Monitoring of the Sources of Environmental Pollution with Crude Oil

The possibility of preliminary identification of sources of environmental pollution with crude oil was studied by IR Fourier spectroscopy, gamma-ray spectrometry, chromatography-mass spectrometry, and capillary gas-liquid chromatography with oil samples from six fields of the Khanty-Mansi Autonomous District and samples of soil and ground water contaminated with these oils.     

Quantification of Petroleum Products in Soil of Natural Moisture Content by IR Spectrometry

Journal of Analytical Chemistry - A method is proposed for determining petroleum products (PPs) in soil of natural moisture content by IR spectrometry. The results obtained by the proposed IR...     

Reactions of 9-alkyl-3-aminocarbazoles with ethyl-3-oxo-butanoate and identification of the products obtained

The reactions in benzene of 9-alkyl-3-aminocarbazoles with ethyl-3-oxobutanoate yielded ethyl-3-[(9-alkyl-9H-carbazol-3-yl)amino]but-2-enoate condensation products or N-(9-ethyl-9H-carbazol-3-yl)-3-oxobutanamide acylation products. The condensation products were cyclized to the corresponding 4,7-dihydro-pyrido[2,3-c]-carbazol-1-ones upon heating in mineral oil at 240-250 degrees C. The structures of the synthesized compounds were investigated by IR, mass spectrometry, (1)H- and (13)C-NMR spectroscopy and MM2 molecular mechanics and AM1 semi-empirical quantum mechanical methods.     

The determination of petroleum hydrocarbons in soil using a miniaturized extraction method and gas chromatography

A gas chromatographic (GC) method for the determination of petroleum hydrocarbons (PH) in the boiling range from 175°C to 525°C (C₁₀?C₄₀ alkane) in soil was evaluated. The extraction was carried out using minimal amounts of acetone and heptane, prior to a clean up with silica gel. The extraction procedure was tested by means of standard solutions of petroleum products and soil samples. The clean up procedure did not have any significant effect on the amounts of petroleum hydrocarbons present and hydrocarbons of natural origin were removed effectively. The recovery of the extraction and clean up procedure for petroleum products in soil was greater than 90%. The standard deviation for the repeatability was estimated to be less than 10% based on multiple analyses of homogenized soil samples. The detection limit for soil was determined to be 10 mg/kg dry matter. Comparing the GC method with the widely used infrared spectrometry (IR) method in combination with a Soxhlet-extraction using Freon-113, the results obtained are equivalent.     

Cu determination in crude oil distillation products by atomic absorption and inductively coupled plasma mass spectrometry after analyte transfer to aqueous solution

Cu was determined in a wide range of petroleum products from crude oil distillation using flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICP-MS). Different procedures of sample preparation were evaluated: (i) mineralization with sulfuric acid in an open system, (ii) mineralization in a closed microwave system, (iii) combustion in hydrogen–oxygen flame in the Wickbold's apparatus, (iv) matrix evaporation followed by acid dissolution, and (v) acidic extraction. All the above procedures led to the transfer of the analyte into an aqueous solution for the analytical measurement step. It was found that application of FAAS was limited to the analysis of the heaviest petroleum products of high Cu content. In ICP-MS, the use of internal reference method (with Rh or In as internal reference element) was required to eliminate the matrix effects in the analysis of extracts and the concentrated solutions of mineralized heavy petroleum products. The detection limits (in original samples) were equal to, respectively, 10, 86, 3.3, 0.9 and 0.4 ng g^− 1 in procedures i–v with ETAAS detection and 10, 78, 1.1 and 0.5 ng g^− 1 in procedures i–iii and v with ICP-MS detection. The procedures recommended here were validated by recovery experiments, certified reference materials analysis and comparison of results, obtained for a given sample, in different ways. The Cu content in the analyzed samples was: 50–110 ng g^− 1 in crude oil, < 0.4–6 ng g^− 1 in gasoline, < 0.5–2 ng g^− 1 in atmospheric oil, < 6–100 ng g^− 1 in heavy vacuum oil and 140–300 ng g^− 1 in distillation residue.     

