Simultaneous estimation of copper, zinc, cadmium and mercury in biological material by neutron activation analysis

Simultaneous determination of copper, zinc, cadmium and mercury with high sensitivity is possible by neutron activation analysis. After irradiation, the samples are digested and an initial separation of the four elements made by means of an ion-exchange resin. The elements in the separated fractions are then treated to give radio-chemical purity, precipitated, and their activities measured. A purely instrumental technique for the analysis of zinc in samples of biological material is also described. The samples are irradiated for a week and after the activity has decayed for about three months it is measured on a gamma-spectrometer.     

Elucidation of the mechanism of chiral selectivity in diastereomeric salt formation using organic solvent nanofiltration

Organic solvent nanofiltration (OSN) was used to investigate the mechanism of chiral selectivity in diastereomeric salt formation of alpha-phenylethylamine with D-tartaric acid and di-p-toluoyl-D-tartaric acid as resolving agents; results indicate that for these systems chiral selectivity occurs only upon crystallisation and chiral interactions in solution were negligible.     

Zur Kenntnis des Faktors F430 aus methanogenen Bakterien: Struktur des proteinfreien Faktors

Factor F430 from Methanogenic Bacteria: Structure of the Protein-free Factor Factor F430, the porphinoid nickel-containing coenzyme of the methylcoenzyme-M reductase of metanogenic bacteria is shown to be the 3³,8³,12²,13³,18²-pentaacid derivative of the pentamethylester F430M, the structure of which had been determined previously (see structural formulae 1 and 2 ). The structure assignment rests on chromatographic, UV/VIS-, CD-, IR-, and ¹³C-NMR-spectroscopic as well as FAB-mass spectral comparision of F430 with F430M and the pentaacid prepared by acid-catalyzed hydrolysis of F430M. In the cells of Methanobacterium thermoautotrophicum, factor F430 is present in a ‘bound’ and also, depending on the growth conditions, in ‘free’ form, the latter being defined as the part of total F430 that can be extracted from the cells under extremely mild conditions (80% EtOH at 0–4°). From the (protein)-‘bound’ form, F430 is extracted by subsequently treating the cells at 0–4° with 80% EtOH containing (e.g.), 2m LiCi. From both sources, the extracted factor is the same pentaacid, and there is no indication for the existence of a protein-free F430 species that would contain additional (covalently bound) structural elements.     

Mechanism of and Products from the Oxidation of Phenols by Hypervalent Iodine Compounds

Iodobenzene dichloride or diacetate initiates the polymerization of 2,6-dimethylphenolate anion to poly [oxy(2,5-dimethyl)-l, 4-phenylene]. Electron spin resonance spectroscopy was used to identify the polymeric radical that is the growing chain. Infrared and NMR spectroscopy identified the final polymer. The mechanism proposed is probably applicable also to other phenol oxidation processes yielding substituted poly(oxyphenylenes).

The anomalous chemistry of those compounds of xenon, iodine, and tellurium in which the number of bonding electrons exceeds that given by Lewis valence theory has been considered in general terms by Musher [1] who coined the term “hypervalent” to describe these substances. The oxidizing properties of these compounds is in a general way similar to that of peroxides and other strong oxidizing agents, but has not been characterized in any exact fashion. We have observed [2] that the iodobenzene esters have polymeric analogs of the formula, [-I(R)OOCXCOO-], and these compounds are stable oxidizing agents (R = aryl; X = alkylene or arylene). We have been interested in determining if -I(R)OXO- compounds can be formed.

The first question to consider is the stability of bonds in -OI(R)O- compounds. Only acyl derivatives are known [3]. However, the possibility     

Two-photon decay in strong central fields observed for the case of He-like gold

The photon energy differential shape of the second order matrix element for the two-photon (2E1) decay of the 1s2s¹S₀ level in He-like gold has been measured. The results are in agreement with a recent fully relativistic calculation. The corresponding 2E1 matrix element deviates from those in lighter He-like systems due to the strong central field in a heavy two-electron ion.     

Measurement of the electric form factor of the neutron at Q2 = 0.3-0.8 (GeV/ c) 2 ⋆

The electric form factor of the neutron, G_E,n, has been measured at the Mainz Microtron by recoil polarimetry in the quasielastic D(¯e, e¯n)p reaction. Three data points have been extracted at squared four-momentum transfers Q ² = 0.3, 0.6 and 0.8 (GeV/c)². Corrections for nuclear binding effects have been applied.This revised version was published online in March 2005. In the previous version, the email address of one author was inadvertently assigned to multiple authors.     

Knot signature functions are independent

A Seifert matrix is a square integral matrix satisfying

To such a matrix and unit complex number there corresponds a signature,

Let denote the set of unit complex numbers with positive imaginary part. We show that is linearly independent, viewed as a set of functions on the set of all Seifert matrices.

If is metabolic, then unless is a root of the Alexander polynomial, . Let denote the set of all unit roots of all Alexander polynomials with positive imaginary part. We show that is linearly independent when viewed as a set of functions on the set of all metabolic Seifert matrices.

To each knot one can associate a Seifert matrix , and induces a knot invariant. Topological applications of our results include a proof that the set of functions is linearly independent on the set of all knots and that the set of two-sided averaged signature functions, , forms a linearly independent set of homomorphisms on the knot concordance group. Also, if is the root of some Alexander polynomial, then there is a slice knot whose signature function is nontrivial only at and . We demonstrate that the results extend to the higher-dimensional setting.

     

Interlaboratory comparison of actinides in human tissue239Pu and240Pu

An international laboratory intercomparison of actinides in human tissues was organized by the United States Transuranium Registry and the National Institute of Standards and Technology. Five laboratories from the United States, United Kingdom, and Japan participated in the intercomparison. The laboratories were requested to analyze Standard Reference Materials 4351 (Human Lung) and 4352 (Human Liver) for²³⁹Pu and²⁴⁰Pu concentration. Approximately equivalent measurement capabilities were generally found among the participants. The results of this intercomparison were statistically comparable to those used for the original certification of the SRM's and were combined for a re-evaluation of the certified values. The combined data sets provide a better characterization of the inhomogeneity of these reference materials and result in a better basis for certification.Deceased.     

Adjusting for confounding by cluster using generalized linear mixed models

We show how to use generalized linear mixed models to adjust for confounding by cluster of the effect of a within-cluster covariate. We derive estimators for both a cluster-specific causal effect and a population-averaged causal effect.     

A novel approach to modelling counter-current chromatography

Literature lists a number of counter-current chromatography (CCC) models that can predict the retention time and to a certain extent the peak width of a solute eluting from a CCC column. The approach described in this paper distinguishes itself from previous reports by relating all model parameters directly to column dimensions and experimental settings. Most importantly, this model can predict a chromatogram from scratch without resorting to traditional calibration using empirical values. The model validation with experimental results obtained across a range of CCC instruments demonstrated that the solute retention time, peak width, and peak resolution could be predicted within reasonable accuracy. Additionally, the effect of several process parameters, such as mobile phase flow rate, rotational speed of the column or β-value, showed that the model is robust and applicable to a wide range of CCC instruments. Overall, this model proved to be a useful tool for parameter estimation and, most significantly, separation optimisation.