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A Practical Example on Uncertainty Evaluation: Spectrophotometric Determination of pK a 不确定度评定的实例:分光光度法测定钾
Pub Date : 2018-01-01 DOI: 10.20431/2349-0403.0501004
E. J. Díaz-Montaña, Á. Alcázar, J. Jurado, F. Pablos
As it can be read in EURACHEM/CITAC Guide for quantifying uncertainty in analytical measurements [1], many important decisions are based on the results of chemical quantitative analysis and, for this reason, is very important to ensure the quality of analytical methods. Nowadays, there has been a great emphasis on the precision of results obtained using a specified analytical method and in establishing their traceability to a defined standard. For this aim, internal quality control procedures, proficiency testing an accreditation have become very useful tools. Chemists are being asked to demonstrate the quality of their results, including their agreement with others results, being measurement uncertainty one useful measure of this. As a consequence of these requirements, our students are expected to be able to apply measurement uncertainty evaluation and propagation. In this work, we propose a training practical example that can be used by people learning about the evaluation of uncertainty in measurements and its propagation in different cases. The chosen example is the photometric determination of the ionization constant of acetaminophen by measuring the absorbance of an acetaminophen solution at different pH values. According to Hildebrand and Reilley method [2], the next relation can be established:
正如《EURACHEM/CITAC分析测量不确定度量化指南》[1]中所述,许多重要决策都是基于化学定量分析的结果,因此对保证分析方法的质量非常重要。如今,人们非常强调使用特定分析方法获得的结果的准确性,并建立其可追溯性,以确定标准。为此,内部质量控制程序、能力测试和认证已成为非常有用的工具。化学家被要求证明他们的结果的质量,包括他们与其他结果的一致性,测量不确定度是一个有用的测量方法。由于这些要求,我们的学生被期望能够应用测量不确定度评估和传播。在这项工作中,我们提出了一个训练实例,可以用于人们学习测量不确定度的评估及其在不同情况下的传播。所选的例子是通过测量对乙酰氨基酚溶液在不同pH值下的吸光度来测定对乙酰氨基酚的电离常数。根据Hildebrand和Reilley方法[2],可以建立下一个关系式:
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引用次数: 1
Synthesis, and Spectral Studies of Demi-macrocycles of Ligand N2O2 with Ni (II) and Cu (II) Ions Ni (II)和Cu (II)离子配体N2O2半大环的合成及光谱研究
Pub Date : 2018-01-01 DOI: 10.20431/2349-0403.0503003
Sameena Rasheed, A. Dwivedi, M. U. Khan
The new series of demi-macrocycles of the type [C14 H30 N2 O2 (Cl2 O4) 2] having N2O2 as donors ligand were synthesized by the equimolar condensation reaction of ethane-1, 2-diamine in acetone in presenced of perchloric acid. The head unit of demi-macrocycle formed was proposed by the two acetone molecules [M (C14H30N2O2) (ClO4)2] Where, M = Ni(II) and Cu(II) were formed by the reaction of proposed demi-macrocycle with respective metal salts. The complexes formed were characterized by the elemental analysis, conductance and magnetic susceptibilities measurements, and also by spectral methods.
在高氯酸存在下,乙烷- 1,2 -二胺在丙酮中进行等摩尔缩合反应,合成了以N2O2为给体配体的新系列[C14 H30 N2O2 (Cl2 O4) 2]型半大环。提出了两个丙酮分子[M (C14H30N2O2) (ClO4)2]形成半大环的头单元,其中M = Ni(II)和Cu(II)是由所提出的半大环与各自的金属盐反应形成的。通过元素分析、电导、磁化率测量和光谱方法对所形成的配合物进行了表征。
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引用次数: 0
Phosphotungustic Acid Catalysed Oxidation of Aliphatic Hydroxy Acids by N-chlorosuccinimide in Aqueous Acetic Medium 磷钨酸在水乙酸介质中催化n -氯琥珀酰亚胺氧化脂肪族羟基酸
Pub Date : 2018-01-01 DOI: 10.20431/2349-0403.0506001
N. Khan, K. Khan, A. Dwivedi, H. Dwivedi
Kinetics of phosphotungustic acid catalysed oxidation of aliphatic hydroxy acids such as lactic, tartaric and tartronic acids by N-chlorosuccinimide have been studied in aqueous acetic acid medium. The order of [N-chlorosuccinimide] was found to be one and fractional-order with respect to catalyst [PTA]. However, the order of [hydroxy acids] changed from unity to a fractional one in presence of PTA. The insignificant change in rate was observed with [H] and neutral salts. The basis of kinetics features, the probable and activation mechanism are discussed and individual rate parameters evaluated.
