GC–MS analysis of phenolic compounds in fuels after conversion to trifluoroacetate esters

The GC–MS characteristics of trifluoroacetate esters of phenolic compounds are discussed. Linear temperature programmed retention indices and total ion current MS response factors of over 120 phenolic esters are reported. The main GC advantages from analysis of trifluoroacetate esters as compared to plain phenols are enhanced volatility and improved resolution. For example, the elution temperature of a given phenol is typically 50 °C greater than that of the corresponding trifluoroacetate ester. Also, while retention of compounds with two trifluoroacetate groups is only moderately greater than mono esters, underivatized dihydroxy compounds are very difficult to elute from any GC column. Complete resolution of isomeric C₀-, C₁- and C₂-alkylphenol esters is readily achieved on conventional fused silica GC columns; resolution of the corresponding underivatized compounds requires specialized GC columns with low temperature limits. In general, mass spectra of trifluoroacetate esters are more characteristic of a given structure than those of the corresponding phenols and may be more rigorously interpreted towards structural elucidation. A table in the report summarizes some of the more important spectral features used in compound identification. Example applications in analysis of coal-, shale- and petroleum-derived materials are presented. Selected ion monitoring is used to determine individual phenolic components in whole distillates; reconstructed ion chromatograms are used to illustrate distributions of selected species as a function of fuel storage and thermal stress.     

Shotgun proteomics‐based clinical testing for diagnosis and classification of amyloidosis

Shotgun proteomics technology has matured in the research laboratories and is poised to enter clinical laboratories. However, the road to this transition is sprinkled with major technical unknowns such as long‐term stability of the platform, reproducibility of the technology and clinical utility over traditional antibody‐based platforms. Further, regulatory bodies that oversee the clinical laboratory operations are unfamiliar with this new technology. As a result, diagnostic laboratories have avoided using shotgun proteomics for routine diagnostics. In this perspectives article, we describe the clinical implementation of a shotgun proteomics assay for amyloid subtyping, with a special emphasis on standardizing the platform for better quality control and earning clinical acceptance. This assay is the first shotgun proteomics assay to receive regulatory approval for patient diagnosis. The blueprint of this assay can be utilized to develop novel proteomics assays for detecting numerous other disease pathologies. Copyright © 2013 John Wiley & Sons, Ltd.     

Untersuchung von Mehl

Ohne Zusammenfassung     

Invertible symmetric 3 × 3 binary matrices and GQ(2, 4)

We reveal an intriguing connection between the set of 27 (disregarding the identity) invertible symmetric 3?×?3 matrices over GF(2) and the points of the generalized quadrangle GQ(2,?4). The 15 matrices with eigenvalue one correspond to a copy of the subquadrangle GQ(2,?2), whereas the 12 matrices without eigenvalues have their geometric counterpart in the associated double-six. The fine details of this correspondence, including the precise algebraic meaning/analogue of collinearity, are furnished by employing the representation of GQ(2,?4) as a quadric in PG(5,?2) of projective index one. An interesting physics application of our findings is also mentioned.     

The influence of statistical error in radioactivity counting on the precision of isotope dilution analysis,I

The influence of the statistical error in measuring radioactive samples in direct isotope dilution analysis is analytically studied for several practically important sets of conditions. Formulas are given to calculate the optimum amount of radioactive substance to be added in order to minimize the error involved. Both cases with negligible background count rates and cases where the background must be considered are treated. In some cases recommendations are given for the times of measurement of background, undiluted and diluted sample.     

Study of the production of a strange (S = −1) dibaryon in the interactions of K− and π+ on deuterium below 1.5GeV/c

The production of a strange dibaryonic system called H⁺₁ (M = 2.13 GeV/c², S = ?1), has been studied with a missing mass spectrometer, at the CERN Proton Synchrotron, in the reaction K^?d → π^?H⁺₁ and in the line-reversed reaction π⁺d → K⁺H⁺₁ between 0.9 and 1.4 GeV/c.The reactions

$\text{K}{}^{\mathrm{?}}\text{d}\text{→ π}{}^{\mathrm{?}}\text{X}{}^{\mathrm{+}}$

,

$\text{π}{}^{\mathrm{<mtext>d</mtext>}}\text{→}\text{K}{}^{\mathrm{+}}\text{X}{}^{\mathrm{+}}$

,have been studied in a missing mass spectrometer at CERN. The experiment (PS159) is well adapted to search for a signal in the missing mass X⁺ (B = 2, S = ?1) produced in the backward c.m.s. direction, between 2.0 and 2.3 GeV/c². The two reactions have been analysed at three different beam settings: 1.4, 1.06 and 0.92 GeV/c for reaction (1) and 1.4, 1.2 and 1.06 GeV/c for reaction (2).     

Neurotoxicity of tetraphenylporphinesulfonate (TPPS4) and a hematoporphyrin derivative (Photosan) in organotypic cultures of chick embryonic dorsal root ganglia

The neurotoxic effect of tetraphenylporphinesulfonate (TPPS4) and a hematoporphyrin derivative (HPD, Photosan) has been studied in organotypic cultures of chick dorsal root ganglia maintained in a semi-solid culture medium. The changes in two characteristics of neurite outgrowth, the mean radial length of neurites growing out from the ganglia and the area of neurite outgrowths, are used as parameters to evaluate the toxic effect. The porphyrins are tested over the concentration range 10-160 micrograms ml-1. TPPS4 is slightly more toxic than the HPD Photosan. The median inhibitory concentration (IC50) for TPPS4 is 45-50 micrograms ml-1 and for the HPD Photosan 50-60 micrograms ml-1, respectively. Nevertheless, the toxicity of the two drugs is relatively low compared to that of commonly used anticancer drugs, such as cisplatin or taxol.     

Precise determination of the neutron scattering length of lead isotopes <Superscript>204</Superscript>Pb, <Superscript>207</Superscript>Pb and <Superscript>208</Superscript>Pb by neutron interferometry

Excited states of ⁶⁸Ga have been investigated through the ⁵⁵Mn(¹⁶O, 2pn) reaction at projectile energy 55 MeV. The level scheme has been extended up to 7.8 MeV. Altogether six new excited levels could be identified and twelve previously unobserved γ-transitions have been placed in the modified level scheme. Received: 19 June 2000 / Accepted: 20 October 2000     

The influence of the statistical error in radioactivity counting on the precision of isotope dilution analysis,II

Three types of direct isotope dilution analysis (IDA) are mathematically treated: substoichiometric dilution analysis, the determination of sorbent capacity, and direct IDA with a constant amount of substance lost in the separation step. Tables and graphs are given for an easy determination of the amount of radioisotopeW ₀ to be added and for the estimated error involved.     

A Generalization of Strassen’s Theorem on Preordered Semirings

Order - Given a commutative semiring with a compatible preorder satisfying a version of the Archimedean property, the asymptotic spectrum, as introduced by Strassen (J. reine angew. Math. 1988), is...