Chromatographic Determination of Polyiodohalides of Organic Nitrogen Bases

The following biologically active polyiodohalides of organic nitrogen bases were synthesized and studied: trimethylbenzylammonium, triethylbenzylammonium, and N-cetylpyridinium diiodochlorides; tetramethylammonium, tetrabutylammonium, and N-cetylpyridinium diiodobromides; and butylcholinium triiodide. A method for the identification of the above compounds was proposed based on the dependence of their thin-layer chromatographic mobility and IR, UV, and NMR spectrometric properties and on the nature of the organic cation and the structure of the polyiodide anion. Reversed-phase high-performance liquid chromatography in a 1 : 1 methanol–water mixture (pH 6.86) was used for determining the compounds under study. The developed procedure is characterized by high sensitivity (0.09–0.51 g) at RSD of no worse than 10%.     

Transport Properties of Selective Membranes Reversible to Nitrogen-Containing Organic Base Cations: Permeability and Ion Flow

Main transport properties were studied for selective membranes with low dielectric constants based on liquid ion exchangers involving nitrogen-containing organic base cations. Permeabilities and ion flows through a membrane were calculated for major and interfering ions. Dependences of the transport properties of membranes on the concentrations of the ion exchanger and near-membrane solution and their potentiometric characteristics are presented. It was demonstrated that the transport properties of liquid membranes are determined by two main factors: the transfer of counterions through the phase boundary by the extraction–exchange mechanism and the leaching of the ion exchanger from the membrane.     

Selective Spectrophotometric Determination of Aluminium in the Presence of Beryllium and Lanthanide Cations

 A spectrophotometric method for the selective determination of Al(III) in the presence of Be and lanthanide cations is proposed. It is based on the selective reaction of Semi-Xylenol Orange with Al(III) at pH 2.6. The presence of 8% v/v of 1,2- ethanediol serves to stabilize the chelate formed by heating for 5 min at 100 °C. 0.5 mg each of Be(II), Ce(III), La(III), 4 mg of Mn(II), 1.2 mg of Pb(II), 1 mg of Tl(I), 40 mg each of Ca(II) and Mg(II) and 1.9 mg of sodium dihydrogen phosphate are tolerable. A ligand buffer of HEDTA-Pb is incorporated to further enhance the selectivity of the color reaction. Under the specified condition Semi-Xylenol Orange reacts with Al(III) to form a 1:1 chelate, its molar absorptivity at 526 nm was found to be 3.3 × 10⁴ L mol⁻¹ cm⁻¹. The linear regression equation for 2–20 μg of Al(III) is A = 0.04458C + 0.0112 (here C stands for the concentration of Al(III), μg per 25 mL), and correlation coefficient γ = 0.9988. The RSD at a level of 10 μg (n = 10) and LOQ were found to be 3.5% and 2 μg respectively. Author for correspondence. E-mail: weston@online.sh.cn Received November 15, 2002; accepted February 11, 2003 Published online June 13, 2003     

Selective Spectrophotometric Determination of Aluminium in the Presence of Beryllium and Lanthanide Cations

A spectrophotometric method for the selective determination of Al(III) in the presence of Be and Ln (lanthanide) cations is proposed. It is based on the selective reaction of SXO (Semi-Xylenol Orange) with Al(III) at pH 2.6. The presence of 8%v/v of 1,2-ethanediol serves to stabilize the chelate formed by heating at 100°C for 5min. 0.5mg each of Be(II), Ce(III), La(III), 4mg of Mn(II), 1.2mg of Pb(II), 1mg of Tl(I), 40mg each of Ca(II) and Mg(II) and 1.9mg of sodium dihydrogen phosphate are tolerable. A ligand buffer of HEDTA-Pb is incorporated to further enhance the selectivity of the color reaction. Under the specified conditions SXO reacts with Al(III) to form a 1:1 chelate. Its molar absorptivity at 526nm was found to be 3.3×10⁴Lmol^–1cm^–1. The linear regression equation for 2–20µg of Al(III) is A=0.04458C+0.0112 (where C stands for the concentration of Al(III), µg per 25mL) and correlation coefficient =0.9988. The RSD at the level of 10µg (n=10) and LOQ were found to be 3.5% and 2µg, respectively.     

