysis of synthetic musks in environmental samples, the determination of these compounds is not very demanding and can be carried out by a standard analytical laboratory specialising in trace analysis of organic pollutants. Owing to the pheromone-like behavior of some synthetic musks, the induction of receptors in olfactory systems should be investigated. For HHCB (1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethylcyclopenta[g]-2-benzopyran, e.g., Galaxolide), three-dimensional structural similarities with androstenone (5 alpha-androst-16-en-3-one), a mammalian steroid pheromone, were found, which support the hypothesis of HHCB as an artificial pheromone. Owing to their environmental abundance, their relation to human activities and their potential for pheromone-like environmental behavior, synthetic musks are especially valuable as future indicator chemicals for environmental monitoring.     

Removal of atrazine and four organophosphorus pesticides from environmental waters by diatomaceous earth-remediation method

A new viable remediation technique based on the use of diatomaceous earth is proposed to improve the ecological system. Its ability to remove atrazine and the four organophosphorus pesticides parathion-methyl, chlorpyriphos, fenamiphos and methidathion from river and waste waters has been proven. A series of experiments including variable conditions, such as temperature, pH, contact time, pesticide concentration and adsorbent quantity, were performed to demonstrate the efficiency of pesticide removal from three different water samples. The batch experiments showed that diatomaceous earth was able to remove 95% of chlorpyriphos, 75% of methidathion and parathion-methyl and 55% of atrazine and fenamiphos from all types of waters tested. The individual adsorption of each pesticide on diatomaceous earth could be described by the Freundlich isotherm and a tentative adsorption mechanism was proposed. The Freundlich coefficient (Kf) and Freundlich constant (1/n) appeared to be closely related to the physicochemical properties (Kow, solubility) of the compounds. The actual results support the conclusion that diatomaceous earth has the potential to serve as an extractant in remediation techniques.     

Developing an environmental water quality monitoring program for Haraz River in Northern Iran

Water quality management plans are an indispensable strategy for conservation and utilization of water resources in a sustainable manner. One common industrial use of water is aquaculture. The present study is an attempt to use statistical analyses in order to prepare an environmental water quality monitoring program for Haraz River, in Northern Iran. For this purpose, the analysis of a total number of 18 physicochemical parameters was performed at 15 stations during a 1-year sampling period. According to the results of the multivariate statistical methods, the optimal monitoring would be possible by only 3 stations and 12 parameters, including NH₃, EC, BOD, TSS, DO, PO₄, NO₃, TDS, temperature, turbidity, coliform, and discharge. In other words, newly designed network, with a total number of 36 measurements (3 stations × 12 parameters = 36 parameters), could achieve exactly the same performance as the former network, designed based on 234 measurements (13 stations × 18 parameters = 234 parameters). Based on the results of cluster, principal component, and factor analyses, the stations were divided into three groups of high pollution (HP), medium pollution (MP), and low pollution (LP). By clustering the stations, it would be possible to track the water quality of Haraz River, only by one station at each cluster, which facilitates rapid assessment of the water quality in the river basin. Emphasizing on three main axes of monitoring program, including measurement parameters, sampling frequency, and spatial pattern of sampling points, the water quality monitoring program was optimized for the river basin based on natural conditions of the study area, monitoring objectives, and required financial resources (a total annual cost of about US $2625, excluding the overhead costs).     

连续流动分析快速测定环境水样中的硫化物

用新型的连续流动分析对环境水样中的硫化物进行分析测定。与传统的分析方法相比,该方法具有快速、灵敏度高、检出限低的特点。该方法的分析频率可达60次/小时,检测下限为0.006mg/L,大大提高了实验室自动化程度。     

New kinetic-spectrophotometric method for monitoring the concentration of iodine in river and city water samples

A new kinetic method has been developed for the determination of iodine in water samples. The method is based on the catalytic effect of I^? with the oxidation of Indigo Carmine (IC) by KBrO₃ in the sulfuric acid medium. The optimum conditions obtained are 0.16 M sulfuric acid, 1?×?10^?3 M of IC, 1?×?10^?2 M KBrO₃, reaction temperature of 35°C, and reaction time of 80 s at 612 nm. Under the optimized conditions, the method allowed the quantification of I^? in a range of 12–375 ng/mL with a detection limit of 0.46 ng/mL. The method was applied to the determination of iodine in river and city water samples with the satisfactorily results.     

Voltammetric determination of platinum at a lead film electrode in environmental water samples

The paper presents the first report on the application of a lead film electrode for the determination of ultratrace concentrations of platinum. The procedure is based on preconcentration of the Pt(IV)-formaldehyde complexes at an in situ plated lead film electrode held at ?0.9 V (vs. Ag/AgCl), followed by a negatively sweeping differential pulse voltammetric scan. The composition of the supporting electrolyte, the influence of accumulation potential and time on the sensitivity of platinum responses are discussed. The detection limit of Pt(IV) with the accumulation time of 60 was equal to 9.2?×?10^?12 mol L^?1. The application of this method was tested by recovery of Pt(IV) from spiked environmental water samples.     

