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Showing papers in "Fresenius Journal of Analytical Chemistry in 1988"


Journal ArticleDOI
TL;DR: A modified method in which mercaptoethanol was replaced by N,N-dimethyl-2-mercaptoethylammonium chloride results in long-term stability of the extinction values („plateauing“ > 1 h).
Abstract: In the analysis of biological matrices, the application of o-phthaldialdehyde in the presence of a thiol component (OPA-method) for the quantitative determination of free α- and e-amino groups in amino acids, peptides and proteins as well as their hydrolytic or proteolytic products, respectively, is well known The most frequently used thiol compound is mercaptoethanol The use of this substance has the disadvantage that the initially generated isoindole often undergoes intramolecular rearrangement which often leads to a decrease in extinction at the monitoring wavelength of 340 nm The present paper describes a modified method in which mercaptoethanol was replaced by N,N-dimethyl-2-mercaptoethylammonium chloride The use of the new thiol component in the OPA reaction results in long-term stability of the extinction values („plateauing“ > 1 h) The modified method is further characterized by high accuracy and precision

127 citations


Journal ArticleDOI
TL;DR: In this paper, an ICP-AES method for the determination of 12 rare earth elements and Y is described, following a Na2O2-sinter dissolution of silicate materials the REE and Y were separated and concentrated using ion-exchange chromatography.
Abstract: An ICP-AES method for the determination of 12 rare earth elements and Y is described. Following a Na2O2-sinter dissolution of silicate materials the REE and Y were separated and concentrated using ion-exchange chromatography. The dissolution and separation procedures are described in detail. Numerous tests show good recovery of the REE. Spectral interferences were quantified and discussed. The precision is better than 5% (r.s.d.) for all measured REE, except Pr. The accuracy was tested by analyzing more than 30 international reference samples, the results are in good agreement with published data. In this paper we present our latest data from 6 new reference samples.

86 citations


Journal ArticleDOI
TL;DR: In this paper, the principles of waveguide spectroscopy are briefly outlined, and representative examples of fibre-optic sensors for temper-ature, oxygen, pH, carbon dioxide and electrolytes are given.
Abstract: . Optical fibres can be used for remote sensing ofchemical and physical parameters. The usual approach is to provide the fibre end with a suitable indicator chemistry or a material that responds to the parameter of interest. In con—tact with the sample, the intensity of reflected, scattered,or re—emitted light is the analytical signal. Aside from se—veral advantages of optical sensors over electrochemical ones(for instance, lack of reference cells and immunity towardselectromagnetic interferences), the use of fibres can be ad- vantageous when the samples are inaccessible, for instance, incase of in—vivo experiments. The principles of waveguide spectroscopy are briefly outlined,and representative examples of fibre—optic sensors for temper-ature, oxygen, pH, carbon dioxide and electrolytes are given.Apart from these parameters, which also may be sensed by othertechniques, optical sensors have been developed that are basedon quite new principles and which can make them useful for

68 citations


Journal ArticleDOI
TL;DR: In this paper, the solution to be investigated is nebulized by a pressure of 50 to 400 bar, and the liquid sample (5 Μl to 2 ml) to be analyzed is fed into a sample loop, as is common procedure in HPLC techniques.
Abstract: The solution to be investigated is nebulized by a pressure of 50 to 400 bar. The liquid sample (5 Μl to 2 ml) to be analyzed is fed into a sample loop — as is common procedure in HPLC techniques. But instead of being pressed through HPLC columns, the liquid is now pressed through a special nozzle with an opening of a few micrometers. An aerosol results which is then submitted to a spectroscopical source (flame-AAS; ICP/OES). The aerosol yield is more than 50%; even a saturated solution of cooking salt can be nebulized. The sensitivity of flame-AAS increases by about one order of magnitude (signal area). In addition, an effective on-line coupling of HPLC and atomic spectrometric determination methods is possible.