海水化学需氧量的光度法测定

海水中有机污染物在强碱性条件下可被高锰酸钾氧化,通过对生成物溶液中锰酸钾浓度的吸光度测量（λ-430 nm）,测定海水中化学需氧量（COD）。该法的线性范围为0．40～4．50mg／L（以邻苯二甲酸氢钾＋甲酸钠体系为标准溶液）;测定海水COD的相对标准偏差（RSD）为15．6％,回收率为89％～115％。     

化学法同时测定含氮有机化合物的碳和氮

建立了一个新的化学分析方法，即含氮有机化合物与催化剂、氧化剂相混和，在氧气流下于空气浴上加热分解，Ｃ转变成ＣＯ２，用稀ＮａＯＨ溶液吸收，以标准ＨＣｌ溶液滴定；Ｎ转变成ＮＨ３，以克达尔定氮法测定，测定误差都小于±０．５％。     

Spectrophotometric Determination of Water Content in Alcohol Organic Solvents

In this work, the absorption spectral characteristics and color‐change reaction mechanism of cobalt(II) chloride(CoCl₂) in alcohol organic solvents has been investigated in the presence of water, and then the optimum conditions for determining the water content in the solvents were selected. Results indicated that the absorption spectra of CoCl₂ in alcohols decreased with the increment of water content. At the maximum absorption wavelength of 656 nm, there were good linear relationships between the logarithm of the absorbance and the water content in organic solvents such as ethanol, n‐propanol, iso‐propanol and n‐butanol with related coefficients in the range of 0.9996?0.9998. For determining water content in organic solvents, this method is simple, rapid, sensitive, reproducible and environmentally friendly. Furthermore, the linear range cannot restrict determination of the water content in organic solvents. This method had been applied to determine the water content in ethanol and n‐butanol with satisfactory recovery of water in n‐butanol between 98.41%?101.29%.     

苯芴酮分光光度法测定有机锗饮料中的锗

介绍了测定有机锗饮料中的锗的苯芴酮分光光度法。     

有机溶剂中微量水分的测定

绕丹宁与水在有机溶剂中发生诱导荷移反应,产生吸收光谱移动且吸收峰增大。基于此,优化了实验条件,建立了一种快速、简便、灵敏的测定有机溶剂中微量水分的新方法。甲醇、醋酸溶剂中的水分含量分别在3％-10％（φ）、0～4％（φ）范围及乙醇、1-丙醇、丙酮、乙酸乙酯溶剂中水分含量在0～5％（φ）范围内与吸光度（A）呈线性关系。其相关系数分别是0．9992、0．9996、0．9992、0．9982、0．9990和0．9995。使用本方法测定了灯用酒精中水分含量,结果令人满意。     

等色点光度法测定指示剂类有机试剂的纯度

等摩尔连续变化法中部分吸收光谱（ＣＲ〉ｎＣＭ）相交形成一个等色点,另一部分光谱（ＣＲ〈ｎＣｍ）则不交于该等色点。我们利用等色点吸光度值与另一部分光谱在该波长吸光度值之比,可计算出试剂纯度。方法不依金属为基准,操作简单,结果可靠。     

有机溶剂中微量水的荷移光谱法测定

研究了氯冉酸与有机溶剂中水的反应，确定了反应条件，氯冉酸与水的络合物的最大吸收波长为530nm。在乙醇、甲醇，正丙醇，异丙醇、正丁醇，正庚醇，正己醇溶剂中，水的含量分别在0－5％（V／V）或0－8％（V／V）范围内呈线性关系，相关系数为0．998或0．999；该方法重现性好，灵敏度高，操作简单，用于测定乙醇中微量水的含量，与标准值相符；加入回收法测得甲醇中水的回收率分别为98％－103％，结果令人满意。     

