Instructions for Philips PW1830.pdf

Instructions for use of Philips PW1830 X-ray Diffractometer
Table of Contents
STEP 1: ARRIVING AT THE MACHINE .................................................................................. 2
STEP 2: PREPARING THE EQUIPMENT FOR USE ............................................................... 2
STEP 3: SAMPLE PREPARATION ............................................................................................. 3
STEP 4: DIFFRACTOMETER USAGE ........................................................................................ 3
STEP 5: WHEN THE SCAN IS FINISHED ................................................................................ 5
TURNING OFF THE MACHINE ................................................................................................... 5
TROUBLESHOOTING ..................................................................................................................... 6
ALL USERS OF X-RAY EQUIPMENT MUST BE AUTHORISED BY THE X-RAY LAB MANAGER
AND REGISTERED AS A WORKER WITH IONISING RADIATIONS.
This system is protected by a series of safety interlocks – these must never be overridden. All users must fill
the instrument log book at the beginning of each experimental booking and remove all specimens from the
XRD SRF within 24 hrs.
These instructions can be downloaded from http://uspace.shef.ac.uk/community/xrdlab

STEP 1: ARRIVING AT THE MACHINE
Make sure the machine is on:
1. Are the power setting displays showing 40kV and 30mA? If so – the machine is on,
and most likely ready to use - proceed to Step 3!
2. If the kV and mA displays are blank, the machine is switched off. Check for any
notices that the machine is not working. If there are none, proceed to Step 2 to turn
the instrument on.
3. If the displays are reading 0kV and 0mA, check the LCD display next to the
‘Shutters’ button. If this is reading ‘Error 42’ there is a problem with the cooling
water supply – most likely the water filter needs changing!
STEP 2: PREPARING THE EQUIPMENT FOR USE
1. Make sure water supply on (anticlockwise).
- Check flow between 3.5 L/min and 6 L/min on flow rate meter mounted on the
rear of the diffractometer.
2. Make sure that the power is on at the isolator switch.
3. Press ‘POWER ON’.
- When switched ON, the generator will perform a SELF TEST; once completed the
message ‚TARGET 15kV 10mA‛ should appear on the LCD display.
4. Switch on HT by pushing ‘HT ON‘ button.
- The generator should go automatically to 15 kV and 10 mA.
5. If the shutter is open, press CLOSE SHUTTER, ‘4’ and then ENTER.
6. Turn the voltage (kV) and current (mA) up to the working values:
- Turn the ‘kV’ dial to 40.
- Turn the ‘kV’ dial to 30.
REMEMBER: THE mA SHOULD ALWAYS BE LOWER THAN THE kV!

STEP 3: SAMPLE PREPARATION
Note that ALL sample prep should be done in I6b, not in I6. All samples MUST be
labelled with your name! Unlabelled samples will be treated as hazardous waste and
disposed of immediately. When prepared, proceed to Step 4.
For powder samples:
1. Make sure your powder is well-ground.
2. Select the biggest Aluminium specimen tray that you can fully fill. The correct
holders have the aperture for powder towards the TOP of the holder.
3. Remove the back cover, and place on to a glass microscope slide. Completely fill
the aperture with powder. Use a microscope slide to ensure that the specimen
surface is level with the top of the holder. Replace the back cover, and carefully
turn over. Remove the glass slide very carefully to expose your specimen surface.
4. Label the specimen holder with your name using a marker pen.
For bulk samples:
1. Make sure your sample has at least one surface which is level and smooth.
2. Remove or add Apiezon putty to the brass specimen holder as necessary, and
mould the putty so that your sample can sit on top of a mound of putty.
3. Place the sample on to the putty and press down lightly to help it stick.
4. Turn the holder upside down; gently press down on both sides on to a flat surface.
The top of the sample MUST BE LEVEL with the top of the holder.
Key point #1: incorrect specimen height WILL result in specimen height displacement
errors in your data, e.g. if the sample is too high, your Bragg reflections will be shifted to
higher angles (and too low, peaks shifted to lower angles). This can make phase analysis
very difficult!
Key point #2: the Apiezon putty is partly crystalline, so will give peaks in your diffraction
pattern should it get in to the beam. Make sure your specimen is mounted on the putty,
and not embedded too deeply into it!

