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1、 Reference number ISO 11877:2008(E) ISO 2008 INTERNATIONAL STANDARD ISO 11877 First edition 2008-06-01 Hardmetals Determination of silicon in cobalt metal powders Photometric method Mtaux durs Dosage du silicium dans les poudres mtalliques de cobalt Mthode photomtrique Copyright International Organi
2、zation for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/24/2008 22:50:15 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11877:2008(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance w
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5、ery care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2008 All rights reserved. Unless otherwise specif
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7、e postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2008 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 N
8、ot for Resale, 07/24/2008 22:50:15 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11877:2008(E) ISO 2008 All rights reserved iii Contents Page Foreword iv 1 Scope 1 2 Principle1 3 Reagents.1 4 Apparatus and equipment 2 5 Preparation of acid mixture for sample treatment
9、 .2 6 Preparation of solutions for receiver.2 7 Procedure .2 8 Photometric determination.3 9 Preparation of blank and calibration solutions 3 10 Expression of the result3 11 Test report3 Bibliography4 Copyright International Organization for Standardization Provided by IHS under license with ISO Lic
10、ensee=Boeing Co/5910770001 Not for Resale, 07/24/2008 22:50:15 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11877:2008(E) iv ISO 2008 All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards
11、 bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organiza
12、tions, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in t
13、he ISO/IEC 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
14、 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. ISO 11877 was prepared by Technical Committee ISO/TC 119, Powder m
15、etallurgy, Subcommittee SC 4, Sampling and testing methods for hardmetals. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/24/2008 22:50:15 MDTNo reproduction or networking permitted without license from
16、 IHS -,-,- INTERNATIONAL STANDARD ISO 11877:2008(E) ISO 2008 All rights reserved 1 Hardmetals Determination of silicon in cobalt metal powders Photometric method 1 Scope This International Standard specifies a photometric method to be used for the determination of the mass fraction of silicon in the
17、 range of 20 g/g to 300 g/g in cobalt metal powders. 2 Principle After treatment of the sample with a mixture of acids, the so-formed silicon tetrafluoride is distilled into a mixture of boric acid and sodium molybdate. The obtained molybdatesilicate complex is extracted with methyl- isobutylketone
18、and the absorbance of the solution is measured. 3 Reagents Reagents of the highest purity and only double-distilled water or water of equivalent purity shall be used. 3.1 Hydrofluoric acid, 40 % by mass. 3.2 Nitric acid, 65 % by mass. 3.3 Hydrochloric acid, 30 % by mass. 3.4 Sulfuric acid, 96 % by m
19、ass. 3.5 Perchloric acid , 70 % by mass. 3.6 Sodium hydroxide solution, 30 % by mass. 3.7 Boric acid. 3.8 Sodium molybdate. 3.9 Amidosulfuric acid. 3.10 Methyl-isobutylketone. 3.11 Acetone. 3.12 Water. 3.13 Nitrogen. 3.14 Silicon standard solution, 100 g/ml. Copyright International Organization for
20、Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/24/2008 22:50:15 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11877:2008(E) 2 ISO 2008 All rights reserved 4 Apparatus and equipment All apparatus and equipment in
21、 contact with reagents shall be made of silicon-free material like PTFE (polytetrafluoroethylene), PP (polypropylene), PE (polyethylene) and TPX (methylpenten-polymer). 4.1 Apparatus for acid treatment and distillation, for separation of silicon tetrafluoride. 4.2 Test-tube shaker. 4.3 Refrigerator.
22、 4.4 Platinum thimbles, for weighing the sample. 4.5 Graduated flasks, stock bottles and pipettes. 5 Preparation of acid mixture for sample treatment Mix 30 ml of hydrofluoric acid, 20 ml of nitric acid, 20 ml of perchloric acid and 30 ml of water in a PTFE flask. 6 Preparation of solutions for rece
23、iver 6.1 Solution I Dissolve 37,2 g of boric acid and 14,4 g of sodium molybdate in water in a graduated PP flask and fill up to 1 000 ml with water. 6.2 Solution II Dissolve 19,4 g of amidosulforic acid in a graduated PP flask and fill up to 100 ml with water. 7 Procedure 7.1 Pour 30 ml of solution
24、 I and 1 ml of solution II into a graduated 100 ml flask. 7.2 Pour 3 ml of the acid mixture into the distilling flask, and add 100 mg of the sample weighed to a platinum thimble. 7.3 Connect the receiver and distilling flask and start the nitrogen flow. 7.4 Heat the apparatus to 170 10 C, within app
25、roximately 25 min, and keep it at this temperature for 50 min. Control the purge gas during distillation. 7.5 When the distillation time is over, remove the receiver flask and rinse the inlet tube with water. 7.6 Adjust the pH of the receiver solution to 1,3 to 1,4 with sodium hydroxide (approximate
26、ly 800 l to 1 000 l) and leave it for 1 h. 7.7 Add 2,0 ml of hydrochloric acid and 20 ml of methyl-isobutylketone and shake for 1 min. Fill to the stopcock with water and close the flask. Keep the flask at + 5 C for 1 h. Copyright International Organization for Standardization Provided by IHS under
27、license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/24/2008 22:50:15 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11877:2008(E) ISO 2008 All rights reserved 3 8 Photometric determination Transfer the methyl-isobutylketone phase to an appropriate photome
28、ter and measure against methyl- isobutylketone. Use a wavelength of 345 m. 9 Preparation of blank and calibration solutions 9.1 Blank solution Determine the absorbance of a solution containing all the reagents except the sample material. 9.2 Calibration solution Treat a silicon standard sample as ou
29、tlined in 9.1 and prepare at least three solutions containing silicon in the range of the sample for a calibration curve. 10 Expression of the result 10.1 Calculation After calculating E = EX EB (where E is the extinction, EX is the experimentally measured extinction and EB is the blind value of the
30、 extinction), the mass fraction of silicon w is evaluated graphically or arithmetically using the calibration curve, taking into account the sample mass. 10.2 Final result Report the arithmetical mean of the acceptable determination rounded to 0,001 % by mass. 11 Test report The test report shall in
31、clude 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; d) all operations not specified in this International Standard, or regarded as optional; e) details of any occurrence which ma
32、y have affected the result. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/24/2008 22:50:15 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11877:2008(E) 4 ISO 2008 All rig
33、hts reserved Bibliography 1 ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions 2 ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and r
34、eproducibility of a standard measurement method 3 ISO 5725-3, Accuracy (trueness and precision) of measurement methods and results Part 3: Intermediate measures of the precision of a standard measurement method 4 ISO 5725-4, Accuracy (trueness and precision) of measurement methods and results Part 4
35、: Basic methods for the determination of the trueness of a standard measurement method 5 ISO 5725-5, Accuracy (trueness and precision) of measurement methods and results Part 5: Alternative methods for the determination of the precision of a standard measurement method 6 ISO 5725-6, Accuracy (truene
36、ss and precision) of measurement methods and results Part 6: Use in practice of accuracy values Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/24/2008 22:50:15 MDTNo reproduction or networking permitted
37、 without license from IHS -,-,- Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/24/2008 22:50:15 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11877:2008(E) ICS 77.160 Price based on 4 pages ISO 2008 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Boeing Co/5910770001 Not for Resale, 07/24/2008 22:50:15 MDTNo reproduction or networking permitted without license from IHS -,-,-