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PubMed2004

Optimizing the determination of haloacetic acids in drinking waters.

Three methods are currently approved by the US Environmental Protection Agency for the compliance monitoring of haloacetic acids in drinking waters. Each derivatizes the acids to their corresponding esters using either acidic methanol or diazomethane. This study was undertaken to characterize the extent of methylation of these analytes by these methods, and to fully optimize methylation chemistries to improve analytical sensitivity, precision and accuracy. The approved methods were shown to have little to no esterification efficiencies for the brominated trihaloacetic acids (HAA3). Methylation with acidic methanol was determined to be more efficient and rugged than methylation with diazomethane. A new higher boiling solvent, tertiary-amyl methyl ether, is reported which has significantly improved methylation efficiencies for HAA3. Additional modifications to the method have been made that improve method ruggedness. The revised method, EPA Method 552.3, outperforms the currently approved methods, especially for HAA3.

Acetates↗
PubMed2004

Selective pressurized liquid extraction of polychlorinated biphenyls from fat-containing food and feed samples influence of cell dimensions, solvent type, temperature and flush volume.

Sulphuric acid impregnated silica was used for the lipid free extraction of polychlorinated biphenyls from fat containing food and feed matrices using pressurized liquid extraction on a Dionex ASE300, with 34 mL cells. Data were compared to a previous publication where extractions had been performed on a Dionex ASE200, with 33 mL cells. Four different fat/fat retainer ratios (FFRs) were tested (0.100, 0.075, 0.050 and 0.025) at 50 and 100 degrees C using n-pentane, n-hexane or n-heptane as extraction solvent. The best results were obtained with a FFR of 0.025 when applying a temperature of 100 degrees C. Both n-pentane and n-heptane were capable of replacing n-hexane as extraction solvent. A flush volume of 60% was sufficient as suggested in US Environmental Protection Agency Method 3545. The applicability of the method was demonstrated for naturally contaminated fish meal as well as various spiked and certified materials.

Animal Feed↗
PubMed2004

Supported liquid membrane microextraction with high-performance liquid chromatography-UV detection for monitoring trace haloacetic acids in water.

Supported liquid membrane microextraction (SLMME) with high-performance liquid chromatography (HPLC)-UV detection has been developed for the extraction, preconcentration, and determination of all the nine haloacetic acids (HAAs) in water. The HAAs are extracted into a supported liquid membrane, and then back-extracted into few microliters of an acceptor solution. The extract was directly analyzed by HPLC-UV with a 15-min run. Enrichment factors in the range of 300-3000 were obtained in a 60-min extraction, and detection limits were at low to sub-microg/L level with R.S.D. values between 1.5 and 10.8%. The parameters that affected analyte enrichment were studied. This approach offers an attractive alternative to the current US Environmental Protection Agency standard methods for HAA analysis, which require complex sample preparation and derivatization prior to analysis by gas chromatography. SLMME can also be used in conjunction with other analytical schemes, such as, ion chromatography and capillary electrophoresis.

Acetates↗
PubMed2004

Comparison of series 5 gas chromatography column performances from a variety of manufacturers for separation of chlorinated dibenzo-p-dioxins and dibenzofurans using high-resolution mass spectrometry.

An extended study of seven fused silica capillary gas chromatographic (GC) columns has been conducted with regard to separation of international toxic equivalent factor (I-TEF) isomers (tetra- through octa-chlorinated at 2,3,7,8 positions) of polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans (PCDDs/PCDFs) from closely co-eluted other isomers using high-resolution gas chromatography-high-resolution mass spectrometry (HRGC-HRMS). The data are explicated in mass chromatograms of Series 5 GC columns from a variety of manufacturers (Varian CP-Sil 8 CB LowBleed/MS, Phenomenex ZB-5UMS, Agilent HP-5MS, Restek Rtx-5MS, Supelco Equity-5, J&W Scientific DB-5 and DB-5MS), according to relative retention times, and 2,3,7,8-substituted isomer concentrations for each of the columns tested. Results showed differences between 5% phenyl methyl silicone and 5% silphenylene (Si-arylene) silicone polymer type GC stationary phases in separation of 2,3,7,8-substituted PCDDs/PCDFs from closely co-eluted isomers. The separation differences for Si-arylene type columns resulted in lower toxic equivalence (TEQ) values compared to the siloxane-based columns. Because of differences in product nomenclature and manufacturing practices by various manufacturers, incorrect assumptions and comparisons may be made regarding the interchangeability of these columns for PCCD/PCDF separations. The data presented are the most comprehensive to date and provide a valuable addition to operational criteria for the standard US Environmental Protection Agency methods 1613b and 8290.

