Instrumentation changes

Because they are plotted on an absolute-intensity basis with no correction for background, all standard graphs immediately become obsolete after any instrumental change and must be redone. When many standards are used, restandardization becomes time consuming. 

In the Beckman instrument, change in conductivity is used (28). The instrument uses 14pi for the test but samples from a cup which needs to contain at least 100 pi of serim. 

One practical example of the consequences of change control is that in the regime of system/instrument change control, hardware, software and operational aspects such as routine operation, maintenance and data integrity are locked down in fixed configurations. Any modification that has not been anticipated in the initial qualification requires testing and documentation. 

The feasibility exercise should include preparation of a concentrated (stock) solution as well as diluted standard solutions of various concentrations and establishing a first calibration curve. From the data obtained, preliminary conclusions should be drawn with respect to the approximate precision, its working range and limit of detection. Finally, the results should provide sufficient evidence with respect to the workability of the intended analytical approach. If the method appears inappropriate, it must be optimized by methodological improvements, instrument changes or applica-... 

Initial inspection of the dyed carpet suggested that good color reproducibility and uniformity had been achieved. Ten samples were cut from each of the dyed samples and the color measured on the Diano Colorimeter. Each sample was measured three times to average variations due to instrument changes and sample texture differences. Tristimulus values (X,Y,Z) were calculated from the average of the three measurements. 

The interaction of hydrogen chloride with alumina was also investigated with the same instruments. Changes in the surface hydroxyl groups 29b) were observed that were directly correlated with the active sites. The combination of information from the TOSCA and MARI neutron scattering spectrometers to solve problems in surface chemistry is a powerful method that will undoubtedly be exploited further. It is through an improved awareness of reactant-catalyst interactions that increased efficiencies of industrial chemical processes can be recognized and realized. 

Instrument changes Linearity (working range), LOD, LOQ, system precision. 

Some systematic instrument errors can be found and corrected by calibration. Periodic calibration of equipment is always desirable because the response of most instruments changes with time as a result of wear, corrosion, or mistreatment. Many systematic instrument errors involve interferences in which a species present in the sample affects the response of the analyte. Simple calibration does not compensate for these effects. Instead, the methods described in Section 8C-3 can be used when such interference effects exist. 

Verification or revalidation should be performed when relevant, for example, when there are changes in the process for synthesis of the drug substance changes in the composition of the finished product changes in the analytical procedure when analytical methods are transferred from one laboratory to another or when major pieces of equipment instruments change. 

Instruments Changes in benefits, benefit conditionality and enabling schemes... 

In these experiments oxidation of ethanol with a gas phase concentration of 200 ppm was studied. Figure 2 shows the light-ofF temperatures (temperature at which 50% conversion of the compound in question occurs) for ethanol oxidation over eight supported platinum and palladiiun catalysts as measured with a continuous flame ionization detector. Depending on by-product formation the signal from the instrument changes. The sensitivity for ethanol is for example about twice as high as for acetaldehyde. A marked difference can be observed for the activities of the different supported Pt catalysts. 

Combining Eqs. (26) and (27) and substituting the phase angle, H, corrected for instrument changes, as outlined below, then results in... 

CRMs should, in principle, be systematically used if important modifications are brought to a routinely applied method (e.g., instrument change, new analyst, new batch of consumables, etc.). Finally, the use of CRMs may be required by customers, e.g., when analytical data have to be used as a decision-making tool in the framework of regulations. 

Figure 12. Calibration curve using longer time intervals and an I/Io ratio to correct for instrument changes showing much improved sensitivity.

Depending on the frequency range and on the quality of instrumentation, systematic deviations in the gain and phase shift within the range of measurement may be induced to the data. These instrumental changes can be compensated by measuring lock-in signals 5 P(ct)i) and for a sample which does not... 

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