Dynamic extraction in microcolumn as a method for the sample preparation of oil-contaminated soils

A method is proposed for the sample preparation of oil-contaminated soils based on the dynamic extraction of petroleum products in a microcolumn of special design. By an example of the analysis of GSO (State Standard Sample) 8673-2005 of an oil-contaminated soil and model soil samples, a comparative evaluation of the efficiency of dynamic and batch (shaking in a shaker) extraction for the sample preparation of oil-polluted soils is carried out. The concentration of petroleum products in the extracts was determined by IR spectrometry. It was shown that the recovery of petroleum products into carbon tetrachloride in extraction in a microcolumn is, on the average, 50% higher than that in mixing the sample and reagent in a shaker. The rapid and efficient extraction of petroleum products in a microcolumn is possible because of dynamic extraction occurring at a constant renewal of the reagent.     

Thermal decomposition of basic aluminium potassium sulphate. Part I. Stages of decomposition

The stages of thermal decomposition of basic aluminium potassium sulphate were studied with the use of differential thermal analysis (DTA), thermogravimetry (TG), mass spectrometry (MS), IR spectroscopy (IR), and X-ray diffraction phase analysis (XRD). The individual stages of the decomposition were determined and both solid and gaseous products of the dissociation were identified. On the basis of spectrometric data and thermodynamic calculations the possibility of the occurrence of the SO in the gaseous reaction products is discussed.     

几个新型呋喃氨基腈衍生物的合成及抗菌活性

用5-甲基-4-乙氧羰基呋喃氨基腈与芳醛反应制得Schiff碱,再采用NaBH4还原Schiff碱,得到3个新型5-甲基-4-乙氧羰基呋喃氨基腈衍生物.利用核磁共振谱(1H NMR)、红外光谱(IR),质谱(EI-MS)表征了产物的结构;并初步测定了产物的抗菌活性.结果表明,目标化合物的抗菌活性一般.     

墓头回挥发油化学成分的研究

墓头回也叫箭头风,为败酱科植物异叶败酱[Patrinia Heterophylla Bge.]和糙叶败酱[PatriniuScabra Bge.]的根,能治伤寒、温疟,妇女崩中,赤白带下,跌打损伤等疾病,对艾氏癌细胞有抑制及伤害作用。墓头回挥发油的化学成分尚未见报道。本文采用毛细管气相色谱-质谱法对墓头回挥发油的化学成分进行了研究。色谱分离出50多个组分,质谱确定了其中30个组分的化学成分,占总色谱流出峰面积的56.32％。此外还有10个结构尚未完全确定的倍半萜烯,占色谱总流出峰面积的8.50％;3个倍半萜烯醇,占色谱总流出峰面积的4.71％;2     

Formation of volatile copper carbonyl during the preparation of copper nanoparticles in the copper acetate hydrate-polyacrylonitrile heterogeneous system under IR radiation

The products of reactions induced by IR heating in the copper acetate hydrate-polyacrylonitrile system and the intermediate Cu compounds formed during the preparation of Cu nanoparticles were studied by powder X-ray diffraction, atomic absorption spectroscopy, mass spectrometry, and IR spectroscopy. Mass spectra of the volatile products formed from the nanocomposite contain peaks typical of the CuCO molecular ion. After treatment of the nanocomposite at 500°C, the copper content in the composite decreased 10-fold as a result of evolution of volatile CuCO.     

Monitoring the synthesis of new pitches from coal tar and its fractions by chromatography and related techniques.

The aim of this paper is to study the applications of chromatography and related techniques in the transformation of coal-derived products into pitches for specific uses. Anthracene oil, tar and pitch were thermally treated in the presence of air (and sulfur in the case of anthracene oil) in order to cause the polymerization/condensation of their components. The evolution of the components of the parent materials during the treatments was monitored by gas chromatography-mass spectrometry, gas chromatography-atomic emission detection, probe mass spectrometry and size-exclusion chromatography. From the results obtained, possible mechanisms for the transformation of coal-derived products into new pitches were established.     

Novel Route to 4‐(Adamantan‐1‐yl)quinoline Derivatives Based on the Friedländer Condensation

2,3,4‐Trisubstituted quinolines, substituted with adamantan‐1‐yl or (adamantan‐1‐yl)methyl in the 4‐position, were prepared from the corresponding admantan‐1‐yl 2‐aminophenyl ketones or admantan‐1‐ylmethyl 2‐aminophenyl ketones and ketones with an α‐CH₂ group. These reactions were carried out under neat conditions or in toluene, and the products were obtained in moderate‐to‐excellent yields. The scope and limitations of the examined procedures are discussed. All new compounds are fully characterized by IR and NMR spectroscopy and mass spectrometry. The molecular structures of five new quinolines, obtained via single‐crystal X‐ray diffraction analyses, are discussed.     

