EN ISO 3908-2009 en Hardmetals - Determination of insoluble (free) carbon - Gravimetric method《硬质合金 不溶性(游离)碳含量的测定 重量法［代替 CEN EN 23908］》.pdf

1、BS EN ISO3908:2009ICS 77.160NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDHardmetals Determination ofinsoluble (free) carbon Gravimetric method(ISO 3908:2009)This British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on

2、31 March2010 BSI 2010ISBN 978 0 580 56455 0Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 3908:2009National forewordThis British Standard is the UK implementation of EN ISO 3908:2009. Itsupersedes BS EN 23908:1993 which is withdrawn.The UK participation in its preparation was e

3、ntrusted to TechnicalCommittee ISE/65, Sintered metal components.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.

4、Compliance with a British Standard cannot confer immunityfrom legal obligations.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 3908 October 2009 ICS 77.160 Supersedes EN 23908:1993English Version Hardmetals - Determination of insoluble (free) carbon - Gravimetric method (ISO 3908:2009) Mta

5、ux-durs - Dosage du carbone insoluble (libre) - Mthode gravimtrique (ISO 3908:2009) Hartmetalle - Bestimmung des unlslichen (freien) Kohlenstoffgehaltes - Gravimetrisches Verfahren (ISO 3908:2009) This European Standard was approved by CEN on 29 September 2009. CEN members are bound to comply with t

6、he CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN Management Centr

7、e or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official

8、 versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Sloven

9、ia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN nat

10、ional Members. Ref. No. EN ISO 3908:2009: EBS EN ISO 3908:2009EN ISO 3908:2009 (E) 3 Foreword This document (EN ISO 3908:2009) has been prepared by Technical Committee ISO/TC 119 “Powder metallurgy“. This European Standard shall be given the status of a national standard, either by publication of an

11、 identical text or by endorsement, at the latest by April 2010, and conflicting national standards shall be withdrawn at the latest by April 2010. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be hel

12、d responsible for identifying any or all such patent rights. This document supersedes EN 23908:1993. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, C

13、zech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 3908:20

14、09 has been approved by CEN as a EN ISO 3908:2009 without any modification. BS EN ISO 3908:2009ISO 3908:2009(E) ISO 2009 All rights reserved iiiForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of pr

15、eparing 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 organizations, governmental and non-governmental, i

16、n 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 the ISO/IEC Directives, Part 2. The main tas

17、k 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. Attentio

18、n 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 3908 was prepared by Technical Committee ISO/TC 119, Powder metallurgy, Subcommittee SC 4, Sampling and t

19、esting methods for hardmetals. This third edition cancels and replaces the second edition (ISO 3908:1985), which has been technically revised. BS EN ISO 3908:2009BS EN ISO 3908:2009INTERNATIONAL STANDARD ISO 3908:2009(E) ISO 2009 All rights reserved 1Hardmetals Determination of insoluble (free) carb

20、on Gravimetric method 1 Scope This International Standard specifies a gravimetric method for the determination of the mass fraction of insoluble (free) carbon in carbides and hardmetals. This method is applicable to carbides of hafnium, molybdenum, niobium, tantalum, titanium, vanadium, tungsten and

21、 zirconium, mixtures of these carbides and binder metals, free of lubricant, and all grades of presintered or sintered hardmetals, produced from these carbides, having a mass fraction of insoluble carbon between 0,02 % and 0,5 %. 2 Normative references The following referenced documents are indispen

22、sable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 3907:2009, Hardmetals Determination of total carbon Gravimetric method 3 Principle Decomposi

23、tion of the carbides and determination of the insoluble carbon by a gravimetric method. 4 Reagents During the analysis, use only reagents of recognized analytical grade, and only distilled water or water of equivalent purity. 4.1 Nitric acid, = 1,20 g/ml. Add 2 000 ml of nitric acid, = 1,42 g/ml, to