67 citations


Journal ArticleDOI
TL;DR: In this paper, a number of standard reference materials (SRM's) have been issued by the National Bureau of Standards (NBS) to assist in validating measurements for the determination of polycyclic aromatic hydrocarbons (PAH) and other polycyclically aromatic compounds (PAC).
Abstract: Since 1980 a number of Standard Reference Materials (SRM's) have been issued by the National Bureau of Standards (NBS) to assist in validating measurements for the determination of polycyclic aromatic hydrocarbons (PAH) and other polycyclic aromatic compounds (PAC). These SRM's are certified for selected PAC and range in analytical difficulty from calibration solutions to complex natural matrix materials, such as air and diesel particulate matter, shale oil, and crude oil. In the past year three new SRM's have been introduced: (1) SRM 1647a “Priority Pollutant PAH in Acetonitrile”, (2) SRM 1491 “Aromatic Hydrocarbons in Hexane/Toluene”, and SRM 1597 “Complex Mixture of PAH from Coal Tar”. The SRM's available from NBS for use in the determination of PAC are described and the concentrations of PAC determined in the natural matrix SRM's are summarized and compared. The primary analytical techniques used for the measurement of PAC in these SRM's were gas chromatography, liquid chromatography, and gas chromatography/mass spectrometry.

66 citations


Journal ArticleDOI
TL;DR: Isotope dilution-spark source mass spectrometer (ID-SSMS) has been applied for the simultaneous quantitative determination of about 35 trace elements in rock samples as mentioned in this paper.
Abstract: Isotope dilution-spark source mass spectrometry (ID-SSMS) has been applied for the simultaneous quantitative determination of about 35 trace elements in rock samples. A precision and an accuracy of better than 5% is obtained for most elements. Concentrations down to 0.01–0.1 ppm can be precisely determined for many trace elements.

62 citations


Journal ArticleDOI
TL;DR: In this article, the authors present a systematic, collaborative learning program undertaken by a group of experienced analytical laboratories within the European Economic Community (EEC) to improve the state-of-the-art in the determination of individual chlorobiphenyl congeners in different matrices in preparation for the certification exercises to produce two fish oils as certified reference materials (CRMs).
Abstract: This paper gives an account of the systematic, collaborative learning programme undertaken by a group of experienced analytical laboratories within the European Economic Community (EEC) to improve the state-of-the art in the determination of individual chlorobiphenyl congeners in different matrices in preparation for the certification exercises to produce two fish oils as certified reference materials (CRMs). The choice of individual CB congeners, the critical GC parameters necessary to optimise the chromatographic separation and quantification of the congener is given. An assessment is made of the methods of extraction, separation and clean-up of samples prior to gas chromatographic analysis.

60 citations


Journal ArticleDOI
TL;DR: It is shown that many standard outlier tests are not able to detect gross outliers (masking effect) and an alternative method of evaluation using tests of estimates based on robust statistics is proposed.
Abstract: The paper criticizes the use of standard outlier tests when evaluating interlaboratory data. It is shown that many such tests are not able to detect gross outliers (masking effect). An alternative method of evaluation using tests of estimates based on robust statistics is proposed.

57 citations


Journal ArticleDOI
TL;DR: Water solubility (Sw) and log Kow values have been determined for 154 possible polychlorobiphenyls using the retention indices obtained by RP-HPLC and structurally selected PCB congeners with known log kow values for the regression lines.
Abstract: Water solubility (Sw) and log Kow values have been determined for 154 possible polychlorobiphenyls using the retention indices obtained by RP-HPLC and structurally selected PCB congeners with known log Kow values for the regression lines The water solubility data are melting point corrected

57 citations


Journal ArticleDOI
TL;DR: In this paper, the analysis of the organic compounds adsorbed on diesel particulate is reviewed with special emphasis on the determination of polycyclic aromatic hydrocarbons (PAH), nitro PAH and oxy PAH.
Abstract: Methods developed for the analysis of the organic compounds adsorbed on diesel particulate are reviewed with special emphasis on the determination of polycyclic aromatic hydrocarbons (PAH), nitro PAH and oxy PAH.

