共查询到20条相似文献，搜索用时 546 毫秒
1.
GC/MS Nontarget Analysis to Examine an Organic Groundwater Contamination. Part II: Graphical and Multivariate Methods for Searching Key Substances In the nontarget analysis, a maximum of organic substances was extracted by a sequence which separates high polar, medium polar, and nonpolar compounds. This leads to the detection of 477 different organic substances in the example of the groundwater contamination investigated. To reduce the high expense for an exact identification of 477 compounds as a first step the individual compound is defined as a data set of retention time and the mass spectrum belonging to this retention time. The table of data contains now 477 individual compounds in groundwater samples collected at 10 different locations. The application of mathematical filters helps to reduce the size of the data set. Graphical methods enable large amounts of data to be visualized in a clear manner and enable to detect patterns in a data set. These patterns are the key to select typical compounds as indicator substances for the contamination source as well as the geogenic background. Similarities between the groundwater samples should not be changed by selection of the indicator compounds. Therefore, cluster analysis was applied as a controlling instrument for the final selection of the indicator compounds. The combination of graphical and multivariate data analysis is a useful tool to deduce indicator compounds for monitoring and control of complex environmental pollution states. 相似文献
2.
Humic substances (HS) were isolated from two contaminated groundwater samples (B22 and B53) from a site of a former gas facility. The isolation yielded almost only the fulvic acid fractions (FA). For characterization spectroscopic (UV, fluorescence) and chromatographic techniques (hydrophobic interaction chromatography – HIC as well as size-exclusion chromatography – SEC) were applied. The sample designated B22 FA was collected from the contamination plume whereas the sample B53 FA was collected downstream. Distinct differences were exhibited by these samples. The UV and fluorescence spectra as well as the HIC and SEC chromatograms of the B53 FA sample resemble those of the FA fraction obtained from natural water (groundwater, bog). The HIC and SEC chromatograms reveal the presence of organic compounds in B22 FA which can be derived from coal tar contaminants or their metabolites. Some of the compounds can be extracted from the FA fraction with non-polar organic solvents indicating adsorptive forces between the contaminants and the FA fraction. 相似文献
3.
Mengyan Li Patrick Conlon Stephanie Fiorenza Rock J. Vitale Pedro J.J. Alvarez 《Ground Water Monitoring & Remediation》2011,31(4):70-76
An innovative micro‐extraction of aqueous samples coupled with gas chromatography/mass spectrometry in selected ion‐monitoring mode (GC/MS‐SIM) was developed to selectively analyze for 1,4‐dioxane with low part‐per‐billion detection sensitivity. Recoveries of 1,4‐dioxane ranged from 93% to 117% for both spiked laboratory reagent water and natural groundwater matrices, the later having elevated organic carbon content (8.34 ± 0.31 mg/L as total organic carbon). We observed that freezing the aqueous sample along with the extraction solvent enhanced the extraction efficiency, minimized physical interferences, and improved sensitivity resulting in a limit of detection for 1,4‐dioxane to approximately 1.6 μg/L. This method substantially reduces the labor, time, reagents and cost, and uses instruments that are commonly found in analytical laboratories. This method requires a relatively small sample volume (200 μL), and can be considered a green analytical method as it minimizes the use of toxic solvents and the associated laboratory wastes. 相似文献
4.
A method is described for the detection and identification of dissolved organic compounds (DOCs) in various water samples. Acid treated active silica gel sorbent (pH 3) was packed into a micro‐column and used as a solid‐phase extraction medium for adsorption of DOCs. Silica particles‐adsorbed‐organic species were then divided into equal portions followed by suspension into various organic solvents of different polarities such as methanol, acetone, ethyl acetate, and toluene. Suspended silica‐adsorbed‐organic species were shaken for 1 h at room temperature and the organic extracts were subjected to GC–MS analysis under temperature programming conditions for qualitative detection and identification of these species. Blank solvents and silica samples were also subjected to the same extraction procedures and GC–MS analysis for comparison. The mass spectrum of each eluted chromatographic peak was library searched or manually interpreted to identify the compound. 相似文献
5.
