Determination of pKa values of alendronate sodium in aqueous solution by piecewise linear regression based on acid-base potentiometric titration

As a mono-sodium salt form of alendronic acid,alendronate sodium presents multi-level ionization for the dissociation of its four hydroxyl groups.The dissociation constants of alendronate sodium were determined in this work by studying the piecewise linear relationship between volume of titrant and p H value based on acidbase potentiometric titration reaction.The distribution curves of alendronate sodium were drawn according to the determined p Ka values.There were 4 dissociation constants(pKa_1=2.43,pKa_2=7.55,pKa_3=10.80,pKa_4=11.99,respectively) of alendronate sodium,and 12 existing forms,of which 4 could be ignored,existing in different p H environments.

Spectroscopic study on variations in illite surface properties after acid-base titration

FT IR, Raman microscopy, XRD, 29 Si and 27 Al MAS NMR, were used to investigate changes in surface properties of a natural illite sample after acid base potentiometric titration. The characteristic XRD lines indicated the presence of surface Al Si complexes, preferable to Al(OH) 3 precipitates. In the microscopic Raman spectra, the vibration peaks of Si O and Al O bonds diminished as a result of treatment with acid, then increased after hydroxide back titration. The varied ratio of signal intensity between IV Al and VI Al species in 27 Al MAS NMR spectra, together with the stable BET surface area after acidimetric titration, suggested that edge faces and basal planes in the layer structure of illite participated in dissolution of structural components. The combined spectroscopic evidence demonstrated that the reactions between illite surfaces and acid leaching silicic acid and aluminum ions should be considered in the model description of surface acid base properties of the aqueous illite.

Investigation of a Simple and Cheap Source of a Natural Indicator for Acid-Base Titration: Effects of System Conditions on Natural Indicators

This study investigated a natural indicator for acid-base titration which is extracted from guinea corn leaves popularly called “waakye leaves” in Ghana. Four types of acid-base titration were studied: strong acid versus (v/s) strong base, strong acid versus weak base, weak acid versus strong base, and weak acid versus weak base. The indicator color change, pH range and the average titre values were determined for each type of acid-base titration. These values were comparable to those obtained from three standard indicators: methyl orange, methyl red and phenolphthalein. Total flavonoids (TF) and condensed tannin (CT) from the crude leaves extract were determined which might be the major reasons for the activity of the extract as an indicator for simple acid-base titration. The authors suggest that the natural indicator is cheap, available, simple to extract, user and environmentally friendly and could be an excellent replacement for standard indicators.

Triphenylmethanol and Tris(2-(hydroxymethyl)phenol) Derivatives: Synthesis and Application as Indicators for Acid-Base Volumetric Titration

Polyphenols are naturally occurring compounds found largely in fruits, vegetables, cereals and beverages. Currently, there is much interest in the potential health benefits of dietary plant polyphenols as antioxidants. The effect of polyphenols on human cancer cells is most often protective and induces a reduction in the number of tumors or rate of growth. During our course of study on anticancer prodrugs, twelve triphenylmethanol and one tris(2-(hydroxymethyl) phenol derivatives were synthesized as a carrier of several drugs with optimized lipophilicity. Besides application of these compounds as a foundation for anticancer drug delivery systems, these compounds were evaluated as indicators for the acid-base volumetric titration of a standard solution of hydrochloric acid with a standard solution of sodium hydroxide. The experiments indicated a moderate-to-sharp color transition of the solutions near the neutralization point for most indicators. These indicators may have potential applications for acid-base titrations in a narrow range.

QUANTITATIVE ANALYSIS OF VERY WEAK ACID AND BASE BY pH-FIXED TITRATION METHOD

pH-fixed titration method for the determination of weak acids and bases has been studied in this paper.It is not necessary to know the ionization constant of weak acid or base and the concentration of titrant. This method had been applied to determine phenol,4-aminoantipyrine and glycine,whose ionization constants range from 10^(-10)to 10^(-12).The results were satisfactory.

DIRECT TITRATION OF VERY WEAK ACIDS(BASES)IN AQUEOUS SOLUTION WITH STRONG BASES(ACIDS)USING VISUAL END-POINT INDICATION WITHOUT INDICATOR

This paper reports a new method of titration for very weak acids and bases using the appearance of incisions on oscillopolarogram to indicate the end-point.This method has the advantages of rapidity,simplicity,no indicator needed as well as good precision.

