Bio-regeneration of p-complexation desulfurization adsorbents

More and more stringent regulations of gasoline and diesel oil were proposed with the awareness of environmental protection. Hydrodesulfurization (HDS) is a conventional method to remove sulfur compounds for industrial purpose. The main drawbacks of this …     

Overloaded elution band profiles of ionizable compounds in reversed‐phase liquid chromatography: Influence of the competition between the neutral and the ionic species

The parameters that affect the shape of the band profiles of acido‐basic compounds under moderately overloaded conditions (sample size less than 500 nmol for a conventional column) in RPLC are discussed. Only analytes that have a single pK_a are considered. In the buffer mobile phase used for their elution, their dissociation may, under certain conditions, cause a significant pH perturbation during the passage of the band. Two consecutive injections (3.3 and 10 μL) of each one of three sample solutions (0.5, 5, and 50 mM) of ten compounds were injected on five C₁₈‐bonded packing materials, including the 5 μm Xterra‐C₁₈ (121 Å), 5 μm Gemini‐C₁₈ (110 Å), 5 μm Luna‐C₁₈(2) (93 Å), 3.5 μm Extend‐C₁₈ (80 Å), and 2.7 μm Halo‐C₁₈ (90 Å). The mobile phase was an aqueous solution of methanol buffered at a constant _W^WpH of 6, with a phosphate buffer. The total concentration of the phosphate groups was constant at 50 mM. The methanol concentration was adjusted to keep all the retention factors between 1 and 10. The compounds injected were phenol, caffeine, 3‐phenyl 1‐propanol, 2‐phenyl butyric acid, amphetamine, aniline, benzylamine, p‐toluidine, procainamidium chloride, and propranololium chloride. Depending on the relative values of the analyte pK_a and the buffer solution pH, these analytes elute as the neutral, the cationic, or the anionic species. The influence of structural parameters such as the charge, the size, and the hydrophobicity of the analytes on the shape of its overloaded band profile is discussed. Simple but general rules predict these shapes. An original adsorption model is proposed that accounts for the unusual peak shapes observed when the analyte is partially dissociated in the buffer solution during its elution.     

Headspace SPME–GC Method for Acetone Analysis and its Biomedical Application

A new method for extraction and analysis of acetone in human urine based on headspace solid phase microextraction using a mixture of activated carbon and zeolite as sorbents in a PVC matrix coated on a silver wire and its application to the determination of ketone bodies is described. Unlike commercial fibers, which are coated on fused silica, the coating adheres strongly to the silver wire and is thermally stable up to 250 °C. After optimization of coating composition and microextraction conditions the fiber was used for the analysis of acetone in human urine.     

A Monte Carlo simulation of the heterogeneous adsorption of hydrogen ions on metal oxides: Effect of inert electrolyte

Charging of the surface of an oxide caused by the adsorption of hydrogen ions and ions of inert 1:1 electrolyte was investigated by using grand canonical Monte Carlo simulation technique. In particular, adsorption isotherms of protons as well as of ions of the electrolyte together with the resulting charge density of the surface were obtained for different system parameters. Also, the effect of the surface energetic heterogeneity and the concentration of the background electrolyte on the isotherms and the charge density curves was examined. Furthermore, lateral interactions in the mixed adsorbed phase were taken into account in the modeling of the system behavior. The obtained results, in general, suggest that the three factors mentioned above may have substantial influence on the charging mechanism at the liquid/oxide interface.     

