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141.
The present paper describes the feasibility of on-line preconcentration of nickel ions from aqueous medium on Ni(II)-imprinted cross-linked poly(methacrylic acid) (IIP) synthesised through a double-imprinting method and their subsequent determination by FAAS. The proposed method consisted in loading the sample (20.0 mL, pH 7.25) through a mini-column packed with 50 mg of the IIP for 2 min. The elution step was performed with 1.0 mol L?1 HNO3 at a flow rate of 7.0 mL min?1. The following parameters were obtained: quantification limit (QL) – 3.74 µg L?1, preconcentration factor (PF) – 36, consumption index (CI) – 0.55 mL, concentration efficiency (CE) – 18 min?1, and sample throughput – 25 h?1. The precision of the procedure assessed in terms of repeatability for ten determinations was 5.6% and 2.5% for respective concentrations of 5.0 and 110.0 µg L?1. Moreover, the analytical curve was obtained in the range of 5.0–180.0 µg L?1 (r = 0.9973), and a 1.64-fold increase in the method sensitivity was observed when compared with the analytical curve constructed for the NIP (non-imprinted polymer), thus suggesting a synergistic effect of the Ni(II) ions and CTAB on the adsorption properties of the IIP. The practical application of the adsorbent was evaluated from an analysis of tap, mineral, lake and river water. Considering the results of addition and recovery experiments (90.2–100 %), the efficiency of this adsorbent can be ensured for the interference-free preconcentration of the Ni(II) ions.  相似文献   
142.
The effect of ultraviolet (UV) radiation and copper (Cu) on apical segments of Pterocladiella capillacea was examined under two different conditions of radiation, PAR (control) and PAR+UVA+UVB (PAR+UVAB), and three copper concentrations, ranging from 0 (control) to 0.62, 1.25 and 2.50 μm . Algae were exposed in vitro to photosynthetically active radiation (PAR) at 70 μmol photons m?2 s?1, PAR + UVB at 0.35 W m?2 and PAR +UVA at 0.70 W m?2 during a 12‐h photocycle for 3 h each day for 7 days. The effects of radiation and copper on growth rates, content of photosynthetic pigments and photosynthetic performance were analyzed. In addition, samples were processed for light and transmission electron microscopy. The content of photosynthetic pigments decreased after exposure to radiation and Cu. Compared with PAR radiation and copper treatments modified the kinetics patterns of the photosynthesis/irradiance curve. The treatments also caused changes in the ultrastructure of cortical and subcortical cells, including increased cell wall thickness and accumulation of plastoglobuli, as well as changes in the organization of chloroplasts. The results indicate that the synergistic interaction between UV radiation and Cu in P. capillacea, led to the failure of protective mechanisms and causing more drastic changes and cellular imbalances.  相似文献   
143.
The ligand‐centered radical complex [(CoTPMA)2‐μ‐bmtz.?](O3SCF3)3 ? CH3CN (bmtz=3,6‐bis(2′‐pyrimidyl)‐1,2,4,5‐tetrazine, TPMA=tris‐(2‐pyridylmethyl)amine) has been synthesized from the neutral bmtz precursor. Single‐crystal X‐ray diffraction studies have confirmed the presence of the ligand‐centered radical. The CoII complex exhibits slow paramagnetic relaxation in an applied DC field with a barrier to spin reversal of 39 K. This behavior is a result of strong antiferromagnetic metal–radical coupling combined with positive axial and strong rhombic anisotropic contributions from the CoII ions.  相似文献   
144.
The total Kjeldahl nitrogen (TKN) method was simplified by using a manifold connected to a purge-and-trap system immersed into an ultrasonic (US) bath for simultaneous ammonia (NH3) extraction from many previously digested samples. Then, ammonia was collected in an acidic solution, converted to ammonium (NH4+), and finally determined by ion chromatography method. Some variables were optimized, such as ultrasonic irradiation power and frequency, ultrasound-assisted NH3 extraction time, NH4+ mass and sulfuric acid concentration added to the NH3 collector flask. Recovery tests revealed no changes in the pH values and no conversion of NH4+ into other nitrogen species during the irradiation of NH4Cl solutions with 25 or 40 kHz ultrasonic waves for up to 20 min. Sediment and oil free sandstone samples and soil certified reference materials (NCS DC 73319, NCS DC 73321 and NCS DC 73326) with different total nitrogen concentrations were analysed. The proposed method is faster, simpler and more sensitive than the classical Kjeldahl steam distillation method. The time for NH3 extraction by the US-assisted purge-and-trap system (20 min) was half of that by the Kjeldahl steam distillation (40 min) for 10 previously digested samples. The detection limit was 9 μg g−1 N, while for the Kjeldahl classical/indophenol method was 58 μg g−1 N. Precision was always better than 13%. In the proposed method, carcinogenic reagents are not used, contrarily to the indophenol method. Furthermore, the proposed method can be adapted for fixed-NH4+ determination.  相似文献   
145.
