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1

Influence of distillation time and distillation apparatus on the chemical composition and quality of Lavandula angustifolia Mill. essential oil

Wesołowska Aneta, Jadczak Dorota, Zyburtowicz Karolina

Polish Journal of Chemical Technology

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2023

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Vol. 25, nr 4

36--43

EN

In the study, the influence of distillation time as well as distillation apparatus on the chemical composition and quality of lavender (Lavandula angustifolia Mill.) essential oil were investigated. Two different types of distillation apparatuses: Deryng (popular in Poland) and Clevenger-type (recommended by European Pharmacopoeia) were used for the isolation of the essential oil from dried lavender flowers (Lavandulae flos). Moreover, different distillation times (2, 3 and 4 hours) were also applied. The chemical composition of the isolated oils, determined by gas chromatography coupled with mass spectrometry (GC-MS), revealed the dominance of linalool (11.55–17.19%) and linalyl acetate (12.84–16.78%) in the all analyzed samples. Other important constituents were: caryophyllene oxide (5.66–7.35%), lavandulyl acetate (4.64–5.40%) and borneol (4.62–5.51%). On the basis of the obtained data it was proved that the distillation time and distillation apparatus affect the amounts of some constituents in the lavender oil.

2

Determination of acrylamide in foods by automatic accelerated solvent extraction and gas chromatography-mass spectrometry

Kang Cuicui, Ma Haijian, Li Yuan, Zhang Chizhong, Hong Yueqin, Shao Minghua

Acta Chromatographica

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2021

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Vol. 33, no. 1

64--72

EN

The aim of the experiment is to establish a method for the determination of acrylamide in food by automatic accelerated solvent extraction-gas chromatography-mass spectrometry. D3-acrylamide was used as isotope internal standard, crushed samples were extracted and purified by automatic accelerated solvent, acrylamide was derivatized into 2,3-dibromopropanamide by potassium bromide and potassium bromate under acidic conditions, and then the derivative was extracted by ethyl acetate and detected by gas chromatography-mass spectrometry. The method had a good linear relationship in the concentration range of 10–2000 ng/mL, and the coefficient of determination (R2) was 0.9997. The detection limit of the method was 3 mg/kg. The quantification limit of the method was 10 mg/kg. The standard addition recovery of acrylamide was between 105 and 120%, and the relative standard deviation of the recovery of acrylamide was less than 3.0%. The experimental result showed that the method was simple, sensitive, efficient and accurate, and could be used for the determination of acrylamide in food.

3

Hydrocarbon species in SI and HCCI engine using winter grade commercial gasoline

Elghawi Usama, Mayouf Ahmed, Tsolakis Athanasios

Combustion Engines

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2020

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R. 59, nr 1

17--24

EN

The study provides a qualitative and quantitative analysis of the C5-C11 hydrocarbon species generated in Spark Ignition - Homogeneous Charge Compression Ignition (SI/HCCI) gasoline direct injection (GDI) engine at range of operating conditions. The presented results and data were obtained from the combustion of winter grade commercial gasoline containing 2% w/w ethanol (C2H5OH) for the engine operated in steady-state, fully warmed-up condition. The hydrocarbon analysis in exhaust gases was executed on a Gas Chromatography-Mass Spectrometer (GC-MS) apparatus directly connected to the engine exhaust via heated line. The highest concentration of the total hydrocarbon emissions was obtained under low load HCCI engine operation at stoichiometric fuel-air ratio. The major hydrocarbon compounds detected in the collected samples were benzene, toluene, p-xylene, and naphthalene. Benzene originates from the incomplete combustion of toluene and other alkylbenzenes which are of considerable environmental interest. During the SI engine operation, increase of the engine speed and load resulted in the increase of benzene and the total olefinic species with simultaneous decrease in isopentane and isooctane. The same trends are seen with the engine operating under HCCI mode, but since the combustion temperature is always lower than SI mode under the same engine conditions, the oxidation of fuel paraffin in the former case was less. As a result, the total olefins and benzene levels in HCCI mode were lower than the corresponding amount observed in SI mode. Aromatic compounds (e.g., toluene), except for benzene, were produced at lower levels in the exhaust when the engine speed and load for both modes were increased.

4

Zastosowanie chromatografii jonowej i chromatografii gazowej sprzężonej ze spektrometrią mas do oznaczania wybranych anionów i ftalanów w wodach smakowych

Piątek M., Powałek I., Oszczudłowski J.