Etude de L'oxydation de Polyethylenes Par Analyse Thermique Identification des produits de dégradation par infra-rouge

The oxidation of pure and recycled polyethylene samples was studied by thermal analysis (DTA-TG-DSC): presence of two exothermic peaks and mass loss. The thermo-oxidation products, containing C-O and C=O links, were identified by IR spectrometry and GC-MS spectrometry. The oxidation is easier from low to high density polyethylene. This revised version was published online in July 2006 with corrections to the Cover Date.     

Assessment of priority pesticides,degradation products,and pesticide adjuvants in groundwaters and top soils from agricultural areas of the Ebro river basin

Gas chromatography-mass spectrometry (GC/MS) was employed for the determination of 30 widely used pesticides including various transformation products and alkylphenols in water and agricultural soils with the aim of assessing the impact of these compounds in agricultural soils and the underlying aquifer. The extraction, clean-up, and analytical procedures were optimized for both water and soil samples to provide a highly robust method capable of determining target analytes at the ppb–ppt level with high precision. For water samples, different solid-phase extraction cartridges and conditions were optimized; similarly, pressurized liquid extraction conditions were tested to provide interference-free extracts and high sensitivity. Instrumental LODs of 3–4 pg were obtained. The multi-residue extraction procedures were applied to the analysis of groundwaters and agricultural soils from the Ebro river basin (NE Spain). Most ubiquitous herbicides detected were triazines but some acetanilides and organophosphorus pesticides were also found; the pesticide additive tributylphosphate was found in all water samples. Levels varied between 0.57 and 5.37 μg/L in groundwater, whereas nonylphenol was the sole compound detected in soil. Alkylphenols are used as adjuvants in pesticide formulations and are present in sludges employed as soil fertilizers. Occurrence was found to be similar to other environmental studies.     

Reaction of di-2-chloroethyl 2-chloroethanephosphonate with potassium methacrylate

Reaction of di-2-chloroethyl 2-chloroethanephosphonate with potassium methacrylate at various component ratios was studied with the aim to prepare products containing methacrylate and vinyl functional groups. The structures of the compounds obtained were examined by 1H NMR and IR spectroscopy and by gas chromatography-mass spectrometry.     

Synthesis of substituted anilides of the alkaloid cytisine and molecular structure of <Emphasis Type="Italic">N</Emphasis>-(2′,6′-dichloro-4′-nitrophenyl)-2-<Emphasis Type="Italic">N</Emphasis>-cytisinoacetamide

Anilides of cytisinylacetic acid were synthesized by reaction of the alkaloid cytisine with 2-bromo-N-(2,6-dihalo-4-nitrophenyl)acetamides. The compositions and structures of the products were confirmed by IR and PMR spectroscopy, mass spectrometry, and x-ray structure analysis.     

芸香草精油化学成分的研究

芸香草(Cymbopogon distans(Nees)W.wats)系多年生禾本科香茅属植物,分布于我国甘肃、陕西和西南及印度等地~[1].芸香草含芳香油,可提制香精油,是香料及化妆品工业的重要原料,芸香草还可入药,有较大的开发价值.Melkani等~[2]曾指出,不同地区生长的芸香草精     

Synthesis and properties of aminomethoxy derivatives of 1-(butylsulfanyl)pentane

New aminomethoxy derivatives of 1-(butylsulfanyl)pentane have been synthesized. The structure of the synthesized compounds was studied by elemental analysis, IR and ¹Н NMR spectroscopy, and mass spectrometry. Some specimens of the synthesized compounds were tested as antimicrobial additives to lubricant oil, and as aseptic compounds against bacteria and fungi.     

Proficiency test on the determination of mineral oil from polluted soils

Mineral oil products are abundant sources of environmental contamination. A Finnishproficiency test was carried out to investigate the quality of data provided in an analysis of mineral oil in polluted soils. The homogeneity and stability of the samples were tested. The calculated concentration or the median value of the results was used as the assigned value because of the unavailability of certified reference materials (CRMs). The samples were analysed using an infrared spectroscopy (IR) or gas chromatography (GC) procedure. Even if the participating laboratories had little experience with GC, the results were promising. Hence, the GC procedure will replace IR as the new ISO standard (ISO/DIS 16703) in the near future in many Finnish environmental laboratories. There is a need for CRMs for the determination of mineral oil using the GC method due to common contamination problems caused by mineral oil. Received: 9 December 2001 Accepted: 14 February 2002