Chemical modification of silica surface by immobilization of functional groups for extractive concentration of metal ions

Increased utilization of mechanically stable synthetic matrices particularly silica gel as a solid support and its surface modification either by impregnation of organic ligands directly or covalent grafting through spacer unit for extractive concentration of trace elements are highlighted in the present article. Experimental evidences for existence of surface silanol and its chemical nature have explored the idea of silica surface modification. Recent methods of development in functionalized silica synthesis by attachment of various ligands or organic reagents to the silica surface and techniques of characterization of the modified surface have been reported. Analytical applications of various modified silica surfaces, in particular, adsorption of trace elements taking separation and preconcentration into account from complex synthetic mixture as well as natural water is presented.     

On-line testing of gas chromatographic columns with a programmable computing integrator

Summary A program is described which calculates the number of effective plates and the coating efficiency over the entire range of a test chromatogram. The peak widths at half height are derived by assuming a Gaussian peak shape. The interpolated peak width at k=4 is used for computing a standardized number of effective plates. Plate height, column permeability, overall performance and a novel parameter called sampling efficiency are calculated from 5 other figures — i. e. carrier gas code, pressure drop, column length, column temperature and particle size.Dedicated to Dr. Leslie S. Ettre for his 60th birthday.     

Thermotropic gelation of ovalbumin 1. Viscoelastic properties of gels as a function of heating conditions and protein concentration at various pH values

A study has been undertaken of stress relaxation in ovalbumin thermotropic gels with a concentration of 8–20%, depending on time and temperature of heating (respectively, 20–60 min, 70°–110°C), at pH 2.5–10.0. In all instances, the dependence of the initial gel elasticity modulus on heating has a single maximum. Gelation conditions corresponding to this maximum are considered optimal. Optimal gelation time is 30 min, regardless of pH. On the other hand, the optimal heating temperature depends on pH. To the right and left of the isoelectric point of protein (2.5pH<4.0 and 5.5G) of gels on heating conditions, pH and protein concentration (X ₁,X ₂,X ₃,X ₄), as well as on time of relaxation (t) may be generally described asG(X ₁,X ₁,X ₁,X ₁,t)=G _e(X ₁,X ₂,X ₃,X ₄)f(t), whereG _e is the equilibrium value of the elasticity modulus, and f(t) the relaxation function. Thus, a change in the parameters only affects the value of the equilibrium elasticity modulus, and exerts no effect on the relaxation time spectrum. For this reason, all the relaxation curves obtained may be transformed into two normalized relaxation functions:f(t)=f(t)/f(1)=G(X ₁,X ₂,X ₃,X ₄,t)/G(X ₁,X ₂,X ₃,X ₄, 1)Each of these normalized functions corresponds to one of the homologous groups. Rheological similarity of gels in each homologous group evidently points to their structural similarity. Invariance of the gel relaxationproperties with regard to protein concentration, leads to a concentration dependence of the equilibrium modulus at various pH values. These dependences are curvilinear on a double logarithmic scale. The slope of the curve exceeds 2 in the entire concentration interval studied. In other words, the dependences obtained cannot be described by the usual law of squares. On the other hand, they adequately match Hermans theoretical relation for a network formed by random association of identical polyfunctional particles without cyclization. This simple model evidently gives a true picture of the major regularities of thermotropic gelation for ovalbumin. An agreement between this theory and experiment was achieved for a protein concentration ofC ^*=6.0±1.0% at the gel point regardless of pH. Invariance of gelpoint position with regards to pH demands further confirmation.List of symbols T _h,t _h heating temperature and time - T _h ^* ,t _h ^* optimal heating temperature and time - C protein concentration - C ^* protein concentration in gel-point - G relaxation modulus - G _e equilibrium modulus - f(t) relaxation function - t time of relaxation - f(t) normalized relaxation function - fT _A (t), f _B (t) normalized relaxation functions of groups A and B - G ₁ T _h,t _h-reduced modulus - G ₂ T _h,t _h, pH-reduced modulus - G ₃ C-reduced modulus - b ₁ T _h, t_h reduction parameter of modulus - b ₂ pH reduction parameter of modulus - b ₃ C reduction parameter of modulus - W_g gel-fraction     

纳米Eu0.10Y1.90-xNdxO3-δ的光致发光特性及浓度猝灭研究

使用超声波作用下的均匀沉淀法,制备了Eu0.10Y1.90-xNdxO3-δ纳米晶荧光粉,用X射线粉末衍射、荧光光谱等对其进行表征.研究了掺杂Nd3 离子对Y2O3∶Eu3 晶格常数、晶粒尺寸及室温光致发光特性的影响.由不同掺杂浓度x=0~0.18下样品的发射光谱强度变化曲线得到猝灭浓度值,探讨了掺杂Nd3 的样品荧光浓度猝灭的机理.发光强度与浓度的关系表明,掺杂离子之间存在的Eu3 -Nd3 或Nd3 -Nd3 间交换相互作用,是导致掺杂样品浓度猝灭的主要原因.     

