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1.
萃取光度法测定高纯氧化钐中的铬   总被引:2,自引:0,他引:2  
本文研究了正戊醇-高氯酸-Cr(Ⅵ)-二苯碳酰二肼体系的各种萃取条件,建立了萃取光度法测定微量铬的新方法。在高氯酸介质中,正戊醇能定量的萃取富集Cr(Ⅵ)-二苯碳酰二肼络合物。萃取前和萃取后络合物的最大吸收波长不变(543nm),而试剂空白在此处均无吸收。校准曲线在0-5μg/mL范围内符合比耳定律。利用EDTA掩蔽稀土基体的干扰,用本法制定了高纯稀土氧经物中的铬含量,并作了加标回收实验结果令人满意。  相似文献   

2.
以干青蒿叶为原料,考察石油醚萃取青蒿素的工艺条件,如温度、时间、溶剂量及超声功率等因素,正交法确定了最佳萃取工艺条件为温度40℃,超声功率90W,时间20min(两次),液固比120∶1(mL.g-1)。紫外分光光度法直接测定不同产地青蒿中青蒿素的含量,结果表明:用超声波强化石油醚萃取青蒿素与常规浸泡法石油醚萃取比较,用超声波可以大大缩短萃取时间,提高了萃取率。  相似文献   

3.
GDX 501-TBP萃取色谱富集分离-原子吸收光谱法测定痕量金   总被引:2,自引:0,他引:2  
以GDX501(二乙烯苯和丙烯腈的聚合物)型树脂浸渍磷酸三丁酯(TBP)为固定相,萃取色谱法富集样品中的微量金,盐酸-硫脲溶液洗脱并用原子吸收光谱法进行测定。方法的回收率在97%-105%之间,相对标准偏差为0.76%-2.3%。用于实际样品中金的测定,结果令人满意。  相似文献   

4.
提出了一种流动注射在线液-液萃取有机相汞还原原子荧光光谱法测定汞的新方法。该法以KI+HNO3+(NH2)2CS/TBP为萃取体系,将汞萃取到有机相中,汞还原反应是在金属络合萃取液与含NaBH4的N,N-二甲基甲酰铵(DMF)溶液和冰乙酸中发生。应用流动注射技术实现了液-液萃取非水介质汞还原反应原子荧光测定的在线分析。研究了反应的最佳条件和流动注射流路及运行程序。该法提高了测定灵敏度并消除了干扰。用于地质样品中汞的测定得到好的准确度和精密度。  相似文献   

5.
叔胺N235萃取柠檬酸的研究   总被引:2,自引:1,他引:1  
用正辛醇-叔胺N235石油醚溶液萃取柠檬酸有协同效应,协萃系数R=2.7萃取为一放热反应,H=-14.6kJ.mol^-1一次萃取率可达92.2%,用稀盐酸反萃率为99.3%。测定了协萃有机相的红外光谱。  相似文献   

6.
本文提出一种确定萃取反应热力学萃取平衡常数的单参数方程(°↑α=4.9),方法简便,用P538萃取硫氰酸钒(Ⅳ)配合物的实验,在较宽的离子强度范围内有良好线性关系,在一般萃取实验条件下,用作图法可求出热力学萃取平衡常数,有普遍意义。  相似文献   

7.
采用二苯碳酰二肼为络合剂,正戊醇为萃取剂,乙醇为助溶剂,建立了微珠析相微萃取-石墨炉原子吸收法测定地质样品中痕量Cr的分析方法。实验详细探讨了微珠析相微萃取的析相条件、石墨炉原子吸收工作参数及共存离子的干扰,优化了体系萃取条件。实验结果表明:微珠析相微萃取既起到了分离富集的作用,在石墨炉升温程序中又起到了基体改进剂的作用;当萃取剂用量为0.2~1.5 mL时,使之与水完全互溶所需助溶剂体积约为水相体积的0.2~0.5倍;方法线性范围为0~10 μg·L-1,检出限为0.057 μg·L-1,相对标准偏差(RSD)为3.3%(c= 2.5 μg·L-1,n=11);当萃取剂用量为1.5 mL、水相体积15 mL时,与直接溶液进样相比其灵敏度可提高10倍。所建立的方法用于地质标准参考物质AGV-2和G-2中Cr的测定,测定值与参考值具有较好的一致性。  相似文献   

8.
沈友 《光谱实验室》2012,29(5):3227-3230
研究了用磷酸三丁酯(TBP)-醋酸纤维富集,I2-CCl4萃取分光光度法测定矿石中的痕量金的方法.实验表明,测定金的回收率为93.0% %-105.0%.与其他测定方法进行比较,此法效果较好.  相似文献   

9.
本文研究了PEG2000铬菁R(NH4)2SO4体系对Co(Ⅱ)、Ni(Ⅱ)的非有机溶剂萃取行为。指出在pH=5的(NaAcHAc)水溶液中,有(NH4)2SO4存在下,Ni(Ⅱ)可被PEG相几乎完全萃取,而Co(Ⅱ)则基本上不被萃取。从而获得了Co(Ⅱ)与Ni(Ⅱ)混合离子的定量分离。  相似文献   

