Thin-Layer Chromatography of Metal Ions Complexed with Anils (V). Detection,Separation and Determination

Abstract

p-Diethylaminoanil of phenylglyoxal a bidentate ligand was used for complexation with Hg(II), UO₂(II), Au(III), Pt(IV) Mg(II), Bi(III), Sb(III) and Be(II) ions. The chelates were characterized by their analysis, molar conductance and infrared spectra. T.L.C. detection, separation and determination of these complexes on starch bound silica gel layers was studied Long persisting dark coloure of the complexes rendered the spots self descernible and no locating agent was required. A maximum four complexes could be resolved and identified. Errors in determinations and maximum separation limits were also deduced.     

Thin Layer Chromatography of Metal Ions Complexed with Anils Part - VI

Abstract

Thin layer chromatographic detection, separation and determination of Ti(IV), UO₂(II), Au(III) and Hg(II) complexes with λ - and β - naphthylanils of methylenediglyoxal have been made on silica gel layers. No locating agent was used as the complex spots were self evident in day light.     

Separation Studies of Metal Ions in Sodium Thioglycolate Medium by Thin Layer Partition Chromatography

Abstract

A thin layer partition chromatographic method has been developed for separation of Fe(III), Ni(II), Zn(II), Cu(II), Pb(II) and Mn(II) on thin layers of silica gel-G as an adsorbent. The R_f values were determined using 0.01–0.2 aqueous solution of sodium thioglycolate as a mobile phase. The dependence of R_f values on the migration time, pH and concentration of mobile phase has been studied. The optimum conditions for possible 3-component separation have been determined. Metal ions have been separated, detected, eluted and quantitatively determined by atomic absorption spectroscopy. The present method was applied to the separation and determination of zinc in forensic samples.     

Separation and Identification op Metal Ions by Reversed Phase Then Layer Chromatography

Abstract

Conditions for the simultaneous separation and identification of as many as ten different metal ions have been established using the technique of reversed-phasethin-layer chromatography. Complete resolution of the ten ions in sub-microgram amounts was achieved using a liquid ion exchanger supported on cellulose. The total time for the analysis was 3–4 hours.     

低压离子分离-化学发光在线检测过渡金属离子

 研究了低压离子 (LPIC)分离 柱后鲁米诺化学发光 (CL)检测方法 ,并分离测定了Cu2 + ,Co2 + ,Cr3 + ,Fe2 + ,Mn2 + 等 5种过渡金属离子。以草酸 柠檬酸混合溶液作为洗脱液 ,Luminol H2 O2 Mn + 作为化学发光检测体系 ,对过渡金属离子进行在线检测。测定的线性范围分别为 (mg·L-1) :Co2 + ,0 0 0 1～ 0 .1;Cu2 + ,0 1～ 6 ;Mn2 + ,0 0 6～ 4 ;Fe2 + ,0 0 3～ 5 ;Cr3 + ,0 0 2 5～ 1。检测限分别为 (μg·L-1) :Co2 + ,0 85 ;Cu2 + ,85 ;Mn2 + ,4 2 ;Fe2 + ,2 1;Cr3 + ,2 0。     

离子相互作用色谱法分离金属离子的研究

离子相互作用色谱在无机离子的分离和分析中潜力很大。它通过离子相互作用试剂,能容易控制或改变柱交换容量或分析物的保留值,分离效率高,可快速完成多组分的同时分离。 在ODS固定相上涂敷阳离子型的十六烷基吡啶(CPI),使金属离子成为阴离子型的氨羧络合物,因不同金属氨羧络合物与CPI的作用程度不同从而可使金属离子分离。金属氨羧络合物亲水性很强,在键合相上的吸附作用可忽略,流动相中不需加入有机溶剂,因此络合物     

Thin Layer Chromatographic Detection and Separation of Metal Ion Complexes with Tridentate Schiff Base

The Tridentate chelating, system present in Salicylidine o-amino benzoic acid was used for complexation with Cu (11), Ni (11), Co (11) and Pd (11). The thin-layer chromatographic (TLC) detection and separation of these complexes on Silica gel (G) layers was studied. The coloured spots of the complexes were quite visible without any visualizing agent. A maximum of four complexes could be resolved and identified. The coloured zones were eluted with solvent and characterise by elemental analysis and spectral studies. Colour of the complexes at λ_max was measured.     

