Microwave (MW) digestion procedures with high sample throughput (simultaneous digestion of 36 or 80 samples) and procedural simplicity (disposable plastic tubes, or re-usable liners with screw-cap) were investigated for their efficiency in routine analyses of biological samples. Different digestion vessel materials were tested for metal leaching/adsorption and thermal resistance: quartz, glass, polyethylene (PE) and polystyrene (PS). For the instrumental quantification of Al, Bi, Cd, Co, Cr, Hg, Mn, Mo, Ni, Pb, Sb, and Tl at ultra-trace levels in urine, serum, and whole blood, sector field inductively coupled plasma mass spectrometry (SF-ICP-MS) was used. The different pretreatment conditions and vessels were evaluated in terms of contamination risk, effective power of detection, accuracy, and precision. Results of analyses of serum, urine and whole blood certified reference materials (CRMs) were fully satisfactory for almost all the analytes. In the case of Hg, Mo, and Tl in serum digested in plastic containers the results were just below the lower limit of uncertainty of the certified range. On the basis of the present data the following MW procedures can be suggested: 1. for urine, digestion with nitric acid at atmospheric pressure in plastic vials; 2. for serum, digestion with nitric acid at atmospheric pressure in glass vessels; and 3. for whole blood, digestion under pressure in quartz tubes.Because of the levels of the procedural blanks, Bi was not measurable at the concentrations expected in human fluids, and Al was accurately detectable in whole blood only. 相似文献
In the framework of the activities of the European Commission Reference Laboratory (CRL) for residues at the Istituto Superiore di Sanità a number of analytical quality control trials on determination of trace analytes are being carried out. As regards trace elements it soon became apparent that the stability of Hg dilute aqueous solutions is rather unsatisfactory. An investigation was thus undertaken to ascertain the conditions under which the concentration of this metal does not appreciably change. Mercury solutions were prepared in high purity deionized water in the concentration range 1–10 ng g−1and the effect of various amounts of HNO3and K2Cr2O7(alone or in combination) was elucidated by measuring the variations with time in the actual concentration of Hg. Determinations were performed by both inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry. Results show that solutions added with 5% (w/w) HNO3and 0.01% (w/w) K2Cr2O7do not undergo any significant alteration in the nominal content of the analyte for at least 1 month. Similar conclusions are reached in the case of solutions enriched in CaCO3, NaCl, NaNO3, KH2PO4, KNO3, and Mg(NO3)2·6H2O to mimic acid digests of meat samples. The improvement ensuing from the adoption of this approach on the performance of the Hg analytical quality control trials is discussed in detail. 相似文献
(NO)2 was detected at ambient temperature in compressed gaseous NO. From the temperature dependence of the UV absorption intensity the enthalpy cha
Abstract
We have shown that van der Waals molecules may be conveniently detected at ambient temperature in a short optical path cell by applying simple high pre 相似文献
In this paper the use of voltage gradient gel electrophoresis (VGGE) in the electrophoretic analysis of apoptotic DNAs is described. The peculiarity of VGGE fractionation in enhancing DNA bands in the gel by reducing their thickness was used to obtain a rapid, more selective and higher-quality electrophoretic fractionation of apoptotic DNA with respect to conventional electrophoresis. The use of VGGE fractionations also allowed a reduced amount of DNA to be used to detect a characteristic apoptotic DNA ladder pattern, in a lower agarose gel concentration, with respect to conventional electrophoretic fractionation 相似文献
Separation of seven organic and inorganic arsenical species, i.e., inorganic arsenite (As III) and arsenate (As V), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), arsenobetaine (AsBet), arsenocholine (AsCh) and p-arsanilic acid (pAs) was carried out by capillary electrophoresis (CE) equipped with one of two different optical path cells, i.e., either the standard detection interface (SDI) or the high sensitive detection cell (HSDC). Separation, identification and quantification of the As species were performed by means of a capillary silica column with an alkaline borate buffer at pH 9.3 and direct UV detection at 192 nm. This methodological approach was tested with the abovementioned types of cells, and the results of the two modes were compared. In both cases, good separation was obtained, and also, repeatability in terms of migration times and peak areas was rather satisfactory. With regard to sensitivity, the HSDC allowed peak areas to be obtained, which were ca. 50 times greater than those afforded by the former cell. This also led to a substantial improvement in the limits of detection (LoDs); by a factor of 9 in the case of AsCh. 相似文献
