Phase identification software

Table 17.3 Available search-match and phase identification software.

XRD Characterization The powder x-ray diffraction of the mechano-chemically milled complex borohydride has been carried out by the Philips X pert diffractometer with Cu-Koi radiation of X= 5.4060 A. The incident and diffraction slit width used for the measurements are 1° and 2° respectively. The sample holder was covered with Polyethylene tape (foil) with an O-ring seal in an N2 filled glove box in order to avoid or at least minimize the 02/moisture pickup during the XRD measurements. The diffraction from the tape was calibrated without the actual sample and found to be occurring at 29 angles of 22° and 24°, respectively. The XRD phase identification and particle size calculation has been carried out using PANalytical X pert Highscore software, version l.Of. 

Sample preparation for XRD is rapid and data is acquired by a computer which also controls the sample changer. A typical acquisition time would be a few hours. For routine operations, such as determining zeolite lattice parameters, it is also possible to process data automatically. Phase identification, aided by a JCPDS database search software, takes a few tens of minutes. 

Most powder diffraction databases only serve angular dispersive X-ray diffraction. Energy dispersive X-ray diffraction data can be transformed into an angular dispersive equivalent that can then be used in conventional search-match software. Users of neutron diffraction data are currently limited to performing phase identification using a list of crystal structures imported into a Rietveld program. It is wise to first run samples destined for neutron diffraction sample in a powder XRD prior to confirm phase purity, and to use calculated patterns to assist in phase identification of possible undesired phases due to ancillary equipment or sample environment. 

X-ray diffraction (XRD) data of the metal product was collected using a Philips PW 1050 fitted with a Philips X PERT powder XRD system which employed a copper target. Phase identification was made using the X Pert High Score Plus software. 

Phase identification and Rietveld QPA were carried out using the X Pert High Score Plus v3.0e software package by PANalytical alternatively the Topas Academic v4.1 software was used to cross-check the quantification results. When similar refinement strategies were followed, the results of both software packages were found to be very similar. 

The major impetus for the development of solid phase synthesis centers around applications in combinatorial chemistry. The notion that new drug leads and catalysts can be discovered in a high tiuoughput fashion has been demonstrated many times over as is evidenced from the number of publications that have arisen (see references at the end of this chapter). A number of )proaches to combinatorial chemistry exist. These include the split-mix method, serial techniques and parallel methods to generate libraries of compounds. The advances in combinatorial chemistry are also accompani by sophisticated methods in deconvolution and identification of compounds from libraries. In a number of cases, innovative hardware and software has been developed tor these purposes. 

Different capillary columns are available for organic acid separation and analysis. In our laboratory, the gas chromatography column in all GC-MS applications is crosslinked 5% phenyl (poly)methyl silicone, 25 m internal diameter 0.20 mm stationary phase film thickness 0.33 pm (Agilent HP-5, DB-5, or equivalent). Several instrument configurations are commercially available, which allow for positive identification of compounds by their mass spectra obtained in the electron impact ionization mode. A commercially available bench-top GC-MS system with autosampler (Agilent 6890/5973, or equivalent) is suitable. Software for data analysis is available and recommended. The use of a computer library of mass spectra for comparison and visualization of the printed spectra is required for definitive identification and interpretation of each patient specimen. 

Prototyping FDA (1995) An approach to accelerate the software development process by facilitating the identification of required functionality during analysis and design phases. A limitation of this technique is the identification of system and software problems and hazards. [Adapted.]... 

The methods for each study are divided into the initial protein separation step, a second separation step if applicable, the type of mass analysis, and the software used for peptide identification. ID = one dimensional polyacrylamide gel electrophoresis, 2D = two dimensional polyacrylamide gel electrophoresis, MS = mass spectrometry (peptide mass fingerprinting), MS/MS = tandem mass spectrometry, MALDI-TOF = matrix assisted laser desorption/ionization-time of flight, MS FIT = software from Protein Prospector, http //prospector.ucsf edu/, ESI = electrospray ionization, Q-TOF = quadrupole-time of flight, PPSS2 =Protana s Proteomic Software Suite (ProtanaEngineering, Odense, Denmark), Mascot = Matiix Science, http //www.matrixscience.com/, TOF-TOF = MALDI plus TOF tandem mass spectrometry, RP-HPLC = reverse phase high performance liquid chromatography, Q-IT = quadrupole ion trap, LIT = linear ion trap. Bioworks = Thermo Electron Corporation. 

A methods file is created for each analysis to specify the standard conditions to be used such as autosampler sequence, use of blanks and QA samples, column temperature programme, mobile phase composition and flow-rate, split ratios, mass range to be scanned, scan rate and sample identification codes. A methods menu leads the analyst through the full set-up sequence. Methods are filed for future reference and for use in routine analysis. The software can be linked to other standard packages such as word processors so the methods data can be linked to the results file and then transferred to the analytical report. 

There are two general approaches for computer-aided identification of infrared spectra of unknown compounds [173,196-199,248-250]. The most common approach uses software designed to identify an unknown spectrum by its similarity to a limited number of reference spectra selected from a general or customized library of reference spectra measured under similar conditions (e.g. vapor phase, solid phase, etc.) Commercial... 

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