54 citations


Journal ArticleDOI
TL;DR: In this article, a method for stable isotope ratio measurements of carbon, nitrogen and sulfur dioxide was developed, consisting in coupling an elemental analyzer with an isotope mass spectrometer.
Abstract: Stable isotope ratio measurements of carbon, nitrogen and sulfur are of growing interest as analytical tool in many fields of research, but applications were somewhat hindered in the past by the fact that cumbersome sample preparation was necessary. A method has therefore been developed, consisting in essential of coupling an elemental analyzer with an isotope mass spectrometer, enabling fast and reliable conversion of C-, N- and S-compounds in any solid or liquid sample into the measuring gases carbon dioxide, nitrogen and sulfur dioxide for on-line isotopic analysis. The experimental set-up and the main characteristics are described in short and examples of application in environmental research, food analysis and clinical diagnosis are given.

Journal ArticleDOI
TL;DR: In this paper, the record of the interaction of cosmic ray particles with meteoroids in space is preserved in these objects in radioactive and stable nuclides and radiochemical separations with high decontamination factors of interfering isotopes have been developed.
Abstract: The record of the interaction of cosmic ray particles with meteoroids in space is preserved in these objects in radioactive and stable nuclides. In order to determine the low concentrations of long-lived radionuclides such as10Be (T1/2=1.6×106a),26Al (T1/2=7.2×105a),36Cl (T1/2=3.0×105a),41Ca (T1/2=1.0×105a),53Mn (T1/2=3.8×106a) and59Ni (T1/2=7.5×104a) in extraterrestrial material by means of accelerator-mass-spectrometry and neutron activation techniques, radiochemical separations with high decontamination factors of interfering isotopes have been developed. Detection limits are achieved down to 1×10−14 for isotopic ratio measurements. For absolute analytical techniques they could be lowered to 10−14g/g. The separation methods applied include ion exchange, solvent extraction as well as classical precipitation methods. The successful application of the procedure to problems in meteorite research is given by example.

Journal ArticleDOI
TL;DR: In this paper, the authors proposed a direct coupling of supercritical fluid extractions with gas chromatography (SFE-GC) for the extraction, concentration, and gas chromatographic analysis of organic analytes from solid samples to be performed in less than 1 h.
Abstract: Direct coupling of supercritical fluid extractions with gas chromatography (SFE-GC) allows the extraction, concentration, and gas chromatographic analysis of organic analytes from solid samples to be performed in less than 1 h. Coupling of the supercritical fluid extraction step with a capillary gas chromatographic column is achieved using a standard on-column injector and requires no modification of the gas chromatograph. Maximum sensitivity is achieved and analyte degradation or loss is minimized since the extracted species are quantitatively transferred into the fusedsilica capillary gas chromatographic column where they are cryogenically focused prior to normal gas chromatographic analysis using flame ionization (SFE-GC/FID) or mass spectral (SFE-GC/MS) detection. SFE-GC analysis yields good chromatographic peak shapes that compare favorably with those obtained using standard on-column injection techniques. Class-selective extractions can be achieved by performing multiple SFE-GC analyses with different extraction pressures. The ability of coupled SFE-GC to yield rapid extraction and analysis of organic analytes is demonstrated for a variety of samples including polycyclic aromatic hydrocarbons (PAHs) from treated wood, urban dust, and river sediment, phenolic species from wood smoke particulates, nicotine from tobacco, biological markers from coal, and flavor components from food products.


