Water Quality. Determination of Selected Polycyclic Aromatic Hydrocarbons (PAH) in Whole Water Samples. Method Using Solid Phase Extraction (SPE) with SPE-Disks Combined with Gas Chromatography Mass Spectrometry (GC-MS) PDF Download
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Author: British Standards Institute Staff
Publisher:
ISBN: 9780580844690
Category :
Languages : en
Pages : 36
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Book Description
Water, Quality, Water testing, Chemical analysis and testing, Determination of content, Polynuclear aromatic hydrocarbons, Aromatic hydrocarbons, Potable water, Chromatography, Thin-layer chromatography, Fluorimetry, Extraction methods of analysis
Author: British Standards Institute Staff
Publisher:
ISBN: 9780580844690
Category :
Languages : en
Pages : 36
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Book Description
Water, Quality, Water testing, Chemical analysis and testing, Determination of content, Polynuclear aromatic hydrocarbons, Aromatic hydrocarbons, Potable water, Chromatography, Thin-layer chromatography, Fluorimetry, Extraction methods of analysis
Author: Mohamed Elrutb
Publisher:
ISBN:
Category :
Languages : en
Pages :
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Book Description
Factors affecting the detennination of PAHs by capillary GC/MS were studied. The effect of the initial column temperature and the injection solvent on the peak areas and heights of sixteen PAHs, considered as priority pollutants, USillg crosslinked methyl silicone (DB!) and 5% diphenyl, 94% dimethyl, 1% vinyl polysiloxane (DBS) columns was examined. The possibility of using high boiling point alcohols especially butanol, pentanol, cyclopentanol, and hexanol as injection solvents was investigated. Studies were carried out to optimize the initial column temperature for each of the alcohols. It was found that the optimum initial column temperature is dependent on the solvent employed. The peak areas and heights of the PAHs are enhanced when the initial column temperature is 10-20 c above the boiling point of the solvent using DB5 column, and the same or 10 C above the boiling point of the solvent using DB1 column. Comparing the peak signals of the PAHs using the alcohols, p-xylene, n-octane, and nonane as injection solvents, hexanol gave the greatest peak areas and heights of the PAHs particularly the late-eluted peaks. The detection limits were at low pg levels, ranging from 6.0 pg for fluorene t9 83.6 pg for benzo(a)pyrene. The effect of the initial column temperature on the peak shape and the separation efficiency of the PARs was also studied using DB1 and DB5 columns. Fronting or splitting of the peaks was obseIVed at very low initial column temperature. When high initial column temperature was used, tailing of the peaks appeared. Great difference between DB! and.DB5 columns in the range of the initial column temperature in which symmetrical.peaks of PAHs can be obtained is observed. Wider ranges were shown using DB5 column. Resolution of the closely-eluted PAHs was also affected by the initial column temperature depending on the stationary phase employed. In the case of DB5, only the earlyeluted PAHs were affected; whereas, with DB1, all PAHs were affected. An analytical procedure utilizing solid phase extraction with bonded phase silica (C8) cartridges combined with GC/MS was developed to analyze PAHs in water as an alternative method to those based on the extraction with organic solvent. This simple procedure involved passing a 50 ml of spiked water sample through C8 bonded phase silica cartridges at 10 ml/min, dried by passing a gentle flow of nitrogen at 20 ml/min for 30 sec, and eluting the trapped PAHs with 500 Jll of p-xylene at 0.3 ml/min. The recoveries of PAHs were greater than 80%, with less than 10% relative standard deviations of nine determinations. No major contaminants were present that could interfere with the recognition of PAHs. It was also found that these bonded phase silica cartridges can be re-used for the extraction of PAHs from water.
Author: Mary C. Olson
Publisher:
ISBN:
Category : Contaminated sediments
Languages : en
Pages : 62
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Book Description
Author: Tomi Schebywolok
Publisher:
ISBN:
Category :
Languages : en
Pages :
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Book Description
Solid-phase microextraction (SPME) coupled with gas chromatography/mass spectrometry (GC/MS) is routinely used to analyze polycyclic aromatic hydrocarbons (PAHs) in water. A common SPME-GC/MS approach quantifies target analytes using isotopically labeled standards (IISs); one IIS is needed for each target analyte. This approach is challenging, even prohibitive since IISs are often expensive; moreover, they are generally not available for each analyte of interest. This study developed a novel SPME-GC/MS approach for the quantification of PAHs in water. The new method, which employs only a small number of IISs, uses relative response factor (RRF) (i.e., analyte corresponding to IIS) to quantify PAHs in water. Possible matrix dependency of RRFs values was examined using water that was modified concerning different physical-chemical characteristics (i.e., ionic strength, pH, suspended solids, humic acid, and biological organic carbon represented by hemoglobin). The results revealed that RRFs are not noticeably affected by changing ionic strength and pH; the other three parameters did affect the RRFs. However, the results also showed that the effect is minimal when the solution is dilute (i.e., low concentrations of suspended solids, humic acid or hemoglobin). Relatively stable RRFs for dilute water solutions indicates that this approach can be used for routine quantification of water that does not contain prohibitive amounts of suspended solids, humic acid, and biological organic matter. The developed method was employed to quantify trace levels of PAHs in three different types of water, namely river water, well water, and bottled water. PAH levels in every kind of water were less than 100 ng/L level (i.e., 0.1 ppb). Analyses of spiked water samples containing 2 ng PAHs revealed correlations between calculated RRFs and the physical-chemical properties of the PAHs investigated (i.e., vapor pressure, boiling point, octanol/water partition coefficient, octanol/air partition coefficient, GC retention time). This implies that RRFs for PAHs not examined in this study can be predicted. Overall, the results presented herein constitute a meaningful contribution to the development of SPME-GC/MS methods for quantitative analysis of PAHs and other chemicals in dilute aqueous solutions. Moreover, the development of methods that alleviate the need for IISs corresponding to each target analyte.
