Showing papers in "International Journal of Environmental Analytical Chemistry in 1979"
TL;DR: A series of petroleum hydrocarbons of geochemical significance (biological markers) such as C20-C40 acyclic isoprenoids and C27-steranes and triterpanes are proposed as passive tags for the characterization of oils in the marine environment as mentioned in this paper.
Abstract: A series of petroleum hydrocarbons of geochemical significance (biological markers) such as C20-C40 acyclic isoprenoids and C27-steranes and triterpanes are proposed as passive tags for the characterization of oils in the marine environment. Mass-fragmentography of samples IS used to make evident there series of components without complex enrichment treatments. The rational choice of the characteristic ions 1s discussed and both molecular and stereoisomeric profiles are considered for identification purposes. Furthermore. computerized gas chromatography-mass spectrometry permits multiple fingerprinting from the same GC run. Hence rapid and effective comparisons between bamples and long term storagr of the results for future examination can be carried out. Differences between oils from the same geographic area and correlations of highly weathered samples are exemplified.
101 citations
TL;DR: An interface between a high pressure liquid chromatograph and a Hitachi Zeeman graphite furnace atomic absorption spectrophotometer for the element-specific detection of trace element compounds is described in this paper.
Abstract: An interface between a high pressure liquid chromatograph and a Hitachi Zeeman graphite furnace atomic absorption spectrophotometer for the element-specific detection of trace element compounds is described. This device was used for the separation of arsenobetaine bromide. arsenocholine bromide, and inorganic arsenic (arsenate/arsenite) from each other.
74 citations
TL;DR: In this article, high-performance liquid chromatography was used for the analysis of phthalate esters dL(2-ethylhexyl) and di-n-butyl phthalates (DEHP and DBP) in three main rivers in The Netherlands.
Abstract: Analysis of the phthalate esters dL(2-ethylhexyl) and di-n-butyl phthalate—DEHP and DBP, respectively—can conveniently be carried out by means of high-performance liquid chromatography in the system silica gel/n-hexane—dichloromethane (containing approx. 0.29.; of ethanol) (1:2, v/v). Detection is done by UV absorption spectrometry at 233 nm; the detection limit for both phthalates is approx. 10 ng. The procedure has been used for a survey of the sediments of three main rivers in The Netherlands. The sediments of the rivers Rhine and IJssel contain 1-70 ppm DEHP and @-15ppm DBP. For the river Meuse, slightly lower levels of 1-17 ppm DEHP and G2 ppm DBP are measured. In several sediments of a nature-reserve, DEHP and DBP contents are below the detection limit of approx. 0.5 ppm. The combined data suggest that the phthalate pollution of the river sediments is mainly due to transport of these pollutants via the river, and not via the atmosphere.
42 citations
TL;DR: In this article, eight open and eight wet-only rain samplers were placed together on an open field near Den Helder, the Netherlands, were sampled three times a week.
Abstract: Eight open and eight wet-only rain samplers. placed together on an open field near Den Helder. The Netherlands, were sampled three times a week. Greatest care in sampling and analysis procedures was taken to avoid contamination. The samples were analysed for H+, NH+ 4, Na, K, Ca, Mg, Fc, Zn, Pb, Cd, Cu, Mn, Al, V, SO2- 4, NO− 3, Cl−, Br− and F− by wet chemical techniques. AAS and instrumental neutron activation analysis. For many species the difference between the results of open and wet-only samplers was negligible. The correlation between some cations and anions was computed and indications were found for the presence of HNO3 and (NH4)2SO4 in the atmosphere. whereas little H2SO4 or NH4NO3 seems to be present. It is possible to detect whether various pollutants are of continental or marine origin.
40 citations
TL;DR: Analytical techniques based on thin-layer chromatography and high-pressure liquid chromatography were employed to separate, identify and quantitate individual metabolites from fish exposed to radiolabeled naphthalene and 2,6-dimethylnaphthalenes.