Aparatura Badawcza i Dydaktyczna

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2016

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T. 21, nr 2

65--70

PL

Obecnie powszechne jest spożywanie różnego rodzaju wód smakowych, a informacje o ich składzie chemicznym nie należą do najbardziej szczegółowych. W związku z tym warto przeprowadzić pełną analizę tych wód w celu określenia ich składu. Założeniem badań przedstawionych w niniejszej pracy było oznaczenie istotnych anionów nieorganicznych i niektórych ftalanów w próbkach rzeczywistych wybranych wód smakowych. Zgodnie z tą koncepcją określono skład ilościowy następujących anionów: fluorkowych, chlorkowych, azotanowych (V), siarczanowych (VI) i fosforanowych (V), z zastosowaniem chromatografii jonowej (IC). Przeprowadzono również jakościowe i ilościowe oznaczenie ftalanów, wykorzystując chromatografię gazową ze spektrometrem mas (GC/MS). Stwierdzono stosunkowo wysokie stężenia jonów siarczanowych (VI) i chlorkowych. W wodach smakowych o pH poniżej 3 wykryto śladowe ilości niektórych ftalanów, które mogły migrować z powierzchni plastikowych butelek.

EN

Much as it is common today to consume different kinds of flavored waters, information about their chemical composition is not the most detailed. Therefore it is worth conducting a full analysis of these waters in order to determine their composition. The assumption of the research presented in this paper was to determine the major inorganic anions and certain phthalates in some real samples of flavored waters. According to this concept, there was estimated the concentration of fluoride, chloride, nitrate (V), sulphate (VI) and phosphate (V) ions, using ion chromatography (IC). The determination of phthalates was conducted by means of gas chromatography mass spectrometry (GC/MS). There were found relatively high concentrations of sulfate (VI) and chloride ions. There were also detected trace amounts of certain phthalates, which may have migrated from the surface of plasti botts in fl voured waters having a pH value below 3.

5

Analysis of essential oil of Nardostachys chinensis Batal by GC-MS combined with chemometric techniques

Wang F., Liu S., Luo M. Y, Qin Y., Lei P, Liu Y. H, Liang Y. Z

Acta Chromatographica

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2015

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Vol. 27, no. 1

157--175

EN

The essential oil extracted from Nardostachys chinensis Batal (NCB) was analyzed by gas chromatography-mass spectrometry (GC-MS) combined with two chemometric resolution methods (CRM), heuristic evolving latent projections (HELP), and selective ion analysis (SIA). Qualitative analysis was performed by comparing the obtained pure mass spectra with those in National Institute of Standards and Technology (NIST) mass spectra database. Identification of some compounds was assisted by comparison of programmed temperature retention indices (PTRIs). The quantitative results were obtained by overall volume integration (OVI). A total of 69 compounds in the essential oil of N. chinensis Batal were identified, accounting for 93.98% of the total content. The major compounds were (−)-spathulenol, epiglobulol, trans-longipinocarveol, and patchouli alcohol which contribute to the antimicrobial and antioxidant activity. The results showed that the efficiency and reliability were greatly improved by use of chemometric techniques and programmed temperature retention index as assistants of GC-MS in identification of the plant essential oil.

6

Organic geochemistry of Upper Carboniferous bituminous coals and clastic sediments from the Lublin Coal Basin (Poland)

Karger M., Gazda L., Grafka O.