Acid-base characterization of foursulfide minerals

The amphoteric properties of four sulfide minerals were characterized byacidimetric-alkalimetric titration. Chalcocite, galena, and sphalerite were found to bediprotic acids, while pyrite was determined to be a triprotic acid. Intrinsic acidity con-stants for the four minerals are as follows: chalcocite-pK_(a1)=5.25, pK_(a2)=9.68;galena- pK_(a1)=5.26, pK_(a2)=9.62; sphalente- pK_(a1)= 5.08, pK_(a2)= 9.13;and pyrite - pK_(a1) = 3.50,pK_(a2)=5.32, pK_(a3)=9.81.

Modeling of titration experiments by a reactive transport model

Acid mine drainage（AMD） is commonly treated by neutralization with alkaline substances.This treatment is supported by titration experiments that illustrate the buffering mechanisms and estimate the base neutralization capacity（BNC） of the AMD.Detailed explanation of titration curves requires modeling with a hydro-chemical model.In this study the titration curves of water samples from the drainage of the As Pontes mine and the corresponding dumps have been investigated and six buffers are selerted by analyzing those curves.Titration curves have been simulated by a reactive transport model to discover the detailed buffering mechanisms.These simulations show seven regions involving different buffering mechanism.The BNC is primarily from buffers of dissolved Fe,Al and hydrogen sulfate.The BNC can be approximated by：BNC = 3（C_（Fe） ＋ C_（Al）） ＋ 0.05C_（sulfate）,where the units are mol/L.The BNC of the sample from the mine is 9.25×10^（-3） mol/L and that of the dumps sample is 1.28×10^（-2） mol/L

Python在酸碱滴定分析教学中的应用

基于Python自主设计开发的图形用户界面(GUI)酸碱滴定学习软件,实现了一元强酸(碱)、一元弱酸(碱)、多元酸(碱)和混合酸(碱)等不同酸碱体系滴定曲线图像的可视化绘制,化学计量点和滴定突跃范围以及滴定误差的计算。软件的运用使得教学内容更加直观、形象化,有助于获得滴定曲线变化的感性认识,深刻理解其概念与原理。

Interaction of bovine serum albumi with two alkylimidazolium-based ionic liquids investigated by microcalorimetry and circular dichroism

The interactions of bovine serum albumin (BSA) with two alkylimidazolium-based ionic liquids, 1-butyl-3-methylimidazolium tetrafluoroborate ([bmim]BF4) and 1-butyl-3-methylimidazolium hexafluorophosphate ([bmim]PF6), in buffer solutions at pH 7.0 were investigated by isothermal titration calorimetry (ITC) and circular dichroism (CD). CD spectra showed that the two ionic liquids changed the secondary structure of BSA. Data process was based on the supposition that there were several independent types of binding sites on each BSA molecule for the two ligand molecules. The results obtained by using this supposition combined with Langmuir adsorption model showed that there were two types of such binding sites. One was the high affinity binding site, and the other was the low affinity binding site. The binding constants, changes in enthalpy, entropy and Gibbs free energy for the two types of binding were obtained, which showed that the two types of binding were driven by a favorable entropy increase. Furthermore, for either the ionic liquids, the number of the high affinity binding sites is much smaller than that of the low affinity ones. These results were interpreted with the molecular structure of BSA and the different substituent groups on imidazole ring of the two ionic liquid molecules.

萃余水相中酸和铀的连续测量方法

萃余水相中的酸浓度、铀浓度一般需分开检测,操作步骤繁琐,工作量大。本研究建立了连续测量萃余水相中酸浓度和铀浓度的新方法:先以强碱为滴定剂,通过指示剂的变色指示滴定终点,检测酸浓度;再加入硫酸和偶氮胂Ⅲ溶液,使溶液显色,在650 nm处测量显色溶液的吸光度。结果显示,酸浓度测量的精密度为1.53%,示值误差为1.69%;铀质量浓度测量精密度为1.13%,示值误差为1.52%。在实际水样测量中,本方法和实验室现行方法测量数据基本一致,酸浓度测量的加标回收率为97.0%~102.5%,铀质量浓度测量的加标回收率为97.0%~102.0%,本方法可准确、快速、连续监测萃余水相中的酸浓度和铀浓度。

