A Simple and Efficient Device for Treatment of Fluoride Samples in Analysis by the Selective Electrode Method.

Abstract

A simple, efficient and economic device for fluoride mass transference is presented in this study. Hexamethyldisiloxane (HMDS) is used to volatilize fluoride and, in addition to 0.05M NaOH, 0.3M citrate/phosphate/1 M KCl, pH 7.8 (buffer A) and 0.5 M citrate pH 5.5 (buffer B) are used as the trapping solution with the aim of an additional gain when concentration is a limiting condition in the use of the selective electrode. Using 0.05M NaOH, the fluoride mass transferred was in the range of 40 - 0.2 μg, and with buffer A the mass transferred was around 0.2 μg, with a total recovery in a few hours. The influence of interfering substances on fluoride volatilization was assessed. Fluoride was transferred from standard solutions in either the absence or presence of interfering substances (ethanol, propyleneglycol, glycerol, sorbitol, artificial saliva), and the respective recoveries were determined. Due to its simplicity and low cost several device units can be assembled allowing simultaneous analysis for rapid and accurate comparison of different samples. This device is useful for eliminating interfering substances, to concentrate samples as a function of the limit of method, and/or to attenuate gradative loss of the electrode sensitivity.     

Determination of Traces of Vanadium with 5-Bomosalicylhydroxamic Acid by Solid-Phase Spectrophotometry

Abstract

A microdetermination method at μg 1^?1 levels for vanadium by solid-phase spectrophotometry has been developed. 5-Bromosalicylhydroxamic acid was used as chromogenic reagent to form a 1:2 violet complex which is easily sorbed and concentrated on a dextran-type anion-exchange resin. The resin-phase absorbances at 560 and 850 nm were measured directly. Vanadium can be determined in the 5 - 60 μg 1^?1 range with a RSD of 4.3%. The method is applied to the determination of vanadium in pet roleiim crudes and natural water, samples.     

Petroleum Absorbers Based on CNSL,Furfural and Lignin – The Effect of the Chemical Similarity on the Interactions among Petroleum and Bioresins

Summary: The petroleum has become our most important source of energy since the mid-1950s. It is due to its high energy density, easy transportability and relative abundance. However, along extraction, storage or transportation of oil, spill accidents may happen. This kind of accident causes severe impacts on the environment, being directly responsible for the destruction of the marine life, which affects the fishing and even tourism industries. Main goal of this work is related to the use of renewable sources aiming to obtain “absorbent green materials”. These materials were synthesized by a typical phenolic resin polycondensation route using cashew nut shell liquid (CNSL) as main phenolic compound. Focused on keep the green characteristic of the materials, furfuraldehyde from hemicellulose was used as aldehyde and the reaction was catalyzed using a small amount of sulfuric acid. Resins were characterized using Optical Microscopy, Scanning Electron Microscopy, Infrared Spectroscopy with Fourier Transformed (FTIR) and density tests. In addition, contraction of the oil spilled was studied in presence of resins. Obtained results demonstrated that synthesized resins present a good chemical similarity with oil, which produces a good interaction among resins and oil, making easy the contraction of the oil spot on the water and, consequently, the removal process of oil spilled on water.     

镁铝混合氧化物负载镍催化剂上液化石油气的预重整

采用共沉淀-浸渍法并在较低温度(400～700℃)下焙烧制备了镁铝混合氧化物(MgmAl)负载的Ni催化剂.X射线衍射和程序升温还原结果表明,Ni物种高度分散于催化剂表面,没有形成尖晶石NiAl2O4.在650℃可被还原成金属Ni纳米晶粒,在400℃和较低水/碳摩尔比(S/C=2)条件下表现出较好的催化液化石油气(LP...     

核磁共振岩屑含油饱和度分析技术的实验研究

含油饱和度是油田勘探开发中的重要油层物理参数之一,目前油田现场岩屑常规录井方法只能定性给出岩屑的含油级别,无法给出岩屑含油饱和度的定量结果. 提出了利用核磁共振技术进行现场岩屑含油饱和度快速定量分析. 在室内实验基础上,采用添加弛豫试剂的方法进行了岩屑含油饱和度的核磁共振定量分析,研究摸索了一套利用核磁共振技术进行现场岩屑含油饱和度分析的方法,给出了弛豫试剂的优选方案,同时给出了核磁共振岩屑含油饱和度的测量精度.     

