Experiments recovery

I and the measured line intensities are fitted to an exponential expression. S (-e) =A + B exp(-i / T ). The inversion-recovery experiments are often perfonned for multiline spectra of low-natural abundance nuclei,... 

Figure Bl.13.3. The inversion-recovery experiment. (Reproduced by pennission of VCFI from Banci L, Bertini I and Luchinat C 1991 Nuclear and Electron Relaxation (Weinlieim VCFI).)...

In this chapter, we will review the effects of shock-wave deform.ation on material response after the completion of the shock cycle. The techniques and design parameters necessary to implement successful shock-recovery experiments in metallic and brittle solids will be discussed. The influence of shock parameters, including peak pressure and pulse duration, loading-rate effects, and the Bauschinger effect (in some shock-loaded materials) on postshock structure/property material behavior will be detailed. 

The structure/property relationships in materials subjected to shock-wave deformation is physically very difficult to conduct and complex to interpret due to the dynamic nature of the shock process and the very short time of the test. Due to these imposed constraints, most real-time shock-process measurements are limited to studying the interactions of the transmitted waves arrival at the free surface. To augment these in situ wave-profile measurements, shock-recovery techniques were developed in the late 1950s to assess experimentally the residual effects of shock-wave compression on materials. The object of soft-recovery experiments is to examine the terminal structure/property relationships of a material that has been subjected to a known uniaxial shock history, then returned to an ambient pressure... 

Shock-recovery experiments by Gray [10] were conducted to assess directly if the strain-path reversal inherent to the shock contains a traditional microstructurally controlled Bauschinger effect for a shock-loaded two-phase material. Two samples of a polycrystalline Al-4 wt.% Cu alloy were shock loaded to 5.0 GPa and soft recovered in the same shock assembly to assure identical shock-loading conditions. The samples had two microstructural... 

G.T. Gray III, Shock Recovery Experiments An Assessment, in Shock Compression of Condensed Matter—1989 (edited by S.C. Schmidt, J.N. Johnson, and L.W. Davison), North-Holland, Amsterdam, 1990, 407 pp. 

P.S. Decarli and M.A. Meyers, Design of Uniaxial Strain Shock Recovery Experiments, in Shock Waves and High Strain Rate Phenomena in Metals, (edited by M.A. Meyers and L.E. Murr), Plenum, New York, 1981, 341 pp. 

The shock-induced micromechanical response of <100>-loaded single crystal copper is investigated [18] for values of (WohL) from 0 to 10. The latter value results in W 10 Wg at y = 0.01. No distinction is made between total and mobile dislocation densities. These calculations show that rapid dislocation multiplication behind the elastic shock front results in a decrease in longitudinal stress, which is communicated to the shock front by nonlinear elastic effects [pc,/po > V, (7.20)]. While this is an important result, later recovery experiments by Vorthman and Duvall [19] show that shock compression does not result in a significant increase in residual dislocation density in LiF. Hence, the micromechanical interpretation of precursor decay provided by Herrmann et al. [18] remains unresolved with existing recovery experiments. 

To answer questions regarding dislocation multiplication in Mg-doped LiF single crystals, Vorthman and Duvall [19] describe soft-recovery experiments on <100)-oriented crystals shock loaded above the critical shear stress necessary for rapid precursor decay. Postshock analysis of the samples indicate that the dislocation density in recovered samples is not significantly greater than the preshock value. The predicted dislocation density (using precursor-decay analysis) is not observed. It is found, however, that the critical shear stress, above which the precursor amplitude decays rapidly, corresponds to the shear stress required to disturb grown-in dislocations which make up subgrain boundaries. 

An important aspect of micromechanical evolution under conditions of shock-wave compression is the influence of shock-wave amplitude and pulse duration on residual strength. These effects are usually determined by shock-recovery experiments, a subject treated elsewhere in this book. Nevertheless, there are aspects of this subject that fit naturally into concepts associated with micromechanical constitutive behavior as discussed in this chapter. A brief discussion of shock-amplitude and pulse-duration hardening is presented here. 

Along a different line of research on shock compression of solids, namely, recovery experiments, great progress was also being made. Shock-induced recovery-type chemical reactions in encapsulated samples were first reported by Riabinin in 1956. Shock-induced metallographic transformation and the observation of twin bands in iron were first reported by Smith in 1958. Another major breakthrough was the shock-induced synthesis of diamond in 1961 by DeCarli and Jamieson. 