流动注射法检测枸杞中二氧化硫残留量的方法比较及风险评估

近年来自动化检测设备以及对应方法相继涌现,本研究使用在线蒸馏-流动注射法与国标中酸碱滴定法、离子色谱法对枸杞中二氧化硫残留量进行检测比较。结果表明,三种方法的测定结果并无显著性差异。在线蒸馏-流动注射法RSD在1.5%~2.4%之间,加标回收率在86.1%~92.7%之间,因其具有自动化程度高、检测周期短的优势,更适合大批量样品的快速准确检测。用在线蒸馏-流动注射法对106批次红枸杞中的二氧化硫残留量进行检测分析,并对枸杞中的二氧化硫残留量进行暴露风险评估。结果显示,二氧化硫超标率达21.7%,枸杞中二氧化硫残留尚未对健康构成威胁。

采用酸碱滴定法测定葡萄发酵饮料中二氧化硫含量结果的不确定度评定

对酸碱滴定法测定葡萄发酵饮料中二氧化硫含量不确定度进行有效评定,找出影响其不确定度的关键因素。通过酸碱滴定法测定葡萄发酵饮料中二氧化硫的含量,建立相关的数学模型,并对各不确定度分量进行计算和评定。结果显示:当置信水平为95%,包含因子为k=2时,葡萄发酵饮料中二氧化硫的含量为(39.1±0.4)mg/L。检测结果的不确定度主要来源于样品重复性测定和滴定过程,另外,标准溶液的标定和稀释过程也是影响不确定度的关键因素。

酸碱滴定教学中的动态演示探讨

酸碱滴定是《分析化学》课程中的重点内容,因其涉及分布系数、酸碱平衡的计算、指示剂的变色原理等难点,知识点及相关公式较多,计算复杂,概念也比较抽象,笔者研发了基于C#编程语言的酸碱滴定曲线虚拟动态演示系统,包括酸碱组分分布系数、酸碱滴定曲线及酸碱指示剂三个动态演示模块、将晦涩难懂的理论知识转变为具有动态可视化和趣味性的虚拟平台,以提高学生的计算及创新应用能力。

酸碱滴定法优化香蕉磷脂酶A活性测定及炭疽病胁迫下其活性变化研究

植物磷脂酶A(phospholipase A,PLA)是细胞膜磷脂代谢中的关键酶,可以催化磷脂分子上多个功能基团发生裂解生成信号分子,参与调节植物生长发育以及环境和生物胁迫,具有重要研究价值。本研究主要考察底物浓度、反应温度、缓冲溶液pH、缓冲溶液体积、反应时间等多种因素对香蕉PLA催化卵磷脂水解活性的影响,从而优化磷脂酶A活性测定方法,进一步根据最佳测定条件研究炭疽病胁迫下香蕉PLA活性的变化趋势。结果表明,酸碱滴定法测定香蕉PLA活性的优化条件:反应体系pH 9,底物浓度为4 g/L,反应温度为55℃,底物为15 mL,酶粗提液为3 mL,提取缓冲液体积与果皮重量的比值(mL/g)为3,反应时间为7 h。在最优条件下对炭疽病胁迫下的香蕉果皮组织进行PLA活性测定,发现果皮的病害程度与PLA活力呈正相关,即随着病害程度加深,PLA活性增大,且远大于对照组。表明PLA活性大小可能与果实的抗性有关,随着果实病害程度加深,PLA活性增大,膜磷脂降解,细胞膜的完整性被破坏,从而导致果实腐烂。本研究明确了一种方便可行的香蕉PLA活性测定方法,为深入研究香蕉PLA的催化作用机制奠定基础。