RESEARCH OF REGULARITY OF THROWING MOVEMENT FOR SOLID PARTICLE ON THE SHAKER’S SCREEN

By means of Delta-function & unit step function to express the force of solid particle on plane inertial shaker’s screen, an mathematical model of the differential equation type was set up and solved. According to analysis of the solution, the relation is given between the throw period & displacement with the parameters of shaker design & solid particle. The method of numerical value calculation & analysis for the relation is given too.     

Thermo-kinetic Investigation of Optimum Growth Temperature of Petroleum Bacteria

The power-time curves of the growth of three strains of petroleum bacteria at different temperatures have been determined. A novel equation of a power-time curve has been proposed in this paper. The general formula to calculate the rate constant of the bacterial growth has been derived. The rate constants of the bacterial growth at different temperatures, the heat production per newly formed bacterium, the bacterial number at the end of the bacterial growth and the deceleration rate constant of the bacterial growth at 50.00°C, have been calculated. The optimum growth temperatures of the three strains have been obtained.This revised version was published online in November 2005 with corrections to the Cover Date.     

反相高效液相色谱二极管阵列检测器对戊四硝酯粉质量的研究

建立了戊四硝酯粉含量及有关物质的RP-HPLC测定法。采用ODS色谱柱,甲醇/水(70∶30)为流动相,使戊四硝酯与有关物质基线分离,二极管阵列检测器检测波长206nm。本方法操作简便,重现性好。     

离子对反相高效液相色谱法分离伊班膦酸钠及其有关物质

采用离子对反相高效液相色谱法研究了伊班膦酸钠及其有关物质的色谱分离方法。以Inertsil C8色谱柱为固定相,乙腈．甲醇．12mmol／L乙酸铵缓冲液（含35mmol／L正戊胺,pH7．0）（8：4：88）为流动相,流速为1．0mL／min,分析物以通用型的蒸发光散射检测器（ELSD）测定。在该色谱条件下,伊班膦酸钠及其有关物质分离良好且能够被同时检测。本方法采用的可挥发离子对试剂和缓冲液的流动相系统,同时解决了伊班膦酸钠及其有关物质的分离与检测的问题,简单快速、专属性强,适用于伊班膦酸钠的有关物质检测,为该药的质量控制提供了简便可靠的分析手段。     

Phase transitions in polymesomorphic compounds

Summary The results of a X-ray diffraction study, performed on N(p-n-pentyloxy benzylidene)p′-n-octylaniline (50.8) and N(p-n-pentyloxy benzylidene)p′-n-decylaniline (50.10) are presented. The investigated compounds exhibit smecticB, smecticA and nematic phases in between solid and isotropic liquid phases. In addition, after a thermal cycle the 50.8 compound exhibits a smecticG phase at room temperature. The interlayer and the in-plane intermolecular distances were obtained as functions of temperature through all the mesophases. A phase coexistence has been observed during the solid to smecticB and the smecticB to smecticA phase transitions of the 50.8 compound. The nematic to smecticA phase transitions are found to be of second order for both compounds. Pretransitional effects due to cybotactic-cluster formation in the nematic region are observed.

---

Riassunto Si presentano i risultati di uno studio effettuato mediante la diffrazione dei raggi X sul N(p-n-pentilossi benzilidene)p′-n-ottilanilina (50.8) e sul N(p-n-pentilossi benzilidene)p′-n-decilanilina (50.10). Tra le fasi solida ed isotropica i composti esaminati presentano le mesofasiS _B ,S _A e nematica. Inoltre, dopo un ciclo termico il composto 50.8 presenta una faseS _G a temperatura ambiente. Sono state misurate le distanze tra i piani smettici e le distanze laterali tra le molecole in tutte le mesofasi in funzione della temperatura. Una coesistenza di fase è stata osservata durante le transizioni solido →S _B eS _B →S _A del composto 50.8. Le transizioni nematico-S _A sono risultate del second'ordine per entrambi i composti. Nelle fasi nematiche sono stati osservati effetti pretransizionali dovuti alla formazione di gruppi cibotattici.