Methods for the determination of three compound classes, i. e. diaminotoluenes, nitrophenols, and chloroaromatics in groundwater of a former ammunition plant are reported. Diaminotoluenes were extracted by discontinuous liquid/liquid-, nitrophenols by continuous liquid/liquid-extraction using dichloromethane, and chloroaromatics by solid-phase extraction. These compound classes may be analyzed by gas chromatography (GC) or gas chromatography coupled to mass spectrometry (GC/MS) without derivatization or after derivatization with N-methyl-bis(trifluoroacetamide) (MBTFA) or heptafluorobutyric anhydride (HFBA) in the case of diaminotoluenes and HFBA or acetic anhydride in the case of nitrophenols. An atomic emission detector (AED) coupled to a gas chromatograph may be employed for the analysis of chloroaromatics. High selectivity can be achieved using the characteristic wavelengths of chlorine. A variety of these compounds were identified and quantified in a groundwater sample from the former ammunition plant Elsnig (Saxony, Germany). Concentrations were in the lower ppb range. Thus, dichlorobenzenes which may have been used as substituents at the end of World War II could be identified in groundwater samples at this site. 相似文献
6.
Behaviour of Some Pharmaceuticals during Artificial Groundwater Recharge – Elimination and Effects on Microbiology The behaviour of bezafibrate, carbamazepine, clofibric acid, diclofenac, ibuprofen, and gemfibrozil during artificial groundwater recharge was investigated with different test systems simulating field conditions. The given concentrations of the pharmaceuticals were 100 μg/L in the influent of the systems. Concentrations in the influent as well as in the effluent were measured by GC‐MS. These column experiments indicated a significant elimination of bezafibrate, diclofenac, and ibuprofen (60 to 80%) during slow sand filtration. The results showed a moderate elimination of clofibric acid and gemfibrozil (40 to 60%) but a rather low elimination of carbamazepine (<40%). The adaptation times until the elimination processes started were about 5 days. Only the elimination of carbamazepine needed a lag phase up to 17 days. Additional column experiments with groundwater model systems indicated a high persistence of pharmaceuticals under aerobic and anaerobic groundwater conditions. The elimination was less than 20%. Only diclofenac was eliminated with rates between 60% and 80% in aerobic systems and between 40% and 60% in anaerobic systems. Analysis of eubacterial 16S‐rDNA by PCR and DGGE demonstrated changes in the microbial community structure in slow sand filters after application of pharmaceuticals. Adaptation processes may cause these changes, e.g. the appearance or disappearance of single species. Also differences between the populations of water and of the solid phase in slow sand filters could be demonstrated by DGGE pattern. 相似文献
7.
Dawn A. Zemo Kirk T. O'Reilly Rachel E. Mohler Asheesh K. Tiwary Renae I. Magaw Karen A. Synowiec 《Ground Water Monitoring & Remediation》2013,33(4):44-56
Polar metabolites resulting from petroleum biodegradation are measured in groundwater samples as TPHd unless a silica gel cleanup (SGC) is used on the sample extract to isolate hydrocarbons. Even though the metabolites can be the vast majority of the dissolved organics present in groundwater, SGC has been inconsistently applied because of regulatory concern about the nature and toxicity of the metabolites. A two‐step approach was used to identify polar compounds that were measured as TPHd in groundwater extracts at five sites with biodegrading fuel sources. First, gas chromatography with mass spectrometry (GC‐MS) was used to identify and quantify 57 individual target polar metabolites. Only one of these compounds—dodecanoic acid, which has low potential human toxicity—was detected. Second, nontargeted analysis was used to identify as many polar metabolites as possible using both GC‐MS and GC×GC‐MS. The nontargeted analysis revealed that the mixture of polar metabolites identified in groundwater source areas at these five sites is composed of approximately equal average percentages of organic acids, alcohols and ketones, with few phenols and aldehydes. The mixture identified in downgradient areas at these five sites is dominated by acids, with fewer alcohols, far fewer ketones, and very few aldehydes and phenols. A ranking system consistent with systems used by USEPA and the United Nations was developed for evaluating the potential chronic oral toxicity to humans of the different classes of identified polar metabolites. The vast majority of the identified polar metabolites have a “Low” toxicity profile, and the mixture of identified polar metabolites present in groundwater extracts at these five sites is unlikely to present a significant risk to human health. 相似文献
8.
A method for the determination of organohalogens by gas chromatography using electron capture (EDC) and mass-spectrometric (MS) detection was developed for sediments from lakes and sludges of water treatment plants. The method was described and separate techniques for sample preparation were investigated to compare the retrieval rates and the best approach to the “real value”. With the help of solid-liquid-phase- and liquid-liquid-phase extraction sulphur, most of the organosulphur compounds and carbon acids were effectively removed. The compounds were identified by comparing temperature programmed retention indices with those of reference compounds and by high-resolution GC/MS. 相似文献
9.