Abstract: Aquatic organisms convert aromatic hydrocarbons into a variety of conjugated and nonconjugated derivatives. Analytical techniques based on thin-layer chromatography (TLC) and high-pressure liquid chromatography (HPLC) were employed to separate, identify and quantitate individual metabolites from fish exposed to radiolabeled naphthalene and 2,6-dimethylnaphthalene. Significant differences in profiles of individual metabolites were found in relation to the type of biological sample analyzed. Liver of naphthalene-exposed salmonids contained eight polar derivatives, as shown by HPLC. Two nonconjugates (1-naphthol and 1,2-dihydro-1,2-dihydroxynaphthalene) and three conjugates (1-naphthyl glucuronic acid, 1-naphthyl sulfate and 1-naphthyl glucoside) were identified. HPLC revealed that brain of 3H-naphthalene-exposed trout contained essentially the nonconjugated derivatives, 1-naphthol and 1,2-dihydro-1,2-dihydroxynaphthalene. TLC showed that the metabolites from trout urine were 1-naphthol, 1,2-dihydro-1,2-dihydroxynapthalene, and 1-naphthyl glucuronic acid (99% of the total metabolites detected). Major components of the metabolite fractions of tissues and biological fluids were 1,2-dihydro-1,2-dihydroxy and glucuronic acid derivatives. Dihydrodiol derivatives arise from the corresponding arene oxides, some of which have been shown to be cytotoxic to certain mammalian systems.
27 citations
TL;DR: In this paper, the analysis of the phthalate esters di-(2-ethylhexyl) and di-n-butyl phthalates (DEHP and DBP) was carried out by means of high-performance liquid chromatography (HPLC) in the system silica gel/hexane-dichloromethane (1:2, v/v) containing 0.1-0.2% of ethanol, and (b) GC on 4% OV-101 on Chromosorb W (HP) at a temperature of 240
Abstract: Analysis of the phthalate esters di-(2-ethylhexyl) and di-n-butyl phthalate—DEHP and DBP. respectively—has been carried out by means of (a) high-performance liquid chromatography (HPLC) in the system silica gel/hexane-dichloromethane (1:2, v/v) containing 0.1-0.2% of ethanol, and (b) gas chromatography (GC) on 4% OV-101 on Chromosorb W (HP) at a temperature of 240°C. Detection was done by U.V. absorption spectrometry at 233 nm and flame ionization, respectively. The procedure has been used to analyse series of water samples of the Dutch rivers Rhine, IJssel and Meuse. Since the phthalate levels of the samples rapidly decrease with time, extraction invariably was performed without delay at the sampling station. The DEHP values on an average are approx. 1 ppb for all three rivers; for DBP, values of 0.3-0.5 ppb are found for the rivers Rhine and Meuse, while a somewhat high value of 2 ppb is reported for the river IJssel. The results obtained by HPLC and GC show good agreement; the former technique...
25 citations
TL;DR: In this article, the products from the chlorination of water from a southern USA reservoir were investigated using size HPLC with aqueous solvent and passivated controlled porosity silica columns, showing that the ratio of non-volatile halogen to trihalomethane halogen is at least 2:1.
Abstract: Several analytical methods have been utilized to study the products from the chlorination of water from a southern USA reservoir Low molecular weight fragments have been assayed by GC/MS following resin accumulation under acidic or basic conditions High molecular weight products before and after chlorination have been investigated using size HPLC with aqueous solvent and passivated controlled porosity silica columns The results show a slight lowering of average molecular weight after chlorination, but more importantly, a nearly uniform level of organic chlorine through the polymer Total organic halogen measurements confirm that the ratio of non-volatile halogen to trihalomethane halogen is at least 2:1 in all cases studied The oronation and photolytic oronation products of 246,2′,4′6′-hexachloro-biphenyl have been determined and a reaction scheme proposed
20 citations
TL;DR: A critical study of the solution conditions and other parameters affecting the reliability of the ammonium pyrrolidinedithiocarbamate-methyl isobutyl ketone (APDC-MIBK) extraction system for Ag, Cd, Co, Cr, Cu, Fe, Mn, Ni, and Pb was made as discussed by the authors.
Abstract: A critical study of the solution conditions and other parameters affecting the reliability of the ammonium pyrrolidinedithiocarbamate-methyl isobutyl ketone (APDC-MIBK) extraction system for Ag, Cd, Co, Cr, Cu, Fe, Mn, Ni, and Pb was made. The following parameters were investigated in detail: pH of the aqueous phase prior to extraction, amount of APDC added to the solution following pH adjustment, the length of time needed for complete extraction and the time-stability of the chelate in the organic phase. Except for Ag and Cr which were quantitatively extracted only in a very narrow pH range (1.0-2.0 and 1.8-3.0, respectively), and Cd and Pb which were stable in the extracted MIBK phase only for 2-3 hrs, the solution conditions for quantitative extraction were not critical for the other metals. Simultaneous extraction of all the metals except Cd and Pb was also investigated, Good recoveries (100±10%) were obtained for a number of spiked raw, treated and distributed drinking water samples covering...
