The procedure for simultaneous extraction from soil and determination by means of GC-ECD insecticides: aldrin, dieldrin, endrin and herbicide: atrazine was worked out. The proposed GC-ECD technique provides limits of detection in range 12 μg/mL - 18 μg/mL and 2 μg/mL, for insecticides and atrazine, respectively. Two different types of extraction: microwave assisted extraction (MAE) and ultrasound assisted extraction (UAE) with different solvents were tested to choose the procedure that provides the highest recoveries of analytes and low detection limits, typical for trace analysis (100 ppm or 100 mg/g, IUPAC). On the basis of recoveries and precision both extraction methods were compared. The insecticides recovery from soil samples obtained by UAE were in range 40-85%, coefficient of variation (CV): 1.3-5.0%, whereas for atrazine recovery was below 15% (CV: 8-18%). The most efficient and precise extraction procedure turned out to be MAE with n-hexane: acetone. The recoveries were in range 70-85% for insecticides and 84% for atrazine, CV: 0.4-2.2% and 5.3% for insecticides and atrazine, respectively. The presented MAE-GC-ECD procedure enables extraction and determination of aldrin, dieldrin, endrin and atrazine in soil samples with high recoveries, precision and limits of detections in range 6 ng/g - 8 ng/g in the case of insecticides and 1.5 ng/g for atrazine.
The MAE-GC-ECD procedure was applied for the above mentioned pesticides determination in environmental samples. Soils were collected in agricultural as well as rural areas in Poland. In all cases atrazine was determined in concentration range: 0.0187 mg/g - 0.1107 mg/g. Aldrin and dieldrin was detected in soil samples from two locations.
This paper aims at presenting the possibilities of applying gas chromatography for the determination of pharmaceutical residues in different matrices. Section one of the study underscores the environmental advantages of employing GC for such analyses. Section two presents the innovative methods for determining pharmaceuticals in the environment. The last section discusses the results of the analysis of the GC and GC-MS market in Poland.
According to the literature data, the described methods were applied for the analysis of real samples: wastewaters, surface waters, soil samples. The samples were collected from the Pomerania region and the Gulf of Gdańsk. The pharmaceuticals were determined in various environmental samples. The highest concentrations were found in raw wastewater, medium – in a treated wastewater, and the lowest – in surface water. The most frequently detected pharmaceuticals were: ibuprofen, paracetamol, diclofenac and naproxen, all belonging to NSAIDs.
Furthermore, the results of the study of the Polish GC market indicate that a very limited number of entities are currently using chromatographic techniques, and pharmaceutical residues tests are exceptions, mainly due to the lack of the legal requirements in this field and the lack of own laboratories.
Analyses of the ground waters in respect of presence of residues of plant protection products, i.e. active substances as well as environmental metabolites thereof are performed in the Institute of Plant Protection since the end of 80ties of the past Century. Based on the results obtained in 1993–1994 for 40 wells located in administrative territories of former Poznań, Toruń and Bydgoszcz voivodeships, in the vicinity of intensive agricultural production areas (orchards, farms), wells where significant amounts of residues of triazines group and dealkylated metabolites thereof had been found previously were qualified to further studies. There were 6 wells in which triazine residues were determined most often. Additionally, based on hydrogeological maps, directions of underflows in the areas of well’s locations were determined as well. The aim of the above was to find the additional places for sampling waters distant from pollution sources and estimation of the level of residues of target compounds depending on distance from the basic wells. Seven triazine compounds including basic active substances (atrazine, simazine) and their metabolites [desethyl atrazine, desisopropyl atrazine, desethyldesisopropyl atrazine, hydroxyatrazine and hydroxysimazine] were selected for the presented studies. Residues were analyzed using methodologies designed in the Institute, i.e. solid-phase extraction (SPE) followed by determination by chromatographic techniques HPLC-PDA, GC-NPD and GC-MS. Generally, during 11 years of investigations (1993–2003) samplings were performed 52 times and 323 samples of groundwater including that from additional wells were analyzed. Most often residues of atrazine and deethylatrazine in wells located in environs of Poznań were detected.