10.
采用动态激光光散射(DLS)、Fourier变换红外光谱(FTIR)、核磁共振波谱(31P-/1H NMR)等谱学技术,研究了TBP-Pd(Ⅱ)-HCI萃取有机相中微乳的形成以及溶液聚集态结构的变化.结果表明:(1)伴随钯的萃取,TBP萃取有机相中形成微乳.(2)萃取有机相中酸含量的变化导致溶液结构发生相应改变:胶团聚集体平均流体力学半径随有机相中酸含量的增加先增大而后又减小.微乳"内核水"的O-H伸缩振动吸收谱带逐渐宽化,与邻近的C-H伸缩振动区形成交迭,且有机相含酸量越高,交迭程度越大.水分子O-H-O弯曲变角振动吸收峰形也发生很大变化.TBP的P=O伸缩振动明显向低频移动.核磁共振31P化学位移与活泼氢1H化学位移变化行为相反,说明TBP分子与酸和水分子发生缔合,形成RP=0·H 或RP-O·H3O ,并与PdC2-4存在相互作用.(3)有机相形成微乳水团后,由于大量H 的进入,微乳水团中酸浓度表现出明显的"增浓效应".微乳水池内部微观环境的改变是导致钯萃取行为变化的主要原因.  相似文献   

11.
This paper deals with an application of Zipf law in climatology. This analysis allows the extraction of information not available by standard methods. In particular, rainfall temporal aggregation patterns associated with different climates are characterized by means of exponents derived from the resulting scaling laws. The analogy with linguistic analysis is obtained using a particular coding of precipitation as a discrete variable with four states (corresponding to four standard precipitation thresholds); each weekly symbolic sequence of observed precipitation is considered as a “word”, and each local station defines a “language” characterized by the observed words in a period representative of the climatology. To characterize these precipitation languages, we obtained characteristic exponents derived from the Zipf law for a set of representative stations of the main Köppen's climates and subclimates. We found different scaling behaviors for different subclimates, given by a single exponent in the range 0.60.6 (humid tropical climates) to 1.41.4 (polar climates); some humid middle-latitude subclimates exhibit a crossover with two different characteristic exponents corresponding to high and low frequency aggregation patterns (no explanation for this behavior is provided).  相似文献   

12.
Z. Ali  Abu Zuhri 《光谱学快报》2013,46(4):333-341
Abstract

A new spectrophotometric method was employed for the determination of lead (II) based on the ternary complex formation with 2-(5-Bromo-2-Pyridylazo)-5-diethylaminophenol(5-BrPADAP) and cetyltri-methyl-ammonium bromide (CTAB). At pH 7.00 a violet ternary complex, whose molar absorptivity is 5.1×104 1.mole?1 cm?1 at 575 nm, is formed. Beer's law range (0.5 ? 4.9 μg ml?1 of lead), the apparent stability constant (log β=9.90) and δG° were evaluated. A large number of ions do not interfer at pH 7.00 because they form complexes with 5-Br-PADAP at higher pH's (< 9.40) or at lower pH's (> 4.86). The method offers the advantages of simplicity and requires no extraction.  相似文献   

13.
The use of deep eutectic solvents (DESs) as a new extraction medium is a step towards the development of green and sustainable technology. In the present study, nine DESs based on choline chloride acids, alcohols, and sugar were screened to study the extraction of curcuminoids from Curcuma longa L. Choline chloride and lactic acid DES at 1:1 M ratio gave the maximum extent of extraction. Further, DES based extraction was intensified using ultrasound. The impact of various process parameters such as % (v/v) water in DES, % (w/v) solid loading, particle size, ultrasound power intensity, and pulse mode operation of ultrasound was studied. The maximum curcuminoids yield of 77.13 mg/g was achieved using ultrasound assisted DES (UA-DES) based extraction in 20% water content DES at 5% solid loading and 0.355 mm particle size with 70.8 W/cm2 power intensity and 60% (6 sec ON and 4 sec OFF) duty cycle at 30 ± 2 °C in 20 min of irradiation time. Kinetics of UA-DES extraction was explained using Peleg’s model and concluded that it is compatible with the experimental data. Additionally, anti-solvent (water) precipitation technique was applied, which resulted in 41.97% recovery of curcuminoids with 82.22% purity from UA-DES extract in 8 h of incubation at 0 °C. The comparison was made between conventional Soxhlet, batch, DES and UA-DES based processes on the basis of yield, time, solvent requirement, temperature, energy consumption, and process cost. The developed UA-DES based extraction can be an efficient, cost effective, and green alternative to conventional solvent extraction for curcuminoids.  相似文献   

14.
The supercritical fluid extraction of chlorophylls and carotenoids from marine algae Fucus vesiculosus and Laminaria digitata with carbon dioxide was studied. Complete extraction of carotenoids with carbon dioxide was achieved at a pressure of 250 atm and a temperature of 80°C after 20 min in the absence of a cosolvent. Extraction of chlorophylls in high contents required the use of a polar co-solvent (ethanol, 10–15 vol %) or extraction time increased to 50–90 min (at a co-solvent consumption of <5 vol %). The proposed method is more express compared with extraction in a Soxhlet apparatus.  相似文献   

