磷酸钛离子交换薄层色谱分离无机离子(英文)

The chromatographic behavior of 30 inorganic cations has been studied on thin layers of titanium phosphate ion-exchanger using several aqueous,organic and mixed mobile phases.The separation of one ion from several other ions and also ternary and binary separations have been developed.Some important analytical separations are reported.The effect of pH of the mobile phase on retention factor(Rf)values of the cations in the presence of complex-forming anion along with the separation power of the ion-exchanger were studied.This ion-exchanger exhibits high sorption capacity and varying selectivity towards metal ions and makes it a suitable stationary phase in thin layer chromatography.     

镍钼杂多酸制备NiMo/γ-Al2O3催化剂及硼、钴或镍改性氧化铝的影响（英文）

A hydrotreating NiMo/γ-Al2O3 catalyst(12 wt% Mo and 1.1 wt% Ni) was prepared by impregnation of the support with the Anderson-type heteropolyoxomolybdate(NH4)4Ni(OH)6Mo6O18.Before impregnation of the support,it was modified with an aqueous solution of H3BO3,Co(NO3)2,or Ni(NO3)2.The catalysts were investigated using N2 adsorption,O2 chemisorption,X-ray diffraction,UV-Vis spectroscopy,Fourier transform infrared spectroscopy,temperature-programmed reduction,temperature-programmed desorption,and X-ray photoelectron spectroscopy.The addition of Co,Ni,or B influenced the Al2O3 phase composition and gave increased catalytic activity for 1-benzothiophene hydrodesulfurization(HDS).X-ray photoelectron spectroscopy confirmed that the prior loading of Ni,Co or B increased the degree of sulfidation of the NiMo/γ-Al2O3 catalysts.The highest HDS activity was observed with the NiMo/γ-Al2O3 catalyst with prior loaded Ni.     

卡尔曼滤波伏安分析法同时测定钴(Ⅱ)、镍(Ⅱ)、锌(Ⅱ)

卡尔曼滤波（ＫＹ）用于解析互相干扰离子的Ｃｏ（Ⅱ）、Ｎｉ（Ⅱ）、Ｚｎ（Ⅱ）的伏安重叠峰。用该法对钢铁试样中的这些离子进行了测试，效果良好。设计了ＢＡＳＩＣ程序，将有关数据输入后，直接给出结果。为保证结果准确度，程序中设置了两个监控出口。     

钴萃取研究 Ⅸ.有机磷(膦)酸萃取剂结构与萃取分离钴(Ⅱ)、镍(Ⅱ)性能的研究

本文就三种典型的有机磷(膦)酸萃取剂P_(204)、P_(507)、P_(272)在高氯酸盐体系中对Co(Ⅱ)、Ni(Ⅱ)萃取分离能力进行了比较。 在萃取体系有机相中,上述三种萃取剂与Co(Ⅱ)形成的萃合物均存在粉红色八面体与蓝色四面体构型转化的平衡反应。随着萃取剂分子中氧烷基被烷基取代,反应基团磷氧酰基氧原子上电子云密度增加,酸性降低,与Co(Ⅱ)形成的四面体萃合物稳定性增强,对Co(Ⅱ)/Ni(Ⅱ)分离的能力增加。Co(Ⅱ)四面体萃合物的稳定性是影响Co(Ⅱ)/Ni(Ⅱ)分离效果最主要的因素。这一结论还可通过Co(Ⅱ)/Ni(Ⅱ)萃取分离温度效应与Co(Ⅱ)萃合物构型转化温度效应的一致性得到证实。在所研究的三类有机磷(膦)酸萃取剂结构因素中,磷氧酰基氧原子上的电子云密度是影响Co(Ⅱ)/Ni(Ⅱ)分离效果的关键因素。     

仲辛基苯氧基乙酸萃取钴(Ⅱ)和镍(Ⅱ)的机理研究

确定萃取机理和萃合物组成时,两相滴定法比斜率法快速简便。本实验利用两相滴定法,首次研究了新型萃取剂仲辛基苯氧基乙酸(CA-12)从盐酸介质中萃取Co(Ⅱ)和N i(Ⅱ)的机理。确定了298 K时萃合物的组成分别为CoA2.4.1HA和N iA2.4.3HA,该温度下相应的萃取反应平衡常数分别为pKCo=2.91和pKN i=2.64。     

Dimerization of Propylene by Nickel (Ⅱ) and Cobalt (Ⅱ) Catalysts Based on Bidentate Nitrogen-phosphino Chelating Ligands

The catalytic property of propylene dimerization by several nickel (Ⅱ), cobalt (Ⅱ) complexes containing N-P bidentate ligands was studied in combination with organoaluminum co-catalysts. The effects of the type of aluminum co-catalysts and its relative amount, the nature of precursors in terms of ligand backbone and metal center were investigated. The results indicated that precursor I (N,N-dimethyl-2-(diphenylphosphino)aniline nickel (Ⅱ) dichloride) exhibited high activity in propylene dimerization in the presence of the strong Lewis acid Et3Al2Cl3, whereas low productivity by its cobalt analogues was observed under identical reaction conditions.     