STEP 4: DIFFRACTOMETER USAGE
1. Make sure the computer is switched on.
2. Load sample in to the diffractometer. Old samples must be removed, tipped in to
aluminium foil, labelled with the date and name of whoever ran the sample, then
placed in to the used specimen box for collection.
3. Place chamber door onto goniometer.
4. Ensure that all shielding is correctly positioned and close doors.
5. Make sure the shutter is closed, then launch the ‘HBX’ software, if not running.
- Note: If you try to launch the HBX software, and it appears to already be running,
simply press Ctrl, Alt and Delete, and close the HBX software before trying again.
6. Set the scanning parameters:
(i) Starting angle, in degrees 2θ (> 3º).
(ii) Finish angle, in degrees 2θ (< 160º).
(iii) Step size, in degrees 2θ (> 0.01º; 0.02 is a good standard, though 0.05 is often
best for quick, good quality data for phase analyses. Use 0.01 for cell refinement).
(iv) Scan speed in degrees per minute (between 0.1 and 2 degrees/minute).
(v) Enter comment, if desired, for your own reference.
(vi) Enter sample name (8 or less characters, no ‘special’ characters).
(vii) Save your data in your folder on the hard drive by selecting ‘Options’/’Data
Path and Type’ and then selecting your data folder.
7. Press ‘Begin Scan’ on the PC.
8. When prompted, open the shutter by holding the SHUTTERS button, and then
pressing the ‘OPEN’ button for shutter 2.
Note: if the shutter fails to open, the most common cause is the enclosure door being poorly
fitted.
9. Use mini-monitor to check for any radiation leaks.
10. MAKE SURE THAT YOU FILL IN THE LOG BOOK.
The scan may be stopped at any time with ‘STOP+SAVE’ or ‘ABORT SCAN’.

STEP 5: WHEN THE SCAN IS FINISHED
1. Close the shutter: On the front of the diffractometer, press CLOSE SHUTTER,
enter ‘4’ and then press ENTER.
2. The data will be saved automatically to the hard drive. If you cannot find your
data, it is most likely operator error! Use of special characters (&, +, etc) will cause
data not to be saved – or perhaps the ‘Data Path and Type’ wasn’t selected
(correctly). Try using the ‘Search’ function in Windows to look for your file.
3. Remove sample.
NOTE: Used samples MUST be removed from the XRD Lab within 24 hours of being run!
TURNING OFF THE MACHINE
The diffractometers are normally in use around the clock, seven days a week. If for some
reason it is necessary to turn the machines off:
1. Lower mA then kV if not starting new scan immediately. To do this:
- Press ‘mA’ and enter 10, and press ‘ENTER’.
- Press ‘kV’ and enter 15, and press ‘ENTER’.
REMEMBER: THE mA SHOULD ALWAYS BE LOWER THAN THE kV!
2. Press ‘FUNCTION’, enter ‘2’ then press ‘ENTER’.
3. Press ‘STANDBY’.
The equipment is now on standby mode. To isolate the instrument completely:
1. Turn the isolator switch on the wall to ‘OFF’.
2. Turn the water off (clockwise).

TROUBLESHOOTING
The shutter will not open! Try putting the chamber door on again – the round button on
The ‘No waterflow’ light is
lit, and the machine
appears to be off.
The shutter is closing
automatically of its own
accord!
the side of the X-ray tube housing must be fully pressed in
before the instrument will recognise that it is safe to unleash
the X-rays.
If this button is fully in, check all the housing doors are fully
closed and all interlocks in contact.
There is also an interlock underneath the ‘top hat’
arrangement (just on the chamber side before the secondary
beam monochromator) – try pinching that closed.
Finally, if the problem still persists, it is likely that one or
both of the ‘Shutter Open’ bulbs has blown. Contact the Lab
Manager.
Last revised by N. Reeves-McLaren, 5 h January 2012.
Low water pressure. Report to the Lab Manager.
Probably someone has pressed the Shutter 2 ‘Clock’ button.
Press the ‘∞‘ button, and try again.