A rapid and sensitive extractive spectrophotometric determination of copper(II) in pharmaceutical and environmental samples using benzildithiosemicarbazone.

Benzildithiosemicarbazone (BDTSC) is proposed as a sensitive and selective analytical reagent for the extractive spectrophotometric determination of copper(II). BDTSC reacts with copper(II) in the pH range 1.0-7.0 to form a yellowish complex. Beer's law is obeyed in the concentration range 0.5-0.4 microg cm(-3). The yellowish Cu(II)-BDTSC complex in chloroform shows a maximum absorbance at 380 nm, with molar absorptivity and Sandell's sensitivity values of 1.63 x 10(4) dm3 mol(-1) cm(-1) and 0.00389 microg cm(-2), respectively. A repetition of the method is checked by finding the relative standard deviation (RSD) (n = 10), which is 0.6%. The composition of the Cu(II)-BDTSC complex is established as 1:1 by slope analysis, molar ratio and Asmus' methods. An excellent linearity with a correlation coefficient value of 0.98 is obtained for the Cu(II)-BDTSC complex. The instability constant of the complex calculated from Edmond and Birnbaum's method is 7.70 x 10(-4) and that of Asmus' method is 7.66 x 10(-4), at room temperature. The method is successfully employed for the determination copper(II) in pharmaceutical and environmental samples. The reliability of the method is assured by analyzing the standard alloys (BCS 5g, 10g, 19e, 78, 32a, 207 and 179) and by inter-comparison of experimental values, using an atomic absorption spectrometer.     

Substitution of calcium by strontium within selected calcium phosphates

Sr incorporation in the molecules of amorphous calcium phosphate, apatitic tricalcium phosphate, hydroxyapatite, octacalcium phosphate and dicalcium phosphate dihydrate was investigated. The concentration of Sr ranged from 225 to 1010 μ g / g, i.e. it overlapped with the physiological range of Sr concentrations in human bone. The leading experimental technique was extended X-ray absorption fine structure (EXAFS) at the Sr K edge. Results of these studies demonstrated the following: (1) Sr incorporation in the calcium phosphates is compound-dependent, (2) the coordination of incorporated Sr atoms in the Ca-P molecules is similar to that of Ca atoms, but interatomic distances are ≈0.015 nm larger, (3) in apatitic tricalcium phosphate, hydroxyapatite and octacalcium phosphate lattices Sr atoms may occupy selected Ca sites, which was not the case for dicalcium phosphate dihydrate, (4) in the apatite lattice Sr atoms are coordinated by 6 PO₄ tetrahedrals and (5) EXAFS spectra at the K edge of the incorporated Sr may be used to distinguish the structures of amorphous calcium phosphate, dicalcium phosphate dihydrate as well as apatite and its derivatives (apatitic tricalcium phosphate, octacalcium phosphate).     

X-ray induced fluorescence spectrometry at grazing incidence for quantitative surface and layer analysis

Summary Single layers and layer systems on diverse substrates were measured by Total Reflection X-Ray Fluorescence (TXRF) spectrometry. The angular dependence of the fluorescence intensities at grazing incidence allows the elemental composition, density and thickness of the layers to be evaluated using model calculations.     

Theoretical and experimental investigation of the linear optical response of YBa2Cu4O8 The relevance of LDA calculations

We report results of ellipsometric measurements of the dielectric tensor of YBa₂Cu₄O₈ as well as calculations employing density functional theory in the local density approximation (LDA). For the computation of the one-electron eigenvalues and states the linear-muffin-tin-orbital method (LMTO) was used. Measured and calculated results show good agreement. In particular, the calculation predicts different band structures for YBa₂Cu₃O₇ and YBa₂Cu₄O₈ in the vicinity of the Fermi energy which lead to significant differences in the optical spectra. One such difference is a region of small ε₂ in the near infrared which is a fingerprint of the high (relative to the top of the highest fully occupied band) Fermi energy as compared to the situation in YBa₂Cu₃O₇. Our experimental results confirm the theoretical findings.     

Input control in nonnegative matrix equations

In this paper we consider the nonnegative matrix system c_iA+u_iB=c_i+1 where the nonnegative matrix A is allowed to vary, within bounds. The cone control problem is to find a nonnegative matrix B such that if C_i is a nonnegative vector in a specified cone, then there is a nonnegative vector u_i such that c_i+1 is in that cone. We extend this problem to input control by finding a B such that the cone, generated by the rows of B, is as small as possible. Thus, the percent distribution of ∣u_iB∣ through the states of the sustem by u_iB is either constant or varies little.     

Flow and reactive transport in porous media induced by well injection: Similarity solution

The authors study concentration profiles of solutes undergoingequilibrium absorption in the vicinity of a water well. Forthe case of a contamination event, the limit problem of vanishingwell radius, which is of self-similar nature, is analysed indetail. Existence, uniqueness, and qualitative properties ofsolutions of the corresponding ordinary differential equationsare shown. Some numerical examples are also presented.     

NATA: 50 years experience with accreditation

 Laboratory accreditation is becoming increasingly accepted around the world as a means of identifying technically competent laboratories. It is also being used as a mechanism for the acceptance of test data both nationally and internationally. The concept and mechanisms of accreditation have been developed over the past 50 years. The first national laboratory accreditation system appeared in Australia in 1947. This organisation, known as the National Association of Testing Authorities (NATA), has since taken a leading role in developing accreditation practices that are now used world-wide in evaluating testing, measurement and calibration laboratories. This paper examines the development of the world's first and largest laboratory accreditation system, and looks at the difficulties and triumphs in gaining acceptance and recognition by government and industry of the benefits of laboratory accreditation. Received: 24 June 1996 Accepted: 25 June 1996