Journal ArticleDOI
TL;DR: Sodium tetrahydroborate(III) is equivalent to or better than tin(II) chloride as a reducing agent for mercury in cold vapor atomic absorption spectrometry using collection on gold as mentioned in this paper.
Abstract: Sodium tetrahydroborate(III) is equivalent to or better than tin(II) chloride as a reducing agent for mercury in cold vapor atomic absorption spectrometry using collection on gold. Concentrations of copper, silver, nickel, iodide, antimony, arsenic, bismuth and selenium typically found in water or waste water do not interfere. Prerequirements for satisfactory performance are that the gold is at a temperature below 100‡C during collection of mercury and that the gas from the reaction flask is washed with sodium hydroxide and dried with magnesium perchlorate. All determinations were carried out in 5 mol l−1 hydrochloric acid and in the presence of 200 mg l−1 iron(III). Detection limits (3σ) of 0.15 ng absolute, and of 15 ng l−1 or 3 ng l−1, using 10 ml or 50 ml solution, respectively, are obtained. The analytical curve is linear to 40 ng, and the relative standard deviation in the optimum working range is better than 2%.


Journal ArticleDOI
TL;DR: A flow-system utilizing a miniature column packed with silica-immobilized 8-hydroxyquinoline (I-8-HOQ) was used for the preconcentration of Cd, Pb, Zn, Cu, Fe, Mn, Ni, and Co from seawater prior to their determination by graphite furnace atomic absorption spectrometry (GFAAS).
Abstract: A flow-system utilizing a miniature column packed with silica-immobilized 8-hydroxyquinoline (I-8-HOQ) was used for the preconcentration of Cd, Pb, Zn, Cu, Fe, Mn, Ni, and Co from seawater prior to their determination by graphite furnace atomic absorption spectrometry (GFAAS). Enrichment factors sufficient to permit the analysis of an open ocean seawater reference material using 50 ml sample volumes (100 ml for Co determinations) were obtained. Recoveries of the above elements from seawater averaged 93% (range 87–97%) with absolute blanks ranging between 0.04 ng (Ni) and 4.0 ng (Fe). Estimated detection limits for these elements vary from 0.2 ng l−1 (Co) to 40 ng l−1 (Fe) based on a 50 ml sample volume (100 ml for Co).

Journal ArticleDOI
TL;DR: The mechanism of the sorption of U on TiO2 · x H2O is investigated in absence and in presence of carbonate as function of pH in this paper, where the state of the surface of TiO 2 x H 2O is taken into account.
Abstract: The mechanism of the sorption of U on TiO2 · x H2O is investigated in absence and in presence of carbonate as function of pH. Speciation of U in solution and the state of the surface of TiO2 · x H2O are taken into account. In the experiments the mole fractions of the U species in presence of carbonate are the same as in seawater. Below pH 5 the sorption of U can be described in absence and in presence of carbonate by ion exchange of UO22+or alternatively by sorption of UO2OH+, because hydrolysis and sorption are occurring simultaneously. Above pH 5 in absence of carbonate, first pH-independent sorption of (UO2)3(OH)7−and then (above the isoelectric point of TiO2 · x H2O) pH-dependent sorption of (UO2)3(OH)7−are observed. In the same pH range, but in presence of carbonate, two species of U are dominating in solution, first UO2CO3OH− and then UO2(CO3)34−· UO2CO3OH− is not sorbed in measurable amounts which causes a drastic decrease of the sorption ratio. UO2(CO3)34−, which begins to dominate above pH 6 (depending on the carbonate concentration), is sorbed either by formation of ≥ TiOUO2 bonds or (at carbonate concentrations >10−2 mol/l) via carbonate bridges.

Journal ArticleDOI
TL;DR: The TXRF-spectra, like fingerprints, facilitate the easy characterization of samples and turn out to be very suitable for screening and monitoring tasks.
Abstract: Different biomaterials were prepared as thin sections (up to 20 Μm thick, 8 mm in diameter) by means of a freezing microtome on a quartz-glass carrier and analyzed directly by total-reflection X-ray fluorescence (TXRF). They were originally available either as compact samples, as powder material or as solutions. About 20 elements with atomic numbers between 15 and 40 (P and Zr) and between 57 and 92 (La and U) were determined simultaneously with detection limits of some Μg/g. — The method was applied to the analysis of plant and animal foodstuff (nuts, mushrooms, shrimps) and of different organic tissue (human lung). The TXRF-spectra, like fingerprints, facilitate the easy characterization of samples and turn out to be very suitable for screening and monitoring tasks.

