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41.
Samuel Melaku Ilse Gelaude Frank Vanhaecke Luc Moens Richard Dams 《Mikrochimica acta》2003,142(1-2):7-12
Microwave digestion reduction-aeration and pyrolysis combined with cold vapour atomic absorption and cold vapour atomic fluorescence
are compared for the determination of total mercury in several biological and environmental matrices. The biological samples
were digested in a mixture of HNO3/H2O2, the environmental samples in a mixture of HNO3/HClO4. After reduction with SnCl2, the mercury was collected by two-stage gold amalgamation. After microwave digestion reduction-aeration, detection limits
of 1.4 ng g−1 and 0.6 ng g−1 were obtained for cold vapour atomic absorption spectrometry (CVAAS) and cold vapour atomic fluorescence spectrometry (CVAFS),
respectively, for 250 mg of environmental samples. For biological samples (500 mg) the detection limits were 0.7 ng g−1 (CVAAS) and 0.4 ng g−1 (CVAFS). After pyrolysis, detection limits of 3.5 ng g−1 and 1.6 ng g−1 for CVAAS and CVAFS, respectively, were obtained for a 10 mg sample. Pyrolysis can only be applied when the organic content
of the sample is not too high. Accurate results were obtained for 8 certified reference materials of both environmental and
biological origin. In addition, a real sludge sample was analysed.
Author for correspondence. E-mail: richard.dams@rug.ac.be
Received September 18, 2002; accepted December 3, 2002
Published online May 5, 2003 相似文献
42.
Simplified method for the Re-Os dating of molybdenite using acid digestion and isotope dilution ICP-MS 总被引:1,自引:0,他引:1
An analytical method was developed for Os-Re dating of molybdenite. The method is based on determination of Os and Re concentrations in molybdenite by isotope dilution inductively-coupled plasma mass spectrometry (ID-ICP-MS). Sample digestion and sample/spike equilibration were achieved by a two-stage autoclave-based procedure using a mixture of nitric and sulphuric acids. Os was separated from the sample digest by modified single-stage distillation of osmium tetraoxide (OsO4) using elevated temperature and on-line addition of hydrogen peroxide. OsO4(g) was trapped in a mixture of 0.05% thiourea in 0.05 M sodium hydroxide. An anion-exchange column was used to separate Re from excess Mo in the solution remaining after distillation. Os and Re isotope ratio measurements were performed by single-collector, double focusing inductively-coupled plasma mass spectrometry (ICP-MS) with on-line mass-bias correction. Typical instrumental precision was in the range 0.02-0.2% relative standard deviation (R.S.D.) depending on the analyte concentrations. Notorious Os memory effects in the ICP-MS introduction system were eliminated using 5% ammonia solution, both as matrix for final dilution of the trap mixture as well as for washing between the samples. The reproducibility of the entire analytical procedure was accessed by replicate dating of two molybdenite standards and three molybdenite separates, and was found to be in the range 0.87-1.52% R.S.D. Though accuracy of the method is limited by difficulties in evaluating exact concentration of Os in spike solution, ages obtained in the course of these work agrees well with previously published data. 相似文献
43.
J. Hernández-Borges M. A. Rodríguez-Delgado F. J. García-Montelongo 《Chromatographia》2006,63(3-4):155-160
Several improvements in sample pretreatment for the determination of organic pollutants (i.e. n-alkanes, polycyclic aromatic hydrocarbons, PAHs) in marine biota (mussels) are presented. The use of liquid nitrogen and
homogenization of the samples are shown to be an alternative to the time consuming liophilization step required for the analysis
of biota samples. Microwave-assisted hydrolysis and extraction are combined to isolate organic pollutants (19 n-alkanes and 27 PAHs) from biota matrices. Experimental design (ED) and artificial neural networks (ANNs) were used to optimize
the experimental conditions. NIST-CRM 2978 was used to test the validity of the developed method which shows a good agreement
with certified values. 相似文献
44.
