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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. 

Содержание PC-APD PW-1710

Страница 1: ... 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 ...

Страница 2: ...ollection settings example V 40 kV I 35 mA Be careful not exceed 45 kV and 40 mA 8 Mount your sample in a suitable X ray specimen holder I suggest our Plexiglas holders or glass slides Double stick tape or Vaseline can be used to attach powder specimens Clean silly putty can be used for bulk specimens If using aluminum sample holders make sure you are using the holders with the larger openings oth...

Страница 3: ...reen should now display the current computer setup including which ports are in use and the directories where data will be stored It will appear something like Figure D IF YOU ENCOUNTER ANY PROBLEMS PLEASE CONSULT DR WEAVER 16 Press the escape key Esc to return to the SYSTEM PREPARATION menu 17 Choose DIFFRACTOMETER PARAMETERS D 18 The model number for the electronics will appear in the lower righ...

Страница 4: ...tify programs if necessary 30 Enter the sample identification and a filename where the data will be stored in the appropriate fields 31 Check for the following Sample should be on the stage Instrument door should be closed Power should be set to desired levels Shutter should be open See instructions for turning on generator if it is not on or at the proper power 32 Push F1 to start the measurement...

Страница 5: ...ware Data directory C APD DATA Temporary files C APD TMP Graphics Adapter VGA Graphics hard copy device PRINTER Monitor COLOUR Number of pens Serial port Used for Baudrate Databits Stopbits Parity Addr Check 1 MOUSE 2 DIFFRACTOMETER 4800 3 NOT PRESENT 4 NOT PRESENT Esc Last menu F5 Show names F10 Help FIGURE D Schematic of SYSTEM PARAMETERS menu ...

Страница 6: ...grammable generator PW1825 NO Generator tension kV 45 Generator current mA 40 Divergence slit 1 12 Separate θ drive NO Receiving Slit mm 0 2 Monochromator YES Lower level 30 Upper level 80 Maximum 2θ 120 000 Temperature control unit NONE Esc Last menu F1 Save current settings F10 Help FIGURE 2 Schematic of SYSTEM PARAMETERS menu ...

Страница 7: ...ram CONTINUOUS Step size 2θ 0 020 Start Angle 2θ 10 000 Maximum d value Å 8 83820 End Angle 2θ 70 000 Minimum d value Å 1 34298 Scan time h m s 0 50 00 Number of steps 3000 Time per step s 1 000 Scan speed 2θ s 0 020 Automatic analysis NO Esc Last menu F9 Print Program F10 Help FIGURE 3 ...

Страница 8: ...se then S twice and verify that the data directory listed is the one where the data is stored If this is not the case enter the appropriate directory 4 In the lower right portion of the screen there is a parameter titled weights and levers this should be set to 3 use the or key 5 Press F1 to start the alpha 2 stripping A file with the same name as the raw data file but with an A2 extension has now...

Страница 9: ...o automatic slit intensities NO Esc Menu F1 Start F5 Show Names F10 Help FIGURE 1 13 Adjust the parameters in the peak search that apply to problem with peak search For example If there were too many peaks present make the minimum peak tip width larger or if there were too few peaks make it smaller If less intense peaks are not being detected make the minimum significance lower 14 After making the...

Страница 10: ...lete a peak use the F1 and F2 keys to page through the listing of peaks Then use the arrow keys to highlight the 2 theta value of the peak to be deleted Press F3 to delete the peak To move a peak highlight it in the list and choose F8 for graphics mode Position the cursor on the peak tip and select F1 to accept the new position 20 Press ESC twice to return to the main menu 21 Exit PC APD and X MEN...

Страница 11: ... will be brought to the PC Identify main window Figure 3 Figure 3 PC Identify main window 24 Choose IDENTIFY I and press F1 or ENTER You will be prompted with a highlighted entry box as indicated in Figure 4 ...

Страница 12: ...appropriate data directory and press ENTER 26 Enter the name of the desired DI file or press F5 to select from a list of available DI files 27 Press F1 to continue with analysis You will be prompted with the following screen ...

Страница 13: ...eneral 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 Refer to the PC IDENTIFY Users Manual for more details 29 Press F1 to start the analysis 30 The entire ICDD JCPDS database will now be searched This will take a minute Afterwards you will be prompted with a screen similar to the Figure 6 ...

Страница 14: ...Figure 6 31 Press F8 to go to graphics mode You will be prompted with a screen similar to Figure 7 Figure 7 ...

Страница 15: ...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 ...

Страница 16: ...T 5 MINUTES 2 Lower the voltage to 10 kV i e lowest kV 3 Turn off the X ray generator by pressing the STOP button Turn off the power by pressing the OFF button 4 Feel the top of the x ray tube when it is cool the water chiller may be turned off 5 Data analysis and manipulation may be performed now if desired Otherwise exit the software by pressing Esc until the main menu is reached Then press X to...

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