固定化单宁对酒类营养成分的吸附性能研究

采用固定化单宁对酒中可能存在的营养成分蛋白质、氨基酸、糖类、有机酸、乙醇和铁离子等进行吸咐试验。结果表明：固定化单宁对不同营养成分的吸附率差别明显，它通过氢键和疏水作用对蛋白质有较大的吸附率，通过多个酚羟基与中心铁离子形成螯合物而对其有较大的吸附率，对氨基酸、糖、有机酸和乙醇等营养成分或风味物质吸附率不大，固定化单宁可以作为一种较为理想的酒类处理剂。     

Determination of styrene in olive oil by an automatic purge-and-trap system coupled to gas chromatography-mass spectrometry

Summary A new gas chromatographic method using an automatic purge-and-trap system coupled to a GC with mass selective detection to analyze styrene at the parts-per-trillions (ng kg^–1) level is described. The method shows a good sensitivity and the detection limit is 10 ng kg^–1 with a relative standard deviation (RSD) of 4.7% for 164 ng kg^–1 styrene in olive oil. This analytical method has been successfully applied to the analysis of styrene in extra-virgin olive oil from the European market.     

Critical evaluation of gas standards based on hydrogen

Summary Six commercial hydrogen standards containing helium, oxygen, nitrogen, methane and carbon dioxide at trace levels were analyzed by gas chromatography, for periods up to 105 days. The concentrations, in the range of 0–120 μmol mol⁻¹, were stable (with the exception of oxygen) but often significantly different from the certified values provided by the suppliers, especially for helium, oxygen and nitrogen. Concurrently, some experiments were carried out to verify the stability of gas mixtures based on hydrogen stored in cylinders submitted to different chemical and physical treatments. The causes that led to the deviations observed, as well as the decreases in oxygen, are discussed. Presented at the 21^st ISC held in Stuttgart, Germany, 15^th–20^th September, 1996.     

Insertion of benzothiazolium compounds into montmorillonite interlayers

Benzothiazolium compounds exhibit pronounced antimicrobial activities and stimulation effects on plant growth. When applied to fields they can pollute soil colloids. In contact with the soil they can potentially interact with a clay fraction giving rise to clay organocomplexes. Model intercalation complexes were prepared using monoionic montmorillonite and a variety of water-soluble benzothia zolium salts. It was found that the adsorption into the silicate interlayer space proceeds via a cation exchange process. Substantial differences were observed in the extent of the reaction between non-substituted andN-substituted species. The sulphur atoms present in the benzothiazolium molecules repel the surface oxygen atom: this is considered to be the factor responsible for prevention of insertion of the guest cations perpendicular to the layers.     

Automated derivatization for on-line solid-phase extraction-gas chromatography; phenolic compounds

An automated system for derivaatization was coupled on-line with solid-phase extraction-gas-chromatography (SPE-GC). The system was optimized for the determination of phenol and chlorinated phenols in aqueous samples. The test analytes were acetylated with acetic anhydride; proper buffering of the sample was a critical factor. Next, the phenol acetates were enriched on a SPE cartridge and transferred to a GC; two appraoaches were studied. In the first approach, the derivatives were enriched on disposable C18 cartridges (ASPEC type) and desorbed with methylacetate. Aan aliquot of the final eluate was injected on-line the GC by means of a loop-type interface. In the second approach, trace enrichment was performed on 10 × 2 mm i.d. LC-type precolumn packed with polystyrenedivinylbenzene copolymer (PLRP-S) this precolumn was dried with a mitrogen purge and the phenol acetates were desorbed with ethyl acetate which was injectedon-line into the retention gap of the GC under partially concurrent solvent evaporation (PCSE) conditions. The Derivatization-SPE-GC system which was based on the loop-type interface has the advantage of simplicity and easy operation, the main drawback is the impossibility to determine phenol acetates which elute prior to trichlorophenol acetates. With the derivatization-SPE-GC approach using PCSE-based desorption, even the most volatile analyte of the test series, phenol acetate, can be determined successfully. The entire procedure, including the derivatization step, was fully automated and integrated in one set-up. The precision data for the integrated on-line derivatization-SP-FID system were fully satisfactory, with RSD values of 1–12 % at the 1 μg/1 level. When a sample volume of 2.2 ml was analyzed, The detection limits for the chlorinated phenol acetates were in the 0.1–0.3 μg/1 range.