1、BRITISH STANDARDBS ISO 11877:2008Hardmetals Determination of silicon in cobalt metal powders Photometric methodICS 77.160g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g4
2、4g42g43g55g3g47g36g58BS ISO 11877:2008This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 July 2008 BSI 2008ISBN 978 0 580 56322 5National forewordThis British Standard is the UK implementation of ISO 11877:2008. The UK participation in its pr
3、eparation was entrusted to Technical Committee ISE/65, Sintered metal components.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its co
4、rrect application.Compliance with a British Standard cannot confer immunity from legal obligations.Amendments/corrigenda issued since publicationDate CommentsReference numberISO 11877:2008(E)INTERNATIONAL STANDARD ISO11877First edition2008-06-01Hardmetals Determination of silicon in cobalt metal pow
5、ders Photometric method Mtaux durs Dosage du silicium dans les poudres mtalliques de cobalt Mthode photomtrique BS ISO 11877:2008ii iiiContents Page Foreword iv 1 Scope 1 2 Principle1 3 Reagents.1 4 Apparatus and equipment 2 5 Preparation of acid mixture for sample treatment .2 6 Preparation of solu
6、tions 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 report 3 Bibliography 4 BS ISO 11877:2008iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of nation
7、al standards 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. Internatio
8、nal organizations, 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 rule
9、s given in the 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 l
10、east 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. ISO 11877 was prepared by Technical Committee ISO/TC 1
11、19, Powder metallurgy, Subcommittee SC 4, Sampling and testing methods for hardmetals. BS ISO 11877:20081Hardmetals 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 frac
12、tion of silicon in the 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 m
13、ethyl-isobutylketone 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 Sul
14、furic acid, 96 % by mass. 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. BS ISO 11877:20082 4
15、 Apparatus and equipment All apparatus and equipment in 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
16、 tetrafluoride. 4.2 Test-tube shaker. 4.3 Refrigerator. 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 wat
17、er in a PTFE flask. 6 Preparation of solutions for receiver 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 10
18、0 ml with water. 7 Procedure 7.1 Pour 30 ml of solution 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 nitrog
19、en flow. 7.4 Heat the apparatus to 170 10 C, within approximately 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 so
20、lution to 1,3 to 1,4 with sodium hydroxide (approximately 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. BS ISO 11877:200838 Phot
21、ometric determination Transfer the methyl-isobutylketone phase to an appropriate photometer 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 exc
22、ept the sample material. 9.2 Calibration solution Treat a silicon standard sample as outlined 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 ex
23、tinction, EX is the experimentally measured extinction and EB is the blind value of the 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 accep
24、table determination rounded to 0,001 % by mass. 11 Test report 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; d) all operations not specified in this
25、 International Standard, or regarded as optional; e) details of any occurrence which may have affected the result. BS ISO 11877:20084 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 (tru
26、eness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility 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 o
27、f a standard measurement method 4 ISO 5725-4, Accuracy (trueness and precision) of measurement methods and results Part 4: 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: A
28、lternative methods for the determination of the precision of a standard measurement method 6 ISO 5725-6, Accuracy (trueness and precision) of measurement methods and results Part 6: Use in practice of accuracy values BS ISO 11877:2008blankBS ISO 11877:2008BSI Group Headquarters389 Chiswick High Road
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