19 citations
TL;DR: The use of Amberlite XAD-2 macroreticular resin to extract PAHs from drinking water is shown to be effective, although the recovery of individual PAHS from artificially loaded XAD -2 resin varied from 57 to 100%.
Abstract: Samples of Ottawa drinking water, collected in January and February 1978 were analysed by Gas Chromatography/Mass Spectrometry (GC/MS) for fifty polycyclic aromatic hydrocarbons (PAH) and five oxygenated polycyclic aromatic hydrocarbons (O-PAH), following extraction of the organic species using Amberlite XAD-2 macroreticular resin. In the January sample, thirty PAHs, ranging in concentration from 0.05 to 14 ng/L with a mean value of 3.8 ng/L and a total weight of 114 ng/L and four O-PAHs, ranging in concentration from 0.10 to 1.8 ng/L with a mean value of 0.91 ng/L and a total weight of 3.7 ng/L, were detected. In the February sample, thirty-six PAHs, ranging in concentration from 0.05 to 8.1 ng/L with a mean value of 1.4 ng/L and a total weight of 50.4 ng/L and five O-PAHs, ranging in concentration from 0.20 to 2.4 ng/L with a mean value of 1.0 ng/L and a total weight of 5.2 ng/L, were detected. Twenty-eight PAHs and four O-pahs were common to the two samples. The use of Amberlite XAD-2 macroreticular resin to extract PAHs from drinking water is shown to be effective, although the recovery of individual PAHs from artificially loaded XAD-2 resin varied from 57 to 100%.
18 citations
TL;DR: The analytical performance of a chelation/extraction procedure for concentrating trace metals from natural water samples has been investigated in this article, where the chelates were found to be stable in the organic phase for at least ten days.
Abstract: The analytical performance of a chelation/extraction procedure for concentrating trace metals from natural water samples has been investigated. The metals (Cd, Co, Cu, Ni, Pb, Zn), chelated with ammonium pyrrolidine dithiocarbamate, were concentrated by solvent extraction in methyl isobutyl ketone at a sample pH of 4; the organic phase was analyzed by flame atomic absorption spectrophotometry. Sensitivity of the method tested was adequate for surface waters and precision proved to be good. The chelates were found to be stable in the organic phase for at least ten days. In the two rivers studied, the recovery of spiked metals proved to be independent of sampling stations but slightly dependent on sampling dates; this latter dependence suggests the existence of weak matrix effects. No significant interferences from linear alkyl sulphonate (1 mg/l) or from humic acid (3mgC/l) were detected.
17 citations
TL;DR: In this paper, the suitability of HPLC with UV or post-column reaction detection for the analysis of organomercurials was investigated systematically, and it was shown that HPLC is best carried out on a reversed phase system with a C-8 bonded phase material as the stationary phase and acetonitrile-aqueous sodium bromide mixtures as the mobile phase.
Abstract: The suitability of HPLC (normal and reversed phase adsorption) with UV or post-column reaction detection for the analysis of organomercurials was investigated systematically. The separation of organomercurials is best carried out on a reversed phase system with a C-8 bonded phase material as the stationary phase and acetonitrile-aqueous sodium bromide mixtures as the mobile phase. The precision and detection limit of the method and the efficiency of the extraction procedure were established. For the alkylmercury compounds the lowest limit of detection (80ppb) was obtained with the dithizone reaction detection and for the phenylmercury compounds with UV detection (60ppb). A chromatogram of a spiked fish (2ppmHg) and a river water sample (50ppbHg) is shown.
TL;DR: In this paper, the results of the analysis for SO2 4, CI−, NO+,3 NH+ 4 Na+, Pb2+ and pH of the daily samples agreed my well.
Abstract: Twenty-one raincollectors were placed together in a flat area. From 11 collectors samples were taken on a daily basis and from 10 collectors on a monthly basis. The results of the analysis for SO2 4, CI−, NO+,3 NH+ 4 Na+, Pb2+ and pH of the daily samples agreed my well. The results of the monthly samples, analysed for CI−, Na+, Ca2+, Fe3+, F−, Pb2+, Zn2+, Cd2+, and Cu2+, were less satisfactory. Differences up to 507; are found between the results of daily and monthly samples.