研究了磷钨酸在醋酸水溶液中催化乳酸、酒石酸和酒石酸等脂肪羟基酸被n -氯琥珀酰亚胺氧化的动力学。发现[n -氯琥珀酰亚胺]对催化剂[PTA]为一阶和分数阶。然而,在PTA的作用下,羟基酸的顺序由单一变为分数。[H]和中性盐的反应速率变化不大。在动力学特征的基础上,讨论了反应的可能性和活化机理,并对各速率参数进行了评价。
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引用次数: 0
Determination of Diethylstilbestrol in Water Samples by Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Droplet Followed UV Spectrometry 基于悬浮液滴固化的分散液液微萃取-紫外光谱法测定水样中的己烯雌酚
Pub Date : 2018-01-01 DOI: 10.20431/2349-0403.0507001
Z. Niu, Yingying Wen
A dispersive liquid–liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) combined with ultraviolet spectrometry (UV) method was developed for the determination of diethylstilbestrol (DES) in water samples. Several parameters including sample pH, extraction solution type and volume, dispersion solution type and volume, centrifugation speed and time were systematically investigated. The optimal extraction conditions of DLLME-SFO were: sample pH 3; extraction solution, 200 μL 1-dodecanol; dispersion solution, 400 μL ACN; Centrifugation speed and time, 2500 rpm and 15 min . Under the optimum extraction and determination conditions, good responses for DES were obtained in a range of 0.5 – 12.5 μg/mL, with linear coefficients greater than 0.99. The recoveries of the DES ranged from 70% to 97%. The limits of detection based on a signal-to-noise ratio of 3 was 0.15 μg/mL. The method was applied to the determination of DES in tap and lake water samples with a satisfactory result. The results demonstrated that this DLLME-SFO-UV method was successfully applied to determine DES in water samples.
建立了一种基于悬浮有机液滴固化(DLLME-SFO)的分散液液微萃取-紫外光谱法(UV)测定水样中己烯雌酚(DES)的方法。系统考察了样品pH、萃取液类型和体积、分散液类型和体积、离心速度和离心时间等参数。DLLME-SFO的最佳提取条件为:样品pH为3;提取液为200 μL -十二醇;分散液,400 μL ACN;离心速度和时间,2500转/分钟,15分钟。在最佳提取和测定条件下,DES在0.5 ~ 12.5 μg/mL范围内具有较好的提取效果,线性系数均大于0.99。DES的加样回收率为70% ~ 97%。信噪比为3的检出限为0.15 μg/mL。将该方法应用于自来水和湖泊水样中DES的测定,结果满意。结果表明,DLLME-SFO-UV法可用于水样中DES的测定。
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引用次数: 1
Fluorescence Spectroscopic Study of the Interaction between the Baltic Amber Extract and BSA 波罗的海琥珀提取物与牛血清白蛋白相互作用的荧光光谱研究
Pub Date : 2018-01-01 DOI: 10.20431/2349-0403.0507003
K. Yin, Kaihong Xie, Zhenzhen Liu, Sufang Sun
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引用次数: 0
Synthesis, Spectral and Kinetic Study of Demi-macrocycle of N 2 O 2 with Complex of Co (II) Ion Co (II)离子配合物n2o半大环的合成、光谱及动力学研究
Pub Date : 2018-01-01 DOI: 10.20431/2349-0403.0502004
Sameena Rasheed, M. U. Khan, S. S. Parihar, A. Dwivedi
Macrocyclic metal chelating agents are useful for detecting tumor lssions. 4,5 The chemistry of macrocyclic complexes is also important due to their use in dyes and pigments as-well-as in study of NMR shift reagents etc. 2. EXPERIMENTAL All reagents and solvents used in the present investigation were of analytical grade. 1,2diaminoethane, perchloric acid (HClO4), acetone (CH3COCH3) etc. of Loba, Merck and Aldrich brand. The preparation of solutions, standardization, and procedures for demi-macrocyclic complex formation and their spectral kinetic studies have been performed. The carbon, hydrogen and nitrogen analysis of the samples were carried out microanalytically. Oxygen was determined by different methods. Metal and chloride were determined gravimetrically. The IR spectra (4000-400 cm -1 ) was recorded on a Jasco model 4100 FTIR spectrometer as KBr discs. UV-visible spectra was recorded on a shimedzu 1700 pharmaspectrometer. Conductivity measurements were made in DMSO or nitromethane (10 -3 mho) at room temperature on systronics conductivitymeter. Magnetic susceptibility was measured at 8000 G in a Evans magnetic susceptibility balance using Co[(Hg(SCN)4)] as calibrant and the experimental susceptibilities were corrected for diamagnetic correction with pascal constants.