A monitoring system was developed to gain information on the present level of pollutants in the Lake Balaton, Hungary. Determination of 13 polycyclic aromatic hydrocarbons (PAHs) and inorganic pollutants (mostly toxic metals) in aerosol, precipitation and sediment samples was carried out. The aim of collecting aerosol and precipitate samples in the same site at the same period was to determine the distribution of elements in two depositions. For the fractionation by particle size, aerosols were sampled by a cascade impactor. A simple three-stage sequential leaching procedure was applied to establish the distribution of metals among environmentally mobile, bound to carbonates and oxides, and environmentally immobile, (bound to silicates) fractions in aerosols. Sediment samples were collected from 17 different sites inside of the lake and 10 sites at harbors at 30–70 cm in depth. Core samples were cut to 10-cm pieces, dried at room temperature, and finally passed through a 63-μm sieve. Total concentrations of elements were determined by atomic absorption spectrometry (AAS) after an acidic digestion. The concentrations of PAHs were determined by HPLC method with fluorescence detection.In aerosol samples collected from September 6, 2002 to January 26, 2003, concentration of Cd was <0.1 μg/m3, and the majority of Cd has been found in the mobile fraction. Cadmium was associated to particles between 0.25 and 2 μm indicating the anthropogenic origin. Similar distribution of Pb was obtained in all seasons, and the highest concentration of Pb was found as 8.6 ng/m3 in particle size of 0.7 and 1.4 μm. Results of total concentration of elements of bottom sediments of the Lake Balaton and harbors were compared to Interim Sediment Quality Guideline (ISQG) values and the Probable Effect Level (PEL) values. Data showed that the average concentrations of elements were usually less than those of ISQGs and other background data for soils and geochemical values. The sediment is not polluted and its disposal is feasible. There is no direct correlation between the concentration of elements deposited onto the surface of the lake from dry and wet deposition and the upper part of the sediment. So, from the budget of the deposition, the concentration of elements in the upper layer of the sediment cannot be predicted.Seasonal changes of the concentration of PAHs in aerosol was observed, samples collected at winter contained the highest values. In December–January 2002/2003, the wet deposition was found as 64 μg/m2 period. Among the individual compounds, the wet deposition rate of phenantrane, fluoranthene and pyrene was dominant, while for dry deposition, these compounds were fluoranthene and pyrene. The concentrations of ∑PAHs found for all sites and depth of sediment samples ranged from 11 to 1734 μg/kg dry weight with an average of 132 μg/kg. These values represent a quite low pollution level compared to other sediment with anthropogenic influence. Based on the results, it can be definitely confirmed that the chemical quality of the water and sediment of the Lake Balaton is satisfactory. 相似文献
45.
The pretreatment of waste-activated sludge (WAS) by electron beam irradiation was studied in order to improve anaerobic sludge
digestion. The irradiation dose of the electron beam was varied from 0.5 to 10 kGy. Batch and continuous-flow stirred tank
reactors (CFSTRs) were operated to evaluate the effect of the electron beam pretreatment on anaerobic sludge digestion. Approximately
30–52% of the total chemical oxygen demand (COD) content of the WAS was solubilized within 24 h after electron beam irradiation.
A large quantity of soluble COD, protein, and carbohydrates leached out from cell ruptures caused by the electron beam irradiation.
Volatile fatty acids production from the irradiated sludge was approx 90% higher than that of the unirradiated sludge. The
degradation of irradiated sewage sludge was described by two distinct first-order decay rates (k
1 and k
2). Most initial decay reaction accelerated within 10 d, with an average k
1 of 0.06/d for sewage sludge irradiated at all dosages. The mean values for the long-term batch first-order decay coefficient
(k
2) were 0.025/d for irradiated sewage sludge and 0.007/d for unirradiated sludge. Volatile solids removal efficiency of the
control reactor fed with unirradiated sewage sludge at a hydraulic retention time (HRT) of 20 d was almost the same as that
of the CFSTRs fed with irradiated sludge at an HRT of 10 d. Therefore, disintegration of sewage sludge cells using electron
beam pretreatment could reduce the reactor solid retention time by half. 相似文献
46.
Efforts were made to assess the efficiency of an anaerobic filter packed with porous floating ceramic media and to identify
the optimum operational condition of anaerobic filter as a pretreatment of swine wastewater for the subsequent biological
removal of nitrogen and phosphorus. A stepwise decrease in hydraulic retention time (HRT) and an increase in organic loading
rate (OLR) were utilized in an anaerobic filter reactor at mesophilic temperature (35°C). The optimum operating condition
of the anaerobic filter was found to be at an HRT of 1 d. A soluble chemical oxygen demand (COD) removal efficiency of 62%
and a total suspended solids removal efficiency of 39% at an HRT of 1 d were achieved with an OLR of 16.0 kg total COD/(m3·d), respectively. The maximum methane production rate approached 1.70 vol of biogas produced per volume of reactor per day
at an HRT of 1 d. It was likely that the effluent COD/total Kjeldahl nitrogen ratio, of 22, the COD/total phosphorous ratio
of 47, and the high effluent alkalinity >2500 mg/L as CaCO3 of the anaerobic filter operated at an HRT of 1 d was adequate for the subsequent biological removal of nitrogen and phosphorus. 相似文献
47.
