A simple,rapid and sensitive method based on modified multiwalled carbon nanotube for preconcentration and determination of lead ions in aqueous media in natural pHs

In this study, multiwalled carbon nanotube (MWCNT) was modified by the pyridine group using a silane agent and characterized by infrared spectroscopy (IR), thermal analysis (TG/DTA), and elemental analysis (CHN) and scanning electron microscopy (SEM). The application of this sorbent was investigated in determination of lead ions in aqueous samples, using flame atomic absorption spectrometry (FAAS). Through this study, different parameters such as pH and sample flow rate on adsorption process and eluent concentration, volume and flow rate were optimized. The limit of detection (LOD), the relative standard deviation and the recovery of the method were 2 ng mL^?1, 1.3% and 99.7%, respectively. Two standard reference materials (NIST 1571 and NIST 1572) were used to verify accuracy of this method. Finally, the sorbent was successfully applied for extraction and determination of low levels of Pb(II) ions in aqueous samples.     

基于多线程技术的监控系统的设计

详细介绍在32位操作系统Windows95／98下，用C Builder3．0开发基于多线程技术的监控系统的有关方法。     

Complete systems, elementary submodels and the tightness of upper hyperspaces

We introduce and study some completeness properties for systems of open coverings of a given topological space. A Hausdorff space admitting a system of cardinality κ satisfying one of these properties is of type Gκ. Hence, we define several new variants of the ?ech number and use elementary submodels to determine further results. We introduce M-hulls and M-networks, for M elementary submodel. As an application, we give estimates for both the tightness and the Lindelöf number of a generic upper hyperspace. Two recent results of Costantini, Holá and Vitolo on the tightness of co-compact hyperspaces follow from ours as corollaries.     

Synthesis and characterisation of bis(pentafluorophenyl)antimony(V) cations, [(C6F5)2SbL3]

Pentacoordinate complex cations of the general formula [(C₆F₅)₂SbL₃]³⁺ stabilized as solid salts in combination with tetraphenylborate (BPh₄), tetrafluorobroate (BF₄) anions, where L=DMSO, Ph₃AsO, PyO, DMF, α-, β- and γ-picoline have been isolated. The newly formed complexes were characterized by elemental analysis, molar conductance measurements, solid-state IR and and NMR. From these results, a five-fold coordination around antimony was required.     

Counterpoise-corrected potential energy surfaces of simple H-bonded systems

Geometries and stabilization energies of various simple H-bonded complexes (water dimer, hydrogen fluoride dimer, formamide dimer, formic acid dimer) have been determined by a gradient optimization that eliminates the basis set superposition error (BSSE) by the counterpoise (CP) method in each gradient cycle as well as by the standard gradient optimization. Both optimization methods lead to different potential energy surfaces (PES). The difference depends on the theoretical level used and is larger if correlation energy is considered. Intermolecular distances from the CP-corrected PES are consistently longer, and this difference might be significant (∼0.1 ?); also angular characteristics determined from both surfaces differ significantly. Different geometries were obtained even when passing to larger basis sets (aug-cc-pVDZ). The standard optimization procedure can result in a completely wrong structure. For example, the “quasi-linear” structure of the (HF)₂ (global minimum) does not exist at the standard MP2/ 6-31G** PES (where only cyclic structure was detected) and is found only at the CP-corrected PES. Stabilization energies obtained from the CP-corrected PES are always larger than these from the standard PES where the BSSE is added only a posteriori for the final optimized structure; both energies converge only when passing to a larger basis set (aug-cc-pVDZ). Received: 11 March 1998 / Accepted: 19 June 1998 / Published online: 4 September 1998 RID=" ID=" <E6>Acknowledgements.</E6> The project was supported by the Grant Agency of the Czech Republic (Grant No. 203/98/1166). RID=" ID=" <E5>Correspondence to</E5>: P. Hobza     

Highly diastereoselective chemoenzymatic synthesis of (2′R)- and (2′S)-2′-deoxy[2′-H]guanosines

In an effort to develop an efficient synthetic method of highly diastereoselective (2′R)- and (2′S)-2′-deoxy[2′-²H]guanosines, chemoenzymatic conversion was investigated. The synthesis of (2′R > 98% de)-2′-deoxy[2′-²H]guanosine was achieved by biological transdeoxyribosylation using (2′R > 98% de)-2′-deoxy[2′-²H]uridine, 2,6-diaminopurine, and Enterobacter aerogenes AJ-11125, followed by treatment with adenosine deaminase. (2′S > 98% de)-2′-Deoxy[2′-²H]guanosine was synthesized from (2′S > 98% de)-2′-deoxy[2′-²H]uridine and 2,6-diaminopurine using thymidine phosphorylase and purine nucleoside phosphorylase instead of E. aerogenes AJ-11125.     

