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1.
A method was proposed for the simultaneous determination of trace cadmium and mercury by vapor generation non-dispersive atomic fluorescence spectrometry using an intermittent flow system. The effects of the parameters on the performance were studied systematically. The parameters such as acid concentration of the reaction medium, flow rate of the carrier gas and shield gas, the observation height and the atomizer temperature, etc. which affected the sensitivity, were optimized. Ascorbic acid, cobalt ion and thiourea were used as enhancement reagents or masking agents to enhance the generation efficiency of the volatile species of Cd and Hg. The mechanisms of their effects on vapor generation were investigated. In the presence of thiourea and ascorbic acid, the influences of some coexisting elements on the determination of cadmium and mercury were investigated. The detection limits (3sigma) were 0.010 microg l(-1) for Cd and 0.019 microg l(-1) for Hg, respectively. The relative standard deviations for Cd and Hg at 1.00 microg l(-1) were 2.6% and 0.97% (n = 11), respectively. The proposed method has been satisfactorily applied to the determination of trace cadmium and mercury in Chinese herbal medicine. 相似文献
2.
由二硫代肼基甲酸酯衍生的铜(Ⅱ)的希夫碱配合物的合成,结构和抑菌活性的研究 总被引:4,自引:0,他引:4
从S—苄基和S—甲基二硫代肼基甲酸酯衍生出的两种亚苄基丙酮希夫碱为配体,合成了铜(Ⅱ)配合物。经化学分析、磁性、红外、电子和EPR光谱的研究表明配合物有Cu(TSB)_2的形式,其中配体为双齿单价阴离子。在固态时,两种配合物分别为平面正方形和平面菱形结构。在溶液中,两者都为平面正方形。由EPR光谱分析得到的磁参数和键参数的值表明配合物中的键有较高的共价特征。对四种细菌的抑菌试验发现配体及其配合物均有抑菌活性,其中配合物的活性较高并研究了介质,pH对抑菌作用的影响。 相似文献
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The development of highly active and stable reversible oxygen electrocatalysts is crucial for improving the efficiency of metal-air battery devices. Herein, an efficient liquid exfoliation strategy was designed for producing silk-like FeS2/NiS2 hybrid nanocrystals with enhanced reversible oxygen catalytic performance that displayed excellent properties for Zn-air batteries. Because of the unique silk-like morphology and interface nanocrystal structure, they can catalyze the oxygen evolution reaction (OER) efficiently with a low overpotential of 233 mV at j = 10 mA cm?2. This is an improvement from the recently reported catalysts in 1.0 M KOH. Meanwhile, the oxygen reduction reaction (ORR) activity of the silk-like FeS2/NiS2 hybrid nanocrystals showed an onset potential of 911 mV and a half-wave potential of 640 mV. In addition, the reversible oxygen electrode activity of the silk-like FeS2/NiS2 hybrid nanocrystals was calculated to be 0.823 V, based on the potential of the OER and ORR. Further, the homemade rechargeable Zn-air batteries using FeS2/NiS2 hybrid nanocrystals as the air-cathode displayed a high open-circuit voltage of 1.25 V for more than 17 h and an excellent rechargeable performance for 25 h. The solid Zn-air batteries exhibited an excellent rechargeable performance for 15 h. This study provided a new method for designing interface nanocrystals with a unique morphology for efficient multifunctional electrocatalysts in electrochemical reactions and renewable energy devices. 相似文献
5.
气相色谱法研究配位化合物的热稳定性——ⅩⅢ.普鲁士蓝化合物的热分解及其加氢反应研究 总被引:2,自引:0,他引:2
普鲁士蓝化合物的热分解过程,可分为三个阶段:(1)脱水;(2)Fe3+还原至Fe2+;(3)C≡N-键的断裂。H2气中的热分解由于发生了一系列的加氢反应,分解产物及所对应的分解温度都不同于He气中的情况,其产物的种类增加,C≡N-键的断裂温度降低。普鲁士蓝化合物中,CN-呈典型的双端基配位,可看作是一种双金属配位的活化模型,与CN-呈单端基配位的K3[Fe(CN)6]相比,C≡N-键的活化程度增加,不仅断裂温度降低,且能发生更深度的加氢反应。 相似文献
6.
