Separation of Some Herbicides by Two Dimensional Thin Layer Chromatography on Calcium Sulphate

Abstract

Two dimensional thin layer chromatography is being used for the last forty years¹ and now it has became an important tool for the separations of varying complexity. Various coating materials such as alumina, cellulose, kieselgel G, silica gel, silufol and polyamide have been used and studied for the separation of organics such as alkaloids, amino acids, carbohydrates, fatty acids, glycopeptides, glycolipids, lipids, phospholipids, pigments, protiens, peptides, pesticides, steroids and inorganics such as oxy acids of phosphorus, metal ions. Our previous work^{2′3′4′5′6} shows that calcium sulphate coated paper and glass plates have a great separation potential for herbicides containing carboxyl group. Therefore now an attempt is made to test the separation potential of calcium sulphate alone and calcium sulphate containing aluminium oxide active neutral, calcium carbonate and p-dimethylaminobenzaldehyde for some nerbicides by two dimensional thin layer chromatography. The results obtained are discxissed in this paper.     

离子色谱法测定硫酸钙样品中的硫酸根

用碳酸钠将硫酸钙样品中的钙沉淀为碳酸钙,释放出硫酸根,用阴离子型离子色谱仪,在40℃柱温下,以6.3 mmol/L Na HCO3–1.7 mmol/L Na2CO3缓冲盐为淋洗液,采用电导检测器测定其中硫酸根的浓度,以间接得到硫酸钙含量。实验结果表明,该法与经典的沉淀重量法测定结果相吻合,两者之间的相对误差为0.29%。样品加标回收率在96.0%~105.3%之间,测定结果的相对标准偏差为0.26%(n=6)。该方法精密度与准确度高,可快速、稳定、可靠地分析脱硫灰渣及石膏样品中的硫酸根含量。     

Paper Chromatography of 34 Organic Acids on Calcium Carbonate and Calcium Sulphate Impregnated Papers

Abstract

Paper chromatographic separations of 34 organic acids on calcium carbonate and calcium sulphate impregnated paper has been developed. Tricarboxylic acids, dicarboxylic acids, amino acids, and keto acids and their derivatives can be separated in simple solvents such as acetone, ethanol, water, aqueous sodium chloride, ammonium chloride and calcium nitrate. Important separations achieved are: Adipic from maleic and malonic, cis-aconitic from I-cystine and nicotinic, citric or tartaric from ascorbic, gallic, malic and salicylic, I-aspartic from arginine-HCl, fumaric and glutamic, barbituric from hippuric and α-ketoglutaric, benzoic from ρ- & m-nitrobenzoic and cis-aconitic from trans-aconitic.     

Sequential Thin-Layer Chromatography of 2,4-D and Related Compounds

Abstract

Separations and identification of carboxylic herbicidal substances such as 2,4-dichlorophenoxyacetic acid, trichloroacetic acid, 2,4,5-trichlorophenoxyacetic acid and plant growth regulators such as benzoic acid, cinnamic acid, indole-3-acetic acid, β-naphthaleneacetic acid, β-naphthoxyacetic acid, phenoxyacetic acid have been made by sequential thin-layer chromatography on calcium sulphate layer with acetone, benzene, carbon tetrachloride, chloroform, ethyl acetate, dioxan, propanol as solvents and bromophenol blue as detector.     

Dipole Moments and Intermolecular Association of Some Carbonyl Compounds in Nonpolar Solvents

The aggregation of some aldehydes in nonpolar solvents was investigated using the static dielectric method. The molecular association of acetone and two of its derivatives (acetophenone and benzophenone) in cyclohexane solvent were also investigated by this method. Analysis of the static dielectric data for solution of these materials indicated a high molecular association. It was found that benzaldehyde and its derivatives have a strong tendency for antiparallel molecular association, whereas acetone and its derivatives have a tendency for parallel alignment. The experimental results show that there is a sensitive relationship between the molecular association and molecular structure of these materials. The influence of solvent on the molecular association of the solute molecules was studied and compared.     

Planar Chromatography in Studies of the Hydrophobic Properties of Some New Herbicides

JPC – Journal of Planar Chromatography – Modern TLC - Reversed-phase planar chromatography has been used to study the hydrophobic properties of sixteen new herbicides. Solute retention...     

离子色谱法同时测定那屈肝素钙中氯离子和硫酸根离子的含量

建立了一种抑制电导检测器离子色谱法同时测定那屈肝素钙中氯离子和硫酸根离子含量的方法.采用强阴离子交换柱,3 mmol/L碳酸钠溶液为流动相,流速2.0 mL/min,柱温30℃,进样量25μL,检测器为配有化学抑制器的电导检测器.结果表明,氯离子和硫酸根离子在1～20μg/m L浓度范围内线性关系良好,氯离子线性方程为...     