48.
Microwave-assisted desorption (MAD) coupled to in situ headspace solid-phase microextraction (HS-SPME) was first proposed as a possible alternative pretreatment of samples in absorbent collected from workplace monitoring. Aniline collected on silica gel was investigated. Under microwave irradiation, the aniline was desorbed from silica gel and directly absorbed onto the SPME fiber in the headspace. Having been sampled on the SPME fiber, and desorbed in the GC injection port, aniline was analyzed using a GC-FID system. Parameters that affect the proposed extraction efficiency, including the extraction media and its pH, the microwave irradiation power and the irradiation time as well as desorption parameters of the GC injector, were investigated. Experimental results revealed that the extraction of a 150-mg silica gel sample using a 0.8-ml aqueous solution (pH 12) and a PDMS/DVB fiber under medium-high-powered irradiation (345 W) for 3 min maximized the efficiency of extraction. Desorption of aniline from the SPME fiber was optimal at 230 °C held for 3 min. The detection limit was 0.09 ng. The proposed method provided a simple, fast, and organic solvent-free procedure to analyze aniline from a silica gel matrix. 相似文献
49.
《Arabian Journal of Chemistry》2020,13(10):7289-7301
Black pepper oils have been investigated frequently in the recent years. However, there is a significant variation in physicochemical properties and bioactivity of oils depended on extraction techniques. In this study, the systemic investigation of four various extraction methods was performed to evaluate the physicochemical characterizations, antioxidant and antibacterial activity. The investigation of 1H NMR, FTIR and UV–Vis spectra confirmed presence of non-volatile components in oils extracted through supercritical CO2 and hexane-soaking extractions which induced their typical thermal properties. The isothermal behaviour of extracted oils related to evaporation was within range of 3.2–7.3% (w/w) at 27 °C. The SEM images of the black pepper confirmed different operation manners of mechanism between extractions using the solvents and heating process. The lowest MIC for both essential oils from conventional hidrodistillation and microwave-assisted hidrodistillation against two bacteria including E. coli and B. subtilis were found to be 137 µg mL−1. The non-isothermal decomposition kinetics were investigated on the essential oil of microwave-assisted hydrodistillation extraction. The activation energies and pre-exponent factors of non-isothermal decomposition were found to be in range of 36.5–73.7 KJ mol−1 and 4.98 × 103–1.97 × 108 s−1, respectively, dependent on conversional fractions of the oil. The results revealed that chemical components, physicochemical properties and bioactivity of black pepper essential oils depended on the extraction techniques. 相似文献
50.
Low volume microwave digestion for the determination of selenium in marine biological tissues by graphite furnace atomic absorption spectroscopy 总被引:2,自引:0,他引:2
A microwave digestion method for the determination of marine biological tissues has been developed to allow determination of selenium in small sample sizes (< 0.1 g). The benefits of this technique include maintaining concentrates in extracts without the subsequent over dilution encountered when using larger vessels, increased sample throughput and reduced loss of volatile material. Freeze dried biological material (< 0.1 g) and nitric acid (1 ml) were placed into 7 ml screw top Teflon vessels which are completely sealed on capping. Two 7 ml vials were placed into larger 120 ml vessels fitted with a Teflon spacer and 10 ml of distilled water. The effects of microwave power and time, and sample mass on selenium recovery from three marine standard reference materials (NIST SRM 1566a Oyster Tissue, NRCC DORM-1 Dogfish Muscle and NRCC TORT-1 Lobster Hepatopancreas) were examined. The optimum conditions: 600 W, 2 min; 0 W, 2 min; 450 W, 45 min, allowed quantitative recoveries of selenium from these and three other standard reference materials (NRCC DOLT-1 Dogfish liver, NIST RM-50 Albacore tuna and IAEA MA-A-2 fish flesh). Studies on sample mass showed that the analysis of sample masses from 0.025 to 0.1 g gave selenium concentrations within the certified range. Six species of selenium: selenite, selenate, selenomethionine, selenocysteine, selenocystamine, and trimethyl selenonium were added to oyster, dogfish, and lobster tissues. Recoveries were near quantitative for all species (94–105%) except trimethyl selenonium (90–101%). 相似文献