Dynamic mechanical tests experimental measurements

Dynamic mechanical properties are measured to evaluate melt rheology of thermoplastics with and without additives which may modify rheological characteristics of these compositions. " Dynamic oscillatory shear rheometers are used for these purposes. Two geometries of test fixtures are used including parallel plates and cone and plate. Instrument use for these measurements must be capable of measuring forces (stress or strain) and frequency. Temperature must be controlled in a broad range and various modes of temperature sweeps should be available. Sample geometry is not specified but it should be suitable for measurement in particular experimental setup. 

Dynamic mechanical measurements for elastomers that cover wide ranges of frequency and temperature are rather scarce. Payne and Scott [12] carried out extensive measurements of /a and /x" for unvulcanized natural mbber as a function of test frequency (Figure 1.8). He showed that the experimental relations at different temperatures could be superposed to yield master curves, as shown in Figure 1.9, using the WLF frequency-temperature equivalence, Equation 1.11. The same shift factors, log Ox. were used for both experimental quantities, /x and /x". Successful superposition in both cases confirms that the dependence of the viscoelastic properties of rubber on frequency and temperature arises from changes in the rate of Brownian motion of molecular segments with temperature. 

Recently there has been an increasing interest in self-oscillatory phenomena and also in formation of spatio-temporal structure, accompanied by the rapid development of theory concerning dynamics of such systems under nonlinear, nonequilibrium conditions. The discovery of model chemical reactions to produce self-oscillations and spatio-temporal structures has accelerated the studies on nonlinear dynamics in chemistry. The Belousov-Zhabotinskii(B-Z) reaction is the most famous among such types of oscillatory chemical reactions, and has been studied most frequently during the past couple of decades [1,2]. The B-Z reaction has attracted much interest from scientists with various discipline, because in this reaction, the rhythmic change between oxidation and reduction states can be easily observed in a test tube. As the reproducibility of the amplitude, period and some other experimental measures is rather high under a found condition, the mechanism of the B-Z reaction has been almost fully understood until now. The most important step in the induction of oscillations is the existence of auto-catalytic process in the reaction network. 

Becanse there are many factors involved in the dynamic mechanical compression of polyolefin foams, the Taguchi method was employed in a Perkin Elmer DM A7 dynamic mechanical analyser to establish a method to improve the measurement process. The signal-to-noise ratio was measured to determine how the variability could be improved. Control and noise factors were evaluated and levels chosen, with details being tabulated. Appendix A describes some of the factors. Tests were conducted on two closed cell foams. NA2006 foam is 48 kg/cu m LDPE and NEE3306 foam is 32 kg/cu m EVA. Different factors were shown to influence results for E and tan delta but an optimum combination is proposed for the simultaneous measurement of both properties. The results were less variable as frequency was increased. Small differences in the dynamic response of different materials should be measurable because of the low variability in the experimental results. 18 refs. 

Composition profiles generated by interdiffusion in the concentrated regime between polyphenylene oxide-polystyrene blend pairs were experimentally determined by two techniques. Three-point bending moment measurements over a convenient temperature range (dynamic mechanical analysis (DMA)) were used to determine interphase composition profiles. Confocal micro-Raman spectroscopy was also used to measure local compositions along a direction which was perpendicular to the original interface. The study included some limiting cases to test accuracy, precision and flexibility of the DMA method. 4 refs. 

In the second example, in which desolvation influences were considered, Reddy et al. used a computer-assisted ligand design method that combines molecular mechanics, molecular dynamics, FEP calculations, synthesis, and biochemical testing of peptidomimetic inhibitors, plus crystallographic structure determination of the protein-inhibitor complexes. This combination of techniques successfully led to the design of novel inhibitors for the HIV-1 protease enzyme. This study involved a large set of molecules whose relative binding affinities, predicted via the FEP method prior to synthesis, were later confirmed by experimental measurements. 

A complete description of the viscoelastic properties of a material requires information over very long times. Creep and stress relaxation measurements are limited by inertial and experimental limitations at short times and by the pa-tienee of the investigator and structural changes in the test material at very long times. To supplement these methods, the stress or the strain can be varied sinusoidally in a dynamic mechanical experiment. The frequency of this alternation is V cycles/s or co = 2nv) rad/s. An alternating experiment at frequency w is qualitatively equivalent to a creep or stress relaxation measurement at a time t = ( /w) sec. 

Generally, two different types of measurement are applied to determine the linear viscoelastic behavior, namely static (or equilibrium) and dynamic mechanical measurements. Static tests involve the imposition of a step change in stress and the observation of any subsequent development in time of the strain, whereas dynamic tests involve the application of a harmonically varying strain. In ordinary thermoplastic polymer systems, test conditions such as strain or frequency must be in the linear range otherwise, the results will be dependent on the experimental details rather than on the material under test. 

Standard Test Method for Measuring the Dynamic Mechanical Properties of Plastic Using Three Point Bending (The relevant experimental conditions were Frequency IHz, Heat Up Rate 2°C/min)... 

Laboratory simulations of aqueous-phase chemical systems are necessary to 1) verify reaction mechanisms and 2) assign a value and an uncertainty to transformation rates. A dynamic cloud chemistry simulation chamber has been characterized to obtain these rates and their uncertainties. Initial experimental results exhibited large uncertainties, with a 26% variability in cloud liquid water as the major contributor to measurement uncertainty. Uncertainties in transformation rates were as high as factor of ten. Standard operating procedures and computer control of the simulation chamber decreased the variability in the observed liquid water content, experiment duration and final temperature from 0.65 to 0.10 g nr3, 180 to 5.3 s and 1.73 to 0.27°C respectively. The consequences of this improved control over the experimental variables with respect to cloud chemistry were tested for the aqueous transformation of SO2 using a cloud-physics and chemistry model of this system. These results were compared to measurements made prior to the institution of standard operating procedures and computer control to quantify the reduction in reaction rate uncertainty resulting from those controls. 

---