Acta Geologica Polonica

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2013

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Vol. 63, no. 3

425--442

EN

Bituminous coals and clastic rocks from the Lublin Formation (Pennsylvanian, Westphalian B) were subjected to detailed biomarker and Rock-Eval analyses. The investigation of aliphatic and aromatic fractions and Rock-Eval Tmax suggests that the Carboniferous deposits attained relatively low levels of thermal maturity, at the end of the microbial processes/initial phase of the oil window. Somewhat higher values of maturity in the clastic sediments were caused by postdiagenetic biodegradation of organic matter. The dominance of the odd carbon-numbered n-alkanes in the range n-C25 to n-C31 , high concentrations of moretanes and a predominance of C28 and C29 steranes are indicative of a terrigenous origin of the organic matter in the study material. This is supported by the presence of eudesmane, bisabolane, dihydro-ar-curcumene and cadalene, found mainly in the coal samples. In addition, tri- and tetracyclic diterpanes, e. g. 16β(H)-kaurane, 16β(H)-phyllocladane, 16α(H)-kaurane and norisopimarane, were identified, suggesting an admixture of conifer ancestors among the deposited higher plants. Parameters Pr/n-C17and Rdit in the coal samples show deposition of organic matter from peat swamp environments, with the water levels varying from high (water-logged swamp) to very low (ephemeral swamp). Clastic deposits were accumulated in a flood plain environment with local small ponds/lakes. In pond/lake sediments, apart from the dominant terrigenous organic matter, research also revealed a certain quantity of algal matter, indicated, i.a., by the presence of tricyclic triterpanes C28 and C29 and elevated concentrations of steranes. The Paq parameter can prove to be a useful tool in the identification of organic matter, but the processes of organic matter biodegradation observed in clastic rocks most likely influence the value of the parameter, at the same time lowering the interpretation potential of these compounds. The value of Pr/Ph varies from 0.93 to 5.24 and from 3.49 to 22.57 in the clastic sediments and coals respectively. The microbial degradation of organic matter in both type of rocks and during early stages of diagenesis is confirmed by a high concentration of hopanes, the presence of drimane homologues, bicyclic alkanes and benzohopanes. Moreover, bacteria could also have been connected with the primary input of organic matter, which is shown by the presence of e.g. C30 neohop-13(18)-ene.

7

Spektrometria mas w badaniach skażeń mikrobiologicznych środowiska . Część I. Kwas muraminowy jako biomarker ścian komórkowych bakterii

Mielniczuk Z., Bal K.

Wiadomości Chemiczne

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2012

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[Z] 66, 5-6

445-460

EN

Microorganisms synthesize several monomeric chemical structures that are not found elsewhere in nature, e.g. muramic acid (an amino sugar) and D-amino acids (D-alanine and D-glutamic acid) are ubiquitous in bacterial peptidoglycan (PG). Specific sugars (e.g. heptoses) and 3-hydroxylated fatty acids are found in the endotoxin (lipopolysaccharide, LPS) of gram-negative bacteria [42]. The best way to protect against environmental contamination is microbial control. Methods in current use for monitoring of microorganisms mainly include culturing and direct microscopy. However, several factors including samples collection, growth conditions, incubation temperature and interaction between different organisms all affect culturing results. Additionally, culturing based methods can detect only viable organisms and they are also time consuming, sometimes taking days or weeks. However, since both living and dead microorganisms express irritating and toxic structures, they should all be taken into consideration [17]. Muramic acid (MuAc), an amino sugar, has been suggested for use as a chemical marker in gas chromatography-mass spectrometry (GC-MS) determination of bacterial peptidoglycan in both clinical and environmental samples. Several derivatives of MuAc have been applied, including the alditol acetate [1, 2], aldononitrile [3], trifluoroacetyl [4] and trimethylsilyl [5], and methyl ester O-methyl acetate [6] derivatives. Both the alditol acetate and TMS derivatives have proven suitable for the use with GC-ion-trap tandem MS [7]. The aim of our proposition is a trial of application of gas chromatography-mass spectrometry (GC-MS) method as an alternative or complement to culturing, microscopy and other assays for detection, characterization and monitoring of microbial contamination of environment (e.g. water, air, air-conditioning systems), contamination of biochemical and food production chain processes, packaging for foodstuffs etc. by direct analysis of bacterial muramic acid as a biochemical marker. A method is described for the quantitation of muramic acid, a marker of bacterial peptidoglycan as trimethylsilyl (TMS ) derivatives using GC/MS method. The described methods are fast and simple, and can be applied for monitoring of microbial contamination directly, without prior culturing, in complex environmental samples. This method can also be applied for testing processes of cleaning and disinfection on packaging materials or on both packaging materials/foodstuffs in order to decrease their microbial load and thus to ensure better shelf-life.

8

Zastosowanie chromatografii gazowej i elektroforezy kapilarnej do analizy napojów orzeźwiających

Wideł D., Oszczudłowski J., Witkiewicz Z.