Journal ArticleDOI
TL;DR: In this paper, a review of studies made using biological reference materials for animal and human tissues is presented, and the need to have inter-laboratory studies and certified reference materials in the field of biological monitoring of toxic metals is also discussed.
Abstract: Biological monitoring of toxic metal pollution in the environment requires quality control analysis with use of standard reference materials. A variety of biological tissues are increasingly used for analysis of element bioaccumulation, but the available Certified Reference Materials (CRMs) are insufficient. An attempt is made to review the studies made using biological reference materials for animal and human tissues. The need to have inter-laboratory studies and CRM in the field of biological monitoring of toxic metals is also discussed.

Journal ArticleDOI
TL;DR: A fibre optic biosensor for ethanol was developed, which is based on the enzymatic oxidation of ethanol, and contains an oxygen-sensitive fluorescing indicator which reports the decrease in the local oxygen partial pressure as the result of the enzyme oxidation.
Abstract: SummaryA fibre optic biosensor for ethanol was developed, which is based on the enzymatic oxidation of ethanol. The sensor layer contains an oxygen-sensitive fluorescing indicator which reports the decrease in the local oxygen partial pressure as the result of the enzymatic oxidation. The sensor measures in the 50–500 mmol/l ethanol range, with an accuracy of ± 4 mmol/l at 100 mmol/l. The detection limit is 10 mmol/l ethanol.

Journal ArticleDOI
TL;DR: In this article, a multi-ion FIA assembly for the analysis of Na +, K +, Ca 2+, NO3, CI-, and HCO3 in drinking water is described, as well as indirect ISE potentiometry of A13 + combined with FIA.
Abstract: FlieBinjektionsanalyse mit elektrochemischer Detektion Summary. Examples are given of successful combinations of flow injection analysis (FIA) with simple electrochemical detectors. FIA is especially suitable for ion-selective electrodes (ISE); stability, selectivity and speed of analysis can be significantly enhanced. A multi-ion FIA assembly for the analysis of Na +, K +, Ca 2+, NO3, CI-, and HCO3 in drinking water is described, as well as the indirect ISE potentiometry of A13 + combined with FIA. As an example of an amperometric detector, a secondary harmonic AC polarographic detection in an FIA arrangement which detects traces of ascorbic acid is presented and the reasons are given why FIA is also beneficial in amperometry.

Journal ArticleDOI
TL;DR: In this paper, an annular denuder system for simultaneous determination of gaseous and particulate pollutants in ambient air was developed, where inorganic acids (HCl, HNO3) were collected in a NaF-coated denuder, while organic acids (HCOOH, CH3COOH) were trapped in one coated with KOH.
Abstract: An annular denuder system for simultaneous determination of gaseous and particulate pollutants in ambient air was developed. Inorganic acids (HCl, HNO3) were collected in a NaF-coated denuder, while organic acids (HCOOH, CH3COOH) were trapped in one coated with KOH. NH3 was sampled with a H3PO4-coated denuder tube. Particulate H2SO4 was evaporated at elevated temperature (145°–155°C) and deposited on a NaF-coating together with HCl and HNO3 originating from thermal decomposition of NH4Cl and NH4NO3. NH3 resulting from deammoniation of (NH4)2SO4 as well as NH3 remaining from NH4Cl and NH4NO3 were collected in a H3PO4-coated denuder. The practical collection capacity of the tubes ranged from 0.35 to 1.0 μmol calculated from an experimentally determined sorption efficiency of at least 90%. The precision, expressed as relative standard deviation, of sampling and analytical procedures was determined from duplicate measurements in ambient air. The reproducibility varied from 9% to 14% for the gaseous components, while that of the particulate compounds ranged from 12% to 23%. Aqueous extracts of the denuder coatings were analysed for ionic components by ion chromatography using conductivity detection. The minimum detectable concentration in air was found to be 1.5 to 14 nmol/m3 for the different compounds calculated for 1.6 m3 sample volume, based on 3-h measurements at a flow of 9 l/min.

