Standardization of experimental

Standardization of experimental conditions time of day personnel in charge. 

Perhaps the most elementary consideration that should be satisfied is that the measured rates of enzyme reactions under aU conditions represent initial velocities (vq). The indication that initial rates or linear rates were measured are other ways to convey that this standard of experimentation has been met. One of the original stipulations of the general applicability of the Michaelis-Menten model (as well as many others) is that d[So /dt 0 during the time period over which the rate of product formation is measured. Thus, the measured reaction rate is representative of that taking place initially at the [So] selected. This condition is especially important at low [Sol values, where reaction rates are nearly first order with respect to [Sol- In practice, up to 5 to 10% depletion of [Sol can be tolerated over the time frame used to assay [P] for the purpose of determining reaction rates, because error caused by normal experimental... 

However, it must be underlined that an agreement on omics -derived food standards is presently still lacking and needs, as a first step, the standardization of experimental designs, technical protocols, and results presentation for a comparative analysis and toward the preparation of common databases. 

Section BT1.2 provides a brief summary of experimental methods and instmmentation, including definitions of some of the standard measured spectroscopic quantities. Section BT1.3 reviews some of the theory of spectroscopic transitions, especially the relationships between transition moments calculated from wavefiinctions and integrated absorption intensities or radiative rate constants. Because units can be so confusing, numerical factors with their units are included in some of the equations to make them easier to use. Vibrational effects, die Franck-Condon principle and selection mles are also discussed briefly. In the final section, BT1.4. a few applications are mentioned to particular aspects of electronic spectroscopy. 

There are two fimdamental types of spectroscopic studies absorption and emission. In absorption spectroscopy an atom or molecule in a low-lying electronic state, usually the ground state, absorbs a photon to go to a higher state. In emission spectroscopy the atom or molecule is produced in a higher electronic state by some excitation process, and emits a photon in going to a lower state. In this section we will consider the traditional instrumentation for studying the resulting spectra. They define the quantities measured and set the standard for experimental data to be considered. 

The scientific method, as mentioned, involves observation and experimentation (research) to discover or establish facts. These are followed by deduction or hypothesis, establishing theories or principles. This sequence, however, may be reversed. The noted twentieth-century philosopher Karl Popper, who also dealt with science, expressed the view that the scientist s work starts not with collection of data (observation) but with selection of a suitable problem (theory). In fact, both of these paths can be involved. vSignificant and sometimes accidental observations can be made without any preconceived idea of a problem or theory and vice versa. The scientist, however, must have a well-prepared, open mind to be able to recognize the significance of such observations and must be able to follow them through. Science always demands rigorous standards of procedure, reproducibility, and open discussion that set reason over irrational belief. 

Analysis of Standards The analysis of a standard containing a known concentration of analyte also can be used to monitor a system s state of statistical control. Ideally, a standard reference material (SRM) should be used, provided that the matrix of the SRM is similar to that of the samples being analyzed. A variety of appropriate SRMs are available from the National Institute of Standards and Technology (NIST). If a suitable SRM is not available, then an independently prepared synthetic sample can be used if it is prepared from reagents of known purity. At a minimum, a standardization of the method is verified by periodically analyzing one of the calibration standards. In all cases, the analyte s experimentally determined concentration in the standard must fall within predetermined limits if the system is to be considered under statistical control. 

Even though the rates of initiation span almost a 10-fold range, the values of k, show a standard deviation of only 4%, which is excellent in view of experimental errors. Note that the rotating sector method can be used in high-pressure experiments and other unusual situations, a characteristic it shares with many optical methods in chemistry. 

Variations ia the Hquid-juactioa poteatial may be iacreased whea the standard solutions are replaced by test solutions that do not closely match the standards with respect to the types and concentrations of solutes, or to the composition of the solvent. Under these circumstances, the pH remains a reproducible number, but it may have Httle or no meaning ia terms of the coaveatioaal hydrogea-ioa activity of the medium. The use of experimental pH aumbers as a measure of the exteat of acid—base reactioas or to obtaia thermodynamic equiHbrium coastants is justified only whea the pH of the medium is betweea 2.5 and II.5 and when the mixture is an aqueous solution of simple solutes ia total coaceatratioa of ca <0.2 M. 

Such programs generally concentrate on the technical parts of designing an experiment, and provide limited guidance on the important, softer aspects of experimental design stressed in this article. Also, most computer routines do not allow one to handle various advanced concepts that arise frequently in practice, eg, spHt plot and nested situations, discussed in the books in the bibhography. In fact, some of the most successful experiments do not involve standard canned plans, but are tailored to fit the problem at hand. 

V. L. Anderson and R. A. McLean, Design of Experiments—A Eea/istic Approach, Marcel Dekker, New York, 1974. This book provides an extensive exposition of experimental design at a relatively elementary level. It includes most of the standard material, as well as detailed discussions of such subjects as nested and spHt-plot experiments. Restrictions on randomization receive special emphasis. 

Appendix 6 contains requirements of experimental stress analysis. Appendix 8 has acceptance standards for radiographic examination. Appendix 9 covers nondestructive examination. Appendix 10 gives rules for capacity conversions for safety valves, and Appendix 18 details quahty-control-system requirements. 

Standard Deviation of Experimental Results from pairs of Measurements... 

The estimation of the mean and standard deviation using the moment equations as described in Appendix I gives little indication of the degree of fit of the distribution to the set of experimental data. We will next develop the concepts from which any continuous distribution can be modelled to a set of data. This ultimately provides the most suitable way of determining the distributional parameters. 

Thus, as for XP S, the average surface concentration Na can, in principle, be calculated by measurement of the Auger current, according to Eq. (2.13). Again, as in XPS, relative sensitivity factors are generally used. The Auger current for the same transition XYZ in a standard of pure A is measured under the same experimental conditions as in the analysis of A in M, whereupon the ratio of the atomic concentrations is... 

Rubin and Blossey standardized the experimental conditions for the Serini reaction, using freshly activated zinc in refluxing xylene for 20-24 hr with vigorous stirring yields of68-100 % could then be obtained. They noted, however, that the presence of a 16a- or -methyl group markedly decreased the yield, and that a primary-secondary glycol monoacetate failed to react. 

The satisfactory result shown in Table 12 suggests that one might give a more detailed and quantitative discussion of the variation with temperature. If we are to do this, we need some standard of comparison with which to compare the experimental results. Just as wq compare an imperfect gas with a perfect gas, and compare a non-ideal solution with an ideal solution, so we need a simple standard behavior with which to compare the observed behavior. We obtain this standard behavior if, supposing that. /e is almost entirely electrostatic in origin, we take J,np to vary with temperature as demanded by the macroscopic dielectric constant t of the medium 1 that is to say, we assume that Jen, as a function of temperature is inversely proportional to . For this standard electrostatic term we may use the notation, instead of... 

To obtain comparative values of the strengths of oxidising agents, it is necessary, as in the case of the electrode potentials of the metals, to measure under standard experimental conditions the potential difference between the platinum and the solution relative to a standard of reference. The primary standard is the standard or normal hydrogen electrode (Section 2.28) and its potential is taken as zero. The standard experimental conditions for the redox... 

The most common direct methods are the oven, the distillation, and the Fischer methods. They can be made precise by careful standardization of the experimental procedures their accuracy can be assured only by calibration against some accurate reference method. 

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