Aparatura Badawcza i Dydaktyczna

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2012

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T. 17, nr 3

79-84

PL

Wykonano analizę wybranych lotnych związków organicznych w czterech napojach orzeźwiających metodą chromatografii gazowej ze spektrometrią mas. Dodatkowo zbadano zawartość wybranych anionów nieorganicznych oraz organicznych we wspomnianych napojach metodą elektroforezy kapilarnej. Lotne związki organiczne wyizolowano z fazy nadpowierzchniowej napojów techniką mikroekstrakcji do fazy stacjonarnej. We wszystkich próbkach wykryto D-limonen, odpowiedzialny za aromat cytrynowy.

EN

Gas chromatography-mass spectrometry method was applied for selected volatile organic compounds analysis of four similar refreshing drinks. The presence of selected inorganic and organic anions in mentioned drinks were additionally determined by capillary electrophoresis method. Solid phase microextraction was applied to isolate volatile organic compounds from drinks head space. D-limonene, responsible of lemon flavour, was determined in all samples.

9

Comparison of headspace solvent microextraction, hydrodistillation solvent microextraction, and solid-phase microextraction for the study of volatile components of Kelussia odoratissima Mozaff. by GC-MS

Hashemi P., Yarahmadi A, Shamizadeh M, Khademi K

Acta Chromatographica

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2012

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Vol. 24, no. 1

97--109

EN

Kelussia odoratissima Mozaff. is a wild and endangered endemic plant found only in limited areas of central Zagros mountains, Iran. Three microextraction methods, that is, headspace solvent microextraction (HS-SME), hydrodistillation solvent microextraction (HD-SME), and solid-phase microextraction (SPME), and a conventional hydrodistillation method were used and compared for the extraction and gas chromatography- mass spectrometric (GC-MS) analysis of volatile components of the plant. In the HS-SME and HD-SME methods, a suspended n-heptadecane microdroplet was used for the extraction from the sample headspace, while in the SPME method, a PDMS fiber was applied. The highest extraction efficiency was obtained for the SPME method, with the highest number of identified components and best precision. As a consequence, the SPME method was used for the comparison of the volatile components of seeds, leaves, and pedicles of K. odoratissima collected from three different regions. One of the major components of the plant was butyl phthalide. The levels of this compound in the extractions from leaves, pedicles, and seeds were 34.1, 23.8, and 12.9%, respectively. The results also showed considerable variation between the volatile components of the samples collected from different areas.

10

Geochemical features of fossil fuel contaminants found in urban wastes (Siemianowice Śląskie, Poland)

Wojtoń A., Fabiańska M.

Mineralogia

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2011

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Vol. 42, iss. 1

19--32

EN

In sludge samples collected in the "Centrum" wastewater treatment plant in Siemianowice Śląskie, Poland, the composition of aliphatic- and aromatic hydrocarbons and polar compound fractions were investigated by gas chromatography-mass spectrometry (GC-MS). Samples collected in accordance with Polish standards were extracted, the extracts were separated into fractions with preparative thin layer chromatography (TLC), which next were investigated by GC-MS. The following compound groups of the geochemical origin were identified: n-alkanes in the range of n-C14 to n-C.39, acyclic isoprenoids (mainly pristane and phytane), steranes, tri- and pentacyclic triterpanes. Based on the distribution of biomarkers and their parameters, it was established that the dominant component of extractable organic matter in sluge is petroleum material of an unspecified origin. Its geochemical features indicate that its most likely source was crude oil (or its products) of a relatively high degree of thermal maturity (catagenic stage of thermal evolution corresponding to vitrinite reflectance 0.7-0.8%). Aromatic hydrocarbons probably originated from petroleum also, though some of them can be attributed to the products of combustion or to sources such as bituminous coals, the ash from coal/biofuel combustion or coal wastes stored nearby.

11

Integrated approach - the effective tool for pollution level control of sediments from Lake Turawskie

Franke S., Sagajdakow A., Wolska L., Namieśnik J.

Ecological Chemistry and Engineering. S

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2009

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Vol. 16, nr 3

313-321

EN

Lake Turawskie, an artificial reservoir on the Mała Panew River, was selected for a preliminary project financed by the Province Environment Protection Fund in Opole (Poland). The aim of this project was to assess the ecological state of this lake, and testing aqueous extracts from bottom sediments for toxic effects was one of the approaches. The toxicity of aqueous extracts of sediments was assessed applying the measurements of bioluminescence inhibition of Vibrio fischeri bacteria. In addition, analyses of organic compounds in sediment extracts obtained by aqueous and subsequent dichloromethane extraction were performed. The chromatograms from coupled gas chromatography - mass spectrometry (GC/MS) indicated a very complex composition of the examined dichloromethane extracts. The GC/MS non target screening analyses were conducted on a set of selected samples as an attempt to identify chemical substances responsible for the observed toxicity effects. However, the differences in sediment toxicity were not reflected in the results of the GC/MS analyses and it was not possible to correlate sediment toxicity with specific organic compounds.

