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制备了甘氨酸-壳聚糖复合膜修饰玻碳电极(Gly-CTS/GCE),研究了抗坏血酸(AA)和尿酸(UA)在该修饰电极上的电化学行为。结果表明在pH=5.59的磷酸盐缓冲溶液中,AA、UA在Gly-CTS/GCE上均产生灵敏的不可逆氧化峰,其峰电流与浓度在一定范围内呈良好的线性关系。对AA和UA混合溶液平行测定7次,相对标准偏差分别为4.6%、2.9%,表明该电极重现性和稳定性良好。AA、UA在Gly-CTS/GCE电极上的氧化峰峰电位相差340mV,据此可实现对二者的同时检测,并可应用于实际样品测定。 相似文献
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C70X2(X=H,F, Cl)的稳定性和电子光谱 总被引:1,自引:0,他引:1
用INDO方法研究C70H2四种异构体的稳定性, 表明其最稳定异构体为1, 9-C70H2和7, 8-C70H2, 两者能量差为16.3KJ.mol^-^1, 与实验值及ab initio计算值接近; 光谱计算表明, 其特征吸收峰与实验值一致。在此基础上预测C70F2和C70Cl2的稳定性和电子光谱, 表明C70F2四种异构体的稳定性顺序与C70H2一致, 而C70Cl2则以21, 42-异构体最为稳定。二者的电子光谱与C70H2极其相似只是在500nm以上有细微差别。 相似文献
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Francisco D. Avila Orozco Nikolay Kovachev Miguel Ángel Aguirre Pastor Claudia E. Domini Beatriz S. Fernández Band Antonio Canals Hernández 《Analytica chimica acta》2014
A simple and fast method for determining the content of Na, K, Ca, Mg, P, and 20 heavy metals in biodiesel samples with inductively coupled plasma optical emission spectrometry (ICP OES) using a two-nozzle Flow Blurring® multinebulizer prototype and on-line internal standard calibration, are proposed. The biodiesel samples were produced from different feedstock such as sunflower, corn, soybean and grape seed oils, via a base catalyst transesterification. The analysis was carried out without any sample pretreatment. The standards and samples were introduced through one of the multinebulizer nozzles, while the aqueous solution containing yttrium as an internal standard was introduced through the second nozzle. Thus, the spectral interferences were compensated and the formation of carbon deposits on the ICP torch was prevented. The determination coefficients (R2) were greater than 0.99 for the studied analytes, in the range 0.21–14.75 mg kg−1. Short-term and long-term precisions were estimated as relative standard deviation. These were acceptable, their values being lower than 10%. The LOQ for major components such as Ca, K, Mg, Na, and P, were within a range between 4.9 ng g−1 for Mg (279.553 nm) and 531.1 ng g−1 for Na (588.995 nm), and for the other 20 minor components they were within a range between 1.1 ng g−1 for Ba (455.403 nm) and 2913.9 ng g−1 for Pb (220.353 nm). Recovery values ranged between 95% and 106%. 相似文献
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Claudia Domini Lorena Vidal Giancarlo Cravotto Antonio Canals 《Ultrasonics sonochemistry》2009,16(4):564-569
Simultaneous direct irradiation with microwaves and ultrasound was used to determine total Kjeldahl nitrogen. The method involves chemical digestion in two steps, mineralization with sulfuric acid and oxidation with H2O2. The most influential variables for the microwave/ultrasound (MW/US)-assisted digestion were optimized using tryptophan as the model substance. The optimum conditions were: H2SO4 volume, 10 mL; H2O2 volume, 5 mL; weight of sample, 0.05 g; MW power, 500 W; US power, 50 W; digestion time, 7 min (i.e., 5 min mineralization and 2 min oxidation). A modification of the classical Kjeldahl (Hach) method and an US-assisted digestion method were used for comparison. The latter was also optimized; the optimum conditions were: H2SO4 volume, 10 mL; H2O2 volume, 5 mL; sonication time with H2SO4, 15 min; sonication time with H2O2,10 min; US power, 50 W; weight of sample, 0.05 g. Five pure amino acids and two certified reference materials (NIST standard reference materials 1547 (peach leaves), and soil, NCS DC 73322) were analyzed to assess the accuracy of our new MW/US-assisted digestion method, that was successfully applied to five real samples. The significant reduction in digestion time (being 30 min and 25 min for classical Kjeldahl and US-assisted digestion methods, respectively) and consumption of reagents show that simultaneous and direct MW/US irradiation is a powerful and promising tool for low-pressure digestion of solid and liquid samples. 相似文献
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In the present work manganese(III) has been used as oxidant and microwave radiation and ultrasound energy have been assessed to speed up and to improve the efficiency of digestion step for the determination of chemical oxygen demand (COD). Microwave (MW) and ultrasound-assisted COD determination methods have been optimized by means of experimental design and the optimum conditions are: 40 psi pressure, 855 W power and 1 min irradiation time; and 90% of maximum nominal power (180 W), 0.9 s (s?1) cycles and 1 min irradiation time for microwaves and ultrasound, respectively. Chloride ion interference is removed as hydrochloric acid gas from acidified sample solutions at 150 °C in a closed reaction tube and captured by bismuth-based adsorbent suspended above the heated solution. Under optimum conditions, the evaluated assisted digestion methods have been successfully applied, with the exception of pyridine, to several pure organic compounds and two reference materials. COD recoveries obtained with MW and ultrasound-assisted digestion for five real wastewater samples were ranged between 86–97% and 68–91%, respectively, of the values obtained with the classical method (open reflux) used as reference, with relative standard deviation lower than 4% in most cases. Thus, the Mn(III) microwave-assisted digestion method seems to be an interesting and promising alternative to conventional COD digestion methods since it is faster and more environmentally friendly than the ones used for the same purpose. 相似文献
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Summary Orientational effects can exert profound influences over processes carried out inmicelles. A new approach for determining solute orientation within micelles is possible. Lyotropic nematic micelles are anisometrically
shaped and therefore can be oriented. Orientational information about guest molecules can thus be obtained by linear dichroism
or other techniques based on physical processes of rank two (e.g. DNMR, EPR). This information can be transferred to classical spherical micelles to drive reactions by tailoring the reactant
orientations. One more step is recommended for future investigations of micellar catalysis: Why not reactions in nonspherical
micelles instead of the ?classical? spherical micelles?
Work presented at the First USSR-Italy Bilateral Meeting on Liquid Crystals held in Portonovo, Ancona (Italy), September 30–October
2, 1987. 相似文献
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The fracture of thick laminated graphite/epoxy composites has been the subject of an extensive research program. The program
was divided into three major areas of investigation which included laminate thickness, laminate stacking sequence, and part-through
surface flaws. The results from this program are reviewed with emphasis placed on their applicability to the design of thick
laminated composite structures.
Paper was presented at 1985 SEM Spring Conference on Experimental Mechanics held in Las Vegas on June 9–14, 1985. 相似文献
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