The corporate purpose of Wismut GmbH is to decommission its former mining holdings and to rehabilitate the landscape and the environment. Sample taking and analysing the value of contaminants are necessary steps for the remediation of waste rock piles, the recycling of contaminated areas, controlled flooding of uranium mines. Main emphasis lies on the determination of heavy metals and radionuclides of natural decay chains of U‐238 and U‐235. Yearly about 60 000…70 000 determinations of radionuclides in waters were done. Facing this high output of determinations it is a permanent task for laboratory and quality management to ask: Are the results of different methods comparable to each other? Is there a preferred analytical technology? Which matrix influences exist? and What about the analytical costs? Answers to these important questions are given in this report. Summarizing our investigations done in the last few years it is possible to say that – by using different analytical methods the results of radionuclides in water samples (surface or groundwater) are comparable, – a not negligible influence of Ra‐223, Ra‐224 and Ra‐228 may exist by using the DIN 38404 C18 method to determine Ra‐226, – a preferred method cannot be defined, – the choice of the analytical method should include analytical questions (the sample matrix, the occurrence of other disturbing radionuclides, the necessary detection limit) and economical questions (costs, other parameters to be determined). 相似文献
10.
Chlorinated‐solvent compounds are among the most common groundwater contaminants in the United States. A majority of the many sites contaminated by chlorinated‐solvent compounds are located in metropolitan areas, and most such areas have one or more chlorinated‐solvent contaminated sites. Thus, contamination of groundwater by chlorinated‐solvent compounds may pose a potential risk to the sustainability of potable water supplies for many metropolitan areas. The impact of chlorinated‐solvent sites on metropolitan water resources was assessed for Tucson, Arizona, by comparing the aggregate volume of extracted groundwater for all pump‐and‐treat systems associated with contaminated sites in the region to the total regional groundwater withdrawal. The analysis revealed that the aggregate volume of groundwater withdrawn for the pump‐and‐treat systems operating in Tucson, all of which are located at chlorinated‐solvent contaminated sites, was 20% of the total groundwater withdrawal in the city for the study period. The treated groundwater was used primarily for direct delivery to local water supply systems or for reinjection as part of the pump‐and‐treat system. The volume of the treated groundwater used for potable water represented approximately 13% of the total potable water supply sourced from groundwater, and approximately 6% of the total potable water supply. This case study illustrates the significant impact chlorinated‐solvent contaminated sites can have on groundwater resources and regional potable water supplies. 相似文献
11.
Waste water from ammunition production sites and aqueous samples (ground and surface water) on or near former military sites on which explosives were produced or filled, e.g. into shells, may be contaminated by the original explosives—mainly nitrotoluenes (such as dinitrotoluenes, trinitrotoluene (TNT)) and nitramines (such as hexogen (RDX), octogen (HMX), and tetryl) or hexyl, but also by byproducts and compounds formed by biodegradation of the explosives such as aminonitrotoluenes, chlorinated nitrobenzenes and nitrophenols. These compounds can be extracted from aqueous samples by liquid/liquid extraction (using dichloromethane or toluene) or by solid phase extraction using C-18 adsorbents with high recoveries (usually ≥85%) provided they contain only one amino group. Nitrotoluenes, chlorinated nitrobenzenes and aminonitrotoluenes (nitrotoluidines) may be determined by gas chromatography (GC) using selective detectors such as an electron capture detector (ECD), a nitrogen-phosphorus detector (NPD) or a chemiluminescence detector (thermal energy analyzer, TEA). The use of combined gas chromatography/mass spectrometry (GC/MS) under electron impact conditions is even more specific. Detection limits comparable to an ECD or NPD, however, are only achieved if the mass spectrometer is operated under selected ion monitoring (SIM). Nitrophenols are derivatized after extraction by heptafluorobutyric anhydride or by acetic anhydride where the latter method can be directly applied to the aqueous sample. The nitramine explosives, such as RDX, HMX, and tetryl, hexyl, the nitrate esters, such as nitropenta (PETN) and nitroguanidine as well as picric acid cannot, or only with difficulty, be analyzed by gas chromatography. They may be determined by high performance liquid chromatography (HPLC) with UV-detection. The HPLC analysis can be extended to include also nitrotoluenes and nitroaminotoluenes. 相似文献
12.