Benzofurans↗
PubMed2005

Multivariate optimization of a solid-phase microextraction method for the analysis of phthalate esters in environmental waters.

A solid-phase microextraction method (SPME) coupled to gas chromatography-mass spectrometry (GC-MS) has been developed for the determination of the six phthalate esters included in the US Environmental Protection Agency (EPA) Priority Pollutants list in water samples. These compounds are dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), butylbenzyl phthalate (BBP), di-2-ethylhexyl phthalate (DEHP) and di-n-octyl phthalate (DOP). Detailed discussion of the different parameters, which could affect the extraction process, is presented. Main factors have been studied and optimized by means of a multifactor categorical design. Different commercial fibers, polydimethylsiloxane (PDMS), polydimethylsiloxane-divinylbenzene (PDMS-DVB), polyacrylate (PA), Carboxen-polydimethylsiloxane (CAR-PDMS) and Carbowax-divinylbenzene (CW-DVB), have been investigated, as well as the extraction mode, exposing the fiber directly into the sample (DSPME) or into the headspace over the sample (HS-SPME), and different extraction temperatures. The use of this experimental design allowed for the evaluation of interactions between factors. Extraction kinetics has also been studied. The optimized microextraction method showed linear response and good precision for all target analytes. Detection limits were estimated considering the contamination problems associated to phthalate analysis. They were in the low pg mL(-1), excluding DEHP (100 pg mL(-1)). The applicability of the developed SPME method was demonstrated for several real water samples including mineral, river, industrial port and sewage water samples. All the target analytes were found in real samples. Levels of DEP and DEHP were over 1 ng mL(-1) in some of the samples.

Chemical Fractionation↗
PubMed2005

Determination of chloro-s-triazines including didealkylatrazine using solid-phase extraction coupled with gas chromatography-mass spectrometry.

Chloro-s-triazines are a class of compounds comprising atrazine, simazine, propazine, cyanazine and their chlorinated metabolites. The US Environmental Protection Agency (EPA) has determined that selected chloro-s-triazines--atrazine, simazine, propazine, deethylatrazine, deisopropylatrazine, and didealkylatrazine--have a common mode of toxicity related to endocrine disruption. In this paper, a dual-resin solid-phase extraction (SPE) gas chromatography-mass spectrometry (GC-MS) method is reported that provides for each of these chloro-s-triazines including the polar metabolite, didealkylatrazine. The method utilizes deuterated internal standards for quantitation and terbuthylazine as a recovery standard. The limit-of-detection was 0.01 microg/L for simazine, deethylatrazine, deisopropylatrazine and didealkylatrazine, and 0.02 microg/L for atrazine and propazine in surface water. Mean recoveries for 0.5 and 3.0 microg/L spikes for atrazine, simazine, propazine, deethylatrazine, deisopropylatrazine and didealkylatrazine were 94, 104, 103, 110, 108 and 102%, respectively, in surface water. The method was also validated by matrix spikes into fourteen different raw and treated natural surface waters. This method is useful for monitoring "total chloro-s-triazines" in both raw and treated drinking waters.

Gas Chromatography-Mass Spectrometry↗
PubMed2005

Development of an improved analytical method for the determination of carcinogenic polycyclic aromatic hydrocarbons in transformer oil.