TL;DR: In this article, the preconcentration of 10 cations, Ag, As, Co, Cr, Cu, Fe, Hg, Mn, Pb and Zn was studied.
Abstract: In recent years, considerable progress has been made in the field of metal ion preconcentration from environmental water samples. The methods most widely used include ion-exchange, precipitation (and coprecipitation), adsorption and chelation with immobilized and non-immobilized reagents. As the mechanisms underlying the various methods are different. it is expected that these methods perform differently with respect to the enrichment factor. sensitivity and recovery of trace metal ions. In this investigation, the preconcentration of 10 cations. Ag, As, Co, Cr, Cu, Fe, Hg, Mn, Pb and Zn was studied. The methods of preconcentration include (1) cation-exchange resin-loaded filter paper. (2) precipitation with sodium diethyldithiocarbamate, (3) precipitation with ammoniumpyrrolidinedithiocarbamate. (4) chelation with oxine with subsequent adsorption on activated carbon and (5) chelation with diethyldithiocarbamate immobilized on controlled pore glass. Among the factors compared are the detection lim...
TL;DR: In this paper, a method was developed and used to determine B[a]P and perylene quantitatively, and to identify several other PAH in a range of sediments from south-east Australia.
Abstract: Polycyclic aromatic hydrocaroons (PAH) are present in bottom sediments of rivers. estuaries and coastal waters. Few analyses of sediments for PAH have been reported previously, and they have generally determined benzo[a]pyrene (B[a]P) only. The method described here was developed and used to determine B[a]P and perylene quantitatively, and to identify several other PAH in a range of sediments from south-east Australia. A sequence of liquid-liquid extraction using cyclohexane and dimethylsulphoxide, and two stages of thin-layer chrornatography, was used for purification and separation of individual PAH which were identified and determined by spectrofluorimetry. The minimum concentrations detectable using this method were 2.5μg/kg for B[a]P and 1.5μg/kg for perylene starting with a 30g sample of dried sediment. At the 500 μg/kg level both PAHs were determined with a coefficient of variation of 5-7%.
TL;DR: More than 20 trace and minor elements were determined in water samples and in the suspended load of the river Aare (Switzerland) using a simple sample preparation technique and subsequent instrumental neutron activation analysis as mentioned in this paper.
Abstract: More than 20 trace and minor elements were determined in water samples and in the suspended load of the river Aare (Switzerland) using a simple sample preparation technique and subsequent instrumental neutron activation analysis. The water samples were irradiated without preconcentration. The interfering activity of 24Na was eliminated with hydrated antimony pentoxide. The trace elements were co-precipitated as sulfides and hydroxides and were analyzed on Ge(Li)gamma-ray spectrometers. Particulate matter was filtered off in the field, irradiated and assayed by γ-ray spectroscopy. Main results: (a) the concentrations of all the elements investigated are much lower than WHO-limits for drinking water; (b) human activities are responsible for an increase of some elements along the river: (c) concentrations of dissolved trace elements are anticorrelated to the amount of water; (d) concentrations of trace elements in particulates (μg/l) are correlated to the amount of water: (e) significant correlation...
TL;DR: In this article, the effects of transportation and storage of air particulate filters on sample composition were investigated by GC and GC/MS analysis of 42-Hi-Vol filter samples taken in a large metropolitan city.
Abstract: Effects of transportation and storage of air particulate filters on sample composition were investigated by GC and GC/MS analysis of 42-Hi-Vol filter samples taken in a large metropolitan city. One-half of the filters were transported and stored using paper envelopes while the others were individually wrapped in aluminum foil before transportation. One half of each filter received was extracted and analyzed immediately while the other half was stored in a refrigerator for later analysis. Significant losses of organic material from stored filters was observed for filters stored in paper envelopes and filters sealed in aluminum foil, although losses were less for filters wrapped in metal foil. There is some indication that metal foil may protect filters from external contamination after sampling.
TL;DR: The safe development of landfill sites is daily increasing in importance as discussed by the authors, in which the analysis of soil gases especially for methane is vital, and techniques have been developed for the sampling of such gases and their subsequent analysis at the v.p.m. level by gas chromatography.
