DIN EN ISO 13944-2013 Lubricated metal-powder mixes - Determination of lubricant content - Soxhlet extraction method (ISO 13944 2012) German version EN ISO 13944 2012《含润滑剂的金属粉末混合物 .pdf

1、March 2013 Translation by DIN-Sprachendienst.English price group 7No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 7

2、7.160!$qk“1957872www.din.deDDIN EN ISO 13944Lubricated metal-powder mixes Determination of lubricant content Soxhlet extraction method (ISO 13944:2012);English version EN ISO 13944:2012,English translation of DIN EN ISO 13944:2013-03Metallpulver mit Gleitmittelzusatz Bestimmung des Gleitmittelanteil

3、s Extraktionsverfahren nach Soxhlet (ISO 13944:2012);Englische Fassung EN ISO 13944:2012,Englische bersetzung von DIN EN ISO 13944:2013-03Mlanges de poudres mtalliques lubrifies Dtermination de la teneur en lubrifiant Mthode dextraction au Soxhlet (ISO 13944:2012);Version anglaise EN ISO 13944:2012,

4、Traduction anglaise de DIN EN ISO 13944:2013-03SupersedesDIN EN ISO 13944:2006-06www.beuth.deDocument comprises 9 pagesIn case of doubt, the German-language original shall be considered authoritative.02.13DIN EN ISO 13944:2013-03 2 A comma is used as the decimal marker. National foreword This docume

5、nt (EN ISO 13944:2012) has been prepared by Technical Committee ISO/TC 119 “Powder metallurgy”, Subcommittee SC 2 “Sampling and testing methods for powders (including powders for hardmetals)” in collaboration with Technical Committee CEN/SS M11 “Powder metallurgy” (Secretariat: CCMC). The responsibl

6、e German body involved in its preparation was the Normenausschuss Werkstofftechnologie (Technology of Materials Standards Committee), Working Committee NA 145-01-02 AA Probenahme und Prfverfahren fr Pulver (einschlielich Pulver fr Hartmetalle). Amendments This standard differs from DIN ISO 13944:200

7、6-06 as follows: a) the key to Figure 1 has been extended and revised; b) the word “modified” has been deleted from the title; c) Subclause 3.4 “Automated system for Soxhlet extraction method” has been added; d) Clause 5 “Procedure” has been revised; e) the standard has been editorially revised. Pre

8、vious editions DIN ISO 4495: 1987-08 DIN ISO 13944: 1998-07, 2006-06 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 13944 November 2012 ICS 77.160 Supersedes EN ISO 13944:2006English Version Lubricated metal-powder mixes - Determination of lubricant content - Soxhlet extraction method (ISO

9、 13944:2012) Mlanges de poudres mtalliques lubrifies - Dtermination de la teneur en lubrifiant - Mthode dextraction au Soxhlet (ISO 13944:2012) Metallpulver mit Gleitmittelzusatz - Bestimmung des Gleitmittelanteils - Extraktionsverfahren nach Soxhlet (ISO 13944:2012) This European Standard was appro

10、ved by CEN on 13 August 2012. CEN members are bound to comply with the 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

11、standards may be obtained on application to the CEN-CENELEC Management Centre 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 a

12、nd notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hung

13、ary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Manageme

14、nt Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 13944:2012: EDIN EN ISO 13944:2013-03 EN ISO 13944:2012 (E) 2Contents Page Foreword . 3 1 Scope . 4 2 Principle . 4 3 Apparatus a

15、nd materials 4 Test portions . 5 5 Procedure 5 6 Expression of results . 7 7 Test report . 7 4Foreword 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 publica

16、tion 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

17、be 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,

18、 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, Spain, Sweden, Switzerland, Turkey

19、and 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. DIN EN ISO 13944:2013-03 EN ISO 13944:2012 (E) 3 1 ScopeThis International Standard specifies a method for the determination of the lubricant content of a p

20、owder mix. The method is also suitable for preparing samples for measuring the content of elements, 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 concern

21、ed is known and available.2 PrincipleThe lubricant is extracted from a weighed test portion using a 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 d

22、etermine, by the normal methods, the content of other constituents, without any interference from the 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 apparat

23、us, as shown in Figure 1, with ungreased joints, consisting of the following parts.3.2.1 Allihn (bulb-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

24、wool and a length of glass tubing with a diameter of about 30 mm and long enough to serve the purpose 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 ca

25、pacity of 500 ml, containing a boiling aid.3.2.5 Heating mantle, of sufficient power to evaporate the 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

26、in ISO 4793:1980, Laboratory sintered (fritted) filters Porosity grading classification and designation .DIN EN ISO 13944:2013-03 EN ISO 13944:2012 (E) 43.4 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 o

27、f an automated system should be the same as for the manual test set-up described 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 f

28、rom the powder in the as-received condition.4.3 The mass of each test portion 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 an

29、d a plug of glass wool in the mouth of the crucible to the nearest 1 mg (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

30、 crucible, and cover with the plug of glass wool. Weigh the crucible plus 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 wit

31、h the upper bend of the syphon.5.4 Introduce about 300 ml of the solvent 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 esta

32、blish the minimum time required for complete extraction. In general, this 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.

33、The time established in the preliminary test will apply to all further tests 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 aga

34、in. As a final washing operation, fill the crucible with diethyl ether (make 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 place

35、d in a drying oven, where it is kept at 110 C for 30 min.As an alternative 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 b

36、y means of a small spoon from the powder remaining after the extraction for 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 Dete

37、rmination of oxygen content by reduction methods ). Before taking a test portion, the remaining sample shall be homogenized since the extraction procedure might have segregated the sample.DIN EN ISO 13944:2013-03 EN ISO 13944:2012 (E) 5 Key1 Soxhlet extractor (see 3.2.2) 6 boiling aid (see 3.2.4)2 s

38、intered-glass filter crucible (Type P 160) (see 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)DIN EN ISO 13944:2013-03 EN ISO 13944:2012 (

39、E) 66 Expression of results6.1 The lubricant content, expressed as a percentage by mass, is given by the formulammmm2321100wherem1is 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 filter paper plus glass wool p

40、lus 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 with fresh test portions.6

41、.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 tested;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.DIN EN ISO 13944:2013-03 EN ISO 13944:2012 (E) 7