24、 3 000 ml of water. 4.2 Hydrofluoric acid, = 1,12 g/ml. BS EN ISO 3908:2009ISO 3908:2009(E) 2 ISO 2009 All rights reserved5 Apparatus Ordinary laboratory apparatus and the following. 5.1 Apparatus, as specified in ISO 3907. 5.2 Platinum dish, of capacity 200 ml. 5.3 Filter device: ceramic filter dev

25、ice or bed of suitable refractory fibrous or powder material in a Gooch crucible. NOTE If necessary, pretreat the refractory material at 800 C to 1 000 C under strongly oxidizing conditions for a minimum of 3 h. If pretreated, store it in a desiccator. 5.4 Vacuum filtration assembly. 6 Sampling 6.1

26、The sample shall be crushed to a powder in a mortar made of a material which does not alter the sample composition. The powder shall pass through a 180 m sieve. 6.2 The analysis shall be carried out on two or three test portions. 7 Procedure 7.1 Test portion Weigh, to the nearest 0,01 g, approximate

27、ly 2,5 g of the test sample. 7.2 Attack Transfer the test portion (7.1) into the platinum dish (5.2). Add 75 ml of the nitric acid (4.1) and place the dish on a steam bath for 5 min. Add, drop by drop, 10 ml of the hydrofluoric acid (4.2), and leave the dish on the steam bath for about 1 h until com

28、plete dissolution is obtained. Cool the solution to ambient temperature. CAUTION Hydrofluoric and nitric acids are very dangerous chemicals. Any contact with these acids or inhalation of their vapours shall be avoided. All operations with these acids shall be carried out in a fume-cupboard with good

29、 ventilation. 7.3 Preparation of the Gooch crucible Insert the ceramic filter device (5.3) into the crucible. If a refractory material is used, fill the crucible to a depth of approximately 8 mm to 10 mm and press it down so that the residue will be retained on the refractory material and the time o

30、f filtering will not be too slow. BS EN ISO 3908:2009ISO 3908:2009(E) ISO 2009 All rights reserved 37.4 Filtering Before filtering, add a limited quantity of water to avoid the precipitation of tungstic acid. Filter the contents of the dish (see 7.2) through the filter device (5.3). Then rinse the d

31、ish twice with small volumes of water. Be sure that all particles of carbon are transferred to the filter device. Rinse the dish again with water at least twice and then wash the filter device free from acid with hot water (about 500 ml is usually needed). Remove the wet filter device from the Gooch

32、 crucible and transfer the wet filter device into a boat (see ISO 3907:2009, 4.1.5). Dry it at 110 C. 7.5 Blank test Carry out two blank tests for each series of determinations. Prepare the Gooch crucible in accordance with 7.3. Filter through the filter device (5.3) a mixture of 75 ml of the nitric

33、 acid (4.1) and 10 ml of the hydrofluoric acid (4.2) and proceed in accordance with 7.4. 7.6 Determination Burn the filter device (5.3) in a stream of oxygen in accordance with ISO 3907. Use a furnace with an inner temperature of the tube of approximately 1 200 C. 8 Expression of results 8.1 Calcula

34、tion The mass fraction of carbon , expressed as a percentage, is given by the formula 21027,29mmm where m0is the mass, in grams (g), of the test portion; m1is the mass, in grams (g), of carbon dioxide obtained from the blank test; m2is the mass, in grams (g), of carbon dioxide obtained from the comb

35、ustion of the test portion; 27,29 is the carbon dioxide to carbon conversion factor, multiplied by 100. 8.2 Tolerances The deviation between two or three independent determinations shall not exceed the values shown in Table 1. Table 1 Tolerances Total carbon mass fraction Range for two determination

36、s Range for three determinations % % % from 0,02 to 0,1 0,02 0,03 over 0,1 to 0,5 0,04 0,05 BS EN ISO 3908:2009ISO 3908:2009(E) 4 ISO 2009 All rights reserved8.3 Final result Report the arithmetical mean of acceptable determinations rounded to the nearest 0,01 % (mass fraction). 9 Test report The te

37、st report shall include the following information: a) a reference to this International Standard; b) all details necessary for the identification of the test sample; c) the result obtained; d) all operations not specified in this International Standard, or regarded as optional; e) details of any occ

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