Polynuclear aromatic hydrocarbons (PAHs) are natural constituents of transformer oils and are essential in prolonging transformer in-service lifetime. Issues concerning PAH carcinogenicity demand methods that provide qualitative and quantitative information on the PAH composition of new and in-service oils to allow informed operational decisions to be made. However, current analytical methods focus on PAH fingerprinting, as opposed to quantitative analysis and are also cumbersome, relying on the use of large (>100 ml) volumes of organic solvents, some of which are hazardous. This paper reports a method for the improved quantification of carcinogenic PAHs in transformer oils that is both simple and repeatable. The method uses commercially available solid-phase extraction columns and millilitre volumes of relatively non-hazardous solvents. Extraction efficiencies of > or =74% were obtained for the Environmental Protection Agency priority PAHs. The method has potential for automation and high-throughput analysis and thus is of interest to industries that use transformer oils.

Carcinogens↗
PubMed2005

Trace level perchlorate analysis by ion chromatography-mass spectrometry.

Perchlorate is commonly used as an oxidant in solid fuel propellant for rockets and missiles. Recently perchlorate contamination was found in many aquifers associated with Colorado River and other sites. Perchlorate was also found at elevated level in crops that use contaminated water for irrigation. Ion chromatography with conductivity detection could be used to measure perchlorate levels in drinking and wastewaters as per United States Environmental Protection Agency method 314, but at lower levels and with complexity of the matrix there could be false positive and/or false negative. This study was done to demonstrate the detection of perchlorate with lower detection limit with high ionic matrix by ion chromatography-mass spectrometry.

Chromatography, Ion Exchange↗
PubMed2006

Determination of polycyclic aromatic sulfur heterocycles in diesel particulate matter and diesel fuel by gas chromatography with atomic emission detection.

The sulfur content of diesel fuel is of environmental concern because sulfur can facilitate the formation of diesel particulate matter (DPM) and sulfur dioxide (SO2) in the exhaust can poison catalytic converters. The US Environmental Protection Agency (EPA) has established more stringent regulations to reduce the sulfur content of diesel fuels in the near future. In this study, various types of organosulfur compounds in DPM extracts and the corresponding fuels have been determined by gas chromatography with atomic emission detection. The diesel fuels used have sulfur contents of 2284 and 433 ppm, respectively, and are labeled as high-sulfur and low-sulfur diesel fuels. The compounds identified are mainly polycyclic aromatic sulfur heterocycles (PASHs). In the fuels tested, trimethylbenzothiophenes (TMBTs), dibenzothiophenes (DBTs), and 4-methyldibenzothiophene (4-MDBT) were the most abundant sulfur compounds, while larger PASH compounds were more abundant in DPM extracts. The high-sulfur diesel fuel contained a larger proportion of PASHs with one or two rings (lighter PASHs). In DPM, the concentrations of total organic sulfur and individual PASHs are higher for the high-sulfur diesel fuel, and the relative percentage of one or two-ring PASHs is higher as well. The influence of engine load on the DPM composition was also examined. With increasing load, the PASH concentration in DPM decreased for lighter PASHs, increased for heavier PASHs, and had a bell-shaped distribution for PASHs in between.

Chromatography, Gas↗
PubMed2006

Low-pressure gas chromatography-ion trap mass spectrometry for the fast determination of polycyclic aromatic hydrocarbons in air samples.

A low-pressure gas chromatography-ion trap mass spectrometry (LPGC-ITMS) method was investigated to shorten the analysis time for 18 US Environmental Protection Agency priority listed polycyclic aromatic hydrocarbons (PAHs). Their elution was optimised with a short, wide-bore column coupled to a deactivated capillary at the inlet end and with a long, conventional column to compare their analytical performance. The analytical figures of merit under optimal LPGC-ITMS conditions were determined with respect to chromatographic separation, S/N ratio, limit of detection and precision. The peak width at half height of 1.5s matched the ITMS duty cycle. Up to 16 PAHs in the molecular weight (MW) range of 128-278 Da could be separated in a very short time, i.e. less than 13 min using LPGC-ITMS, whereas with conventional GC-MS, it took approximately 40 min. However, LPGC-ITMS has a limited loss of separation power compared to that of conventional GC-MS due to the occurrence of three critical pairs for high-MW PAHs. For a practical evaluation, the LPGC-ITMS approach was applied to the determination of PAHs in gas and aerosol phase samples collected in the ambient air of Hasselt, Belgium.

