Determination of lead by selective chelatometric titration with HEDTA after separation as its sulphate by an improved method of precipitation

A selective titrimetric determination of Pb after separation by a modified method of precipitation as its sulphate is proposed. Pb(II), present as the perchlorate, is precipitated by gentle boiling in 3.6M H(2)SO(4) presaturated with PbSO(4) and free from any extraneous anions. The customary time-consuming evaporation to fumes of sulphuric acid is dispensed with. The precipitate is collected, and dissolved in excess of HEDTA, the surplus of which is back-titrated with Zn(II) at pH 5.0-5.5. Use of Catechol Violet and Xylenol Orange as a mixed indicator gives a sharper end-point. The standard deviation of the proposed method for 60 mg of lead is 0.35 mg. The method has been successfully used to determine Pb in non-ferrous alloys.     

Determination of total arsenic in serum and packed cellsof patients with renal insufficiency

In order to investigate the arsenic level in serum and packed cells of patients with renal insufficiency, total arsenic (As) concentrations were determined with hydride generation atomic absorption spectrometry (HGAAS) in serum (S) and packed cells (PC) of 31 non-dialyzed patients. The accuracy of the method was tested by the analysis of arsenic in 3 certified reference materials. Patients showed a three-fold increase of arsenic concentrations in serum and a two-fold increase of arsenic in packed cells compared with controls. Patients (n=10) with higher serum creatinine (>2.0 mg/dL), urea (>0.70 g/L) and urinary protein (mean+/-SD: 1.12+/-0.82 g/L) showed higher arsenic concentrations (5.8+/-3.3 microg/L in serum and 18.0+/-16.7 microg/kg in packed cells) compared with those with lower creatinine (<1.6 mg/dL), urea (<0.6 g/L) and urinary protein (mean+/-SD: 0.27+/-0.82 g/L) (n=16, serum arsenic 1.2+/-1.2 microg/L, packed cells arsenic 2.6+/-1.9 microg/kg). The significant differences (both p < 0.001) in S and PC-arsenic levels of patients in group I and II implies a relationship between the arsenic level and the degree of chronic renal insufficiency.     

Chemische Vitamin D<Subscript>3</Subscript>-Bestimmung in Lebertran

The different aspects of Vitamin D₃ determination and the data reported in the literature are discussed. The spectrophotometric determination of Vitamin D₃ in cod-liver oil is carried out after the alkaline saponification, extraction of unsaponified parts, precipitation of accompanying sterols and the column- and thin-layer chromatographic purification and separation of vitamin D₃ on 40 cm plates from other vitamins. The dyestuff α-naphtholbenzein is suited well as standard substance for the better location and identification of vitamin D₃ zone on the thin-layer plate. The results obtained from the chemical method were checked through the simultaneous biological determination.     

Theoretical study of the effect of frit quality on chromatography using computational fluid dynamics

Summary Frits at both ends of a chromatographic column, especially for a preparative column, have significant influence on the flow distribution within the column and thus the column efficiency. However, frits have received little attention from chromatographers in the past. Here a theoretical study was conducted with the aid of CFD software FLUENT to investigate the effect of frits on the performance of homogeneous and heterogeneous chromatographic columns. A dimensionless number,FQ, was applied to characterize frit quality. This study visualized how frit quality affects the flow distribution and the concentration band, the shape of eluted pulse at the colum exit and column efficiency. Simulation results show that the development length of the flow distribution is related toFQ but has nothing to do with the packing heterogeneity. The curvature of the concentration band in a column depends onFQ and packing quality. This study shows column efficiency can be improved significantly by increasingFQ and/or frit permeability.     

Determination of panaxadiol and panaxatriol in ginseng and its preparations by capillary supercritical fluid chromatography (SFC).

Capillary supercritical fluid chromatographic (SFC) method has been developed for the determination of panaxadiol and panaxatriol in ginseng and its preparations. 0.1 g ginseng or an appropriate amount of its preparations was hydrolysed by 15% H2SO4 in an ethanol:water (1:1 v/v) solution for 4 h followed by 15% NaOH for 0.5 h. The mixture was extracted by cyclohexane. The cyclohexane extracts were purified by a partition column and concentrated by an adsorption column and then analysed by SFC. Methyltestosterone was used as the internal standard.     