Author: Justyna Płotka-Wasylka
Publisher: Springer
ISBN: 981139105X
Category : Science
Languages : en
Pages : 449
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Book Description
The book explains the principles and fundamentals of Green Analytical Chemistry (GAC) and highlights the current developments and future potential of the analytical green chemistry-oriented applications of various solutions. The book consists of sixteen chapters, including the history and milestones of GAC; issues related to teaching of green analytical chemistry and greening the university laboratories; evaluation of impact of analytical activities on the environmental and human health, direct techniques of detection, identification and determination of trace constituents; new achievements in the field of extraction of trace analytes from samples characterized by complex composition of the matrix; “green” nature of the derivatization process in analytical chemistry; passive techniques of sampling of analytes; green sorption materials used in analytical procedures; new types of solvents in the field of analytical chemistry. In addition green chromatography and related techniques, fast tests for assessment of the wide spectrum of pollutants in the different types of the medium, remote monitoring of environmental pollutants, qualitative and comparative evaluation, quantitative assessment, and future trends and perspectives are discussed. This book appeals to a wide readership of the academic and industrial researchers. In addition, it can be used in the classroom for undergraduate and graduate Ph.D. students focusing on elaboration of new analytical procedures for organic and inorganic compounds determination in different kinds of samples characterized by complex matrices composition.Jacek Namieśnik was a Professor at the Department of Analytical Chemistry, Gdańsk University of Technology, Poland. Justyna Płotka-Wasylka is a teacher and researcher at the same department.
Author: Wang Huiyong
Publisher:
ISBN:
Category : Extraction (Chemistry)
Languages : en
Pages : 232
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Book Description
Polycyclic aromatic hydrocarbons (PAH) are important environmental pollutants originating from a wide variety of natural and anthropogenic sources. Because many of them are highly suspect as etiological agents in human cancer, chemical analysis of PAH is of great environmental and toxicological importance. Current methodology for PAH follows the classical pattern of sample preparation and chromatographic analysis. Sample preparation pre-concentrates PAH, simplifies matrix composition, and facilitates analytical resolution in the chromatographic column. Among the several approaches that exist to pre-concentrate PAH from water samples, the Environmental Protection Agency (EPA) recommends the use of solid-phase extraction (SPE). High-performance liquid chromatography (HPLC) and gas chromatography-mass spectrometry (GC-MS) are the basis for standard PAH identification and determination. Ultraviolet (UV) absorption and room temperature fluorescence detection are both widely used in HPLC, but the specificity of these detectors is modest. Since PAH identification is solely based on retention times, unambiguous PAH identification requires complete chromatographic resolution of sample components. When HPLC is applied to "unfamiliar" samples, the EPA recommends that a supporting analytical technique such as GC-MS be applied to verify compound identification and to check peak-purity HPLC fractions. Independent of the volume of extracted water, the approximate time required to separate and determine the sixteen "priority pollutants" (EPA-PAH) via HPLC is approximately 60min. If additional GC-MS analysis is required for unambiguous PAH determination, the total analysis time will reach 2-3 hours per sample. If the concentrations of target species are found to lie outside the detector's response range, the sample must be diluted and the process repeated. These are important considerations when routine analysis of numerous samples is contemplated. Parent PAH are relatively inert and need metabolic activation to express their carcinogenicity. By virtue of the rich heterogeneous distribution of metabolic products they produce, PAH provide a full spectrum of the complexity associated with understanding the initial phase of carcinogenesis. PAH metabolites include a variety of products such as expoxides, hydroxyl aromatics, quinines, dihydrodiols, dioepoxides, tetrols and water soluble conjugates. During the past decades tremendous efforts have been made to develop bio-analytical techniques that possess the selectivity and sensitivity for the problem at hand. Depending on the complexity of the sample and the relative concentrations of the targeted metabolites, a combination of sample preparation techniques is often necessary to reach the limits of detection of the instrumental method of analysis. The numerous preparation steps open ample opportunity to metabolite loss and collection of inaccurate data. Separation of metabolites has been accomplished via HPLC, capillary electrophoresis (CE) and GC-MS. Unfortunately, the existence of chemically related metabolic products with virtually identical fragmentation patterns often challenges the specificity of these techniques. This dissertation presents significant improvements in various fronts. Its first original component--which we have named solid-phase nano-extraction (SPNE)--deals with the use of gold nanoparticles (Au NPs) as extracting material for PAH. The advantages of SPNE are demonstrated for the analysis of PAH in water samples via both HPLC and Laser-Excited Time-Resolved Shpol'skii Spectroscopy (LETRSS). The same concept is then extended to the analysis of monohydroxy-PAH in urine samples via SPE- HPLC and In-Capillary SPNE-CE. The second original component of this dissertation describes the application of Shpol'skii Spectroscopy to the analysis of polar PAH metabolites. The outstanding selectivity and sensitivity for the direct analysis of PAH at trace concentration levels has made Shpol'skii spectroscopy a leading technique in environmental analysis. Unfortunately, the requirement of a specific guest-host combination--typically a non-polar PAH dissolved in an n-alkane-- has hindered its widespread application to the field of analytical chemistry. This dissertation takes the first steps in removing this limitation demonstrating its feasibility for the analysis of polar benzopyrene metabolites in alcohol matrixes.