Matt A. Limmer Gregory D. Martin Christopher J. Watson Camilo Martinez Joel G. Burken 《Ground Water Monitoring & Remediation》2014,34(1):49-56
Phytoscreening has been proven to rapidly delineate subsurface contaminant plumes for semiquantitative site assessment, with minimal impact to property or ecology through the collection and analysis of tree cores. Here, three phytoscreening methods were applied concurrently to identify multiple chlorinated volatile organic compounds (cVOCs) in a phytoremediation treatment system at a contaminated industrial facility. Tree coring, in planta gas chromatography–mass spectrometry (GC‐MS), and in planta passive sampling showed general agreement, with the in planta GC‐MS providing the quickest but least quantitative results. The portable GC‐MS sampling and analysis method identified six cVOCs in the xylem of hybrid poplars (Populus sp.) in the phytoremediation plot. These real‐time data can permit onsite identification and delineation of the contaminants, allowing for adaptive sampling during a single mobilization to a site. The in vitro methods provided quantitative data across two sampling campaigns, as relative cVOC concentrations remained similar between the two trips, despite a decrease in absolute cVOC concentrations from August to October. Overall, this research demonstrates the advantages and limitations of three phytoscreening techniques. 相似文献
13.
The flood in the Odra river in 1997 has led to considerable additional pollution of the Stettin Lagoon and the Baltic Sea with contaminated suspended solids. For some priority substances, the pollutant entries via suspended solids during the flood period are estimated to be approximately 1/3 of the usual annual load. Among these priority pollutants there are total organic carbon (TOC), nitrogen, and the heavy metals Cu, Pb and Zn. For the concentrations of the priority pollutants in suspended solids accumulation factors from 2 to 4 in the comparison with normal conditions were observed. On the basis of the analysis of sediments sampled after the flood, main sources of the pollutants should be evaluated. As reference area with an industrial background as well as a typical pollutant pattern the region around Glogow/Legnica is proposed. 相似文献
14.
广州市海珠区地表水中致嗅物质及毒性分析 总被引：1，自引：1，他引：0
为研究广州市海珠区地表水中的致嗅物质及其毒性,在海珠区珠江前后航道与湖泊池塘采集了21个水样,采用液液萃取气质联用法对其中的土臭素、二甲基异茨醇等5种致嗅物质进行含量检测,并根据水样相关富营养化指标,探究这些致嗅物质的分布和来源.研究结果表明:海珠区地表水中含量最高的两种致嗅物质依次是土臭素(4.0~69.0 ng/L)和二甲基异茨醇(4.1~24.9 ng/L);异臭味问题最严重的地表水体是珠江水,其次为湖泊池塘,水厂取水口的异臭味问题不明显;珠江前航道中致嗅物质的含量高于后航道,其中含量最高的河段为鳌洲码头段至广州大桥段,含量高达40.2~69.0 ng/L;致嗅物质的含量和分布与水体的污染和富营养化程度密切相关,广州市海珠区地表水的净化和治理形势严峻.另外,在可检出的浓度范围内,土臭素和二甲基异茨醇对发光细菌抑制率较高. 相似文献
15.
Phoebe Zito Rana Ghannam Barbara A. Bekins David C. Podgorski 《Ground Water Monitoring & Remediation》2019,39(4):25-31
The extraction efficiency of petroleum-derived dissolved organic matter (DOM) was examined for groundwater samples from an aquifer contaminated with crude oil. Five different types of extraction techniques were investigated to determine which method is best suited for the analysis of potentially toxic petroleum-derived DOM. The five types were a liquid-liquid extraction (LLE) with dichloromethane (DCM) and total petroleum hydrocarbons-diesel range (TPHd) with DCM (EPA method 3510C), and three solid-phase extraction (SPE) stationary phases that are routinely used for extraction of polar analytes from water. For the LLE and TPHd, that is selective for nonpolar compounds, the extraction efficiency of petroleum-derived DOM decreased downgradient as the petroleum-derived DOM becomes increasingly polar due to biodegradation. In contrast, the average extraction efficiency by the SPE methods was greater than 65% across the gradient. The results showed that SPE is more efficient for extracting petroleum-derived DOM at hydrocarbon-contaminated sites. The use of a method with greater extraction efficiency for partially oxidized hydrocarbons may prove useful in determining relationships between their composition and structure and potential for risks to human health or the environment. 相似文献
16.