PL

Turawski zbiornik retencyjny został wytypowany do projektu pilotażowego spośród 14 obiektów zlewni Odry w ramach programu: "Stan ekologiczny jezior zaporowych w dorzeczu Odry i działania na rzecz jego poprawy". Celem projektu jest ocena stanu ekologicznego Jeziora Turawskiego dla uzyskania niezbędnych informacji mających służyć do zaprojektowania i wyboru metody jego remediacji. Jezioro Turawskie jest nizinnym zbiornikiem retencyjnym na rzece Mała Panew. Potencjalnymi źródłami zanieczyszczeń wód Małej Panwi jest działalność rolnicza, ścieki komunalne i odpady przemysłowe. Działalność przemysłowa (również w przeszłości) w zlewni rzeki obejmuje między innymi: eksploatację . hutnictwo srebra, cynku i ołowiu, produkcję celulozy, produkcję chemiczną w (tym barwników dla przemysłu włókienniczego i materiałów wybuchowych), hutnictwo żelaza oraz hutnictwo szkła. Celem przedstawionych badań była ocena poziomu zanieczyszczenia osadów jeziora oraz poszukiwanie korelacji pomiędzy oszacowaną toksycznością a wynikami analiz chemicznych (na przykładzie wybranych próbek). W ekstraktach z próbek osadów oznaczano między innymi związki organiczne. Do izolacji związków o charakterze polarnym zastosowano ekstrakcję rozpuszczalnikiem (dichlorometan). Do rozdzielenia związków wykorzystano chromatografię gazową, a następnie analizowano je w detektorze spektrometrii mas (GC-MS; tryb pracy: SCAN). Badania ekotoksykologiczne przeprowadzono, korzystając ze standardowego testu bakteryjnego MicrotoxŽ wykorzystującego zjawisko bioluminescencji bakterii z rodzaju przecinkowców (gatunek Vibrio fischeri).

12

Triterpenes in traditional and supercritical-fluid extracts of Morus alba leaf and stem bark

Böszörményi A, Szarka Sz., Héthelyi É, Gyurján I, László M, Simándi B, Szőke É, Lemberkovics É

Acta Chromatographica

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2009

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Vol. 21, no. 4

659--669

EN

Our objectives were to establish a GC method capable of quantitative analysis of terpenoids without derivatisation and to examine the amount of β -sitosterol extracted from Morus alba L. leaf and stem bark by use of traditional organic solvent extraction and supercritical-fluid extraction (SFE). To measure β -sitosterol content without derivatization, GC-FID was used with 5- α -cholestan-3-one as internal standard. To identify terpenoid constituents, GC-MS was used; β -sitosterol, phytol, lanost-7-en-3-on, α -amyrin, β -amyrin, and lupeol were identified. We established that for Morus leaf the best SFE method for β -sitosterol was pilot scale SFE; the β -sitosterol content of this extract was higher than that of the hexane solvent extract. Among analytical SFE conditions, 200 bar for 90 min and 300 bar for 60 min resulted in extraction of the most β -sitosterol. For mulberry stem bark, solvent extraction with hexane and SFE at 400 bar and 40°C for 60 min proved the best methods.

13

Preparation of wastewater samples for GC-MS analysis of PAHs

Włodarczyk-Makuła M.

Archives of Environmental Protection

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2008

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Vol. 34, no. 3

259-264

EN

Standard EPA Method 8310 recommends the use of liquid chromatography with fluorescence detection for the determination of PAH compounds. Taking into consideration the advantages of gas chromatography - mass spectrometry (GC - MS) it is important to carry out investigations to optimise wastewater preparation for qualification and quantification of PAHs using this method. The aim of the investigation was to verify the procedure of wastewater preparation for PAHs analysis using GC-MS. The method was evaluated based on experimental recovery values of individual compounds. The experiments were carried out using both raw and biologically treated wastewaters collected from a municipal treatment plant.