大环金属螯合剂在检测肿瘤损伤方面是有用的。大环配合物的化学性质也很重要,因为它们可以用于染料和颜料以及核磁共振移位试剂等的研究。本研究中所用的试剂和溶剂均为分析级。Loba、Merck、Aldrich品牌的1,2 -二氨基乙烷、高氯酸(HClO4)、丙酮(CH3COCH3)等。溶液的制备、标准化和半大环络合物形成的程序及其光谱动力学研究已经完成。对样品进行了碳、氢、氮微量分析。氧的测定方法不同。用重量法测定金属和氯化物。红外光谱(4000 ~ 400 cm -1)在Jasco型4100 FTIR光谱仪上以KBr光盘的形式记录。在shimedzu 1700型药谱仪上记录紫外可见光谱。在室温下用DMSO或硝基甲烷(10 -3 mho)在系统电导率仪上测量电导率。以Co[(Hg(SCN)4)]为标定剂,在埃文斯磁化率天平上测量了8000g下的磁化率,并用帕斯卡常数对实验磁化率进行了反磁校正。
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引用次数: 1
Study of the Adsorption Kinetics of Iron Ion from Wastewater using Banana Peel 香蕉皮对废水中铁离子的吸附动力学研究
Pub Date : 2018-01-01 DOI: 10.20431/2349-0403.0503001
S. Shrestha
There is a growing concern for the effective treatment of wastewater contaminated with heavy metal. Most of the heavy metals are highly toxic even in trace concentration [1]. Most of the common methods used to remove heavy metals from wastewater are chemical reduction followed by precipitation, membrane filtration, ion-exchange and adsorption onto activated carbon. Among these, adsorption by activated carbon has been used as an effective method to remove these heavy metals in trace concentration. However, the activated carbon is expensive and requires chelating agents to enhance its performance, thereby increasing treatment cost. For this reason, it is desirable to develop low cost and efficient adsorbent for removal of heavy metals from wastewater. Recently, adsorptions of metals by using bio-adsorbents are in progress [2, 3]. Different types of industrial and agricultural bio-wastes are investigated as bio-adsorbent such as sugarcane bagasse [4], rice husk [5], olive stone [6], clay minerals [7-9], used tea leaves [10], wheat straw [11], chitin and chitosan [12]. They are easily available, economically acceptable and chemically less polluting substances often with high affinity and binding capacity of metals. In adsorption process, metal ions from solution are transported to the surface of the adsorbent and then attached due to the physical and chemical interaction between the metal ions and the functional groups on the surface of the adsorbent [13-19].
重金属污染废水的有效处理日益受到人们的关注。大多数重金属即使在微量浓度下也具有剧毒[1]。去除废水中重金属的常用方法有化学还原、沉淀、膜过滤、离子交换和活性炭吸附等。其中,活性炭吸附法是去除痕量重金属的有效方法。然而,活性炭价格昂贵,需要螯合剂来增强其性能,从而增加了处理成本。因此,开发低成本、高效的吸附剂去除废水中的重金属是迫切需要的。近年来,生物吸附剂对金属的吸附研究进展迅速[2,3]。研究了不同类型的工农业生物废弃物作为生物吸附剂,如甘蔗甘蔗渣[4]、稻壳[5]、橄榄石[6]、粘土矿物[7-9]、废茶叶[10]、麦秸[11]、几丁质和壳聚糖[12]。它们是容易获得、经济上可接受和化学污染较少的物质,通常具有高亲和力和金属的结合能力。在吸附过程中,由于金属离子与吸附剂表面官能团之间的物理化学相互作用,溶液中的金属离子被输送到吸附剂表面并附着在吸附剂上[13-19]。
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引用次数: 6
Pharmacokinetic Study of Hibiscus Rosa-sinenses-L 芙蓉的药动学研究
Pub Date : 2018-01-01 DOI: 10.20431/2349-0403.0505004
B. Pandey, A. Dwivedi, S. Nigam, S. S. Paihar
The pharmacokinetic study of medicinal plants Hibiscus Rosa-sinenses-L (HRS) of malvaceae family in vitro condition have been carried out electrochemically using Ag-Zn pair of electrodes in vitro condition in three different seasons. The investigation shows first to zero order kinetics for complex oscillatory reactions occurring in the system at long span of time. The reaction velocity enhanced by charge transfer of Zwitter ions between biomass and electrodes. The measured activation parameters fully explained the suggested mechanism and activity.