15.
Benford’s law, also called the first-digit law, states that in lists of numbers from many quite disparate databases, the leading digit is distributed in a non-uniform but actually logarithmic way. We have investigated the first-digit distribution of experimental cross-sections of A(n,a \alpha)B reactions. In the case of below-barrier a \alpha -particle emission from compound nucleus, it is found that the (n,a \alpha) reaction cross-sections approximately follow the first-digit distribution indicated by Benford’s law. The origin of this first-digit distribution is discussed within the framework of the statistical model. In addition, Benford’s law is used to test the evaluated cross-sections of A(n,a \alpha)B reactions.  相似文献   

16.
Among the approaches available for structural analysis, the J-integral has received an excellent feedback as a fracture parameter under elastic-plastic conditions. In the literature and dealing with the crack case, it is proposed to evaluate the J-integral as a sum of elastic and plastic contributions. However, some uncertainties arise when applying this method to a Ramberg-Osgood law, especially under large scale yielding conditions.The aim of the present paper is to discuss how the J-integral evaluation can be performed for elastic-plastic cracked components. Two different non-linear behaviours have been considered for the material: the Ramberg-Osgood law and power law. Numerical and finite element results from different approaches have been accurately compared, proving that the most appropriate way to evaluate the J-integral for a material obeying Ramberg-Osgood law is to perform two finite element analyses evaluating separately the elastic contribution (through a linear elastic analysis) and the plastic contribution (through a nonlinear analysis considering power law behaviour).  相似文献   

17.
In this work, two new possibilities for standard probe diagnostics are described. The first one can be used to study isotropic, collisionless low-pressure plasma in which the electron energy distribution function is close to a Maxwellian one. In such plasmas, the Boltzmann law, Bohm effect, and 3/2 power law are valid. Use of corresponding system of equations for cylindrical Langmuir probes allowed for measurements of probe sheath thicknesses and the mean ion mass. The solution of this task was provided by accurate probe diagnostics of inductive xenon plasma at pressure p = 2 mTorr that resulted in the determination of the Bohm coefficient CBCyl = 1.22. The second possibility of probe diagnostics includes a method and device for evaluation of ion current density to a wall under a floating potential using a radially movable plane wall Langmuir probe simulator. This measurement in the same xenon plasma served as the basis for development of an ion source in which the given wall was represented by an ion extracting electrode of the ion extraction grid system.  相似文献   

18.
The rigged Hilbert space formalism of quantum mechanics provides a framework in which one can identify resonance states and obtain the typical exponential decay law. However, there remain questions of the interpretation and extraction of physical information through the calculation of expectation values of observables. The Lax-Phillips scattering theory provides a mathematical construction in which resonances are assigned with states in a Hilbert space, thus no such difficulties arise. The original Lax-Phillips structure is inapplicable within standard nonrelativistic quantum theory. Through the powerful theory of H p spaces certain relations between the two theories are uncovered, which suggest that a search for a unifying framework might prove useful.  相似文献   

19.
This paper discusses a new turn in the 148-year old electrodynamic force law controversy between the 1822 Ampère force law of the Newtonian electrodynamics and Grassmann's 1845 law which has become the electrodynamic force law of relativistic electromagnetism. Faced with the infallibility of Ampère's empirical law, defenders of relativity theory now argue that Ampère's law is equivalent to the relativistic law. This paper demonstrates that, far from being equivalent, the laws require two different mechanics of solid bodies, disagree on internally generated stresses, and predict different force distributions.  相似文献   

20.
《Ultrasonics sonochemistry》2014,21(4):1461-1469
The effects of acoustic energy density (6.8–47.4 W/L) and temperature (20–50 °C) on the extraction yields of total phenolics and tartaric esters during ultrasound-assisted extraction from grape marc were investigated in this study. The ultrasound treatment was performed in a 25-kHz ultrasound bath system and the 50% aqueous ethanol was used as the solvent. The initial extraction rate and final extraction yield increased with the increase of acoustic energy density and temperature. The two site kinetic model was used to simulate the kinetics of extraction process and the diffusion model based on the Fick’s second law was employed to determine the effective diffusion coefficient of phenolics in grape marc. Both models gave satisfactory quality of data fit. The diffusion process was divided into one fast stage and one slow stage and the diffusion coefficients in both stages were calculated. Within the current experimental range, the diffusion coefficients of total phenolics and tartaric esters for both diffusion stages increased with acoustic energy density. Meanwhile, the rise of temperature also resulted in the increase of diffusion coefficients of phenolics except the diffusion coefficient of total phenolics in the fast stage, the value of which being the highest at 40 °C. Moreover, an empirical equation was suggested to correlate the effective diffusion coefficient of phenolics in grape marc with acoustic energy density and temperature. In addition, the performance comparison of ultrasound-assisted extraction and convention methods demonstrates that ultrasound is an effective and promising technology to extract bioactive substances from grape marc.  相似文献   

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