Air Pollutants↗
PubMed2006

Analysis of polycyclic aromatic hydrocarbons in pine needles by gas chromatography-mass spectrometry: comparison of different extraction and clean-up procedures.

Three extraction methodologies (Soxhlet, ultrasonic and pressurized liquid extraction) and several clean-up procedures (Florisil, silica and alumina in cartridges or glass column format) were tested and compared to extract 16 US Environmental Protection Agency (EPA) polycyclic aromatic hydrocarbons (PAHs) from Pinus pinea L. needles. Quantification was done by gas chromatography with mass spectrometry, by internal standard method using five deuterated PAH surrogate standards. Among the several extraction and clean-up procedures tested, ultrasonic extraction followed by alumina cartridge clean-up was the preferred method, yielding recoveries between 72 and 100% and limits of detection between 0.22 and 0.71 ng/g dry weight. The performance of the method was tested to determine PAHs in naturally contaminated samples.

Chemical Fractionation↗
PubMed2006

Validated analytical strategy for the determination of polycyclic aromatic compounds in marine sediments by liquid chromatography coupled with diode-array detection and mass spectrometry.

The aim of this work was to optimise and validate the experimental conditions for the analysis of 20 polycyclic aromatic compounds (PACs) [19 polycyclic aromatic hydrocarbons (PAHs) and dibenzothiophene as polycyclic aromatic sulphur heterocycle (PASH)] in marine sediments by reversed-phase high-performance liquid chromatography (LC) coupled to photodiode array detection (DAD) and to mass spectrometry (MS). The LC-MS interface used was atmospheric pressure chemical ionization (APCI) in the positive ion mode. The operational parameters of the APCI interface and MS detection, such as organic modifier, fragmentation voltage, gain, vaporizer temperature, corona current, capillary voltage, drying gas (N2) and nebulizer pressure, were studied. The sediments were subjected to microwave-assisted solvent extraction (MAE) and clean-up by solid-phase extraction (SPE). The relevance of the selected PACs lies in the fact that 16 PACs are classified by the US Environmental Protection Agency as priority pollutants; 17 PACs are detected in the Prestige oil spill; and 8 PACs are included in the priority substance list of the EU water policy. Recoveries from 47% to 102% were obtained for SRM 1944 certified reference sediment. The limits of quantitation were lower than 100 ngg(-1) dry weight for most PACs, and good precision was achieved.

Atmospheric Pressure↗
PubMed2006

Investigation of a variety of cationic surfactants attached to cation-exchange silica for hydrophobicity optimization in admicellar solid-phase extraction for high-performance liquid and gas chromatography.

A series of cationic surfactants were attached to cation-exchange silica that included silica modified with sulfopropyl groups and unmodified silica to create hydrophobic solid-phase extraction sorbents. Various chain lengths and chain numbers of amine, ammonium and pyridinium-based cationic surfactants were investigated to reach sufficient sorbent hydrophobicity to capture US Environmental Protection Agency (EPA) priority polycyclic aromatic hydrocarbons (PAHs). Of the tested surfactant/silica combinations, dihexadecyldimethylammonium cations attached to unmodified silica resulted in the sorbent having the greatest hydrophobicity. This sorbent provided strong hydrophobic attraction of PAHs and also efficient elution because the PAHs were removed together with the surfactant using a very mild 5% acetic acid in methanol rinse solution. This admicellar solid-phase extraction procedure was applied for the determination of these PAHs for both high-performance liquid and gas chromatography. The detection limits of these PAHs were below the EPA's maximum contaminant level of 0.2 microg/L.

Cation Exchange Resins↗
PubMed2006

Simultaneous determination of methyl tert-butyl ether, its degradation products and other gasoline additives in soil samples by closed-system purge-and-trap gas chromatography-mass spectrometry.

