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LABORATORY MANUAL AND INSTRUCTIONS
Version 1.3
Metallurgical & Materials Engineering
Dr. M.L. Weaver
W.S. Rollings
September 6, 2000
This manual describes operation of the Philips PW-1710 X-ray generator using PC-APD,
techniques for data collection and analysis, and for instrument shutdown. All users should refer
to the proper manuals for detailed information.
IMPORTANT!
DO NOT STORE YOUR DATA ON THE C: OR D: DRIVE OF THE COMPUTER. THE
HARD DRIVE WILL BE PURGED WEEKLY. STORE YOUR DATA ON YOUR OWN
FLOPPY DISK.
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Summary of Contents for Philips PC-APD PW-1710
- Page 1 Dr. M.L. Weaver W.S. Rollings September 6, 2000 This manual describes operation of the Philips PW-1710 X-ray generator using PC-APD, techniques for data collection and analysis, and for instrument shutdown. All users should refer to the proper manuals for detailed information.
- Page 2 INSTRUCTIONS FOR PHILIPS X-RAY GENERATOR TURNING ON THE X-RAY GENERATOR 1) SIGN THE LOG SHEET! 2) Turn on the water chiller and wait 1 minute. The water pressure should be ≥ 40 psi. 3) On the x-ray generator, set the voltage and current to the lowest available setting (i.e., turn the kV and mA knobs all of the way to the left).
- Page 3 11) The instrument is now ready to collect data. Setup your data collection program in PC-APD and run it. SEE THE NOTES FOR PC-APD ON THE ACCOMPANYING PAGES. 12) Turn on the computer. In the Windows 3.1 environment, open the Philips folder and double click the “XMENU” icon.
- Page 4 25) Alter the field to collect a standard powder measurement. See Figure 3. 26) Press [Esc] twice to return to the main APD menu. 27) Choose DATA COLLECTION (D). 28) Choose IDENTIFY MEASUREMENT (I). 29) Enter the name of the identify program that was just created. Press [Enter]. Press F5 to see a list of available identify programs if necessary.
- Page 5 S Y S T E M P A R A M E T E R S Licensee: Some Laboratory Tuscaloosa, AL Identification: Philips Analytical PC-APB, Diffraction software Data directory: C:\APD\DATA Temporary files: C:\APD\TMP Graphics Adapter: VGA Monitor: COLOUR Serial port...
- Page 6 PARAMETERS FOR PW3710 BASED DIFFRACTOMETER Programmable generator (PW1825): NO Generator current [mA]: Temperature control unit: Esc=Last menu F1=Save current settings F10=Help FIGURE 2. Schematic of SYSTEM PARAMETERS menu. Sample Changer: NO Spinner: NO Tube Anode: Cu Focus: NF (Normal Focus) Generator tension [kV]: Divergence slit: 1/12°...
- Page 7 I D E N T I F Y : S C A N P A R A M E T E R S New program: Type of Program: Step size [°2θ]: Start Angle [°2θ]: End Angle [°2θ]: Scan time [h:m:s]: Number of steps: Time per step [s]: Scan speed [°2θ/s]:...
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Page 8: Analyzing Data
The following procedures explain the use of the APD and IDENTIFY software to analyze collected data. Patterns must be treated using the APD software prior to identification using the IDENTIFY sofware. Choose APD from X-MENU and from the main menu select PATTERN TREATMENT (P). - Page 9 P E A K S E A R C H Input file: Create background file: Create peak data file: Creeate smoothed data file: Create second derivative file: Start angle [°2θ]: End angle [°2θ]: Minimum peak tip width [°2θ]: Maximum peak tip width [°2θ]: Peak base width [°2θ]: Minimum significance: Converty fixed slit intensities...
- Page 10 Enter the name of the DI file (this file was created when the peak search was performed and has the same name as the raw data file but a DI extension) to be edited. Press F1 to edit the lines. Peaks can be added, deleted or moved.
- Page 11 You will be brought to the PC-Identify main window (Figure 3). Choose IDENTIFY (I) and press F1 or ENTER. highlighted entry box as indicated in Figure 4. Figure 3. PC-Identify main window. You will be prompted with a...
- Page 12 Select the appropriate data directory and press ENTER. Enter the name of the desired DI file or press F5 to select from a list of available DI files. Press F1 to continue with analysis. screen: Figure 4 You will be prompted with the following...
- Page 13 Use the ‘+’ or ‘-‘ keys to toggle the parameters setting to ‘Normal’, ‘Precise’ or ‘User defined’ depending upon the type of analysis that you want to do. A ‘Normal’ setting is appropriate for general analysis. The ‘User defined’ option can be used to limit the scope of your search to select ICDD cards or to compounds containing selected elements.
- Page 14 Press F8 to go to graphics mode. You will be prompted with a screen similar to Figure 7. Figure 6 Figure 7...
- Page 15 The list of patterns can now be compared to both the DI file and the raw data file. Pressing the ‘+’ and ‘-‘ keys steps through the list of candidates and pressing F4 and F3 insert and delete the reference patterns from the raw data field.
- Page 16 TURNING OFF THE X-RAY GENERATOR 1. Close the shutter by turning the appropriate knob on the Shutter Control Box (Figure C) to off. Lower the current to the lowest mA by turning the mA knob all of the way to the left. Reduce the voltage to 25 kV.