Applications of Ion-Selective Electrodes in Organic Microanalysis: Potentiometric Determination of Organic Cations Precipitated by Tetraphenylborate

Summary Sodium tetraphenylborate has been used in the potentiometric precipitation titration of various water-soluble organic cations, mostly containing a quaternary ammonium moiety. Emf's were monitored with a fluoroborate ion-selective indicator electrode and a double-junction reference electrode. The perchlorate and nitrate electrodes also respond to the various cations. The solid-state cyanide electrode responds to most of the cations investigated. This makes it possible to carry out titrations in partially nonaqueous media. Some of the compounds which can be determined are alkaloids, dyes, and other organic bases.

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Anwendung ionenselektiver Elektroden (ISE) in der organischen Mikroanalyse: potentiometrische Bestimmung organischer Kationen nach Fällung mit Tetraphenylborat

Zusammenfassung Natriumtetraphenylborat wurde zur potentiometrischen Fällungstitration verschiedener wasserlöslicher organischer Kationen verwendet, von denen die meisten einen Rest einer quartären Ammoniumbase enthielten. Die EMK wurde mit Hilfe einer Fluoroborat-ISE und einer double-junction Bezugselektrode gemessen. Perchlorat- und Nitratelektroden eignen sich gleichfalls für verschiedene Kationen. Die Festkörper-Cyanid-Elektrode reagiert mit den meisten der untersuchten Kationen. Infolgedessen kann man die Titrationen in teilweise nicht-wäßrigen Medien durchführen. Zu den analysierbaren Kationen gehören Alkaloide, Farbstoffe u. dgl.

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This paper is dedicated to the memory of my father, Dr. Sigmund Selig, who died in April 1980.

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Work performed under the auspices of the U. S. Department of Energy by the Lawrence Livermore Laboratory under contract number W-7405-ENG-48.     

紫外光降解-离子色谱法测定液晶材料中有机分子上的碱、碱土金属和铵

采用紫外光降解－离子色谱法测定了液晶材料中的阳离子。研究了样品光降解的条件，H2O2及酸的影响，样品基体有机物的去除，并对直接水溶样品，超声提取样品和光解样品和光解样品测定结果进行了对比。结果表明：3种样品中均含有Na^ ,NH4^ ,K^ ,Mg^2 ,Ca^2 5种阳离子，但光解样品中5种阳离子的含量分别是超声提取及直接水溶样品中含量的3．5－19．7倍和10．6－46．6倍。对液晶样品进行光解测定阳离子时无需加入H2O2氧化，光解后无需对样品进行酸化。Na^ ,NH4^ ,K^ 在光解1.5h时响应值达到最大，Mg^2 ,Ca^2 在2h时光解最完全。5种阳离子加标回收率为71．5％－107．6％。本方法对测定有机化合物上结合的阳离子有一定的参考价值。     

Ion-Selective Electrodes for the Determination of Nitrogen-Containing Medicinal Substances

Stoichiometric ratios and solubility products were determined for medicinal substance–tetraphenyl borate ion pairs. The influence of the nature of the medicinal substance cation incorporated into ionophores and the effect of the solvent–plasticizer on analytical characteristics were studied. The optimal composition of membranes was determined. Ion selective electrodes were used for the potentiometric determination of dimedrol, papaverine, novocaine, and lidocaine in medicinal forms.     