14

Investigation of pyrolysis behavior of fenoxycarb using PY-GC-MS assisted with chemometric methods

Wang G., Hou Z., Sun Y., Liu Y., Xie B., Liu S.

Chemia Analityczna

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2007

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Vol. 52, No. 1

141-156

EN

Fenoxycarb is a carbamate-type insect growth regulator. To investigate its pyrolysis behavior, it was pyrolysed at 600°C, 750°C and 9QQ°C. Pyrolysate was directly subjected to GC-MS analysis. The separated components were identified using probability-based matching procedure followed by correlation of the boiling point- Lee retention index. It has been shown that (Py-GC-MS) pyrolysis assisted with chemometric methods is an effective technique for the investigation of carbamate pesticide pyrolysis, 84 components were determined in pyrolysate, which included the products of thermal decomposition of fenoxycarb, a variety of monoaromatics, polycyclic aromatic hydrocarbons, and other oxygenous or nitrogenous compounds. Determination of the components of pyrolysates may provide useful information for understanding of the pyrolysis mechanism of fenoxycarb and other carbamate pesticides.

15

Determination of volatile components of pine needles from Pinus densiflora S. using solid phase trapping extraction-gas chromatography -mass spectrometry

Lee J. G., Lee C. G., Kwag J. J., Rhee M. S., Buglass A. J., Lee G. H.

Chemia Analityczna

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2007

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Vol. 52, No. 3

411-422

EN

Volatile components of the needles from Pinus densiflora were studied by gas chromato-graphy-mass spectrometry (GC-MS) applying a new solid phase trapping extraction (SPTE) method and a Magic Chemisorber™ (MC). In SPTE, a titanium tube of the surface covered with poly dimethyls i loxane (PDMS) was used. The efficiency of SPTE method was studied by varying extraction temperature (20, 35, 50 and 65°C) at a fixed extraction time of 20 min. The optimum temperature was 35°C. Extraction efficiency of SPTE method was compared to that of SPME method under the same optimum conditions (extraction time 20 min, extraction temperature 35°C). For SPTE, extraction efficiency of hydrocarbons increased with the increasing temperature. However, alcohols and carbonyls, such as 2-hexenal, 1-hexanol, and 65-3-hexenol were extracted less efficiently at higher temperatures. Fatty acids, such as capric, lauric, myristic, pentadecanoic, and paimitic were identified by SPTE. but not by SPME under the same (SPTE optimum) experimental conditions.

PL

Związki lotne w igłach sosny Pinus densiflora S. oznaczano za pomocą chromatografii gazowej sprzężonej ze spektrometrią mas. Do oznaczeń zastosowano nową metodę ekstrakcji - półłapkowanie na fazie stałej (SPTE) i Magie ChemisorberTM (MC). W metodzie SPTE użyto rurki tytanowej, której powierzchnię pokryto polidimetylosiloksanem (PDMS). Badano wydajność metody SPTE w funkcji temperatury (20, 35, 50 i 65°C) przy stałym czasie ekstrakcji (20 min). Jako optymalną temperaturę przyjęto 35°C. Wydajność metody SPTE porównano z wydajnością metody SPME (mikroekstrakcja) stosując te same optymalne warunki. W metodzie SPTE wydajność ekstrakcji węglowodorów rosła wraz z temperaturą. Jednakże alkohole i związki karbonylowe, takie jak: 2-heksanol, 1-heksanol i as-3-heksanol ekstrahowały się w wyższych temperaturach z mniejszą wydajnością. Kwasy tłuszczowe takie jak: kaprowy, laurowy, mirystynowy, pentadekanowy i palmitynowy można było zidentyfikować metodą SPTE, natomiast metoda SPME nie dawała możliwości ich identyfikacji w warunkach optymalnych dla metody SPTE.

16

Soxhlet and accelerated solvent extractions of polycyclic aromatic hydrocarbons from date palm samples

Helaleh M. I. H., Al-Omair A., Nisar A., Gevao B., Ballam Z.