Abstract: The safe development of landfill sites is daily increasing in importance. In this context the analysis of soil gases. especially for methane. is vital. Techniques have been developed for the sampling of such gases. and their subsequent analysis at the v.p.m. level by gas chromatography. Factors affecting the gas concentrations are considered.
TL;DR: A cheap and simple, but very sensitive and specific detection tube could be bedeveloped for the hydrolysis of certain esters from horse serum by making use of this biochemical reaction.
Abstract: The enzyme butyrylcholinesterase from horse serum catalyses the hydrolysis of certain esters. The orange-red 2,6-dichloroindophenyl acetate will be converted by the enzyme into a deep blue alcohol. The colour transformation does not occur when the enzyme is inactivated. By making use of this biochemical reaction a cheap and simple, but very sensitive and specific detection tube could be developed. The tube comprises a breakable ampoule with an aqueous buffer solution, a freeze-dried preparation of the chromogenic ester with a filler promoting its dissolution, a freeze-dried preparation of butyrylcholinesterase with a filler promoting its stability, and an indication layer. DDVP can be detected at concentrations as low as 0.4mg/m3, when the sampled airvolume is 21.
TL;DR: In this article, the content of chemically persistent (it. sulphuric acid resistant) chlorinated hydrocarbons in the fatty surface film on water is investigated using a gas chromatograph with an electron capture detector (GC/ECD).
Abstract: The content of chemically persistent (it. sulphuric acid resistant) chlorinated hydrocarbons in the fatty surface film on water is investigated. The sampling method is based on adsorption of the surface film to tenon sheets, and analysis was performed using a gas chromatograph with an electron capture detector (GC/ECD). The results are obtained as gas chromatographic profiles. When comparing chromatographic profiles of surface film and corresponding water samples a significant difference between the two is observed. The results indicate that the atmosphere 1s the main source for chlorinated organic pollutants in the surface, while enrichment of these compounds from the water seems to be of minor importance. Only small differences are observed when comparing pollution profiles of surface samples taken at different times at the same locality. The most predominant chlorinated organic pollutants in all the surface film samples are found to be PCB. It is estimated that the concentration of PCB in the ...
TL;DR: A gas chromatographic technique has been developed and applied to the qualitative and quantitative analysis of fatty acids in the interstitial gases of landfill sites as mentioned in this paper, which may be responsible for the unpleasant smells frequently associated with landfill gases.
Abstract: A gas chromatographic technique has been developed and applied to the qualitative and quantitative analysis of fatty acids in the interstitial gases of landfill sites. Acetic, propionic. and butyric acids were those shown to be present in the highest concentrations. The fatty acid concentrations were higher at a site where landfill had been completed two years ago than at a site where operations had finished twenty-five years ago. The concentrations of fatty acids measured were well above the odour thresholds. These compounds may be responsible for the unpleasant smells frequently associated with landfill gases.
TL;DR: In this paper, the authors used gas chromatography and flame ionization or electron capture detection techniques to trace low molecular weight hydrocarbons, chlorinated and aromatic compounds in ambient air.
Abstract: Low molecular weight hydrocarbons, chlorinated hydrocarbons and aromatics are three groups of volatile organic chemicals that are widely used in industry and constitute a potential danger for the environment. Selective tracing of these pollutants in ambient air was performed with the aid of gas chromatography and flame ionization or electron capture detection, whichever yielded highest sensitivity. Methods of analysis, calibration procedures and sampling techniques are discussed, covering automatic operation in the field as well as discontinuous control by analyses performed in the laboratory. The efficiency of the overall procedure is illustrated by the results obtained during two pollution measuring campaigns, one performed in the neighbourhood of a vinyl chloride plant and the other in an area with an intensive paint industry.
TL;DR: In this article, the possibility of using X-ray techniques for the study of pollution of a marine ecosystem by heavy metals has been investigated, and preliminary results obtained on the concentrations of Cr, Cu, Fe, Mn, Ni, Pb and Zn of various samples of marine organisms, sediments and sea water which have been collected in the Mediterranean sea together with atmospheric particulates on the coast near La Spezia.
Abstract: The possibility of using X-ray techniques for the study of pollution of a marine ecosystem by heavy metals has been investigated. In this preliminary study data are reported, obtained on the concentrations of Cr, Cu, Fe, Mn, Ni, Pb and Zn of various samples of marine organisms, sediments and sea water which have been collected in the Mediterranean sea together with atmospheric particulates on the coast near La Spezia. Improvements in the analytical procedure are proposed.