H.-J. Brauch 《洁净——土壤、空气、水》1993,21(2):84-88
High resolution gas chromatography (HRGC) with ECD, NFID and MSD is a very efficient determination method for pesticides in water. Because of their relatively low concentrations in aquatic systems enrichment and preconcentration procedures are essential. Some examples for pesticide determination by GC methods are given. Potentials and limitations of HRGC for pesticide analysis are also discussed. An extensive pesticide analysis in water has to include different methods like HRGC, HPLC and GC/MS. 相似文献
17.
Identification of Nitrogen-containing Compounds of Low Molecular Weight in Effluents of Biologically Treated Municipal Wastewater Enriching methods based on reversed phases were developed for the investigation of low-molecular compounds containing nitrogen in municipal wastewater effluent. The enriched mixtures were treated gas chromatographically without derivatization under different conditions. By application of the PBM-algorithm to the GC/MS spectra of the enriched samples (concentration factor 1000...20000), 133 nitrogen-containing compounds could be identified with a probability of occurence of at least 30% put out. Seventeen of these compounds were identified with > 90% probability and another ten with 80...90% probability. 9-Methylacridine was found in nine of ten processed samples investigated. The nitrogen content of the 133 identified compounds was estimated at about 20% of the low-molecular fraction of DON (dissolved organic nitrogen). 相似文献
18.
Michaela Ventker Friedrich Werres Peter Balsaa Peter Winterhalter Horst Overath 《洁净——土壤、空气、水》2004,32(1):40-47
Determination of Organophosphorus Pesticides in Water by HPLC‐MS‐MS In the EC Water Framework Directive 2000/60/EG and in CEC 76/464/EEC there are 16 organophosphorus pesticides (insecticides and acaricides) listed which belong to so‐called priority substances. The committed quality aims of these substances frequently require maximum concentrations below 0.1 μg/L. In this paper a HPLC‐MS‐method is described. The reported limits of determination of organophosphorus pesticides are lower than the demanded limits. High analytical sensitivity is reached by solid‐phase extraction (SPE) and by injecting large volumes. For some of these substances no sample enrichment is needed and low detection limits are obtained by direct injection of the original water sample. 相似文献
19.
Zhiguang Song Keith W. Jones Nebojsa Marinkovic Xian Ming Xiao Huan Feng Elli Tchouparova 《洁净——土壤、空气、水》2011,39(12):1041-1049
Dredging and remediation of contaminated Harbor sediments requires characterization of organic pollutants. In this paper, we apply a combination of Fourier transform IR attenuated total reflectance (FTIR‐ATR) and synchrotron FTIR techniques to the investigation of sediments and related materials from New York/New Jersey Harbor and other locations. The FTIR techniques give information on the functional groups of the compounds found in the sediments and make possible measurements with a spatial resolution of about 0.015 mm. Comparisons of natural organic materials namely, river and groundwater humic substances, recent marine and lacustrine sediments, and ancient sedimentary kerogen show that contaminated NY/NJ Harbor sediments display a strong and distinct absorption in their IR spectra at 2850–2950 cm?1 identified as a C? H stretching band, indicative of the presence of anthropogenic hydrocarbons. We suggest that the presence of this band could be used for rapid screening for the presence of contaminant organic compounds in sediments encountered in dredging operations and/or as an indicator for the efficacy of sediment decontamination technologies used for treatment of dredged material. 相似文献
20.
Different types of data can be collected to evaluate whether or not vapor intrusion is a concern at sites impacted with volatile organic compound (VOC) contamination in the subsurface. Typically, groundwater, soil gas, or indoor air samples are collected to determine VOC concentrations in the different media. Sample results are evaluated using a “multiple lines of evidence” approach to interpret whether vapor intrusion is occurring. Data interpretation is often not straightforward because of many complicating factors, particularly in the evaluation of indoor air. More often than not, indoor air sample results are affected by indoor or other background sources making interpretation of concentration‐based data difficult using conventional sampling approaches. In this study, we explored the practicality of compound‐specific isotope analysis (CSIA) as an additional type of evidence to distinguish between indoor sources and subsurface sources (i.e., vapor intrusion). We developed a guide for decision‐making to facilitate data interpretation and applied the guidelines at four different test buildings. To evaluate the effectiveness of the CSIA method for vapor intrusion applications, we compared the interpretation from CSIA to interpretations based on data from two different investigation approaches: conventional sampling and on‐site GC/MS analysis. Interpretations using CSIA were found to be generally consistent with the other approaches. In one case, CSIA provided the strongest line of evidence that vapor intrusion was not occurring and that a VOC source located inside the building was the source of VOCs in indoor air. 相似文献