Determination of Tetracycline and Related Compounds by High-Performance Liquid Chromatography

Abstract

An isocratic high-performance liquid chromatography method for the determination of tetracycline and its related compounds is described. The method uses a reverse phase (C₁₈) column, a modified acetonitrile/water mobile phase, and banzoic acid as the internal standard. Elution of all compounds of interest is complete within seven minutes. Results are presented for thirteen commercial capsule formulations and are compared with results by microbiological assay and thin-layer chromatographic methods.     

Comparison of Retention Indices of Some Explosives and Related Compounds Calculated by Different Mathematical Methods in Reversed-Phase Liquid Chromatography

In reversed phase liquid chromatography, the retention indices of some neutral and acidic explosives and related compounds (nitramines, nitroaromatics, aminoaromatics, and nitrophenols) based on the alkan-2-one, alkyl aryl ketone, and 1-nitroalkane retention index standards have been determined by the application of a new mathematical adaptation method, viz. a multiparametric least-squares regression iterative method. This method was applied to two types of columns. The first group includes six octadecyl-C₁₈ columns with different packing materials and obtained from different manufacturers, while the second group comprises one octyl-C₈ column. The retention indices have been extensively studied using either methanol-water or methanol-phosphate buffer mobile phase systems. The calculated multiparametric retention indices values were compared with those obtained by Guardino's, Grobler's, and Kovàts' methods. The influences of the concentration of the organic modifier in the mobile phase, aqueous mobile phase pH, and the column packing material on the retention indices of the explosives were also investigated. Good agreement was observed between the retention indices calculated by the use of the four mathematical methods for both neutral and acidic explosives.     

乙醇 /水混合溶剂沉淀制备纳米BaF2及粒径控制

采用水和乙醇混合溶剂沉淀的方法制备了不同粒径的BaF₂纳米粉体。用XRD、TEM和FSEM表征了粉体的粒径和形貌。研究了陈化时间、水和乙醇的体积比对BaF₂纳米粉体的粒径和形貌的影响。结果表明，随混合溶剂中乙醇含量升高，沉淀粒径减小。BaF₂沉淀粒径的倒数和溶剂介电常数的倒数呈线性关系，据此关系可以控制BaF₂纳米粉体的粒径。     

乙醇/水混合溶剂体系中碳酸钙晶体晶型和取向的控制

采用（NH₄）₂CO₃分解法,制备得到了晶型和形貌可控的CaCO₃晶体。研究结果表明,乙醇/水混合溶剂、陈化时间和L-半胱氨酸自组装单层模板对CaCO₃晶体的晶型、取向和形貌都具有重要影响。无单层模板情况下,溶液中主要得到了球霰石,球霰石的形貌随陈化时间从花朵外形变为树叶形。同样的醇/水体系中,在自组装单层上却得到了取向为（104）晶面的方解石。这与水溶液中同一自组装单层上主要获得（001）结晶面的方解石有明显不同。方解石的形貌也随陈化时间变化而改变。陈化时间为3h时,得到具有孔洞结构的方解石;陈化时间为12h时,得到表面光滑的菱面体方解石。     

乙醇/水混合溶剂体系中碳酸钙晶体晶型和取向的控制

采用(NH4)2CO3分解法,制备得到了晶型和形貌可控的CaCO3晶体。研究结果表明,乙醇/水混合溶剂、陈化时间和L-半胱氨酸自组装单层模板对CaCO3晶体的晶型、取向和形貌都具有重要影响。无单层模板情况下,溶液中主要得到了球霰石,球霰石的形貌随陈化时间从花朵外形变为树叶形。同样的醇/水体系中,在自组装单层上却得到了取向为(104)晶面的方解石。这与水溶液中同一自组装单层上主要获得(001)结晶面的方解石有明显不同。方解石的形貌也随陈化时间变化而改变。陈化时间为3h时,得到具有孔洞结构的方解石;陈化时间为12 h时,得到表面光滑的菱面体方解石。     

Analysis of Solvent–Solvent Interactions in Mixed Isosteric Solvents by Inverse Gas Chromatography

The Flory–Huggins interaction parameter, χ ₂₃, characterizing the interaction between solvents in a mixed stationary phase has been calculated using inverse gas chromatography (IGC). The χ ₂₃ parameters for four mixed solvent systems formed by mixing a non-polar branched alkane, 19, 24-dioctadecyldotetracontane (C78), with four different polar solvents are analysed as a function of temperature. Two of the polar solvents are formed by replacing one of the –CH₃ groups of C78 by –OH (POH) group and –CN (PCN) group and the other two polar solvents are formed by replacing all the four –CH₃ groups of C78 by four –CF₃ (TTF) groups and four –OCH₃ (TMO) groups. The five solvents have similar structures and nearly the same molar volume and in mixtures, they form regular solutions. For the mixture, C78 + POH, χ ₂₃ was calculated at two compositions and for the remaining three mixtures χ ₂₃ was calculated at equimolar composition. Eight solute probes representing all possible chemical structures and polarity were used under conditions approaching infinite dilution. The effects of temperature, concentration of the mixed solvent and probe solute on χ ₂₃ are presented and discussed. The probe-independent χ ₂₃ values were also calculated by linear regression analysis using the retention data of all the solute probes. In all the mixed solvents considered here the χ ₂₃ values are probe-dependent and decrease with increase of temperature.     