甲烷与含氮有机杂环化合物吸附作用的DFT研究

根据煤中氮的存在形式,提炼出11种具有不同杂化方式及含氮量的有机环状化合物.应用密度泛函理论(DFT)模拟方法对甲烷在这11种含氮化合物上的吸附模型进行结构优化,并结合吸附能、电荷分布及静电势能面的分析,从微观角度考察了甲烷与这些化合物之间的相互作用.计算结果表明:甲烷与含氮化合物的相互作用能在3.81-6.82kJ·mol-1范围内,且通过氢键和静电力相互作用;当化合物中氮的杂化方式为sp2时,其与甲烷的作用能大于sp3杂化方式的;当化合物中的氮含量增加时,可以提供更多的甲烷吸附位点.     

离子色谱法测定高氯、高钠油田回注水中的阴、阳离子及有机酸

建立了高氯、高钠油田回注水中痕量无机阴、阳离子和有机酸的离子色谱分析方法。对高钠基质中痕量阳离子的测定,选用IonPac CS12A分析柱、H2SO4溶液梯度淋洗、电导检测器检测;对高氯基质中阴离子及有机酸的测定,选用对OH-具有高选择性的高容量的IonPac AS11-HC柱、KOH梯度淋洗、电导检测器检测。在优化的梯度淋洗条件下,高氯或高钠的存在不影响痕量阴离子或阳离子的测定。该方法具有良好的线性(r=0.9926~0.9990)和精密度(测定组分峰面积的相对标准偏差(n=7)在8.0%以下),回收率     

On the Problem of the Tetrafluoroborate Ion State in Complexes with Nitrogen-Containing Organic Bases

Using a number of Cu(II), Zn(II), and Cd(II) tetrafluoroborate complexes with nitrogen-containing organic bases as examples, the possible existence of two states of the BF₄ ^– ion, namely, the "half-coordination" and counter-ion states, was studied. It was found that in [ML₂(BF₄)₂] complexes with strong organic bases (L), the "half-coordination" of the anion exists. As the electron-donating ability of the ligand increases, the interaction between the tetrafluoroborate ion and the metal atom becomes more efficient.     

Spectrophotometric Determination of Copper(II) as the Azide Complexes,in the Presence of Iron(III) Cations

Abstract

A method for the spectrophotometrio determination of copper(II), in the presence of iron(III) cations (excess), was stablished. The masking of iron is made with sodium fluoride salt in 50 % (v/v) water/acetone medium. In the recommended conditions, absorbances for cupric complexes are measured at 435 nm where molar absorptivity is 6.00 × 10³ 1 mol^?1 cm^?1.

The stable ayetern obeys Beer's law and is suitable for the copper determination in concentration range from 2.0 to 9.0 mg 1^?l. The iron(III) ion interference (until ca. 600 mg 1^?l) can be completely suppressed. The influence of diverse ions and several others factore were studied.

The results show that copper(II) can be accurately determined by azide apectrophotometric method, if the samples were suitablely treated by the recommended procedure.     

Hydrogen-Bonded Organic Frameworks: Functionalized Construction Strategy by Nitrogen-Containing Functional Group

The construction of hydrogen-bonded organic framework materials by intermolecular hydrogen bonding forces has been rapidly developed in the last decade, among which, the strong intermolecular hydrogen bonding and functional binding sites exhibited by nitrogen-containing functional groups have made them favorites for designing organic components to customize functionalized porous materials. This review systematically introduces the types of nitrogen-containing monomers used to prepare porous hydrogen-bonded organic backbones and the principles of their construction, summarizes the design advantages of crystalline materials from an elemental perspective, and presents the applications of such HOFs in the fields of gas adsorption/separation, molecular recognition, plasmonic conductivity, biomedical, and luminescent materials, etc. Finally, the prospects for the development of such materials are discussed and potential directions for future work are analyzed.     

络合物稳定常数及有机试剂纯度的光度法测定

利用摩尔比法先测出络合物的表观稳定常数，再通过物料平衡及线性回归处理，建立了在不纯试剂体系中同时测定络合物稳定常数及试剂纯度的新方法，方法用于Cu-5-Cl-PADAB体系，结果满意。