A new protocol for the simultaneous determination of methyl tert-butyl ether (MTBE); its main degradation products: tert-butyl alcohol (TBA) and tert-butyl formate (TBF); other gasoline additives, oxygenate dialkyl ethers: ethyl tert-butyl ether (ETBE), tert-amyl methyl ether (TAME) and diisopropyl ether (DIPE); aromatics: benzene, toluene, ethylbenzene and xylenes (BTEX) and other compounds causing odour events such as dicyclopentadiene (DCPD) and trichloroethylene (TCE) in soils has been developed. On the basis of US Environmental Protection Agency (EPA) method 5035A, a fully automated closed-system purge-and-trap coupled to gas chromatography/mass spectrometry (P&T-GC/MS) was optimised and permitted to detect microg/kg concentrations in solid matrices avoiding losses of volatile compounds during operation processes. Parameters optimised were the sampling procedure, sample preservation and storage, purging temperature, matrix effects and quantification mode. Using 5 g of sample, detection limits were between 0.02 and 1.63 microg/kg and acceptable method precision and accuracy was obtained provided quantification was performed using adequate internal standards. Soil samples should be analysed as soon as possible after collection, stored under -15 degrees C for not longer than 7 days if degradation products have to be analysed. The non-preservative alternative (empty vial) provided good recoveries of the most analytes when freezing the samples up to 7 day holding time, however, if biologically active soil are analysed the preservation with trisodium phosphate dodecahydrate (Na(3)PO(4).12H(2)O or TSP) is strongly recommended more than sodium bisulphate (NaHSO(4)). The method was finally applied to provide threshold and background levels of several gasoline additives in a point source and in sites not influenced by gasoline spills. The proposed method provides the directions for the future application on real samples in current monitoring programs at gasoline pollution risk sites where till now little monitoring data for MTBE in soils are available.

Benzene↗
PubMed2006

Comparison of various detection limit estimates for volatile sulphur compounds by gas chromatography with pulsed flame photometric detection.

This paper addresses the variations that presently exist regarding the definition, determination, and reporting of detection limits for volatile sulphur compounds by gas chromatography with pulsed flame photometric detection (GC-PFPD). Gas standards containing hydrogen sulphide (H(2)S), carbonyl sulphide (COS), sulphur dioxide (SO(2)), methyl mercaptan (CH(3)SH), dimethyl sulphide (DMS), carbon disulphide (CS(2)), and dimethyl disulphide (DMDS) in concentrations varying from 0.36ppb (v/v) up to 1.5ppm (v/v) in nitrogen were prepared with permeation tubes and introduced in the gas chromatograph using a 0.25-ml gas sampling loop. After measuring the PFPD response versus concentration, the method detection limit (MDL), the Hubaux-Vos detection limit (x(D)), the absolute instrument sensitivity (AIS), and the sulphur detectivity (D(s)) were determined for each sulphur compound. The results show that the MDL determined by the US Environmental Protection Agency procedure consistently underestimates the minimum concentrations of volatile sulphur compounds that can be practically distinguished from the background noise with the PFPD. The Hubaux-Vos detection limits and the AIS values are several times higher than the MDL, and provide more conservative estimates of the lowest concentrations that can be reliably detected. Sulphur detectivities are well correlated with AIS values but only poorly correlated with MDL values. The AIS is recommended as a reliable and cost-effective measure of detection limit for volatile sulphur compounds by GC-PFPD, since the AIS is easier and faster to determine than the MDL and the Hubaux-Vos detection limit. In addition, this study confirmed that the PFPD response is nearly quadratic with respect to concentration for all volatile sulphur compounds.

Chromatography, Gas↗
PubMed2006

Comparison of a variety of gas chromatographic columns with different polarities for the separation of chlorinated dibenzo-p-dioxins and dibenzofurans by high-resolution mass spectrometry.