酸中性土壤交换性盐基总量检测方法的影响因素

目前,酸中性土壤交换性盐基总量的检测方法主要为乙酸铵交换-中和滴定法,其特点为步骤繁杂、操作难度大,也是全国“三普”内业指标实验中的技术难点之一。通过采用多类土壤标准物质为研究对象,探讨样品质量、交换试剂、检测方式对盐基总量的影响,并对土壤交换性盐基总量与交换性盐基各离子之间的相关性进行分析。结果表明,高含量盐基样品ASA-7a在添加与不添加EDTA的乙酸铵溶液交换下,电感耦合等离子体发射光谱(ICP-OES)测定的加和盐基总量值分别为(34.71±0.10)、(33.26±0.18) cmol/kg,中和滴定检测后一交换液的值则偏高,达到(38.80±0.62) cmol/kg,并且不同交换试剂间和检测方式间均有一定差异性(P<0.05),但样品质量的多少对盐基总量的结果无显著影响(P>0.05)。对于选取土壤样品,尽管ICP-OES测定加和盐基总量的相对误差RE与相对标准偏差RSD分别小于7%、1.2%,其精密度与准确度均优于中和滴定法,两种检测方式结果仍然在标准参考值范围内。但是,对于更多类型和批量样品土壤交换性盐基总量的测定与数据的比对统计分析,建议遵照统一的规程并保持方法的一致性,避免因方法的不同而增大结果的差异性。

自动充氮蒸馏-酸碱滴定法测定食品中二氧化硫

目的 建立自动充氮蒸馏-酸碱滴定法测定食品中二氧化硫残留量的分析方法。方法 称取20 g(或m L)均质试样,加入350 mL纯水后进行充氮酸化蒸馏,以50 mL 3%过氧化氢溶液为吸收液,加盐酸溶液(6 mol/L)10 mL,氮气流量1.50 L/min,蒸馏时间90 min,微沸功率350 W,用0.01 mol/L或0.1 mol/L氢氧化钠标准溶液进行滴定。结果 增加纯水添加量使测定结果轻微下降。加标实验有基质选择性,亚硫酸钠溶液的储存时间与加标回收率负相关。乙酸是阳性干扰物,能使检测结果显著偏高。本方法的相对标准偏差为0.5%~2.1%,回收率范围为86.0%~96.3%,最低检出限和定量限为0.5 mg/kg和5 mg/kg。对9类98批食品进行检测,结果显示百合干和淮山干的检出率与超标率最高。结论 该方法稳定、操作简便,测定结果准确度高、精密度好,适用于食品(不含乙酸)中二氧化硫残留量的测定。

分析化学教学中的课程思政案例研究

对分析化学教学中和实际生活生产过程联系密切的知识点进行充分挖掘和扩展,梳理归纳了一些典型的课程思政案例。这些案例契合教学大纲中教学重点和教学难点的要求,以相应的知识点作为载体,既能让学生掌握大纲要求的理论知识点,又能实现三全育人的目标。通过这些案例的引入和渗透,可以让学生面对充满逻辑性和晦涩难懂的分析化学课程时,感受到课程和实际生产生活的息息相关性,在和风细雨的课堂教学中达到知行合一的境界。

六甲基二硅烷胺钠的合成工艺改进

在已报道的方法上,使用六甲基二硅烷胺和氢化钠在无溶剂条件下合成了六甲基二硅烷胺钠,改进了反应的温度、时间、物料配比,最佳收率能够达到99.2%。目标化合物的结构经核磁氢谱(H nuclear magnetic resonance spectrum,1H NMR)、红外光谱(infra-red spectrum,IR)和高分辨质谱(high resolution mass spectrometer,HRMS)确证。后续阶段新加入洗涤步骤,减少后处理时间,提高了产品摩尔浓度。改进后的工艺操作简便,成本较低,最终产品为清澈透明的淡黄色溶液,且产品摩尔浓度与性状符合市场产品质量的标准。

酸碱滴定终点误差及软件解析

酸碱滴定的终点误差是分析化学理论教学中的重点和难点之一,目前通行的教材均按照不同的滴定体系,导出大量公式进行误差计算,不仅过程复杂,而且大都为近似计算。本文尝试推导一种统一以滴定剂体积表达的终点误差公式,并将滴定剂在到达计量点和滴定终点时所对应的体积予以数值化,以准确求取滴定终点误差值。相关实例显示,该法可大大降低计算难度,有效减轻教学负担。此外,本文提出采用MATLAB将算法程序化,以进一步提升教学效率。