Importance of REP values when comparing the CALUX bioassay results with chemoanalyses results Example with spiked vegetable oils

Differences between chemical activated luciferase gene expression (CALUX) bioassay and chemoanalyses results are observed.This paper shows that calculations of the TEQ values using REP values instead of WHO TEF values give different results. The REP values do affect the results obtained by the CALUX technique. These differences are more marked for the dioxin like PCB compounds (CALUX TEQ values are lower than WHO TEQ values) than for the dioxin compounds (CALUX TEQ values are higher than WHO TEQ values).The CALUX results were compared with the concentrations of the congeners’ spiked into the oil.     

Electron beam crosslinking of non-lead PVC formulations

PVC samples with lead-free and lead-base stabilizer, containing TMPTMA (trimethylolpropane trimethacrylate) as a crosslinker and DOP (2-ethylhexyl phthalate) as a plasticizer, were electron beam treated at different doses (2–200 kGy) and characterized to evaluate crosslinking and other several properties, as a continuation of our previously reported paper, where these PVC formulations, typical for wire and cable applications, underwent gamma irradiation. The PVC was formulated with two different stabilizing systems: Ca/Zn and dibasic lead phthalate for comparison, to use them as jackets for a 22 wire gage (AWG). Small samples of the jacketed wires were irradiated in an industrial Dynamitron electron accelerator for the corresponding doses, along with two dosimetric systems: radiochromic thin film and alanine pellets dosimeters. The maximum dose applied was decided as the crosslinking increased, until the gel content was stable. The dose of 200 kGy was the condition for the highest crosslinking, so most of the wire was irradiated at such dose. Chemical and mechanical evaluations were carried out to the irradiated wire. The results show that 200 kGy was too high dose for the materials, since an important degradation is observed for the Ca/Zn systems. Unfortunately, such dose affects basically to CaZn formulations, which showed much poorer performance than classical lead-containing compositions. The results also indicate that gel content is not the best way of deciding the optimum condition for irradiation.     

Use of NIRS technology with a remote reflectance fibre-optic probe for predicting major components in bee pollen

In the present work, we study the use of near infra-red spectroscopy (NIRS) technology together with a remote reflectance fibre-optic probe for determination of the major components in bee pollen. The method allows immediate control of the bee pollen without prior sample treatment or destruction through direct application of the fibre-optic probe to the sample.The regression method employed was modified partial least squares (MPLS). The calibration results obtained using 45 samples of bee pollen allowed the measurement of protein, moisture, ash, reducing sugars, and pH with multiple correlation coefficients (RSQ) and prediction corrected standard errors (SEPC) of 0.91, 0.56% for protein, of 0.78 and 0.49% for moisture; 0.92 and 0.049% for ash; 0.81 and 1.32 g of glucose/100 g of bee pollen; 0.84 and 0.15 for pH, respectively.The prediction capacity of the pattern was checked by applying it to samples of unknown pollen in external validation.     

Calculation of vertical ionization potentials of difluoramine by perturbation corrections to koopmans' theorem

The vertical ionization potentials of difluoramine are calculated by perturbation corrections to Koopmans' theorem. The calculation shows that difluoraimine has three overlapping bands between 15 and 16 eV. The calculated results compare well with the experimental values. The photoelectron spectrum of difluoramine is compared with that of OF₂ and CH₂F₂.     

Cellulose microfibrils from banana farming residues: isolation and characterization

Cellulose microfibrils have been prepared from banana rachis using a combination of chemical and mechanical treatments. The morphology and structure of the samples were characterized using transmission electron microscopy, atomic force microscopy, and X-ray diffraction. Fourier-transformed infrared spectroscopy (FTIR) was used to characterize the chemical modifications of the samples after each treatment. Suspensions of bundled or individualized 5-nm-wide microfibrils were obtained after homogenization (PH) whereas an organosolv (PO) treatment resulted in shorter aggregates of parallel cellulose microcrystallites. The sharper rings in the X-ray diffraction pattern of the PO-treated sample suggest a higher crystallinity due to a more efficient removal of hemicelluloses and dissolution of amorphous zones by the acid treatment. Both microfibrils and microcrystals prepared by both methods can be used as reinforcing filler in nanocomposite materials.     

Chemical and thermal analysis of the biopolymers in thyme (Thymus vulgaris)

Thyme (Thymus vulgaris) has been known, long time ago, for its aromatic properties. It contains essential oils and polymers such as cellulose (mixture of hemicellulose and cellulose) and lignin. The thyme, studied in this work, was gathered from the same place, in the period from November 1999 to October 2000. The chemical analysis (water, total ash, essential oils, extractive substances, cellulose, holocellulose and lignin) can be used roughly in the characterisation of the four periods that correspond to the four seasons of the year. The cellulose level was found to be more than lignin level in the wet periods (growth of the plant). The opposite was found in the dry periods. The total ash and essential oil levels were found to be high during the period of high pluviometry. The thermal decomposition of cellulose and holocellulose was found to fit well with the first-order kinetics. The activation energy, under air flow, was 185 and 196 kJ mol⁻¹ for cellulose and holocellulose, respectively. The maximum decomposition rate and thermal analysis heating rate of lignin were found to have a direct linear relationship.     

Direct coupling of capillary supercritical fluid chromatography with double-focusing high resolution mass spectrometry

An integral restrictor interface with jet separator for coupling capillary column supercritical fluid extraction – supercritical fluid chromatography with high resolution mass spectrometry (SFE-SFC-MS) has been built and used for the analysis of a fatty acid ester, and of polymer additives with a wide range of masses. The mobile phase used was supercritical carbon dioxide; a flame ionization detector (FID) was used in parallel with the mass spectrometer. Different SFC-MS interface operating conditions, e.g. temperature, restrictor position, flow rate, and sample transfer conditions were optimized to obtain good sensitivity and separation for these applications. In addition, the sensitivity of measurements performed with the direct insertion probe and by SFC-MS interface have been compared.     

土壤环境中铅的化学

论述了环境中铅的背景值、来源、污染、质量标准、化学循环以及环境中铅的烷基化，为铅污染治理提供理论依据。     

Determination of low levels of polymer additives migrating from polypropylene to food simulated liquids by capillary SFC and solvent venting injection

Summary Methods for the determination of specific migration of polymer additives from polypropylene to aqueous acetic acid and isooctane have been studied. The migrants were extracted from aqueous acetic acid and characterized by supercritical fluid chromatography (SFC) with flame ionization detection (FID) and mass spectrometry (MS). The isooctane simulant was concentrated and injected directly into the SFC. Injection of extracts after incubation, using the solvent venting injection technique in the SFC, enabled additive concentrations as low as 10 ppb in 150 ml simulant to be determined, corresponding to a specific migration level of approximately 1 g additive/dm² polymer.     

Potentiometric studies of dithiooxamide with a sulphide-selective membrane electrode

The sulphide-selective electrode is applicable to the determination of dithiooxamide by titration with silver nitrate. The effect of the alkali content of the solutions on the reaction has been studied. The reaction products are silver sulphide, oxalic acid, and nitric acid. If the alkali concentration of the solution is lower than that equivalent to the acid formed during the titration, the amount of sulphide produced by hydrolysis decreases and the equilibrium potential is established more slowly.The determination is rapid and accurate in the presence of 1 M sodium hydroxide.