一维钴(Ⅱ)/镍(Ⅱ)配位聚合物的合成、结构、磁性及荧光传感性质

采用水热法合成了2个新的配位聚合物[Co(L)_0.5(1,4-bib)(H₂O)₃]_n (1)和[Ni(L)_0.5(1,4-bib)(H₂O)₃]_n (2)(H₄L=1,4-二(2,6-二甲基-3,5-二羧基吡啶基)苯,1,4-bib=1,4-双(1-咪唑基)苯),通过X射线单晶及粉末衍射、元素分析、红外光谱分析和热重分析对其结构进行表征。结构分析表明配合物1和2为异质同构,均为一维结构。通过变温磁化率测量发现,配合物b>1和2中的Co(Ⅱ)/Ni(Ⅱ)离子之间存在反铁磁相互作用。此外,配合物 1可通过荧光猝灭法检测头孢克肟(CEF),配合物 2可用来检测四环素(TET),该方法灵敏度高、选择性好,其检出限分别为0.86 μmol·L^-1 (CEF)和0.49 μmol·L^-1 (TET)。     

2-(2-噻吩偶氮)-5-二乙氨基酚反相液相色谱法分离测定铜(Ⅱ)、钴(Ⅱ)、镍(Ⅱ)

本文以2-(2-噻吩偶氮)-5-二乙氨基酚(简称TADAP)作柱前显色剂,反相色谱法分离测定铜(Ⅱ)、钴(Ⅱ)、镍(Ⅱ)离子。用含有1.5×10~(-4)mol/L的TADAP,0.1mol/L氯化锂和0.1mol/L乙酸盐(pH4)的甲醇(60％)-水(40％)溶液作为流动相,流量为0.9ml/min,紫外-可见检测器检测波长为545nm。在此条件下,铜(Ⅱ)、钴(Ⅱ)、镍(Ⅱ)螯合物得到最佳分离,并定量测定了茶叶中铜、钴、镍的含量,与原子吸收分光光度法测定,得到一致的结果。     

一维钴(Ⅱ)/镍(Ⅱ)配位聚合物的合成、结构、磁性及荧光传感性质

采用水热法合成了2个新的配位聚合物[Co(L)_0.5(1,4-bib)(H₂O)₃]_n(1)和[Ni(L)_0.5(1,4-bib)(H₂O)₃]_n(2)(H₄L=1,4-二(2,6-二甲基-3,5-二羧基吡啶基)苯,1,4-bib=1,4-双(1-咪唑基)苯),通过X射线单晶及粉末衍射、元素分析、红外光谱分析和热重分析对其结构进行表征。结构分析表明配合物1和2为异质同构,均为一维结构。通过变温磁化率测量发现,配合物1和2中的Co(Ⅱ)/Ni(Ⅱ)离子之间存在反铁磁相互作用。此外,配合物1可通过荧光猝灭法检测头孢克肟(CEF),配合物2可用来检测四环素(TET),该方法灵敏度高、选择性好,其检出限分别为0.86 μmol·L^-1(CEF)和0.49 μmol·L^-1(TET)。     

锰(Ⅱ)、钴(Ⅱ)、铜(Ⅱ)和镉(Ⅱ)与吡哆醇配合物的结构研究

本文合成了吡哆醇与锰(Ⅱ)、钴(Ⅱ)、铜(Ⅱ)和镉(Ⅱ)的配合物。通过元素分析确定了配合物的组成。通达摩尔电导、比移值,紫外光谱、红外光谱和核磁共振谱的测定和分析,推断了配合物的结构。     

Thin-layer chromatographic separation and identification of some anions on copper sulphate impregnated silica gel layers

Summary Thin-layer chromatographic behaviour of thirteen anions on plain silica gel and silica gel impregnated with copper sulphate solution has been investigated in aqueous-organic solvents containing acetone, some of which have achieved reliable and reproducible separations. The effect of copper sulphate concentration on the mobility of anions has been examined. The results obtained on plain silica gel have been compared with those obtained on copper sulphate impregnated layers. The impregnated layers dramatically change the selectivity and permit separations not possible on untreated silica. Aqueous sodium chloride-acetone (9∶1) and ammonium hydroxide-acetone (9∶1) were the most effective solvent systems for differential migration of anions. Better results in terms of clarity of detection and compactness of spots were found with HCOOH-acetone as compared to HCl-acetone. The effect of anion loading on R_F values has been investigated and identification limits on impregnated layers determined.     