Author: British Standards Institute Staff
Publisher:
ISBN: 9780580845192
Category :
Languages : en
Pages : 34
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Book Description
Water, Quality, Determination of content, Pesticides, Extraction, Gas chromatography, Chromatography, Mass spectrometry, Spectroscopy, Calibration, Mathematical calculations, Potable water, Water testing, Surface water
Author: British Standards Institute Staff
Publisher:
ISBN: 9780580554865
Category :
Languages : en
Pages : 40
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Book Description
Wastes, Sludge, Soils, Soil pollution, Bitumens, Chemical analysis and testing, Determination of content, Aromatic hydrocarbons, Polynuclear aromatic hydrocarbons, Gas chromatography, Mass spectrometry, Extraction methods of analysis
Author: Carlos Andres Manzano
Publisher:
ISBN:
Category : Gas chromatography
Languages : en
Pages : 132
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Book Description
Polycyclic aromatic hydrocarbons (PAHs) are ubiquitous contaminants and are mostly products of the incomplete combustion of organic material. PAHs are often found in environmental samples as a complex mixture of isomers. In addition, the same sources that produce complex PAH mixtures also produce other poorly characterized mixtures of organic compounds, commonly referred to as an unresolved complex mixture (UCM), that act as matrix interferences in the chromatographic analysis of samples. Conventional one-dimensional chromatographic techniques, such as gas chromatography coupled to mass spectrometry (GC/MS), are not sufficient for the analysis and quantitation of complex PAH mixtures present in environmental samples due to the high degree of overlap in compound vapor pressures, boiling points, and mass spectral fragmentation patterns. Therefore, the separation and quantitation of complex mixtures of individual PAH compounds in environmental samples requires high chromatographic resolution. Comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GCxGC/ToF-MS) was used for this study. GCxGC/ToF-MS uses two different gas chromatographic columns, with different separation mechanisms, for the analysis of complex environmental samples. In theory, the peak capacity in GCxGC/ToF-MS is equivalent to the product of the individual peak capacities of each column used. However, in practice, this is rarely obtained because of the existing correlation between the two GC columns used. This dissertation is a compilation of three studies related to analytical method development for the identification and quantitation of complex PAH mixtures (including parent-PAHs, alkyl-PAHs, oxy-PAHs, nitro-PAHs, thio-PAHs, chloro-PAHs, bromo-PAHs and PAHs with molecular weight higher than 300 Da) that may be present in environmental samples using novel column combinations in GCxGC/ToF-MS. The use of a liquid crystal column (LC-50) in the first dimension, followed by a nano-stationary phase column (NSP-35) in the second dimension, was evaluated for the separation of a standard PAH mixture containing 97 different PAHs. Two standard reference materials purchased from NIST (NIST SRM1650b - Diesel Particulate Matter and NIST SRM1975 - Diesel Extract) were used, after extraction and cleanup, for method validation and comparison between the commonly used non-polar x polar column combination and the LC-50 x NSP-35 column combination with high orthogonality. As part of the method validation, an aliquot of NIST SRM1975 (Diesel extract), without sample cleanup was also analyzed for PAHs, showing that the LC-50 x NSP-35 column combination was accurate (with an average absolute percent difference of approximately 30%) for the identification and quantitation of complex PAH mixtures in environmental samples, with reduced sample preparation prior to analysis. In addition, the LC-50 x NSP-35 column combination was used for the analysis of PAHs sorbed to polystyrene pellets deployed in an urban bay area as passive water samplers because one-dimensional GC/MS was ineffective due to the presence of a strong unresolved complex mixture (UCM) and matrix interferences.
Author: British Standards Institute Staff
Publisher:
ISBN: 9780580403576
Category : High performance liquid chromatography
Languages : en
Pages : 32
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Book Description
Water, Quality, Water testing, Chemical analysis and testing, Determination of content, Aromatic hydrocarbons, Polynuclear aromatic hydrocarbons, Liquid chromatography, Extraction methods of analysis, Fluorescence, Potable water, Ground water