Root-knot nematodes, genus Meloidogyne, are among the most plant damaging pathogens worldwide. The action of natural products against plant pathogens has been investigated to assess their effectiveness in the control of diseases. Thus, the present study aimed to evaluate the phytochemistry potential of the Ficus species for the control of Meloidogyne javanica. In vitro inhibitory activity assays were performed with crude ethanolic extracts of leaves and branches from 10 Ficus species. Among these, Ficus carica extracts exhibited strong paralysis activity against second stage juveniles (J2) (EC50 = 134.90 μg ∙ ml–1), after 72 hours. In addition, high efficacy was observed in egg-hatching inhibition at different embryonic stages. Microscopy analysis revealed severe morphological alterations in the nematode tissues at the J2 stage, as well as immotility of juveniles released from eggs in the presence of F. carica extracts. The efficacy of the treatments for the other species was very low. These differences were supported by the variation in the compound classes, mainly for alkaloids and metabolite profiles by Gas Chromatography/Mass Spectrometry (GC/MS) when F. carica was compared with the other species. The results indicated that F. carica is a promising source for the isolation and identification of molecules capable of acting in the control of M. javanica.
The work presents examination results of the common determination of PAHs and PCBs in industrial sludge and supernatants. Sewage sludge was taken from the wastewater treatment plant, and supernatants were obtained by their centrifuging. The prepared samples of sewage sludge and supernatants were subjected to extraction with applying the mixture of organic solvents. Cyclohexane and dichloromethane were used for constant samples, and methanol, cyclohexane and dichloromethane - for liquid. Extracts, after separation from samples of sewage sludge and supernatants, were cleared on the silica gel in vacuum conditions and concentrated in the stream of nitrogen. In such prepared extracts there was conducted the qualitative-quantitative analysis of 16 PAHs using the GC-MS system. Next, the samples were evaporated and poured with water and methanol until the clear solution was obtained. Extracts were cleared on octadecyl C18 columns, and then concentrated in the nitrogen stream. In these extracts PCBs was also determined with the application of the gas chromatograph with mass spectrometer. The range of concentrations 16 PAHs in sewage sludge equalled 10-16 mg/kgd.w. Summary average concentration 16 PAHs in supernatants was reached 17 μg/L. Average recovery of PAHs introduced to sewage sludge in the form of reference mixture was 78% (with consideration of naphthalene). In the case of supernatants, the average value of recovery reached 60%. Average PCBs concentration in supernatants equalled 10 ng/L. For sewage sludge the sum of marked PCBs was an average 1.23 μg/kgd.w.. In the case of particular PCBs the percentage recovery of the reference mixture for supernatants was 86%, while for sewage sludge it was 55%.
Suitability of the given binding agent for the moulding sands preparation depends on the one hand on the estimation of technological properties of the sand and the mould made of it and the obtained casting quality and on the other hand on the assessment of this sand influence on the natural and working environment. Out of moulding sands used in the foundry industry, sands with organic binders deserve a special attention. These binders are based on synthetic resins, which ensure obtaining the proper technological properties and sound castings, however, they negatively influence the environment. If in the initial state these resins are not very dangerous for people and for the environment, thus under an influence of high temperatures they generate very harmful products, being the result of their thermal decomposition. Depending on the kind of the applied resin (phenol-formaldehyde, urea, furfuryl, urea–furfuryl, alkyd) under an influence of a temperature such compounds as: furfuryl alcohol, formaldehyde, phenol, BTEX group (benzene, toluene, ethylbenzene, xylene), and also polycyclic aromatic hydrocarbons (PAH) can be formed and released. The aim of the study was the development of the method, selection of analytical methods and the determination of optimal conditions of formation compounds from the BTEX group. An emission of these components constitutes one of the basic criteria of the harmfulness assessment of binders applied for moulding and core sands. Investigations were carried out in the specially designed set up for the thermal decomposition of organic substances in a temperature range: 5000 C – 13000 C at the laboratory scale. The object for testing was alkyd resin applied as a binding material for moulding sands. Within investigations the minimal amount of adsorbent necessary for the adsorption of compounds released during the decomposition of the resin sample of a mass app. 15 mg was selected. Also the minimal amount of solvent needed for the desorption of compounds adsorbed in the column with adsorbent was found. The temperature range, in which the maximal amounts of benzene, toluene, ethylobenzene and xylenes are released from the resin, was defined. The qualitative and quantitative analyses of compounds from the BTEX group were performed by means of the gas chromatography combined with the mass spectrometry (GC/MS).