Synthesis of the four enantiomers of diethyl 1,2-di(N-Boc-amino)propylphosphonates

A simple and efficient synthetic strategy to all four enantiomerically pure diethyl 1,2-di(N-Boc-amino)propylphosphonates has been elaborated starting from the corresponding N-[(R)-(1-phenylethyl)]aziridine-(2S)- and N-[(S)-(1-phenylethyl)]aziridine-(2R)-carboxaldehydes, employing a one-pot three-components Kabachnik-Fields reaction followed by the hydrogenolytic removal of the chiral auxiliary and aziridine ring opening with simultaneous protection of the amino groups as the N-Boc derivatives.     

Comparative Hydrodynamic Study on Non-Aqueous Soluble Archaeological Wood Consolidants: Butvar B-98 and PDMS-OH Siloxanes

Butvar B-98 and PDMS-OH both have a demonstrable ability as consolidants for archaeological wood. This makes them both potential treatment options for the Oseberg collection, which is one of the most important archaeological finds from the Viking era. Both Butvar B-98 and PDMS-OH are soluble in organic solvents, offering a useful alternative to aqueous-based consolidants. Extensive characterisation studies were carried out on both of these polymers, with the use of analytical ultracentrifugation and viscometry, for the benefit of conservators wanting to know more about the physical properties of these materials. Short column sedimentation equilibrium analysis using SEDFIT-MSTAR revealed a weight-average molar mass (weight-average molecular weight) M_w of (54.0 ± 1.5) kDa (kg · mol⁻¹) for Butvar B-98, while four samples of PDMS-OH siloxanes (each with a different molar mass) had an M_w of (52.5 ± 3.0) kDa, (38.8 ± 1.5) kDa, (6.2 ± 0.7) kDa and (1.6 ± 0.1) kDa. Sedimentation velocity confirmed that all polymers were heterogeneous, with a wide range of molar masses. All molecular species showed considerable conformational asymmetry from measurements of intrinsic viscosity, which would facilitate networking interactions as consolidants. It is anticipated that the accumulated data on these two consolidants will enable conservators to make a more informed decision when it comes to choosing which treatment to administer to archaeological artefacts.     

N1923从碱性氰化液中萃取金(Ⅰ)的研究

采用放射性同位素１９８Ａｕ示踪法研究了伯胺Ｎ１９２３和ＴＢＰ从碱性氰化液中萃取金（Ⅰ）,考察了酸化率、水相ｐＨ值、萃取剂浓度等对萃取率的影响,以及ＮａＯＨ对载金有机相的反萃作用。结果表明,ＴＢＰ含量大于２０％,酸化的Ｎ１９２３与ＫＡｕ（ＣＮ）２摩尔比值在１：１时,金能够完全被萃取。载金有机相可采用０．ｌｍｏｌ·Ｌ－１的Ｎａ０Ｈ溶液定量反萃。机理研究表明,伯胺和ＴＢＰ萃取Ａｕ（ＣＮ）２－,符合ＢＣ类协同萃取机理。当金浓度大于１０ｇ·Ｌ－１时,在萃取有机相中形成纳米级的聚集体。     

Using enantioselective dispersive liquid–liquid microextraction for the microseparation of trans-cyclohexane-1,2-diamine enantiomers

A new chiral separation system effective for the enantioselective extraction of racemic trans-cyclohexane-1,2-diamine is presented. Enantioselective dispersive liquid–liquid microextraction has been used for the chiral microseparation of trans-cyclohexane-1,2-diamine, with a chiral azophenolic crown ether being identified as a versatile chiral selector. The influence of various process conditions on the extraction performance was studied experimentally. It was found that the operational selectivity in one extraction step is mainly related to the type and volume of the solvents, chiral selector concentration, extraction time, temperature of sample solution, and pH. At optimum conditions (300 μL of diethyl ether as the extraction solvent 1 mL of methanol as the disperser solvent, with 5 mmol L^?1 chiral selector concentration, pH of the sample equal to 4.5, 30 min extraction time and a temperature of 10 °C), the distribution ratio of (R,R)- and (S,S)-trans-cyclohexane-1,2-diamine was 18.3 and 1.8, respectively, while the enantioselectivity value of 10.2 was found at the optimum condition.