K3 [Fe(CN)6] and KFe[Fe(CN)6] are classical coordination compounds. However, the mechanism of decomposition reactions has not been well expounded. The gas products of thermal decomposition were examined by gas chroma tography (GC) , and the structure of the solid products by Mossbauer spectroscopy(MS) and X-ray diffraction(XRD). The findings are explained in terms of the theory of coordination chemistry and a decomposition mechanism is proposed in this study. On the basis of various experimental results, the first stage of the decomposition of K3[Fe(CN)6] in He was found to be the evolution of(CN)2 resulting in the reduction of Fe(Ⅲ)12K3 [Fe(CN)6]→9K4[Fe(CN)6] + Fe2 [Fe(CN)6] + 6 ( CN )For KFe [Fe(CN) 6 ], the first stage of decomposition man be represented as6KFe[Fe(CN)6]→3K2Fe[Fe(CN)6] + 2Fe2[Fe(CN)6 + 3(CN)2At higher temperatures, the decomposition of both K3[Fe(CN)6) andKFe[Fe(CN)6] to form KCN and Fe2C was accomplished by the release of(CN)2 and N2. 相似文献
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A multiresidue method has been developed for the simultaneous determination of sulfadiazine, sulfathiazole, sulfapyridine,
sulfamerazine, sulfamethoxydiazine, sulfamethylthiazole, sulfamethazine, sulfamonomethoxine, sulfamethoxypyridazine, sulfisoxazole,
sulfamethoxazole, sulfadimethoxine and sulfaquinoxaline in natural animal casings by HPLC after solid-phase extraction. The
sulfonamides were extracted with acetonitrile and the extract cleaned up with an Oasis MCX SPE cartridge prior to analysis.
Separation was on a ZOBAX Eclipse XDB-C8 column using gradient elution with acetonitrile/methanol/0.1% acetic acid. The effect of separation conditions on chromatographic
behavior and recovery has been studied. Calibration graphs were linear with very good correlation coefficients (r = 0.9983−0.9996) in the concentration range from 0.02 to 1 μg mL−1. The limits of quantitation (LOQ) for the 13 sulfonamides were in the range of 1.5–2.2 μg kg−1. Decision limits (CCα) and detection capabilities (CCβ) were in the range of 105.2–111.0 and 113.0–120.2 μg kg−1, respectively. The recovery for casings spiked with 1.5–100 μg kg−1 ranged from 65.2 to 85.9%. The relative standard deviations (RSDs) of the sulfonamides for six measurements at 100 μg kg−1 were from 2.2 to 7.7%. The applicability of the method to the analysis of salted swine casings, salted sheep casings and
dry casing samples was demonstrated. 相似文献
10.
二乙基二烯丙基氯化铵均聚及其与丙烯酰胺或丙烯酸共聚动力学研究 总被引:1,自引:0,他引:1
采用膨胀计法研究了以过硫酸铵为引发剂,二乙基二烯丙基氯化铵(DEDAAC)在水溶液中的均聚及其与丙烯酰胺(AM)和丙烯酸(AA)共聚动力学,测定了相应的聚合表观活化能;采用元素分析法测定了DEDAAC分别与AM和AA在低转化率下共聚物的组成,并采用氯离子选择性电极法测定了DEDAAC-AM共聚物中的氯离子含量,按Kelen-Tudos方法求得了相应的竞聚率.结果表明,DEDAAC均聚速率方程为RP=k[M]0.99[I]0.76,表观活化能Ea=77.00kJ/mol,说明链终止为单基终止和双基终止并存,引发过程与单体浓度无关;DEDAAC与AM在摩尔比为4∶1时,共聚动力学方程为RP=[M]2.53[I]0.90,表观活化能Ea=67.06kJ/mol,单体竞聚率为rDE=0.31±0.02、rAM=5.27±0.53;DEDAAC与AA在摩尔比为4∶1时,共聚动力学方程为RP=k[M]2.94[I]0.83,表观活化能Ea=70.07kJ/mol,竞聚率为rDE=0.28±0.03、rAA=5.15±0.28;DEDAAC与AM和AA等共聚为非理想共聚,得到的产物均为无规共聚物. 相似文献