Selective separation and determination of isoproterenol on thin layers of bismuth silicate ion-exchanger

A simple and sensitive method for the separation and determination of isoproterenol from other doping drugs has been developed on thin layers of bismuth silicate, a synthetic inorganic ion exchanger as adsorbent in thin layer chromatography (TLC). A mixture of methanol and 0.1 mol/L formic acid (3:7, v/v) was employed as the mobile phase. The development time was 32 min. The quantitative measurement were performed with a Camag TLC Scanner-3 at wavelength (λ) of 410 nm. The isoproterenol recovery in this procedure was 98.9%. The linear correlation coefficient was greater than 0.9871 and the relative standard deviation (RSD) was less than 0.94. The limit of detection (LOD) and limit of quantification (LOQ) were 7.7×10^-7mol/L and 3.85 ×10^-6mol/L, respectively. This method has been applied in the determination of isoproterenol in dosage forms and in biological fluids.     

薄层色谱扫描法测定塑料食品袋中酞酸酯的含量

建立了采用薄层色谱扫描测定塑料食品袋中4种酞酸酯(酞酸二甲酯(DMP)、酞酸二乙酯(DEP)、酞酸二丁酯(DBP)和酞酸二(2-乙基己基)酯(DEHP))的方法。经粉碎的样品先用乙醇浸泡24 h,然后超声提取,经0.45 μm滤膜过滤。点样在以丙酮处理过的硅胶G板上,以乙酸乙酯-无水乙醚-异辛烷(体积比为1∶4∶15)为展开剂展开,以双波长反射吸收飞点扫描测定(λS=275 nm,λR=340 nm),外标法定量。该法的线性关系较好,DMP、DEP、DBP和DEHP的检出限分别为2.1,2.4,3.4和4.0 ng,混合标准品在同一薄层板上的峰面积的相对标准偏差（RSD）为2.8%～3.5%,4种酞酸酯的样品加标回收率为78.58%～111.04%。该方法样品用量少,前处理简单,分离效果好,可用于塑料袋中4种酞酸酯的同时测定。经与气相色谱法的分析结果比较,两种方法对实际样品的分析结果接近。     

Reversed phase partition chromatographic separation of divalent copper with N-n-octylaniline on silica gel

A novel separation method was developed for the extraction and chromatographic separation of copper(II). The quantative extraction of 25.0–125.0 μg copper(II) has been observed from 0.05 to 0.25 mol/L of ascorbic acid at pH 9.0–12.0 with 0.087 mol/L N-n-octylaniline (liquid anion exchanger) coated on silica gel at a flow rate of 1.0 ml/min. The extracted metal ion has been recovered by eluting with 25.0 ml of 1.0 mol/L hydrochloric acid and determined spectrophotometrically by rubeanic acid method. The various influencing parameters viz. acid concentrations, reagent concentration, eluates effect of pH, and effect of flow rate on extraction were studied. The method is free from large number of interferences from cations and anions. A scheme for mutual separation of copper(II), gold(III) and bismuth(III) has been developed. Copper(II) has been separated from ayurvedic (Herbal) medicine and synthetic mixtures corresponding to alloy. The log–log plot of N-n-octylaniline concentration versus the distribution coefficient indicates that the probable extracted species is [.     

A simple and rapid method for the determination of taxol produced by fungal endophytes from medicinal plants using high performance thin layer chromatography

 Taxol is an important anticancer drug used widely in the clinical field. In this study, some endophytic fungi were isolated from selected medicinal plants, and were screened for their potential in the production of taxol, using a rapid separation technique of high performance thin layer chromatography (HPTLC). Of the 20 screened fungi, only 13 fungal species produced taxol in the artificial culture medium. The results of HPTLC showed that the 13 fungal species had identical ultraviolet (UV) characteristics, positive reactivity with a spray reagent, yielding a blue spot, which turned to dark gray after 24 hours, and had Rf values identical to that of the authentic taxol. The amount of taxol was also quantified by comparing the peak area and the peak height of the fungal samples with those of authentic taxol.     