反相高效液相色谱法测定阿奇霉素及其相关化合物

建立了利用简单流动相组成测定阿奇霉素及其相关化合物的反相高效液相色谱法,色谱柱为InertsilODS 3(150mm×4. 6mm, 5μm),流动相为乙腈水(90∶10,V/V),流速0. 8mL/min,柱温30℃;紫外检测波长为205nm。能够明确地分辨阿奇霉素粗品中5种物质:红霉素6, 9亚胺醚、红霉素9, 11亚胺醚、阿奇霉素前体、甲基化硼酸酯和阿奇霉素。该方法简便快捷,线性关系良好,结果准确可靠,对阿奇霉素合成工艺优化和成品的质量检测均具有指导作用。     

Studies on the Complexation of Transition Metal Ions with Macrocyclic Compounds in Mixed Solvents by Competitive Potentiometry and Polarography

Complexation of Cu(II), Zn(II), Ni(II), Co(II), Pb(II), Cd(II), Cr(III) and Fe(III) ions with 15-crown-5, benzo-15-crown-5, 18-crown-6, dibenzo-18-crown-6, dicyclohexano-18-crown-6, dibenzo-24-crown-8, 5,6,14,15-dibenzo-1,4-dioxa-8,12-diazacyclopentadeca-5,14-diene, 1,4,10-trioxa-7,13-diazacyclopentadecane and cyclam has been investigated in 75% (v/v) DMF+water using the silver(I) ion as an auxiliary cation at 0.05?M ionic strength adjusted with tetrabutylammonium perchlorate (TBAP) by competitive potentiometry. Stability constant values obtained for the metal ion–aza macrocyclic complexes are higher than those for the oxa crowns. Shifts in the peak potential and reduction in the peak current in the differential pulse polarography (DPP) method were also used to determine the stability constants of some of the metal ions with aza and tosylated-aza macrocycles using TBAP as supporting electrolyte in 75% (v/v) DMF+water and 90% (v/v) DMSO+water media. Stability constant values determined both by shifts in the potential and by reduction in the peak current were found to be in good agreement with each other.     

乙二醇和水混合溶剂多组分电解质热力学

在乙二醇和水混合溶剂中恒定乙二醇质量分数w=0.1的条件下，应用经典的电动势方法测定无液体接界电池的电动势: Pt，H2 (105 Pa )│HCl (质量摩尔浓度m)， C2H6O2 (w), H2O (1－w)│AgCl-Ag (A) Pt，H2 (105 Pa )│HCl (mA), NaCl(mB), C2H6O2 (w), H2O (1－w)│AgCl-Ag (B) 根据测得电池(A)的电动势，确定混合溶剂中AgCl-Ag电极的标准电极电势，讨论了HCl的迁移性质.利用电池（B）的电动势，计算出HCl的活度系数γA.结果表明，在溶液中总离子强度保持恒定， HCl的活度系数服从Harned规则.在溶液组成恒定时， lgγA是温度倒数1/T的线性函数. 进一步讨论了混合物中HCl的相对偏摩尔焓和介质效应.     

果糖-水混合溶液中多组分电解质热力学

恒定混合溶液总离子强度I=1.0000 mol•kg－1,改变果糖-水混合溶液中果糖的质量分数w=2.5％、5.0％和7.5％的条件下,应用电动势方法测定下列无液体接界电池(A)和(B)在278.15、283.15、288.15、293.15、298.15、303.15、308.15、313.15、318.15 K等9个温度下的电动势: Pt, H2 (105 Pa)│HCl(m), C6H12O6(w), H2O(1－w)│AgCl-Ag (A) Pt, H2 (105 Pa)│HCl(mA), NaCl(mB), C6H12O6(w), H2O(1－w)│AgCl-Ag (B) 根据测得电池的电动势,计算出混合溶剂中AgCl-Ag电极的标准电极电势和HCl的标准迁移吉布斯自由能、迁移熵和迁移焓; 求出四元混合溶液中HCl的活度系数γA.结果表明在溶液中总离子强度I保持恒定,HCl的活度系数服从Harned规则,进一步讨论了混合物中HCl的介质效应.     

The Synthesis of Some 1, 8-Phenanthrolines and Related Compounds

The synthesis of ethyl 4-oxo-1, 4-dihydro-1, 8-phenanthroline-3-carboxylate (2a) and some other 1, 8-phenanthrolines is reported. The ethylation of the above ester yields a thermochromic product 2b and some ethyl 4-ethoxy-1, 8-phenanthroline-3-carboxylate (3b). Reexamination of similar ethylations of analogous esters derived from 1, 7-phenanthroline and 1, 10-phenanthroline indicated formation of the O-ethyl derivative of the former and the N-ethyl derivative of the latter.