Chemia Analityczna

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2006

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Vol. 51, No. 2

229-239

EN

The content of polycyclic aromatic hydrocarbons in the date palm samples purchased at the Kuwait market has been analysed. Soxhlet extraction and accelerated solvent extraction followed by gas chromatography with ion trap mass spectrornetry have been applied for the determination of polycyclic aromatic hydrocarbons in date palm. Samples extracts were passed through a silica SPE cartridge packed with florisil and sodium sulfate for the clean-up. Limits of quantitation were lower than 2 μg L-1 for most of PAHs and an acceptable precision was achieved. The optimised procedure was successfully applied to the extraction and determination of PAHs in different date palm samples. Reliability of the method was evaluated by spiking palm date samples with different amounts of PAHs and calculating percentage recoveries. They ranged between 75.8% and 86.7% for Soxhlet extraction and between 79.4% and 85.9% for accelerated solvent extraction, depending on the molecular mass of PAHs.

PL

Analizowano zawartość wielopierścieniowych węglowodorów aromatycznych (WWA) w daktylach sprzedawanych w Kuwejcie. W WAekstrahowano z daktyli za pomocą aparatu Soxhleta lub przyspieszonej ekstrakcji rozpuszczalnikiem, a następnie analizowano przy użyciu chromatografii gazowej ze spektrometrią mas. Ekstrakty oczyszczano za pomocą kwarcowych kolumienek do ekstrakcji, wypełnionych florisilem i siarczanem sodu, w układzie ciecz-ciało stałe. Oznaczalność większości WWA, przy zadowalającej precyzji, była niższa niż 2 μg L-1. Zoptymalizowaną procedurę z powodzeniem zastosowano do ekstrakcji ioznaczania WWA w próbkach różnych daktyli. Wiarygodność metody oceniono przez dodanie do próbek daktyli różnych ilości WWA i oznaczenie odzysku. Odzysk zawiera! się, w zależności od masy cząsteczkowej WWA, w granicach od 75,8% do 86,7% w przypadku ekstrakcji w aparacie Soxhleta i w granicach od 19,4% do 85,9% w pr/ypadku przyspieszonej ekstrakcji rozpuszczalnikiem.

17

HS-SPME-GC-MS analysis of organic compounds emitted from poly(methyl methacrylate)

Rogalewicz R., Voelkel A.

Chemia Analityczna

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2005

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Vol. 50, No. 6

991-1006

EN

Volatile organic compounds generated during thermal decomposition of poly (methyl meth-aery late) (PMMA) were analysed by capillary gas chromatography with mass spectrometry detection (GC-MS). Decomposition process of PMMA was carried out for 10 min in the closed cell at 100, 150,200,250, and 280°C. Volatile compounds emitted from poly(methyl methacrylate) were trapped onto the SPME (solid phase microextraction) polymeric fibre and further analysed by GC. Qualitative analysis has shown that the emitted vapours are the complex mixture of decomposition products of poly (methyl methacrylate), e.g. methyl methacrylate and several polymer-accompanying compounds as the initiator (2,2'-azobis-(2-methylpropionitrile) - AIBN). chain regulator (dodecanethiol), inhibitor (Topanol OC), and plasticizers (phthalates). Our studies covered identification of the compounds evolved during decomposition of poly(methyl methacrylate) into the headspace phase, optimisation of HS-SPME conditions, e.g. fibre coating, desorption time and temperature, as well as of the conditions of PMMA decomposition, e.g. decomposition time and temperature, or the sample mass. We accomplished also quantitative analysis of main products of PMMA decomposition and of the accompanying compounds present in the studied material.

PL

Lotne związki organiczne powstałe w trakcie rozkładu termicznego poli (metakrylanu metylu) (PMMA) analizowano techniką kapilarnej chromatografii gazowej sprzężonej ze spektrometrią mas (GC-MS). Termiczny rozkład PMMA przeprowadzono w zamkniętym naczyniu przy 100,150, 200,250 i 280°C przez l0 minut. Lotne związki uwalniane z poli (metakrylanu metylu) były zatrzymywane na polimerowym włóknie SPME (mikroekstrakcja do fazy staiej) i dalej analizowane techniką GC. Analiza jakościowa pokazała, że emitowane pary sązfożonąmieszaninąproduktów rozkładu poli (metakrylanu metylu), wśród których zidentyfikowano np.: metakrylan metylu i kilka dodatków stosowanych przy polimeryzacji włącznie 2 inicjatorem (azodiizobulyronitrylem -AiBN). regulatorem długości iańcucha (dodekanotiolem). inhibitorem (Topanolem OC) i plastyfikatorami (ftalanami). W naszych badaniach zidentyfikowaliśmy związki uwalniane podczas rozkładu poli (metakrylanu metylu) w fazie nadpowierzchniowej oraz optymalizowaliśmy warunki HS-PME. jak np.; rodzaj pokrycia włókna, czas i temperaturę desorpcji, oraz warunki termicznego rozkładu PMMA, jak np.: czas i temperatura i masa próbki. Nasze badania miały umożliwić przeprowadzenie analizy ilościowej głównych produktów rozkładu PMMA i obecnych w badanym materiale dodatków.

