1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 13944:2012Lubricated metal-powder mixes Determination of lubricant content Soxhlet extraction methodBS EN ISO 13944:2012 BRITISH STANDARDNational forewordThis British S
2、tandard is the UK implementation of EN ISO 13944:2012. It supersedes BS EN ISO 13944:2006, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee ISE/65, Sintered metal components.A list of organizations represented on this committee can be obtained on reques
3、t to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2012. Published by BSI Standards Limited 2012.ISBN 978 0 580 76769 2 ICS 77.160 Compliance with a British S
4、tandard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 December 2012.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 13944 Novembe
5、r 2012 ICS 77.160 Supersedes EN ISO 13944:2006English Version Lubricated metal-powder mixes - Determination of lubricant content - Soxhlet extraction method (ISO 13944:2012) Mlanges de poudres mtalliques lubrifies - Dtermination de la teneur en lubrifiant - Mthode dextraction au Soxhlet (ISO 13944:2
6、012) Metallpulver mit Gleitmittelzusatz - Bestimmung des Gleitmittelan-teils - Extraktionsverfahren nach Soxhlet (ISO 13944:2012) This European Standard was approved by CEN on 13 August 2012. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for
7、 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-CENELEC Management Centre or to any CEN member. This European Standard exists in three
8、 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-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodi
9、es of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Sp
10、ain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN n
11、ational Members. Ref. No. EN ISO 13944:2012: EBS EN ISO 13944:2012 EN ISO 13944:2012 (E) 3 Foreword This document (EN ISO 13944:2012) 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 publicatio
12、n of an identical text or by endorsement, at the latest by May 2013, and conflicting national standards shall be withdrawn at the latest by May 2013. 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
13、held responsible for identifying any or all such patent rights. This document supersedes EN ISO 13944:2006. According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cr
14、oatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
15、 the United Kingdom. Endorsement notice The text of ISO 13944:2012 has been approved by CEN as a EN ISO 13944:2012 without any modification. BS EN ISO 13944:2012 EN ISO 13944:2012(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodie
16、s (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 organizations,
17、 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 the ISO/
18、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 the mem
19、ber 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 13944 was prepared by Technical Committee ISO/TC 119, Powder metallurgy,
20、 Subcommittee SC 2, Sampling and testing methods for powders (including powders for hardmetals).This second edition cancels and replaces the first edition (ISO 13944:1996), which has been technically revised. ISO 2012 All rights reserved iiiBS EN ISO 13944:2012 EN ISO 13944:2012 (E) BS EN ISO 13944:
21、2012Lubricated metal-powder mixes Determination of lubricant content Soxhlet extraction method1 ScopeThis International Standard specifies a method for the determination of the lubricant content of a powder mix. The method is also suitable for preparing samples for measuring the content of elements,
22、 e.g. graphite and oxygen, the determination of which is interfered with by the presence of a lubricant.A condition of the application of the method is that a suitable solvent for the lubricant concerned is known and available.2 PrincipleThe lubricant is extracted from a weighed test portion using a
23、 suitable solvent. The test portion is reweighed after the extraction, and the percentage mass loss, representing the extracted lubricant, is calculated.The extracted test portion can then be used to determine, by the normal methods, the content of other constituents, without any interference from t
24、he lubricant.3 Apparatus and materials3.1 Analytical balance, capable of weighing the sintered-glass filter crucible (see 3.2.3), together with the test portion, to the nearest 1 mg.3.2 Soxhlet apparatus, as shown in Figure 1, with ungreased joints, consisting of the following parts.3.2.1 Allihn (bu
25、lb-type) condenser.3.2.2 Soxhlet extractor, with a volume of 150 ml to 200 ml.3.2.3 Sintered-glass filter crucible (porosity grade P 1601), filter paper (with a filtering speed of 1 000 mI/min), glass wool and a length of glass tubing with a diameter of about 30 mm and long enough to serve the purpo
26、se mentioned in 5.3.In cases where the lubricant content to be determined is less than 0,5 %, all these items shall be rinsed with organic solvent (3.3) before use.3.2.4 Round-bottomed flask, with a capacity of 500 ml, containing a boiling aid.3.2.5 Heating mantle, of sufficient power to evaporate t
27、he solvent at a rate of not less than 25 ml/min.3.3 Organic solvent, suitable for extraction of the lubricant concerned. Examples of such solvents are xylene, toluene and petroleum ether.1) As defined in ISO 4793:1980, Laboratory sintered (fritted) filters Porosity grading classification and designa