The applicability of 13 different GC columns (Agilent HP-5MS, Restek Rtx-5MS, Rtx-Dioxin2, Supelco Equity 5, SP-2331, Varian VF-5MS, CP-Sil 8 CB LowBleed/MS, J&W Scientific DB-5, DB-225, DB-XLB, DB-5MS, Phenomenex ZB-5MS, and ZB-5UMS) for US Environmental Protection Agency (EPA) methods 1613b, 8290 and European Standard Method EN 1948 for measurement of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) has been evaluated for the separation of all International Toxic Equivalent Factor (I-TEF) isomers (tetra- through octachlorinated at 2,3,7,8 positions) from closely eluting isomers using high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS). The relative performance data are compared based on mass chromatograms using a "visualization approach", absolute retention times, 2,3,7,8-substituted, total dioxins and furans concentrations, as well as TEQ comparisons. None of the columns tested were able to separate all 17 I-TEFs from other co-eluted isomers. Our data indicate that all I-TEFs isomers can be fully differentiated from closely eluting isomers using either of two sets of non-polar and polar stationary phase combinations. One set consists of DB-5 (HP-5MS, Rtx-5MS, Equity-5) and DB-225 GC columns and another set would have a combination of DB-5MS (ZB-5MS, VF-5MS, CP-Sil 8 CB LowBleed/MS) with SP-2331. However, depending on the source of PCDDs/PCDFs a laboratory could choose a single GC column that separates the 2,3,7,8-substituted congeners that contribute most significantly to the overall TEQ. These data are the most comprehensive to date, provide a valuable addition to operational criteria for the standard EPA methods 1613b, 8290, European Standard Method EN 1948 and will allow researches to compare data generated according to the different compliance analytical procedures.

Benzofurans↗
PubMed2005

A review of traffic-related air pollution exposure assessment studies in the developing world.

Exposure assessment studies in the developing world are important. Although recent years have seen an increasing number of traffic-related pollution exposure studies, exposure assessment data on this topic are still limited. Differences among measuring methods and a lack of strict quality control in carrying out exposure assessment make it difficult to generalize and compare findings between studies. In this article, exposure assessment studies carried out in the developing world on several traffic-related air pollutants are reviewed. These pollutants include particulate matter (PM), carbon monoxide (CO), nitrogen dioxide (NO(2)), volatile organic compounds (VOCs), and polycyclic aromatic hydrocarbons (PAHs). In addition, it discusses advantages and disadvantages of various monitoring methods (ambient fixed-site monitoring, microenvironment monitoring, and personal exposure assessment using portable samplers) for these pollutants in exposure assessment studies. Also included in this paper is a brief introduction of standards for these pollutants in ambient air or in occupational settings established by the United States Environmental Protection Agency (USEPA), the United States Occupational Safety and Health Administration (OSHA) and the World Health Organization (WHO). The review ends with a summary of the limitations and gaps in recent studies and suggestions for future research in the developing world.

Air Pollutants↗
PubMed2004

Hair mercury levels versus freshwater fish consumption in household members of Swedish angling societies.

Hair mercury levels were determined in 143 individuals from households of members in angling societies in an area of Sweden with many lakes that have freshwater fish with relatively high mercury levels. Thus, the individuals had a potentially high intake of methyl mercury. The mean mercury concentration of pike and perch was approximately 0.7 microg/g. One-third of the subjects consumed these freshwater fish at least once a week. As could be expected, there was a clear increase in hair Hg with reported freshwater fish consumption (P < 0.001). The median mercury level in hair was 0.9 microg Hg/g for the whole group, and for those who reported consumption of freshwater fish at least once a week it was 1.8 microg/g. The highest hair mercury level was 18.5 microg/g, in a man who consumed pike and perch several times per week. Men had higher hair Hg than women, also when stratified for fish consumption. This was verified in 32 couples, of which the man and woman consumed the same fish and reported the same consumption. The median hair mercury level in these 32 couples was 1.3 microg/g for men and 0.8 microg/g for women (P = 0.002). About half of the subjects had hair mercury exceeding 1 microg/g, corresponding to the reference dose (RfD) of 0.1 microg of mercury per kilogram body weight set by the US Environmental Protection Agency. Although the RfD applies to all populations, the most at-risk group at these levels is pregnant women. There were only 2 women (of 12) of fertile age with hair mercury above 1 microg/g. In Sweden pregnant women are advised not to eat perch and pike at all during pregnancy. Since fish is rich in many important nutrients, it is unsatisfactory that fish consumption must be restricted, and thus there is a need to reduce mercury levels in fish.

Adult↗