Given the advanced state of wave-profile detectors, it seems safe to recognize that the descriptions given by such an apparatus provide a necessary, but overly restricted, picture. As is described in later chapters of this book, shock-compressed matter displays a far more complex face when probed with electrical, magnetic, or optical techniques and when chemical changes are considered. It appears that realistic descriptive pictures require probing matter with a full array of modern probes. The recovery experiment in which samples are preserved for post-shock analysis appears critical for the development of a more detailed defective solid scientific description. 

In an experiment in which a sample is subjected to controlled shock loading and preserved for post-shock analysis, the shock-recovery experiment, the quantification, and the credibility of the experiment rest directly upon the apparatus in which the experiments are carried out. Quantification must be established with two-dimensional numerical simulation and this can only be accomplished if the recovery fixtures are standardized. The standardized fixtures must be capable of precise assembly so that the conditions actually achieved in the experiment are those of the simulation. 

The author s work has included the development of the Sandia Bear and Bertha explosive recovery fixtures, that provide a standardized set of fixtures in which recovery experiments can be routinely carried out at peak shock pressures from 4 to 500 GPa. Shock-induced, mean-bulk temperatures from 50 to 1200°C are achieved with variation in the density of the powder compacts under study. 

The only recourse is to modify the recovery experiments above in the sense that the sample to be tested itself is used as a kind of blank, to which further analyte is spiked. This results in at least two measurements, namely untreated sample and spiked sample, which can then be used to establish a calibration line from which the amount of analyte in the untreated sample... 

Fig. 1.—Diagrammatic Representation of the Recovery of Magnetization along the z-Axis (Mj), from Its Initial Value (-M ) to +Mo, Following Its Inversion by a 180° Pulse. The exponential recovery curve shown in [A] depicts the return of magnetization that would be found in a typical inversion-recovery experiment. The curve in [B] would be obtained from a three-pulse sequence, and is a plot of which decreases from an initial value of...

Figure 4. Recovery experiments for OH AMP at 110, 50, and 20 ppm in the absence (-----) and presence (-----) of polymeric dyes (1 g/dL) (ordinate absorb-...

The effect of alkaline preflush was also studied under two different conditions. All of the oil-recovery experiments were conducted under optimal conditions with a viscous, nonacidic oil and with Berea sandstone cores. 

Various bacterial species have proven useful in MEOR. The principle is based on the species biochemical byproducts produced, such as gases, surfactants, solvents, acids, swelling agents, and cosurfactants, which facilitate the displacement of oil. In field experiments, in situ fermentation is often desirable for producing a great quantity of gases. Clostridium hydrosulfuricum 39E was found to have surface-active properties during simulated enhanced oil recovery experiments [1874]. 

C. hydrosulfuricum 39E was found to have surface-active properties during simulated enhanced oil-recovery experiments [1875]. 

To validate the analytical procedure recovery experiments are performed. To this end, the CRM is spiked with a known mass of the analytes at a variety of concentration levels (at least three different levels) and the concentrations measured are compared to the expected concentrations in at least three separate experiments. The extraction step has been shown to be a critical step in the analytical procedure and it may be responsible for poor recoveries. The efficiency of this step can be assessed either by repetitive extraction of the sample or by the addition of internal standards prior to the extraction step with the assumption that the latter actually represent the behavior of the analytes of interest. 

There are various approaches to determine the trueness of methods. The most common is the performance of recovery experiments. According to the guidance document SANCO/825/00, the mean recovery should be in the range of 70-110%. In justified cases, recoveries outside this range can be acceptable. 

According to SANCO/825/00, a fully validated method consisting of some or all of the components mentioned above must be reported. Provided that sufficient validation data are published by official manuals, further recovery experiments are not necessary. 

A final special case may occur during the validation of common moiety methods. Based on the normal set of recovery experiments (two control samples, five samples fortified at the LOQ and five samples fortified at 10 times the LOQ), in total 12 samples have to be analyzed per matrix and analyte. A typical intention of common moiety methods is their suitability for the parallel determination of residues of the parent compound and a broad spectrum of metabolites. In the common moiety method discussed above for residues of spiroxamine, validation experiments were performed with four compounds. This results in at least 48 experiments per matrix. Assuming a normal... 

On the other hand, some sensible reduction may be acceptable. In the spiroxamine example, an appropriate reduced validation protocol may be as follows a full set of recovery experiments at both levels performed with the intact spiroxamine (which has the longest reaction pathway to the common moiety) and separately with one primary metabolite. Such two complete validations should be an acceptable test of the working range of the common moiety method. 

As the alkylenebis(dithiocarbamates) are not soluble in water or organic solvents, there are two possible procedures to carry out the recovery experiments. The first is to fortify the solid standard onto the untreated sample in the decomposition vessel, and follow the determination procedure as described above. A second option is to... 

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