Instructions for Philips PW1830.pdf

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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!
Page 1: Instructions for use of Philips PW1
Page 5 and 6: STEP 5: WHEN THE SCAN IS FINISHED 1

Instructions for Philips PW1830.pdf

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