河南省地表水环境监测断面优化的原则及其运用

提出和运用了地表水环境监测断面优化的原则,包括网络功能专一化、分类有序优化、监测断面高效、监测断面与监测频率同时优化、监测断面分级管理等。     

PCB congener distribution in estuarine water,sediment and fish samples: implications for monitoring programs

Traditional analyses for PCBs in environmental matrices havefocused on commercial Aroclor mixtures with detection limits inthe 100 to 1000 part per trillion range. This approach hasrecently been supplanted by analyses for specific PCB compoundscalled congeners with detection limits less than 0.5 ppt. At thenational level, total PCB determinations based upon selected PCBcongeners typically characterize analyses of surface water,sediment and tissue. These federal efforts rely on a suite of 18to 20 congeners out of a total of 209 congeners to characterizetotal PCB. The present study compares total PCB estimates basedupon this subset of congeners with estimates based upon anexpanded list of 81 congeners from water, sediment and fishtissue collected from the Delaware Estuary.Analytical data from monitoring programs conducted in theDelaware Estuary by the Delaware River Basin Commission, NOAANational Ocean Service, U.S. Army Corps of Engineers and the U.S.Environmental Protection Agency from 1996 to 1998 were evaluated. Total PCB estimates derived from the different sets of congeners,including the adjustment factor of 2.0 used by NOAA, werecompared. This evaluation indicated that differences existbetween total PCB determinations based upon these approaches, andthat these differences vary depending on the matrix analyzed. The bias associated with using a smaller set of PCB congeners,and the implications for risk assessment are discussed.     

Community air monitoring for pesticides. Part 1: selecting pesticides and a community

The CA Department of Pesticide Regulation (CDPR) developed methods to select pesticides and a community to fulfill criteria for an ambient air monitoring study it conducted as part of the CA Environmental Protection Agency's Environmental Justice Action Plan. Using a scoring system, CDPR evaluated 100 pesticides based on statewide-reported pesticide use, volatility, and priority in CDPR's risk assessment process (indicators of exposure and toxicity) to produce a list of pesticides to consider as candidates for monitoring. The CDPR also evaluated and scored 83 communities based on demographics and health factors, availability of cumulative impacts data, and reported pesticide use to create a list of community candidates. The scores provide relative rankings to distinguish more highly impacted communities from less impacted ones and to identify which pesticides might contribute most to potential adverse health effects. These methods use criteria that can be quantified, validated, and verified in order to provide a transparent and fair selection process. Based on public comments and highest scores, CDPR recommended 40 pesticides (including some of their degradation products) and one community for its yearlong monitoring study. The CDPR then further refined its list of pesticides by soliciting input from local and technical advisory groups. The CDPR plans to use these methods to select pesticides and communities in future monitoring activities.     

锆涂覆石墨管-无火焰原子吸收测定环境水样中微量银

用锆盐对石墨炉进行涂覆处理,同时又将其作为基体改进剂,有效提高了测定环境水样中银的灵敏度和分析精度,方法快速简便,检出限为2 8×10-12g,相对标准偏差小于6 2%。     

Methodologies for determination of antimony in terrestrial environmental samples

Methodologies for the environmental analysis of total antimony and aqueous chemical speciation are critically reviewed, including preparation techniques for aqueous and solid matrices and the determination of solid state partitioning and recommendations are given for future research directions. Concentrations of total antimony commonly present in aqueous and solid environmental samples are readily determined using present day analytical techniques. This has resulted primarily from technological advances in microwave digestion for solid matrices and the development of plasma based analyte detection systems. ICP-AES and ICP-MS techniques are both utilised for the environmental analysis of total antimony concentrations. However, ICP-MS is increasingly favoured as a result of reduced spectral interferences and the potential for analyte detection in the pg mL(-1) range. Determination of aqueous antimony speciation presents a number of complex analytical challenges and highly selective separation and identification techniques are required prior to detection. The majority of published techniques including common applications of hydride generation are insufficiently selective for the determination of intrinsic chemical speciation and often only oxidation state data are obtained. The recent in-line applications of HPLC-ICP-MS offer the potential for highly selective separations of aqueous antimony species and determination of detailed chemical speciation data. However, considerable development work is required to optimise chromatographic separations and identify uncharacterised species resident in environmental systems. Analytical techniques to aid the determination of antimony's associations with solid environmental matrices include the application of chemical extraction procedures and leaching experiments. To date, this area of analytical research has received little attention and further studies are required to elucidate this aspect of antimony's environmental chemistry.     

环境样品中矿物油监测常用萃取剂及其纯化和回收

详细介绍和评述了国内外环境样品中矿物油监测常用萃取剂及其理化性质 ,同时对它们的纯化和回收作了详细评述 ,并展望了矿物油监测用萃取剂研究的可能发展趋势。     

Laser-induced breakdown spectroscopy application in environmental monitoring of water quality: a review

Water quality monitoring is a critical part of environmental management and protection, and to be able to qualitatively and quantitatively determine contamination and impurity levels in water is especially important. Compared to the currently available water quality monitoring methods and techniques, laser-induced breakdown spectroscopy (LIBS) has several advantages, including no need for sample pre-preparation, fast and easy operation, and chemical free during the process. Therefore, it is of great importance to understand the fundamentals of aqueous LIBS analysis and effectively apply this technique to environmental monitoring. This article reviews the research conducted on LIBS analysis for liquid samples, and the article content includes LIBS theory, history and applications, quantitative analysis of metallic species in liquids, LIBS signal enhancement methods and data processing, characteristics of plasma generated by laser in water, and the factors affecting accuracy of analysis results. Although there have been many research works focusing on aqueous LIBS analysis, detection limit and stability of this technique still need to be improved to satisfy the requirements of environmental monitoring standard. In addition, determination of nonmetallic species in liquid by LIBS is equally important and needs immediate attention from the community. This comprehensive review will assist the readers to better understand the aqueous LIBS technique and help to identify current research needs for environmental monitoring of water quality.     

环境样品中 PCBs 的测定

通过碱解、酸洗、萃取、净化、浓缩、脱硫等步骤处理实际样品,利用毛细管柱GC/ECD进行PCBs的定性和定量.方法定性准确,定量良好,具有较高的回收率.各同系物的方法检出限,水样为0.01～0.08ng/L;土壤样为0.003～0.03μg/kg,可以应用于土壤、沉积物、水样、油样等环境样品中PCBs的测定