Instrumental parameters file

We should emphasize that sometimes, not all profile parameters should or could be routinely refined due to the quality of a particular pattern and/or sample crystallinity. For example, U, V, and Wparameters, which define the instrumental part of the FWHM as a function of Bragg angle, can be kept fixed assuming that their values in the instrumental parameters file were... 

Default profile parameters from the instrumental parameter file Scintag.prm as described above in section 7.6. 

For problems 4-9 use instrumental parameters file Scintag.prm located on the CD. 

Direct instrument control (or the lack of it) was an important issue for the earlier version of CDS. The scheme of connecting the detector channels through A/Ds to CDS worked well in analytical laboratories across the pharmaceutical industry. The scheme provided enough flexibility so that the CDS could collect data from a variety of instruments, including GC, HPLC, IC, SFC, and CE. It was equally important that the CDS could be connected to instruments that were manufactured by different vendors. It was not uncommon to find a variety of instruments from different vendors in a global pharmaceutical research company. The disadvantage of this scheme was that the instrument metadata could not be linked to the result file of each sample analyzed. It could not be guaranteed that the proper instrument parameters were used in sample analysis. Another need came from the increased use of... 

To verify the properties of the various acquisition modes call up the files in the folder ACQUIS. These are Raman spectra and interferograms of cyclohexane recorded with different acquisition versions. Find out for yourself which instrumental parameters have been used to record the spectra. Which spectra exhibit artifacts ... 

LC-MS/MS instrument parameters are shown in Table 2. Compound-specific parameters are shown in Table 3. The gradient used for chromatographic separation is shown in Table 4, and the flow rate through the column is 0.6 mL/min (see Note 5). The total run time for the method is 5.2 min. The acquisition file is divided into separate functions in which the number ofSRM transitions monitored is minimized. This provides enhanced sensitivity since the mass spectrometer does not scan the SRM transitions for every compound during the entire run. One isotopically labeled compound is chosen as internal standard for every function (see Note 6). 

Figure 3. The XSophe (v 1.1.4) main Window. The interface allows creation and execution of multiple input files on local or remote hosts. There are macro task buttons to guide the novice through the various menus and two button bars to allow easy access to the menus. For example, the bottom bar (left to right), Experimental Parameters, Spin System, Spin Hamiltonian, Instrumental Parameters, Single Crystal Settings, Lineshape Parameters, Transition Labels/Probabilities, File Parameters, Sophe Grid Parameters, Optimisation Parameters, Execution Parameters and Batch Parameters.

Instruments are controlled by information contained 1n the experimental setup file. For each type of instrument (shear history simulator, rotational viscometer, reciprocating capillary viscometer), the hardware 1s controlled so that the parameters of shear rate, temperature and time comply with the desired test conditions. This involves controlling devices such as pumps, bath heaters, valves and variable-speed motors. The setup and control parameters are recorded in the experiment file along with the resulting measured data. If necessary, the experiment can easily be repeated. 

Before initiating an analysis, the instrument must be programmed for automatic operation and the samples placed in the appropriate positions of the injector. Dialog 16, shown in Figure 2, starts operation of the microcomputer. Intelink communication with the instrument is established and the parameters for the first sample are taken from the sample definition file on the minicomputer and are transmitted to the microcomputer. The microcomputer turns on a ready status light at the instrument to signal to the operator to begin automatic operation of the instrument. 

Values for system peak parameters were found using a narrow distribution polystyrene standard (PS68K) before calculating MWD data for the lignin samples from universal calibration. To check software and instrument operation, several narrow MWD polystyrene and one broad MWD polymethylmethacrylate standards were treated as unknown samples and subjected to analysis with the universal calibration curve assembled from all polymer standards files. It was found that the MWD could be estimated for the recalculated polymer standards with errors between 5 and 10% of the original value indicated by the supplier of the standard (e.g., Mw for PS11K and Mw and M for PMMA17K-6). 

A fundamental objective of a computer system applied to automate a pharmaceutical GMP operation is to ensure the quality attributes of the drug product are upheld throughout the manufacturing process. It is therefore important that quality-critical parameters are determined and approved early in the validation life cycle. The exercise should be undertaken to a written procedure with base information from the master product/production record file examined and quality-critical parameter values and limits documented and approved for the process and its operation. In addition, the process and instrument diagrams (P IDs) should be reviewed to confirm the measurement and control components that have a direct impact on the quality-critical parameters and data. This exercise should be carried out by an assessment team made up of user representatives with detailed knowledge of both the computer system application and process, and with responsibility for product quality, system operational use, maintenance, and project implementation. This exercise may be conducted as part of an initial hazard and operability study (HAZOP) and needs to confirm the quality-related critical parameters for use in (or referenced by) the computer control system URS. 

In contrast, there are just two such files used within the Analyst data acquisition method (DAM) and instrument file format (INS) files. The mapping of the MassChrom and Analyst files is not one to one parameters in the experiment file are split between the INS and DAM files on the Analyst application. 

The frequency of OQ/performance verification depends not only on file type of instrument and tlie stability of tlie performance parameters, but also on file acceptance criteria specified. In general, tlie time intervals should be selected such tliat file probability is high tliat all parameters are still wifiiin file operational specifications. Ofiierwise, analytical results obtained witli tliat particular instrument are questionable. The OQ/perfonnance verification history of file type of instrument can be used to set reasonable test intervals. Here file importance of proper selection of tlie procedures and acceptance limits becomes very apparent. 

---