Page B-8 PW1660/00 Operation Manu: 880830 B.4 METAL POWDER SAMPLES Metal powder samples are made from drillings, filings, shavings and so on, that have been obtained from large pieces of metal. The following methods are generally used: 1. Analysis of loose drilings or filings stuck to adhesive tape (not a commonly used method) 2) It should be noted that in case samples are measured upside down as in most sequential x-ray spectrometers, particles may detach themselves from the tape and fall on the x-ray tube. In this case, this method is certainly not recommended 2. Pelletizing. a) Very frequently, it is possible to pelletize shavings of softer metals such as aluminium and its alloys, lead and tin alloys and solders. In general, quite high pelletizing pressures of up to 100 tons pressure are required. The ensuing pellet is then ready to be put into the spectrometer. 3. Acid solution technique. 2) Usually itis easier to get metals into solution than powders. The same advantages and disadvan- tages apply as mentioned under "Liquid solution technique” 4, Remelting a) Metal shavings can be remelted or cast and the resulting casting treated as a solid sample. Usually either a vacuum or a protective atmosphere type furnace is needed and melting can be done with electrical arc or by RF heating, for instance: Philips PV8920 Sample Preparation Fur- nace. B.5 SOLID METAL SAMPLES This preparation procedure can be divided into two parts: 1. Preparation of samples taken from the melt: ‘The hot metal will have to be cast in either a normal mould or a water cooled one for chillcasting. The sample is then cut in to pieces and the surface is finished. Surface finishing can be carried out on a lathe, a circular sander or a belt sander. Sometimes polishing with diamond paste is necessary after this. Care should be taken to ensure that no smearing takes place when treating the sample surface. The preparation of the sample should not introduce any contamination caused by the grinding agent, lubrication, finger marks and so on. The storage of the sample before measurement should not cause it to be contaminated with moisture, hydrogen sulphide, sulphur dioxide and so on. Spinning the specimen will even out irregularities due to surface finish and slight inhomogeneities. 2. Preparation of samples from round or square stock, ingots, sheets and so on: Usually these samples will have to be brought to the correct size for the spectrometer. The surface treatment is then identical to that described above. It should be noted that if the specimen is a magnetic material there will be interference with the electron beam from the x-ray tube and some inaccuracy of the measurement will result if the mag- netic properties of the unknown specimens differ from the calibration standards.