TL;DR: Oxygen-isotope analyses were made on samples of aerosol sulfates, SO2, water vapor, precipitation water, and precipitation sulfates collected over a two-year period near Chicago, Illinois, U.S.A as mentioned in this paper.
Abstract: Oxygen-isotope analyses were made on samples of aerosol sulfates, SO2, water vapor, precipitation water, and precipitation sulfates collected over a two-year period near Chicago, Illinois, U.S.A. The purpose of this isotopic study was to help to elucidate the mechanisms of sulfate formation in the atmosphere. Oxygen-18 enrichments in precipitation sulfates varied seasonally and in phase with the corresponding enrichments in precipitation water. The ratio of the amplitudes of the enrichment-vs.-time curves indicated isotopic equilibration between SO, and atmospheric water prior to oxidation. Oxygen-18 enrichments in aerosol sulfates appeared to vary randomly with season, but averaged about the same as precipitation sulfates. If aerosol sulfates and precipitation sulfates were formed by the same hydrolysis-oxidation mechanism in clouds, relatively long residence times and transport distances of sulfate aerosols may have provided sufficient mixing to obscure seasonal effects such as were observed in...
TL;DR: In this article, a method for the determination of thallium in natural waters of low and high mineral salt contents is described, in which a sample is made 0.15 M in hydrobromic acid, filtered and after addition of bromine water it is passed through a column of the strongly basic anion exchange resin Dowex 1 on which thalli-bromide complex is adsorbed as the anionic thalli(III)-bromides complex, eluted with an aqueous solution of sulphur dioxide and, after evaporation of
Abstract: A method is described for the determination of thallium in natural waters of low and high mineral salt contents. The sample is made 0.15 M in hydrobromic acid, filtered and after addition of bromine water it is passed through a column of the strongly basic anion exchange resin Dowex 1 on which thallium is adsorbed as the anionic thallium(III)-bromide complex. The thallium is eluted with an aqueous solution of sulphur dioxide and, after evaporation of the eluate, this element is determined by a.a.s. with an air-acetylene flame. The method was used successfully for the determination of thallium in waters suitable for drinking purposes. hydrothermal waters, sea-water and waters from oil-wells.
TL;DR: In this article, a quantitative preconcentration technique for uranium as the uranyl ion is described, which utilizes a silica-cellulose filter material (Whatman SG-81, 20%, w/w silica gel) which has been modified by silylation with Nβ-ethyl-γ-aminopropyl trimethoxysilane (Dow-Corning Z-6020).
Abstract: A quantitative preconcentration technique for uranium as the uranyl ion is described. The method utilizes a silica-cellulose filter material (Whatman SG-81, 20%, w/w silica gel) which has been modified by silylation with N-β-ethyl-γ-aminopropyl trimethoxysilane (Dow-Corning Z-6020). The uranyl solution is extracted after adding ammonium carbonate to form the tris-carbonato uranyl-complex (UO2(CO3)4- 3). This complex forms a strong ion-pair with the protonated diamine group bonded to the silica portion of the filter. The extraction is effective in the pH range 6-8 and recovery was observed to lie in the range of 70-95% as the concentration was varied from 10ppm to 0.5 ppm. The low recovery at high concentration is attributed to loading the functional sites. The uranium content of synthetic samples and extractive mining process samples has been determined using x-ray fluorescence measurements on the filter following extraction. The current procedure shows a 3.5 relative standard deviation and a low...
TL;DR: In this paper, an analytical method has been used to identify some odorous compounds in the air of the water treatment plant Werdholzli, Zurich: sampling of contaminated air with the help of activated carbon, desorption by the solvents carbon disulphide and methylene chloride, separation of the carbon disulfide extract into a polar and a nonpolar fraction by adsorption column chromatography on silica.