Journal ArticleDOI
TL;DR: In this article, the rate of reduction of Se(VI) to Se(IV) by hydrochloric acid was studied as a function of acid concentration, temperature and reaction time.
Abstract: The rate of reduction of Se(VI) to Se(IV) by hydrochloric acid was studied as a function of the acid concentration, temperature and reaction time. The reaction product Se(IV) was measured with the hydride generation-atomic absorption technique. The results show that for 10 mol/l HCl a complete reduction is achieved within 15 min at 60°C. The activation energy of the apparent first-order reaction was calculated from the results, and a value of 83 kJ mol−1 was obtained.

Journal ArticleDOI
TL;DR: In this article, the cephalosporin derivatives moxalactam, cefazolin, Cefuroxime, ceftriaxone and cefotaxime were studied by direct current, sampled direct current and differential pulse polarography and cyclic voltammetry.
Abstract: The cephalosporin derivatives moxalactam, cefazolin, cefuroxime, ceftriaxone and cefotaxime were studied by direct current, sampled direct current, differential pulse polarography and cyclic voltammetry. While moxalactam and cefazolin give rise to one reduction wave, cefuroxime, ceftriaxone and cefotaxime exhibit two reduction waves. The characteristics of corresponding electrode reactions and their analytical parameters are presented and discussed. Optimum pH-ranges for the determination of the five cephalosporins are given. Linear concentration ranges varied from 0.1 to 200 μg/ml and limits of determination were of the order of 0.01 to 0.04 μg/ml depending on the compound of interest. The precision of the proposed method is excellent with relative standard deviation around 1.3% at a concentration of 0.5 μg/ml for all investigated cephalosporins.

Journal ArticleDOI
TL;DR: In this article, the results of ion chromatography and isotope dilution mass spectrometry were compared with the results obtained by the German Antarctic station Georg-von-Neumayer.
Abstract: Nitrate traces in Antarctic snow and hoar-frost samples, which were collected on the Ekstrom ice shelf during January and February, 1987, were determined with ion chromatography at the German Antarctic station “Georg-von-Neumayer”. For comparison, sample preparations for isotope dilution mass spectrometry were also carried out at the German station whereas the mass spectrometric measurements took place in Regensburg. Comparable reproducibilities of 1%–5% were found for both methods of analysing nitrate concentrations in the range of 40–190 ng/g. An excellent agreement of the results of both methods with an average deviation of 0.1% was found in three sets of firn core samples. The average relative deviation of the ion chromatographic values from those of isotope dilution mass spectrometry was −10% for eleven hoar-frost and surface snow samples. The highest nitrate concentrations were analysed in hoar-frost samples with an average value of 548 ng/g. The following order, which corresponds to the age of nitrate depositions, was: new snow (206 ng/g), old surface snow (146 ng/g), and snow from firn cores (61 ng/g). The decreasing concentration with the age of samples is the result of re-emission of nitrate into the atmosphere after its deposition by snow. A seasonal variation of the nitrate concentration with a summer maximum and a winter minimum was observed for firn core samples. Accurate results of analytical data, which are published from all parts of Antarctica today, can only be guaranteed by the application of independent methods, e.g., by ion chromatography and isotope dilution mass spectrometry as it is shown in this work.

