Data collection with integrity

Room-temperature fluorescence (RTF) has been used to determine the emission characteristics of a wide variety of materials relative to the wavelengths of selected Fraunhofer lines in support of the Fraunhofer luminescence detector remote-sensing instrument. RTF techniques are now used in the compilation of excitation-emission-matrix (EEM) fluorescence "signatures" of materials. The spectral data are collected with a Perkin-Elraer MPF-44B Fluorescence Spectrometer interfaced to an Apple 11+ personal computer. EEM fluorescence data can be displayed as 3-D perspective plots, contour plots, or "color-contour" images. The integrated intensity for selected Fraunhofer lines can also be directly extracted from the EEM data rather than being collected with a separate procedure. Fluorescence, chemical, and mineralogical data will be statistically analyzed to determine the probable physical and/or chemical causes of the fluorescence. 

Training of the data collectors is an important step in ensuring reliable data collection. Trainees will have different levels of computer competency but all must be comfortably competent with the system before data collection can start. Entry of practice data for each form is recommended during training. Strict guidelines for the use of the trial computer hardware and software must be established at the outset to ensure system integrity. Table 25.2 illustrates a list of these guidelines. 

Sample preparation, injection, calibration, and data collection, must be automated for process analysis. Methods used for flow injection analysis (FLA) are also useful for reliable sampling for process LC systems.1 Dynamic dilution is a technique that is used extensively in FIA.13 In this technique, sample from a loop or slot of a valve is diluted as it is transferred to a HPLC injection valve for analysis. As the diluted sample plug passes through the HPLC valve it is switched and the sample is injected onto the HPLC column for separation. The sample transfer time typically is determined with a refractive index detector and valve switching, which can be controlled by an integrator or computer. The transfer time is very reproducible. Calibration is typically done by external standardization using normalization by response factor. Internal standardization has also been used. To detect upsets or for process optimization, absolute numbers are not always needed. An alternative to... 

All measured values are normally registered by means of a recorder. In addition, an improved method for data collection and processing is possible today by use of a computer. This has the advantage of automatic, safer data collection in an easy-to-read form. Comparison with standard values, correction of the buoyancy effects, control of linearity, control of standard deviations and peak integrations are thus possible. 

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