Using isothermal microcalorimetry for the prediction and testing of long-term properties of materials and products

The use of isothermal microcalorimetry (MC) as a sensitive monitor for slow reactions is demonstrated in a number of examples. In Example 1 the spontaneous decomposition of a nitrate ester propellant is studied and the absolute degradation rate estimated. Example 2 illustrates how MC can be used for comparing the rate of oxidative ageing at different O₂ concentrations. Synergetic effects between oxygen and moisture in accelerated ageing of nitrile rubber are evaluated from a so-called 4-point test in Example 3. The last example shows a simple MC technique for rapid determination of moisture permeability through a polymeric sealant.     

A Multicontrolled Enamine Configurational Switch Undergoing Dynamic Constitutional Exchange

A multiresponsive enamine‐based molecular switch is presented, in which forward/backward configurational rotation around the C=C bond could be precisely controlled by the addition of an acid/base or metal ions. Fluorescence turn‐on/off effects and large Stokes shifts were observed while regulating the switching process with Cu^II. The enamine functionality furthermore enabled double dynamic regimes, in which configurational switching could operate in conjunction with constitutional enamine exchange of the rotor part. This behavior was used to construct a prototypical dynamic covalent switch system through enamine exchange with primary amines. The dynamic exchange process could be readily turned on/off by regulating the switch status with pH.     

The disordered cubic structure of Ca7Co3Ga5O18

The new mixed oxide having composition close to Ca₇Co₃Ga₅O₁₈ was synthesized from CaCO₃, Co₃O₄ and Ga₂O₃ at 1150 °C in air and studied by neutron and synchrotron X-ray powder diffraction, selected-area electron diffraction and high-resolution electron microscopy. The structure was refined, using time-of-flight (TOF) neutron powder diffraction data, in space group F432, with and Z=8, to R_F=0.7%. It is considerably disordered, with four different tetrahedral sites randomly occupied by Co and Ga atoms at a ratio of 1:2. The tetrahedra form a disordered (Co_1/3Ga_2/3)O₂ 3D-framework inside which isolated CoO₆ octahedra, surrounded by 8 Ca atoms, are located. The structure is related to the ordered structure of Ca₁₄Al₁₀Zn₆O₃₅. Electron diffraction patterns confirmed the symmetry and unit cell and revealed no diffuse scattering. High-resolution electron microscopy images showed the absence of extended structural defects.     

Factors influencing level of hydrogen peroxide in exhaled breath condensate

Hydrogen peroxide (H₂O₂) in exhaled breath condensate (EBC) has been proposed as a marker for oxidative stress in the airways. The aim of the present study was to evaluate the measurement of H₂O₂ in EBC with or without use of a nose clip, and the influence of mouth rinsing, sampling time and storage.An elevated H₂O₂ level was seen during nasal breathing compared to mouth breathing with nose clip (3.4 pmol/s vs. 2.1 pmol/s, p = 0.02). Breathing through the mouth, using a nose clip, was therefore practiced in all experiments. The H₂O₂ levels were increased when mouth rinsing was performed using an acid buffer (1.4 pmol/s vs. 1.9 pmol/s, p = 0.03). 15 min sampling time decreased the H₂O₂ output by almost 50% compared with 2 min sampling time (1.2 vs. 0.6 pmol/s, p = 0.03). When samples were left unattended for 15 min no change in H₂O₂ concentration in the EBC was seen.We found no significant differences in H₂O₂ levels between samples stored for 4 weeks at − 80 °C and samples analysed directly; however, a significant decrease in the levels was seen for samples stored for 4 weeks at − 20 °C.In conclusion, the method of EBC collection and storage plays an important role in reducing variability within and between individuals.     

Reflections regarding uncertainty of measurement, on the results of a Nordic fatigue test interlaboratory comparison

This paper presents the experiences of calculation and reporting uncertainty of measurement in fatigue testing. Six Nordic laboratories performed fatigue tests on steel specimens. The laboratories also reported their results concerning uncertainty of measurement and how they calculated it. The results show large differences in the way the uncertainties of measurement were calculated and reported. No laboratory included the most significant uncertainty source, bending stress (due to misalignment of the testing machine, incorrect specimens and/or incorrectly mounted specimens), when calculating the uncertainty of measurement. Several laboratories did not calculate the uncertainty of measurement in accordance with the Guide to the Expression of Uncertainty in Measurement (GUM) [1].