采用银锌对电极,对锦葵科药用植物芙蓉(hishisus rosa -sinense - l, HRS)在3个不同季节的体外药动学条件进行了电化学研究。研究表明,在长时间内,系统中发生的复杂振荡反应的一级到零级动力学。电极与生物质之间的电荷转移提高了反应速度。测定的活化参数充分解释了所提出的机理和活性。
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引用次数: 0
Study on Catalysed Oxidation of Some Aliphatic Hydroxy Acids by N-chlorosuccinimide in Aqueous Acetic Acid Medium n -氯琥珀酰亚胺在醋酸水溶液中催化氧化某些脂肪族羟基酸的研究
Pub Date : 2018-01-01 DOI: 10.20431/2349-0403.0506003
N. Khan, A. Dwivedi, K. Khan, H. Dwivedi
The phosphotungustic acid catalysed oxidation of aliphatic hydroxy acids by halo -oxidant Nchlorosuccinide (NCS) in aqueous acetic acid lead to the formation of corresponding acetone di-carboxylic acid and acetaldehyde. The reaction follows first to zero order kinetic with respect to [NCS] and rate unchanged by hydrogen ion. The rate of oxidation retards with decrease in dielectric constant of solvent. The study showed curvature due to of complex formation between substrates and postulated species HOCl of oxidant. The stoichiometric ratio 1:1 was determined for the reactions. The correlation between enthalpies and free energies of activation is reasonably linear. A suitable mechanism in conformity with kinetics results was proposed.
磷钨酸在醋酸水溶液中催化光环氧化剂NCS氧化脂肪族羟基酸,生成相应的丙酮、二羧酸和乙醛。相对于[NCS],反应从一级到零级动力学,氢离子的反应速率不变。随着溶剂介电常数的降低,氧化速率减慢。研究表明,弯曲是由于底物和假设的氧化剂HOCl之间的复杂形成。测定了反应的化学计量比为1:1。焓和活化能之间的关系是相当线性的。根据动力学结果提出了一种合适的机理。
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引用次数: 0
In - Vitro Antioxidant Activity of Methanolic Extract of the Roots of Bergenia ciliate 根甲醇提取物的体外抗氧化活性研究
Pub Date : 2018-01-01 DOI: 10.20431/2349-0403.0508001
S. Shrestha, S. Awale, S. K. Kalauni
Bergenia ciliata is a wellknown medicinal herb with thick rootstocks, 3.5 to 16.5 cm long. The plant is distributed throughout Nepal at 1300-3000 m in moist, rocky places (Manandhar, 2002). Medicinal and aromatic plants play vital role in for livelihood health and socio-economic prospects of the country.The majority of Nepal’s population, especially tribal, ethnic groups and mountain people relies on traditional medical practices (Ajayi et al. 2011). In many cases this practice is transmitted orally from generation to generation and confined to certain people (Edeogn et al. 2005). In present study plant sample was collected from Manang district of Nepal to analize its antioxidant activity and total phenol and flavonoid content. Antioxidant research is an important topic in the medical field as well as in the food industry. Antioxidants are compounds that protect cells against the damaging effects of reactive oxygen species, such as singlet oxygen, superoxide, peroxyl radicals, hydroxyl radicals and peroxynitrite (Hafiza et al. 2002). An imbalance between antioxidants and reactive oxygen species results in oxidative stress, leading to cellular damage. Oxidative stress has been linked to cancer, aging, atherosclerosis, ischemic injury, inflammation and neurodegenerative diseases (Arutselvi et al. 2012 & Igbinosa et al. 