Novel Membrane Potentiometric Thiocyanate Sensor Based on Tribenzyltin(IV) Dithiocarbamate

A novel PVC membrane ion‐selective electrode based on tribenzyltin(IV) dithiocarbamate [Sn(IV)–TBDTB] as neutral carrier was developed for thiocyanate (SCN^?) determination. The electrode exhibits a near‐Nernstian response for SCN^? with a slope of 62.8±2.0 mV per decade over a wide concentration range 1.0×10^?1–2.0×10^?6 mol L^?1 and a detection limit of 1.0×10^?6 mol L^?1 in MES–NaOH buffer, pH 6.0, at 25 °C. The electrode prepared with 1.5 wt.% Sn(IV)–TBDTB, 32.5 wt.% PVC and 66.0 wt.% 2‐nitrophenyloctyl ether (o‐NPOE) shows optimal response characteristics. Anti‐Hofmeister selectivity sequence for a series of anions shown by the electrode was as follows: SCN^?>Sal^?>I^?>ClO >phCOO^?>CH₃COO^?>Br^?>Cl^?>NO >NO >Citrate>SO₄^2?. The useful pH range for the electrode was found to be 3–7 with a response time 30–40 s. The electrode has been used for direct determination of thiocyanate in wastewater with satisfactory results.     

聚合物体系散射函数的热力学基础

利用链段浓度和链头浓度的概念，根据热力学涨落理论，给出了聚合物二元共混体系ｄｅＧｅｎｎｅｓ散射函数的一个普遍的热力学证明，指出了这个函数和Ｆｌｏｒｙ－Ｈｕｇｇｉｎｓ共混自由能公式一样，也依赖于忽略构象涨落的假设．     

Objective comparison of concentration profiles in solids by means of mathematical statistics

To compare concentration profiles in solids in an objective manner, a multi-dimensional generalization of the comparison of two means by Student'st-test is proposed. The approach is based on piecewise modelling the profiles using rougha priori information, estimating the model parameters and their covariance matrix and comparing the estimated parameters by use of multidimensional test variables. The piecewise modelling is treated in the most important cases in such a way that the partial functions are straight lines or cubic polynoms (splines) with continuity at all knots in each case. It enables us to compare whole profiles as well as the most relevant parts of them. Two ways of estimating the covariance matrix as a generalization of the variance estimation are discussed. The approach is useful for any kind of line profiles if rough information on the profile type is available. As an example SIMS depth-profiles of aluminum obtained from thin-layer systems after different technological heat treatments are considered. These profiles are modeled by three straight lines.     

Stability of the FID sensitivity during an analysis in capillary GC

The sensitivity of an FID may change when the carrier gas flow rate changes during a chromatographic run. Sample parts which are eluted at reduced FID sensitivity produce a reduced peak area, hence are discriminated as compared to other components. Sensitivity changes were studied for hydrogen as carrier gas. For the detector tested, differences in the carrier gas flow rates of 1 ml/min shifted the FID sensitivity by 1 to 5% (depending on the fuel gas supply). Thus the stability of the sensitivity is no longer ensured as soon as the carrier gas flow rate is changed manually or by an automatic programmer during an analysis. Sensitivity drifts may also occur during temperature programmed runs with a pressure regulated carrier gas supply since the gas flow through the capillary drops with increasing temperature. Such shifts in the response became noticeable as soon as relatively high carrier gas flow rates combined with long range temperature programmes were used. The typical patterns of such discriminations are shown, closing with a discussion on the possibilities for minimizing such undesired effects.     

Formation at low surfactant concentrations and characterization of mesoporous MCM-41

At low concentrations of cetyltrimethylammonium bromide,all silica-based mesoporous materials with hexagonal phase have been synthesized via interactions between self-assembled surfactant molecule aggregates and aniomc silicate polymers.The resulting materials are characterized by XRD,FT-IR,solid state 29Si MAS NMR,thermal analysis and N2 adsorption-desorption measurements.After soluble ions are removed,the interactors between surfactant micelles and silicate polymers are reorganized and then form mesostructures 1 he hexagonal framework is sonsistent with amorphous silica gel.The structures of materials depend on the synthesis conditions Hydrothermal process improves the interactions between molecules and increases the degree of framework silicon atom polymerization The.surface area and the mesopore volume of the material prepared at 100℃ increase by 87% and 71 %,respectively,compared with those obtained at room temperature.