Abstract: The following analytical method has been used to identify some odorous compounds in the air of the water treatment plant Werdholzli, Zurich: sampling of contaminated air with the help of activated carbon, desorption by the solvents carbon disulphide and methylene chloride, separation of the carbon disulfide extract into a polar and a nonpolar fraction by adsorption column chromatography on silica. Hereafter gaschromatographic analysis of the polar fraction on glass capillary column (Ucon HB 5100); detection and identification were achieved by flame ionisation, thermoionic nitrogen selective detector and computerized mass spectrometry (Finnigan 3200 F, data system 6110). The results show the presence of sulfur compounds: thiophenes, thiazoles; nitrogen compounds: pyrazines; oxygen compounds: phenols, alcohols and some unsatured hydrocarbons. The malodorous compounds were sulfur and nitrogen compounds in the range of 0.01-0.1 ppm.
TL;DR: In this paper, the use of combined surface analytical techniques such as X-ray Photoelectron Spectroscopy (XPS) or ESCA to probe the surfaces of diesel particulates is presented.
Abstract: Preliminary studies on the use of combined surface analytical techniques such as X-ray Photoelectron Spectroscopy (XPS or ESCA). Auger Electron Spectroscopy (AES), Secondary Ion Mass Spectrometry (SIMS) and Ion Scattering Spectrometry (ISS) to probe the surfaces of diesel particulates are presented. Studies of two different particulate systems are reported. Results of the first study show common chemical forms associated with the surface of particulate emission. Oxygen, sulfur and nitrogen in various chemical states are seen on the surface of a carbonaceous-graphitic (pyrolytic) center. These elements are postulated as organically bound surface segregated species. Observation of particles extracted for routine adsorbed organic analysis by gas chromatography show that nitrogen and sulfur compounds are left behind, along with residual organics. Trace metals were not seen on any sample. The second study involves samples collected under different running speed conditions of a diesel engine. Typical a...
TL;DR: In this paper, the problem of determining the concentration changes of reactive hydrocarbon immissions as a function of time was solved by means of an automatic gas chromatograph which, without enrichment, could record ethylene and acetylene in ppb concentrations.
Abstract: The problem of determining the concentration changes of reactive hydrocarbon immissions as a function of time was solved by means of an automatic gas chromatograph which, without enrichment, could record ethylene and acetylene in ppb concentrations. At the same time various other pollutants were covered, so that by a mutual allocation of the individual components it was possible to identify certain emitter groups. The results clearly show that ethylene and acetylene primarily originate from the combustion processes of the automobiles, while the handling and storage of petroleum products and their processing do not exert any influence on the immission of the two components. By way of time series measurements during a summer week in 1976 with very intensive solar radiation it was possible to show indirect secondary photochemical reactions.
TL;DR: A special type of cell has been used which gives a better sensitivity compared with the types of cells described in the literature and the method of FAAS analysis has been improved.
Abstract: The determination of mercury in blood by flameless atomic absorption spectrometry (FAAS) has been described. Prior to its analysis. the sample was decomposed by combustion and separated on a copper powder micro-column. A special type of cell has been used which gives a better sensitivity compared with the types of cells described in the literature and the method of FAAS analysis has been improved. The sensitivity of 0.1 ng for 1% absorbance was observed and the standard deviation for six determinations at this level was found to be ±0.05 ng, for 95% probability.
TL;DR: In this article, the Glassy Carbon Electrode was used for Mercury determination in synthetic solutions as well as in river water by stripping Voltammetry and best results were obtained with a supporting electrolyte of the chemical composition 0.1m KSCN, 0.025 n HCl and 20ng/mlCu2+.
Abstract: The Glassy Carbon Electrode was used for Mercury determination in “synthetic solutions” as well as in river water by stripping Voltammetry. Best results were obtained with a supporting electrolyte of the chemical composition 0.1m KSCN, 0.025 n HCl and 20ng/mlCu2+. The optimal pH was found to be 2.8 and the optimal deposition potential-1.0 volt. It is possible to determine at to 1.5ppb Hg2+ in river watersamples. Es wurde die Glas Carbon Elektrode benutzt, urn Quecksilber sowohl in “synthetischen Losungen” als auch in Fluswasser invers-voltammetrisch zu bestimmen. Fur die Bestimmung hat sich ein Grundelektrolyt der Zusammensetzung 0.1m KSCN, 0.025 n HCl und 20ng/ml Cu2+ gut bewahrt. Als optimaler pH-Wert fur die Bestimmung wurde pH[dbnd]2.8 und als optimale Elektrolysespannung-1.0 Volt ermittelt. Durch das Verfahren konnen bis zu 1.5 ppb Hg in naturlichen Wasserproben erfasset werden.