2009). Oxidants are capable of stimulating cell division, which is a critical factor in mutagenesis when a cell with a damaged DNA stand divides. Thus, mutation can arise which in turn is an important factor in carcinogenesis. Both cigarette smoking and chronic inflammation are of the major causes of cancer have strong free radical components in their mechanism of action.Flavonoids may help provide protection against these diseases by contributing, along with antioxidant vitamins and enzymes, to the total antioxidant defense system of the human body. Epidemiological studies have shown that flavonoid intake is inversely related to mortality from coronary heart disease and to the incidence of heart attacks (Tamilarasi et al. 2012). Flavonoids are most commonly known for their antioxidant activity and the capacity of flavonoids to act as antioxidants depends upon their molecular structure. The position of hydroxyl groups and other features in the chemical structure of flavonoids are important for their antioxidant and free radical scavenging activities (Fernandez et al. 2004). Quercetin, the most common dietary flavonol, is a potent antioxidant, because it has all the right structural features for free radical scavenging activity.It is generally assumed that frequent consumption of plant derived phytochemicals from vegetables, Abstract: Bergenia ciliata is an important medicinal plant used in regions where western medicines are inaccessible due to their unavailability and high cost. The methanolic extract of Bergenia ciliataroots was screened for phytochemical constituents and in-vitro antioxidant activity. The plant extract showed the
毛缕草(Bergenia ciliata)是一种著名的药材,根茎粗,长3.5 ~ 16.5厘米。该植物分布在尼泊尔1300-3000米的潮湿、多岩石的地方(Manandhar, 2002)。药用和芳香植物在该国的生计、健康和社会经济前景方面发挥着至关重要的作用。尼泊尔的大多数人口,特别是部落、少数民族和山区人口依赖传统医疗做法(Ajayi等人,2011年)。在许多情况下,这种做法是代代相传的,并且仅限于某些人(Edeogn et al. 2005)。本研究采自尼泊尔马南地区的植物样品,分析其抗氧化活性及总酚和类黄酮含量。抗氧化剂的研究是医学领域和食品工业的一个重要课题。抗氧化剂是保护细胞免受活性氧(如单线态氧、超氧化物、过氧自由基、羟基自由基和过氧亚硝酸盐)损害的化合物(Hafiza et al. 2002)。抗氧化剂和活性氧之间的不平衡会导致氧化应激,从而导致细胞损伤。氧化应激与癌症、衰老、动脉粥样硬化、缺血性损伤、炎症和神经退行性疾病有关(Arutselvi et al. 2012; Igbinosa et al. 2009)。氧化剂能够刺激细胞分裂,这是突变的关键因素,当一个DNA受损的细胞分裂时。因此,突变可能出现,这反过来又是致癌的一个重要因素。吸烟和慢性炎症都是导致癌症的主要原因,在它们的作用机制中都有很强的自由基成分。黄酮类化合物可以通过与抗氧化维生素和酶一起,为人体的总抗氧化防御系统提供保护,从而帮助预防这些疾病。流行病学研究表明,类黄酮摄入量与冠心病死亡率和心脏病发病率呈负相关(Tamilarasi et al. 2012)。类黄酮以其抗氧化活性最为人所知,类黄酮作为抗氧化剂的能力取决于它们的分子结构。羟基在黄酮类化合物化学结构中的位置和其他特征对其抗氧化和清除自由基的活性很重要(Fernandez et al. 2004)。槲皮素是最常见的膳食黄酮醇,是一种有效的抗氧化剂,因为它具有清除自由基活性的所有正确结构特征。摘要/ Abstract摘要:毛缕草(Bergenia ciliata)是一种重要的药用植物,在西药难以获得且价格昂贵的地区被广泛使用。对毛缕根甲醇提取物进行了植物化学成分和体外抗氧化活性的筛选。该植物提取物具有丰富的次生代谢产物来源,具有一定的生物活性。这种植物具有较高的抗氧化活性是由于其含有活性成分,如酚类和类黄酮。采用DPPH自由基清除法测定植物提取物的抗氧化活性。在DPPH自由基清除实验中,纤毛草的IC50值为11.21μg/mL,而标准抗坏血酸的IC50值为45.93μg/mL
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引用次数: 0
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International Journal of Advanced Research in Chemical Science
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