The paper presents the results of thermoanalytical studies by TG/DTG/DTA, FTIR and GC/MS for the oil sand used in art and precision foundry. On the basis of course of DTG and DTA curves the characteristic temperature points for thermal effects accompanying the thermal decomposition reactions were determined. This results were linked with structural changes occurred in sample. It has been shown that the highest weight loss of the sample at temperatures of about 320°C is associated with destruction of C-H bonds (FTIR). In addition, a large volume of gases and high amounts of compounds from the BTEX group are generated when liquid metal interacts with oil sand. The results show, that compared to other molding sands used in foundry, this material is characterized by the highest gaseous emissions and the highest harmfulness, because benzene emissions per kilogram of oil sand are more than 7 times higher than molding sand with furan and phenolic binders and green sand with bentonite and lustrous carbon carrier.
Sand samples with furan binder were prepared using Sand, Furfuryl Alcohol and Toluene Sulfonic Acid with ratio 100:0.85:0.30. To
identify and quantify gases releasing from furan binder various studies like FTIR, TGA and GC-MS were carried out. After analyzing our
materials using above mentioned characterizations the chemical formula of the Resin and Binder and amount of gases releasing from
composition were confirmed. After studying various reports on pyrolysis process of furan binder calculation of the % of various gases
emitting during pyrolysis process of furan was carried out. Sample of gas collected from mold was analyzed using GC-MS. Based on GCMS
measurement various gases emitting from furan sand mold were identified and their amount were calculate and compared with the
international standers of permissible gas emission limits in a foundry. The purpose of this paper is to assist foundries in pollution
prevention by devising clean technologies which maintain or improve the quality of ambient surrounding. This paper aimed at
minimization of pollution of air by using various techniques.
Five cosmetics wastewater samples were treated by Dissolved Air Flotation (DAF) assisted by coagulation. Different aluminum based coagulants were used: (Al2(SO4)3, Al 1019, Al 3010, Al 3030, Al 3035, PAX 16 and PAX 19). The raw wastewater COD values were in the range 285-2124 mg/l. The efficiency of DAF depended on different coagulants and production profi le of factory. COD removal was varied from 11.1 to 77.7%. The efficiency of coagulants was similar during treatment of particular sample. The best results were obtained with Al2(SO4)3 and for sample 5 - lotions and shampoos production. The wastewater from UV fi lter creams production (sample 4) was resistant to treatment by DAF regardless of used coagulant. HS-SPME-GC-MS analysis can be a confirmation of DAF effectiveness
This study investigates the acaricidal, ovicidal, and repellent effects of the Tagetes patula Linn. (Asteraceae) leaf extract against both the adult female and egg stages of Tetranychus urticae Koch (Trombidiformes: Tetranychidae) under laboratory conditions. The Tagetes patula ethanolic leaf extract [TpEtOH70%] was screened for adulticide and ovicide bioassays in order to consider its acute toxicity. One sublethal concentration was used to assess egg-laying capacity (fecundity), repellent, and oviposition deterrent activities. The chemical characterization was conducted by gas chromatography-mass spectrometry (GC-MS) analysis to identify the TpEtOH70% bioactive components. Results showed that the LC50 value of TpEtOH70% leaf extract predicted by Probit analysis against T. urticae adult females at 24 h was 0.99%. The TpEtOH70% leaf extract showed a significant toxic effect as the highest mean mortality rates (± SE) of the treated adult females was 88.9 ± 3.7%. However, the TpEtOH70% leaf extract was insignificant in affecting the egg-laying capacity of the adult females treated with a sublethal dose of 0.5% even after 72 h. The TpEtOH70% leaf extract was classified repellent since the repellent index (RI) value was lower than 1 – SD. In addition, it had a high oviposition deterring effect based on a 100% reduction of the total number of eggs. The TpEtOH70% leaf extract had a significant ovicidal effect on T. urticae eggs, with 56.04% reduction in hatching. Five bioactive compounds from various classes of phytochemicals were identified in the TpEtOH70% leaf extract and the major compound was phytol (62.72%). This pioneering investigation reveals the adulticidal, ovicidal, and repellent activities of the TpEtOH70% leaf extract against T. urticae. A combination of multiple modes of action of different plant components may act alone or in synergism to delay the development of mite resistance.