LC–MS Determination and Pharmacokinetic Study of a Novel Sulfonylurea: Potential Hypoglycemic Agent in Rat Plasma

To support preclinical pharmacokinetic investigation of 1-[4-[2-(4-bromobenzene-sulfonaminoethyl)phenylsufonyl]-3-(trans-4-methylcyclohexyl)urea (G004), a rapid, sensitive and specific high-performance liquid chromatography–electrospray ionization mass spectrometry (LC–ESI-MS) method was developed and validated. Glibenclamide was employed as internal standard. After liquid–liquid extraction the analyte was analyzed on a Kromasil C₁₈ column (150 × 2.0 mm i.d.) with a mobile phase consisted of acetonitrile–water (0.05% acetic acid), 30:70 (v/v). The flow rate was 0.2 mL min⁻¹. Detection was performed on a quadrupole mass spectrometer using an electrospray ionization interface and the selected-ion monitoring (SIM) mode. The retention time was about 3.5 and 4.2 min for Glibenclamide and G004, respectively. The assay was linear over the concentration range of 2.0–500.0 ng mL⁻¹. Extraction Recovery of G004 in rat plasma was more than 87%. The intra- and inter-assay precision was lower than 11.5% (CV). This validated method was successfully applied to the pharmacokinetics of G004 in rats.     

The application of multivariate techniques to data from spanish glass-making objects from the Roman Era

Three multivariate techniques (principal components analysis, correspondence factor analysis and spectral map analsis) are applied to x-ray fluorescence data from glass-making objects from the 5th century AD found in Tarragona (Tarraco in the Roman Empire). The information obtained by displaying th eobjects and variables in each reduced factor space is compared. The presence of redundant information is shown. The visualization of groups of objects and of the relationship between objects and variables allows the formulation of hypotheses concerning the origin of the samples and the presence of local glassworks.     

Systematic studies of fission fragment kinetic energy distributions by Langevin simulations

Fission fluctuation-dissipation dynamics of heavy nuclei has been studied using Langevin Monte Carlo simulations. The covariant form of the fission transport equation and the coefficients related to it are investigated. To learn about the influence of the dynamics from the ground state to the saddle point on the kinetic energy distributions we have studied various systems and compared the calculations both starting from the ground state and from the saddle point. Both the mean total kinetic energy of the fission fragments and its variances can fit with the experimental values in terms of a finite neck radius as scission condition.This work was supported by the National Natural Science Foundation of China.     

Observation of isomeric states in197Bi

The high spin states of¹¹⁹Te, populated in¹¹⁰Pd(¹³C,4n) and¹¹⁰Pd(¹²C,3n) reactions, have been studied through -ray spectroscopy. The level scheme has been established upto a spin of 55/2. Three-quasiparticle states, based on g² _7/2h_11/2 and g_7/2d_5/2h_11/2 configurations, have been identified. The 35/2 and 39/2 states are suggested to be the fully aligned states constituted by five valence h_11/2 ³, g_7/2, d_5/2 quasiparticles.     

An impedance analyzer method to simulate the oscillating characteristic of a series piezoelectric sensor in oscillators with zero or non-zero phases

An impedance analyzer method is employed to simulate the oscillation frequency of a series piezoelectric quartz crystal (SPQC) in electrolyte or non-electrolyte solutions. The influence of the oscillator phase on the oscillation frequency and response sensitivity are theoretically derived and experimentally verified. In non-electrolyte liquids, the oscillator phase has little effect on both the oscillation frequency and the response to the permittivity. But in electrolyte solutions, the oscillator phase has a significant influence on the oscillation frequency and the response sensitivity to the conductivity. Depending on the oscillator phase, the oscillation frequency of the SPQC may increase, be maintained or decrease with increasing conductivity in low or high conductive solutions. The dependence of the oscillation frequency of the SPQC on the supply voltage is explained. As an example of the applications, the SPQC is applied to the determination of the critical micelle concentration of ionic surfactants in aqueous solutions.