The Effect of Substituent Groups on the Migration of Metal Ions in Thin Layer Chromatography

Abstract

A reverse phase thin layer partition chramotography has been performed on metal ions using silica gel G as an adsorbent. The effect of chlorosubstituent groups on the migration of cations has been studied. The use of aqueous solutions of acetic acid, monochloro, dichloro and trichloro acetic acid in the solvent system revealed profound effect of substituent groups on the R_f values of metal ions. The effect of concentration and pH of the mobile phases have been studied. Many qualitative ternary separations have been sucessfully achieved.     

薄层色谱法分离紫杉醇和三尖杉宁碱

建立了用薄层色谱分离紫杉醇和三尖杉宁碱的方法.方法中以正己烷-二氯甲烷-甲醇-三乙胺(体积比4.5∶3.5∶0.5∶1.0)四元体系为展开剂,在硅胶薄层板上成功地分离了紫杉醇和三尖杉宁碱,所得斑点清晰、无拖尾.同时以该体系为展开剂,使用薄层色谱法指导分离提取紫杉醇和三尖杉宁碱过程中反相色谱流分的合并,方法快速、简单、成本低,取得了满意的结果.     

薄层层析分离-紫外分光光度法测定冰清中的环丙沙星

报导了用薄层层析法分离冰清中的环丙沙星 .以VCHCl3 :VCH3OH:VC2 H5 OH:V(NH3·H2 O) =15 :8:8:7混合体系为流动相 ,硅胶G为固定相 ,展开浸取后 ,用紫外分光光度法在 2 73nm处测定其含量 ,回收率为 10 0 .1% ,RSD为0 .72 % .     

离子色谱-直接电导法测定碱土金属和过渡金属离子

本文报道离子色谱-直接电导法测定碱土金属和过渡金属离子。研究了流动相pH值、乙二胺浓度及柠檬酸和酒石酸浓度对金属离子分离的影响。结果表明,以乙二胺-柠檬酸为流动相可以同时分离碱土金属和过渡金属离子。用乙二胺-酒石酸作为流动相可以分离碱土金属离子。方法检出限为0.09~1.88 mg/L,加标回收率为97.6%~98.7%。该方法用于叶面肥试样的分析,结果良好。     

毛细管电泳柱上络合分离、间接紫外检测重金属离子

采用弱络合剂乙醇酸,柱上络合,间接紫外检测毛细管区带电泳(CZE)技术对重金属离子Ba2+、Cr3+、Cd2+、Pb2+及可能存在的干扰离子进行了分离研究。通过对背景电解质种类和浓度、缓冲液pH、有机添加剂等的优化,确定了最佳分离体系为含12 mmol/L络合剂乙醇酸的10 mmol/L吡啶溶液作为背景电解质(pH 4.0)。在电压15 kV,压差进样68.95 kPa.s,260 nm间接紫外检测条件下,采用50 cm(45.5 cm)×50μm(I.D.)石英毛细管,重复性实验(n=9):迁移时间RSD≤1.37%,峰高RSD≤1.70%,峰面积RSD≤3.55%;Pb2+、Ba2+和Cd3+的检出限(S/N=3)为0.2 mg/L,Cr3+的检出限为0.08 mg/L;在检出限至10 mg/L范围内,各离子的浓度与峰面积线性相关系数好于0.998。该方法并应用于实际样品的分析。     

Thin Layer Chromatographic of Metal Ions in Oxalic Acid-Oxalate Systems

Abstract

The adsorption behaviour of 48 metal ions has been studied in Oxalic acid - Oxalate systems using silica gel - G layers. The effect of p_H on R_f values was also investigated. A plot of -log Ksp Vs. R_M and R_f shows the dramatic behaviour of Hg²⁺ ion in 0.1 M Potassium Oxalate + 0.1 M Ammonium Oxalate (1:1) system. A number of interesting separations have been achieved e.g., Fe³⁺ - Ti⁴⁺ zr⁴⁺ - Ti⁴⁺, ce⁴⁺ - La³⁺, zr⁴⁺ - Th⁴⁺, Te⁴⁺ - Se⁴⁺ and Zr⁴⁺ - Y³⁺ - La³⁺. Ti⁴⁺ and Nb⁵⁺ were separated from a mixture of number of ions.     