Journal ArticleDOI
TL;DR: In this article, the cellule reflexion totale attenuee-IR for mesures in situ (avec des films minces, avec des films epais) is described.
Abstract: Descriptions et representations schematiques: 1) de la cellule reflexion totale attenuee-IR pour mesures in situ (avec des films minces, avec des films epais); 2) de dispositifs permettant de determiner les caracteristiques de reponse dynamique des membranes. Avantages de la methode proposee pour suivre la diffusion de constituants, ayant un interet, a travers la membrane dans des conditions presque reelles. Resultats obtenus dans differentes conditions (en particulier avec la membrane PVC/DOS/BME-44)

Journal ArticleDOI
TL;DR: The factors affecting the dispersion obtained in a flow injection system are described and examples given of how control of the various factors can be exploited to produce manifolds for calibration purposes.
Abstract: The role of calibration in the overall analytical procedure is discussed and the potential role of flow injection techniques are assessed The factors affecting the dispersion obtained in a flow injection system are described and examples given of how control of the various factors can be exploited to produce manifolds for calibration purposes Most of these examples concern atomic spectrometry methods for which there is considerable interest at present in developing extended range calibrations and flow injection versions of the standard additions method Several examples of the latter are given

Journal ArticleDOI
TL;DR: Differential pulse anodic stripping voltammetry (DPASV) and isotope dilution mass spectrometry (IDMS) were used to analyse heavy metals in Antarctic snow samples.
Abstract: Differential pulse anodic stripping voltammetry (DPASV) and isotope dilution mass spectrometry (IDMS) were used to analyse heavy metals in Antarctic snow samples. It was possible to determine Pb and Cd with DPASV at the German Antarctic station “Georg-von-Neumayer” whereas the analyses of Pb, Cd, Tl, Cr, Ni, Cu, Zn, and Fe with IDMS were carried out at the University of Regensburg. 80% of the elemental concentrations in surface snow samples analysed with IDMS lay in the following ranges: Pb=3−40 pg/g, Cd<0.2−3 pg/g, Tl<0.2 pg/g, Cr<0.8–15 pg/g, Ni<4.8–40 pg/g, Cu<11−30 pg/g, Zn=30–500 pg/g, and Fe=(0.5–1.5)×103 pg/g. In most cases an acceptable agreement between the DPASV and IDMS results was obtained for Pb and Cd. More than 50% of all Pb analyses agreed within a deviation of 0–10 pg/g. The Cd results between both methods usually deviated by less than 1 pg/g. Slightly higher Pb concentrations were analysed in the average with IDMS compared with DPASV. This effect was not observed for the Cd data. A possible explanation for this fact are non-ionic Pb species in the melted snow samples, which cannot be analysed by DPASV. One particular investigation of Pb concentrations showed that the analysed data with DPASV decreased with the increasing length of sun-shine after a snowfall when samples of the same origin were determined. Blank control is the major requirement for accurate analysis results of heavy metals in this low concentration range. On the other hand, accuracy must always be tested by independent analytical methods. In this work it is shown that Pb and Cd can be analysed directly in the Antarctica with DPASV and that the result of this method is in acceptable agreement with the definitive method IDMS.

Journal ArticleDOI
J. M. Levy1, J. P. Guzowski1
TL;DR: The operational chromatographic conditions that were used for gasoline separations as well as results of quantitative heartcut reproducibility experiments of gasolines and hydrocarbon standards are described.
Abstract: Using packed column supercritical fluid chromatography on-line with capillary gas chromatography, gasolines have been characterized with respect to the separation of hydrocarbon classes as a group as well as a detailed fingerprinting of individual components within the classes. Using selective heartcutting, specific gasoline peaks were transferred to the capillary gas chromatograph as they eluted from the supercritical fluid chromatograph. Quantitative information was collected simultaneously from the flame ionization detectors that were used on both chromatographs. This report will describe the operational chromatographic conditions that were used for gasoline separations as well as provide results of quantitative heartcut reproducibility experiments of gasolines and hydrocarbon standards.