28、tion .INTERNATIONAL STANDARD EN ISO 13944:2012(E) ISO 2012 All rights reserved 13.4 Automated system for Soxhlet extraction method, which can be used as an alternative to the test set-up described in 3.2. The basic principles of an automated system should be the same as for the manual test set-up de
29、scribed in 3.2.WARNING Inhalation of the vapours of organic solvents such as toluene is dangerous.4 Test portions4.1 The determination shall be carried out on two test portions.4.2 In general, the test portions shall be taken from the powder in the as-received condition.4.3 The mass of each test por
30、tion shall be approximately 50 g if the lubricant content is less than or equal to 2 %, or approximately 25 g if the lubricant content is greater than 2 %.5 Procedure5.1 Weigh the filter crucible together with a filter paper and a plug of glass wool in the mouth of the crucible to the nearest 1 mg (
31、m1). It is important to ensure that the filter paper is dry. If needed, the filter paper should be dried before the analysis to avoid errors caused by moisture.5.2 Place the test portion on the filter paper in the bottom of the crucible, and cover with the plug of glass wool. Weigh the crucible plus
32、 filter paper plus test portion plus glass wool together to the nearest 1 mg (m2).5.3 Place the crucible plus contents in the Soxhlet extractor, using the length of glass tubing to bring the upper edge of the crucible level with the upper bend of the syphon.5.4 Introduce about 300 ml of the solvent
33、into the round-bottomed flask, and connect it to the Soxhlet extractor (see Figure 1).5.5 Heat the solvent to its boiling point. It is recommended that a preliminary test be made, for a given type of powder and solvent, to establish the minimum time required for complete extraction. In general, this
34、 time will be less than 30 min. For powders containing 0,8 % zinc stearate and with toluene as the solvent, an extraction time of 10 min to 20 min, concluding at the end of an extraction cycle, has been found to be sufficient. The time established in the preliminary test will apply to all further te
35、sts with the same combination of powder and solvent.5.6 On completion of the extraction, remove the crucible plus contents from the Soxhlet apparatus and suck dry on a Bchner flask. Then fill with fresh solvent and suck dry again. As a final washing operation, fill the crucible with diethyl ether (m
36、ake sure that the temperature of the crucible and its contents is below 30 C in order to avoid ignition) and suck dry. Allow any ether residues to evaporate for about 15 min in order to avoid ignition when the crucible is placed in a drying oven, where it is kept at 110 C for 30 min.As an alternativ
37、e to the final washing operation, the samples can be dried at 125 C for 30 min under inert atmosphere.5.7 After cooling in a desiccator, weigh the crucible plus contents to the nearest 1 mg (m3).5.8 Test portions can be taken by means of a small spoon from the powder remaining after the extraction f
38、or the determination of other constituents of the powder mix (e.g. graphite by means of equipment for the determination of carbon or oxygen by one of the methods described in the various parts of ISO 4491, Metallic powders Determination of oxygen content by reduction methods ). Before taking a test
39、portion, the remaining sample shall be homogenized since the extraction procedure might have segregated the sample.2 ISO 2012 All rights reservedBS EN ISO 13944:2012 EN ISO 13944:2012 (E) Key1 Soxhlet extractor (see 3.2.2) 6 boiling aid (see 3.2.4) 2 sintered-glass filter crucible (Type P 160) (see
40、3.2.3) 7 syphon3 glass tubing (see 3.2.3) 8 cold-water intake4 round-bottomed flask (see 3.2.4) 9 Allihn (bulb-type) condenser (see 3.2.1)5 heating mantle (see 3.2.5) 10 outletFigure 1 Soxhlet apparatus (3.2) ISO 2012 All rights reserved 3BS EN ISO 13944:2012 EN ISO 13944:2012 (E) BS EN ISO 13944:20
41、12 EN ISO 13944:2012(E)6 Expression of results6.1 The lubricant content, expressed as a percentage by mass, is given by the formula m mm m2 32 1100 wherem1is the mass, in grams, of the crucible together with the filter paper and the glass-wool plug; m2is the mass, in grams, of the crucible plus filt
42、er paper plus glass wool plus test portion;m3is the mass, in grams, of the crucible plus contents after the extraction.6.2 The maximum difference between the two determinations shall not exceed 0,1 % (m/m). If the difference exceeds 0,1 % (m/m), discard the results and repeat the two determinations
43、with fresh test portions.6.3 Report the arithmetic mean of the two determinations, rounded to the nearest 0,05 % (m/m).7 Test reportThe test report shall include the following information:a) a reference to this International Standard;b) all details necessary for the identification of the sample test
44、ed;c) the solvent used;d) the extraction time;e) the result obtained;f) details of any operation not specified by this International Standard, as well as any operation regarded as optional;g) details of any incident which may have affected the result;h) the date of the test.4 ISO 2012 All rights res
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