Determination of Neomycin Components by Thin Layer Chromatography with Videodensitometry

Abstract

A method was developed for determination of the three neomycin components, neomycin A, B and C using silica gel thin-layer chromatography with detection with p-dimethylamino benzaldehydeninhydrine reagent and videodensitometry. The method was used to monitor the composition in different stages of production. The results obrained were compared with that of biological determination.     

Separation of Selected Transition Metal Ions and Divalent Metal Ions by HPLC Using UV-VIS Detection

Abstract

The use of ethylenediaminetetraacetic acid, disodium salt, (pH 3-5) has been investigated as an eluant for the separation and detection of nanogram levels of selected divalent and trivalent metal ions. The effect of pH and eluant concentration upon the retention times and resolution of the system are given and the ability to alter the eluant characteristics to optimize the chromatographic results in different situations will be discussed. The method is less complicated than the method frequently used for transition metal ion determinations which uses a post-column derivitization reagent. This method is applicable to a wider range of metal ions and provides detection limits which are generally within two orders of magnitude of the post-column derivitization method.     

薄层色谱综合分离程度的定量量度

薄层色谱对多元组分的分离程度,目前常用信息量~[1]来度量.但由于计算信息量时需人为地固定R_f值的分段,且认为同一区段内的R_f值等同,而不考虑每相邻两组分的R_f差值,也忽略了同一R_f区段内不同R_f值的细微差异.同时,由于薄层色谱分离的信息量并非连续函数,它只能取很有限的若干个分立值.因此,导致有时相同的信息量值却对应着相去甚远     

薄层色谱法分离四苯基卟啉和四苯基钴卟啉

提出了用薄层色谱分离四苯基卟啉和四苯基钴卟啉的方法.方法中以石油醚-二甲苯(体积比为2:1)二元溶剂体系为展开剂,在硅胶薄层板上分离了四苯基卟啉和四苯基钴卟啉,所得斑点清晰、无拖尾.应用此薄层色谱法跟踪检测了四苯基钴卟啉的合成.     

Separation and Quantitative Determination of Aldoses and Alditols by Over-Pressured Layer Chromatography (OPLC)

JPC – Journal of Planar Chromatography – Modern TLC - Anew OPLC method has been established for separation and quantitative determination of three alditols (d-xylitol, L-arabitol, and...     

5H-苯基联苯膦磺化产物的薄层色谱分离

1 引 言5H－苯基联苯膦（5H-phenyl-dibenzophosphole, PDBP）的磺化产物是一种多组分的复杂混合物,在石油化学工业具有很好的应用前景。5H－苯基联苯膦是三苯基膦的衍生物,是三苯基膦经桥连反应生成。经与发烟硫酸/硼酸的无水混合物反应,氢氧化钠中和,生成PDBP磺酸钠的混合物。混合物中除了可能含有目标产物二磺化PDBP和三磺化PDBP外,还可能含有取代位置不同的一磺化产物的异构体,二磺化和三磺化PDBP的氧化物,以及Na2SO4等。有关PDBP磺化产物分离方法的研究,目前尚未见报道。作者尝试用薄层色谱法来分离该混合物,通过…     

Determination of Metal Ions by High Performance Liquid Chromatography

The mixture of metal ions [Bi(III), Fe(III), Fe(II), Cu(II), Zn(II), Ni(II), Co(II), Pb(II), Cd(II), Mn(II)] were separated in the bonded-phase strong cation exchange column (Vydac-401 SA) and monitored at 540 nm after a postcolumn reaction with 4-(2-pyridylazo)-resorcinol (PAR). Citrate, tartrate, lactate and α-hydroxyisobutyrate buffer were used as eluent and it has been found that the elution order of some metal ions were changed with different eluents. The detection limits and the calibration curves of metal ions were also studied.