The sustainable development of human activities is directly related to the protection of the environment by lowering the anthropogenic stress. Pharmaceuticals – due to their growing consumption (use in medicine, veterinary, animal production, cosmetics) and their incomplete removal in wastewater treatment plants – are classified as a group of new and rapidly emerging pollutants which have been proven to have a negative impact onto water organisms. In order to ensure the proper protection of human health and the environment there is an urgent necessity of determining pharmaceuticals in clinical, cosmetic, food and environmental samples. Gas (GC) and high performance liquid chromatography (HPLC) are valuable techniques for such determination, especially when they are coupled with mass spectrometry (GC-MS; LC-MS) or tandem mass spectrometry (GC-MS/MS; LC-MS/MS). The purpose of this paper is to present an analysis of sustainability features of analytical techniques in the light of necessity to determine trace amounts of pharmaceuticals in the aforementioned different matrices. Using the Delphi method we performed an analysis of the key sources of the competitive advantages of the application of GC and GC-MS techniques for determining the pharmaceutical residue in clinical, cosmetic, food and environmental samples – compared to techniques based on HPLC or LC-MS. The analysis covered the following areas: (i) the features of the technique, (ii) the price, and (iii) the applicability in various sectors of economy.
The furan resin offers advantages such as high intensity, low viscosity, good humidity resistance and is suitable for cast different casting
alloys: steel, cast iron and non-ferrous metal casting. For hardening furan resins are used different hardeners (acid catalysts). The acid
catalysts have significant effects on the properties of the cured binder (e,g. binding strength and thermal stability) [1 - 3]. Investigations of
the gases emission in the test foundry plant were performed according to the original method developed in the Faculty of Foundry
Engineering, AGH UST. The analysis is carried out by the gas chromatography method with the application of the flame-ionising detector
(FID) (TRACE GC Ultra THERMO SCIENTIFIC).
The results of investigations of three commercial binders applied in the Alphaset technology marked as: Sample E , Sample T and Sample S are presented in the hereby paper. These samples were subjected to the pyrolysis process at a temperature of 900°C (inert atmosphere, He 99.9999). The gas chromatograph coupled with the mass spectrometer and pyrolizer (Py-GC/MS) were used in the study. The identification of gases emitted during the thermal decomposition was performed on the basis of the mass spectral library. The obtained results indicate a certain diversification of emitted gases. Among the pyrolysis products the following harmful substances were identified: furfuryl alcohol, formaldehyde, phenol and also substances from the BTEX (benzene, toluene and ethylobezneze and xylenes) PAHs (Polycyclic Aromatic Hydrocarbons) and VOC groups (Volatile Organic Compounds). Therefore, from the environment protection point of view performing systematic investigations concerning the harmfulness of binders applied in the moulding and core sands technology, is essential.