18

Bilans WWA w miejskiej oczyszczalni ścieków [komunikat]

Włodarczyk-Makuła M.

Archiwum Ochrony Środowiska

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2004

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Vol. 30, no. 4

119--127

PL

W pracy przedstawiono wyniki oznaczeń jakościowo-ilościowych 16 WWA (rekomendowanych przez EPA) w ściekach i osadach ściekowych z miejskiej oczyszczalni ścieków. Na podstawie pomiarów wielkości przepływów ścieków i osadów obliczono ładunki WWA w ściekach surowych, po mechanicznym i biologicznym oczyszczaniu oraz ładunki tych związków w osadach ściekowych: surowych, przefermentowanych i odwodnionych. Na podstawie otrzymanych wyników można stwierdzić, że mechaniczno-biologiczne procesy oczyszczania ścieków pozwalały na obniżenie ładunku WWA w ściekach o 85%. Mimo to dobowy ładunek tych związków wprowadzany do środowiska był wysoki i stanowił 37% wprowadzanego do oczyszczalni; ze ściekami oczyszczonymi wynosił średnio 46 g/d (w tym związki kancerogenne stanowiły 12%), z osadami odprowadzanymi z oczyszczalni i kierowanymi na składowisko (osady z piaskownika i odwodnione) wynosił średnio 68 g/d (w tym związki kancerogenne stanowiły 17%).

EN

Sewage and sewage sludge from municipal wastewater treatment plant were analyzed for 16 EPA-PAH. The measurements were conducted to investigate the effect of different treatment stages on PAH content in wastewater and sewage sludge. PAH loads in influent, mechanically and biologically treated sewage, as well as in raw, digested and dewatered sludge were calculated. Mechanical and biological treatment was found to remove 85% of PAH from the influent. Despite of this a daily PAH load introduced into environment was high, and reached 37% of the PAH load in the influent. In sewage it was equal to 46 g PAH/d, with carcinogenic PAH content of 12%. In waste sludge (filter pressed sludge and sand from sand trap) PAH total load reached 68 g/d with 17% of carcinogenic PAH.

19

Przemiany WWA w osadach ściekowych poddanych sztucznemu działaniu promieniowania UV

Włodarczyk-Makuła M., Janosz-Rajczyk M., Wiśniowska E., Koćwin K.

Inżynieria i Ochrona Środowiska

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1999

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T. 2, nr 3/4

391-401

PL

Przedstawiono wyniki badań zmian WWA w osadach ściekowych narażonych na działanie promieniowania UV. Analizowano 16 WWA wg listy EPA. W osadach odwodnionych pobranych z oczyszczalni ścieków stwierdzono obecność 10 WWA w ilości sumarycznej 79,8 žg/kg s.m. W osadach naświetlanych UV stwierdzono wzrost zawartości sumy WWA o 116% i wzrost sumy kancerogennych związków o 1030%. W próbie porównawczej przechowywanej w warunkach laboratoryjnych odnotowano spadek zawartości WWA o 32,5%. Wyniki badań wskazują, że podczas składowania osadów może nastąpić chwilowy wzrost koncentracji zawartych w nich WWA.

EN

This paper reports the PAHs concentration changes in filter-pressed sewage sludge exposed to UV rays. Between radiation exposures sludge was stored in daylight. 16 EPA-PAHs have been analysed. In filter-pressed sludge 10 of 16 analysed PAHs were present, including two carcinogenic congeners (benzo(a)anthracene and chrysene). UV radiation increased concentration of total PAHs by 116% (from 79.80 to 172.87 žg/kgd.m) and increased carcinogenic PAHs concentration by 1030% (from 4.84 to 54.75 žg/kgd.m). The conclusion is as follows: during deposition of filter-pressed sewage sludge on disposal sites of sewage treatment plants temporary concentrations of PAHs may occur due to the fact that UV radiation can cause PAHs desorption from complex organic matrixes and microbial cells after their destruction