The interaction of glycyl-phenylalanyl-glycine (GFG) with bilayers formed by cesium perfluorooctanoate (CsPFO) in water was investigated in the isotropic phase by means of 1H NMR and molecular dynamics (MD) simulations. Details on the preferential location of the different residues of GFG were obtained from selective variations of chemical shift with peptide concentration and of line width in the presence of the paramagnetic ion Mn2+. The analysis of 1H NMR spectra recorded at different concentrations and temperatures allowed the association constant and the enthalpy change upon binding to be evaluated. MD simulations highlighted the hydrogen bonds formed between the different GFG functional groups and the micelle. Both NMR and MD gave indications of high affinity of GFG with the micelle, with the N-terminal residue anchoring on the surface via hydrogen bonds with the micelle COO(-) groups. 相似文献
Near-optimal controls are considered for singular problems with a constrained control. These controls result in a higher cost than the optimal cost. Bounds for the additional cost are derived for problems with fixed terminal time or free terminal time and for minimal time problems. An illustrative example is solved of an optimal evasive control of an aircraft against a homing missile. 相似文献
Arterial tissue incompressibility is a common notion used in numerical simulations and analytical studies. However, only a few experimental investigations have been performed to characterize arterial tissue incompressibility. Such studies have used various approaches, ranging from the initial purely mechanical measurements in 1954 to the more recent image-based analyses (2004). The results of these studies are rather diverse because different arteries have been tested (human/dog/mouse, carotid/pulmonary/iliac). This has therefore made accurate comparisons between studies challenging. In the first part of this report, a review of the experimental investigations on the compressibility of arteries is presented, with particular focus on the test rigs that have been used. In the second part of this report, a novel simple apparatus to test samples under physiological or supra-physiological conditions is described. Recommendations for a testing procedure are also provided. Finally, preliminary results on porcine renal arteries indicate significant levels of compressibility are possible (>10 %), thereby suggesting the need for further investigation. 相似文献
The lack of a vascular network and poor perfusion is what mostly prevents three‐dimensional (3D) scaffolds from being used in organ repair when reconstruction of thick tissues is needed. Highly‐porous scaffolds made of poly(L ‐lactic acid) (PLLA) are prepared by directional thermally induced phase separation (dTIPS) starting from 1,4‐dioxane/PLLA solutions. The influence of polymer concentration and temperature gradient, in terms of imposed intensity and direction, on pore size and distribution is studied by comparison with scaffolds prepared by isotropic TIPS. The processing parameters are optimized to achieve an overall porosity for the 3D scaffolds of about 93% with a degree of interconnectivity of 91%. The resulting pore network is characterized by the ordered repetition of closely packed dendrite‐like cavities, each one showing stacks of 20 µm large side lamellar branches departing from 70 µm diameter vertical backbones, strongly resembling the vascular patterns. The in vitro biological responses after 1 and 2 weeks are evaluated from mesenchymal (bone marrow stromal) cells (MSC) static culturing. A novel vacuum‐based deep‐seeding method is set up to improve uniform cell penetration down to scaffold thicknesses of over 1 mm. Biological screenings show significant 3D scaffold colonization even after 18 h, while cellular retention is observed up to 14 d in vitro (DIV). Pore architecture‐driven cellular growth is accompanied by cell tendency to preserve their multi‐potency towards differentiation. Confluent tissues as thick as 1 mm were reconstructed taking advantage of the large perfusion enhanced by the highly porous microstructure of the engineered scaffolds, which could successfully serve for applications aimed at vascular nets and angiogenesis.
(GaN/GaAlN/GaN)//Al2O3(00.1) HEMT heterostructures have been studied by X-ray scattering techniques, transmission electron microscopy and atomic force microscopy. X-ray reflectometry has been used to determine with a high accuracy both the individual layer thicknesses and the interfacial roughness, in spite of the weak electronic density contrast between layers. From the Fourier inversion method and using a simulation software, the roughness of the interface corresponding to the two-dimensional electron gas location has been determined equal to 0.5 nm. Both high resolution X-ray diffraction and transmission electron microscopy experiments have shown the excellent crystallinity of the heterostructures. Finally, the surface morphology has been inferred using atomic force microscopy experiments. 相似文献