ISO INTERNATIONAL STANDARD 17352 Second edition 2008-06-01 HardmetalsDeterminationof siliconin cobalt metal powders using graphite. furnace atomic absorption Dosagedusiliciumdanslespoudresmétalliquesde Metauxdurs cobalt parabsorptionatomiqueafourgraphite Reference number ISO17352:2008(E) ii Contents Page Foreword. 1 Scope 2 Principle... 3 Reagents. 4 Apparatus. 5 Procedure 6 Calibration 7 Calculation. 8 Precision 9 Test report Bibliography ili Foreword IsO (the International Organization for Standardization) is a worldwide federation of national standards bodies technical committees. Each member body interested in a subject for which a technical committee has been International Electrotechnical Commission (IEC)on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/lEC Directives, Part 2 The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. IsO shall not be held responsible for identifying any or all such patent rights. ISO17352was prepared by Technical CommitteeISO/TC119,Powdermetallurgy,Subcommittee SC 4 Samplingandtesting methodsforhardmetals. iv HardmetalsDeterminationofsiliconincobaltmetalpowders using graphite-furnace atomic absorption 1 Scope This International Standard specifies a test method, using graphite-furnace atomic absorption, to determine the mass fraction of silicon in cobalt metal powder with varying compositions within the range of 5 μg/g to 40 μg/g. 2 Principle This test method for the chemical analysis of cobalt metal powder is to be used to determine traces of silicon. It is assumed that all those who use this test method will be trained analysts capable of performing common laboratory procedures skilfully and safely. It is expected that all the work will be performed in a properly equipped laboratory. 3 Reagents Reagents of the highest purity and only double-distilled water or their equivalents shall be used 3.1 Nitric acid, p = 1,4 g/ml. 3.2 Hydrochloric acid, p = 1,15 g/ml. 3.3 Cobalt powder, purity> 99,9 %by mass. 3.4 Si solution, 1,oo0 g/l. 1 4 Apparatus 4.1 Graphite-furnaceatomicabsorptionspectrometer Follow the manufacturer's instruction manual for installation and operation, 4.2 Additional information The following parameters are for information purposes only and have to be adapted to the special requirements of everylaboratory. Lamp: hollow cathode lamp for Si Tube: coated pyrolytic C-tube without a platform Wavelength: 251,6 nm Slit: 0,2 nm Injection volume: 20 μl Temperature program: drying-120℃ ashing—1200°C atomising—2 700 °C conditioning—2750C 5 Procedure 5.1Test portion Weigh, to the nearest 0,001 g, approximately 0,5 g of the test sample and transfer it to a 100 ml polypropylene flask. 5.2 Dissolutionofthetestportion The test sample is dissolved in 10 ml of nitric acid and 2 ml of hydrochloric acid. When the sample is completely dissolved, allow the flask to cool and then fill up to 1oo ml with double-distilled water. Calibration 6 0,500 g of ultrapure cobalt powder is dissolved in the same way as the test sample (see 5.2). The resulting Calculation Compensate for the actual weight of the sample analysed. 8Precision No definite statement on the precision and bias can be made at this time. These values shall be calculated using the results of a round-robin analysis. 2 Test report 9 The test report shall include the following information: a) a reference to this International Standard; b) all details necessary for identification of the test sample; C) the test results obtained; (p all operations not specified in this International Standard, or regarded