The crude extract of the Brazilian brown alga Dictyota crenulata was analyzed by NMR spectroscopy and HRGC-MS techniques. Seven diterpenes were identified: pachydictyol A, dictyodial, 4beta-hydroxydictyodial A, 4beta-acetoxydictyodial A, isopachydictyol A, dictyol C and dictyotadiol. Xeniane diterpenes have previously been found in D. crenulata from the Pacific Ocean. The results characterize D. crenulata as a species that provides prenylated guaiane (group I) and xeniane diterpenes (group III), thus making it a new source of potential antiviral products.  相似文献   
146.
This paper focuses on the analytical performance improvement of the coupled technique HPLC-ICPMS using on-line collision/reaction cell technology for selenium elemental and speciation analyses at the ng (Se) l(-1) level in aquatic environment. Collision/reaction cell operating parameters were optimised, resulting in selected conditions of 5.5 ml min(-1) H(2) and 0.5 ml min(-1) He mixture. The detection limits obtained were around 5 ng (Se) l(-1) for total analysis, and between 7 and 15 ng (Se) l(-1) depending on the species for speciation analysis. The capability of UV irradiation-hydride generation interfacing to increase detector sensitivity was also evaluated for speciation analysis. The detection limits obtained were in the range 2-8 ng (Se) l(-1) depending on the species. Moreover, such interface allowed to prevent bromine introduction to the ICPMS which is particularly convenient for selenium trace analysis in natural waters as (80)Se is preserved free from BrH interferences. The developed method was validated using certified water with low selenium content (TM Rain 95, NWRI, Canada) and applied to the analysis of different waters.  相似文献   
147.
This work presents a comparative study of calibration transfer among three near infrared spectrometers for determination of naphthenes and RON (Research Octane Number) in gasoline. Seven transfer methods are compared: direct standardization (DS), piecewise direct standardization (PDS), orthogonal signal correction (OSC), reverse standardization (RS), piecewise reverse standardization (PRS), slope and bias correction (SBC) and model updating (MU). Two pre-treatment procedures, namely standard normal variate (SNV) and multiplicative scatter correction (MSC), are also investigated. The choice of an appropriate number of transfer samples for each technique, as well as the effect of window size in PDS/PRS and OSC components, are discussed. A broad set of gasoline samples representative of the Northeastern states of Brazil is employed in the investigation. The results show that the use of calibration transfer yields prediction errors comparable to those obtained with complete recalibration of the secondary instrument. Overall, the results point to RS as the best method for the analytical problem under consideration. When storage and/or physical transportation of transfer samples are impractical, MU is more appropriate. The comprehensive investigation carried out in the present work will be of value for practitioners involved in networks of fuel monitoring.  相似文献   
148.
In the previous work, we reported a multitarget Quantitative Structure‐Activity Relationship (mt‐QSAR) model to predict drug activity against different fungal species. This mt‐QSAR allowed us to construct a drug–drug multispecies Complex Network (msCN) to investigate drug–drug similarity (González‐Díaz and Prado‐Prado, J Comput Chem 2008, 29, 656). However, important methodological points remained unclear, such as follows: (1) the accuracy of the methods when applied to other problems; (2) the effect of the distance type used to construct the msCN; (3) how to perform the inverse procedure to study species–species similarity with multidrug resistance CNs (mdrCN); and (4) the implications and necessary steps to perform a substructural Triadic Census Analysis (TCA) of the msCN. To continue the present series with other important problem, we developed here a mt‐QSAR model for more than 700 drugs tested in the literature against different parasites (predicting antiparasitic drugs). The data were processed by Linear Discriminate Analysis (LDA) and the model classifies correctly 93.62% (1160 out of 1239 cases) in training. The model validation was carried out by means of external predicting series; the model classified 573 out of 607, that is, 94.4% of cases. Next, we carried out the first comparative study of the topology of six different drug–drug msCNs based on six different distances such as Euclidean, Chebychev, Manhattan, etc. Furthermore, we compared the selected drug–drug msCN and species–species mdsCN with random networks. We also introduced here the inverse methodology to construct species–species msCN based on a mt‐QSAR model. Last, we reported the first substructural analysis of drug–drug msCN using Triadic Census Analysis (TCA) algorithm. © 2009 Wiley Periodicals, Inc. J Comput Chem 2010  相似文献   
149.
A Quartz Crystal Microbalance (QCM) was used to monitor the mass changes on a quartz crystal surface containing immobilized lectins that interacted with carbohydrates. The strategy for lectin immobilization was developed on the basis of a multilayer system composed of Au–cystamine–glutaraldehyde–lectin. Each step of the immobilization procedure was confirmed by FTIR analysis. The system was used to study the interactions of Concanavalin A (ConA) with maltose and Jacalin with Fetuin. The real-time binding of different concentrations of carbohydrate to the immobilized lectin was monitored by means of QCM measurements and the data obtained allowed for the construction of Langmuir isotherm curves. The association constants determined for the specific interactions analyzed here were (6.4 ± 0.2) × 104 M− 1 for Jacalin–Fetuin and (4.5 ± 0.1) × 102 M− 1 for ConA–maltose. These results indicate that the QCM constitutes a suitable method for the analysis of lectin–carbohydrate interactions, even when assaying low molecular mass ligands such as disaccharides.  相似文献   
150.
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