The use of a new,modified Dittmer–Lester spray reagent for phospholipid determination by the TLC image analysis technique

A new phospholipid‐specific spray reagent is described. A new phospholipid‐specific spray reagent, which is a modification of the Dittmer–Lester reagent, is described in authors' studies. The difference between these two reagents is in the addition of tin (II) chloride to the proposed spray reagent. The use of the described spray reagent together with an image analysis technique allows not only for qualitative, but also for quantitative, determination of major phospholipid classes. Separation of phosphatidylserine (PS), phosphatidylethanolamine (PE) and phosphatidylcholine (PC) was conducted on an HPTLC plate with a mixture of chloroform, methanol and 25% ammonia solution in a volume ratio of 65:25:4 as mobile phase. The calibration curves were linear in the ranges of 5.0–25.0, 1.5–15.0 and 1.0–20.0 µg/spot for PC, PS and PE, respectively. The use of the new spray reagent resulted also in lower limits of detection than the standard molybdenum method for the investigated phospholipids. The proposed method was used to determine the amount of PS in the dietary supplement ‘Session’, and of PS, PE and PC in biological samples, with good results. Copyright © 2012 John Wiley & Sons, Ltd.     

Effects of starvation for 4-20 days on the amino acid content of Biomphalaria glabrata as determined by cellulose HPTLC-densitometry with confirmation of identity using silica gel and RP-18 W plates with two mobile phases causing inversion of the separation mechanism

The effects of starvation at 4, 7, 10, 14, and 20 days on the amino acid content of Biomphalaria glabrata was determined by high performance thin layer chromatography (HPTLC)-densitometry. Cultures of control and starved snails were prepared for each duration of time. Samples were extracted using ethanol-water (70:30), and supernatant was collected after multiple centrifugations. Samples and standards were applied as bands using a CAMAG Linomat 4 onto cellulose HPTLC plates and developed in a 2-butanol-pyridine-acetic acid-water (39:34:10:26) mobile phase before spraying with ninhydrin detection reagent and scanning with a CAMAG 3 scanner to quantify ornithine (Orn), glycine (Gly), alanine (Ala), valine (Val), and leucine (Leu). Amino acid identification was confirmed by HPTLC on silica gel plates and RP-18?W plates using two different mobile phases causing inversion of the separation mechanism. Starvation led to an overall decrease in amino acid content in comparison to the control snails, however, the amount of amino acids in the starved snails had no correlation with the duration of starvation.     

Anodic dissolution of magnetic layers based on cobalt and nickel in conditions of electrodeposition of multilayered nanostructures by a single-bath method

Methods of quartz microgravimetry (in solutions containing no copper ions) and stripping voltammetry (in copper-containing solutions) are used to study the process of anodic dissolution of thin deposits of pure Co and Ni and deposits of these metals with inclusion of copper in the potential region of copper deposition. It is shown that, under these conditions, Ni practically does not dissolve in either the sulfate or chloride-containing electrolytes, whereas Co dissolves in sulfate electrolytes at a rate that is dependent on the potential and increases with its shift into the positive region. Stability of ternary CoNiCu deposits is examined and it is demonstrated that additionally inserting Ni in the composition of a magnetic CoCu layer facilitates suppression of selective dissolution of Co.     

Evaluation of thin layer chromatography—Fast atom bombardment mass spectrometry: Application to the determination of midazolam intoxication by use of 3-glycidoxypropyl-treated thin layer chromatographic plates

Summary The effectiveness of 3-glycidoxypropyl-treated thin layer chromatographic plates in the determination of midazolam intoxication has been studied by thin layer chromatography/fast atom bombardment mass spectrometry. Silica plates treated with 3-glycidoxypropyldimethylethoxysilane were used for the measurement of their physical composition and for chemical analysis. From elemental carbon analysis data, the maximum number of bonded 3-glycidoxypropyl surface groups per gram was calculated to be 0.417×10²¹. Midazolam in human serum from patients suffering from intoxication could be separated on a 3-glycidoxypropyl-treated thin layer chromatographic plate with chloroform as eluent. After applying the technique of diffused spot condensation on the 3-glycidoxypropyl-treated thin layer chromatographic plate, the established thin layer chromatography/fast atom bombardment mass spectrometry method was used for the identification of midazolam intoxication, and improved the detection limit for midazolam in the serum of an intoxication patient by 30 times.