1、Reference numberISO/TS 14423:1999(E)ISO 1999TECHNICALSPECIFICATIONISO/TS14423First edition1999-10-01Carbonaceous materials used in theproduction of aluminium Cold-rammingpastes Determination of effective bindercontent and aggregate content byextraction with quinoline, anddetermination of aggregate s
2、ize distributionProduits carbons utiliss pour la production de laluminium Ptes debrasquage froid Dtermination de la teneur effective en liant et enaggrgats par extraction la quinoline, et dtermination de lagranulomtrieCopyright International Organization for Standardization Provided by IHS under lic
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7、crofilm, without permission in writing from either ISO at the address below or ISOs member bodyin the country of the requester.ISO copyright officeCase postale 56 Gb7 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 734 10 79E-mail copyrightiso.chWeb www.iso.chPrinted in Switzerlandii ISO 1999 All
8、 rights reservedCopyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-ISO/TS 14423:1999(E) ISO 1999 All rights reserved iiiContents PageForeword.ivIntroduction.v1 Scope12 Norma
9、tive references13 Principle14 Terms and definitions .25 Reagents.26 Apparatus.27 Sampling.38 Preparation of test portion39 Procedure.310 Calculation and expression of results.410.1 Effective binder content410.2 Aggregate content.410.3 Aggregate particle-size distribution411 Precision.412 Test report
10、4Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-ISO/TS 14423:1999(E)iv ISO 1999 All rights reservedForewordISO (the International Organization for Standardization) is a
11、worldwide federation of national standards bodies (ISOmember bodies). The work of preparing International Standards is normally carried out through ISO technicalcommittees. Each member body interested in a subject for which a technical committee has been established hasthe right to be represented on
12、 that committee. International organizations, governmental and non-governmental, inliaison with ISO, also take part in the work. ISO collaborates closely with the International ElectrotechnicalCommission (IEC) on all matters of electrotechnical standardization.International Standards are drafted in
13、accordance with the rules given in the ISO/IEC Directives, Part 3.The main task of technical committees is to prepare International Standards. Draft International Standards adoptedby the technical committees are circulated to the member bodies for voting. Publication as an InternationalStandard requ
14、ires approval by at least 75 % of the member bodies casting a vote.In other circumstances, particularly when there is an urgent market requirement for such documents, a technicalcommittee may decide to publish other types of normative document:Gbe an ISO Publicly Available Specification (ISO/PAS) re
15、presents an agreement between technical experts in anISO working group and is accepted for publication if it is approved by more than 50 % of the members of theparent committee casting a vote;Gbe an ISO Technical Specification (ISO/TS) represents an agreement between the members of a technicalcommit
16、tee and is accepted for publication if it is approved by 2/3 of the members of the committee casting avote.An ISO/PAS or ISO/TS is reviewed every three years with a view to deciding whether it can be transformed into anInternational Standard.Attention is drawn to the possibility that some of the ele
17、ments of ISO/TS 14423 may be the subject of patent rights.ISO shall not be held responsible for identifying any or all such patent rights.ISO/TS 14423 was prepared by Technical Committee ISO/TC 47, Chemistry, Subcommittee SC 7, Aluminiumoxide, cryolite, aluminium fluoride, sodium fluoride, carbonace
18、ous products for the aluminium industry.Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-ISO/TS 14423:1999(E) ISO 1999 All rights reserved vIntroductionIn order to determi
19、ne the particle-size distribution of the aggregate used in cold-ramming pastes, it is necessary toobtain the aggregate in a binder-free state. The most practicable way to achieve this is by extraction of the binderby a suitable solvent, and the most effective common solvent for coal-tar and bitumino
20、us binders is quinoline. Mostcoal tars are not totally soluble in quinoline, but have a small content of insoluble matter which principallycomprises infusible solid carbonaceous particles smaller than approximately 50 G6dm. This insoluble matter iseffectively part of the solid aggregate of the cold-
21、ramming paste and is measured as such by this method. Theeffective binder is defined as that proportion of the product which is soluble in quinoline.Although quinoline is the most effective common solvent for the present purpose, it has the disadvantage of beingexpensive and of having a high boiling
22、 point which makes the removal of the last traces from the extracted residuedifficult by normal drying processes. However, when the most complete separation of the binder from the aggregateis required, e.g. for referee purposes, quinoline is the solvent of choice, and the method given in this Techni
23、calSpecification should be employed.NOTE The procedure described in this Technical Specification utilizes dichloromethane, but only to remove residual tracesof quinoline solvent from filters prior to oven drying.Copyright International Organization for Standardization Provided by IHS under license w
24、ith ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-TECHNICAL SPECIFICATION ISO/TS 1
25、4423:1999(E) ISO 1999 All rights reserved 1Carbonaceous materials used in the production of aluminium Cold-ramming pastes Determination of effective binder contentand aggregate content by extraction with quinoline, anddetermination of aggregate size distribution1 ScopeThis Technical Specification de
26、scribes a method for determining the content and particle-size distribution of thesolid aggregate component, and also for determining the effective binder content, of cold-ramming pastes used inaluminium manufacture.The method is applicable to cold-ramming pastes made with coal-tar or bituminous bin
27、ders but not applicable toresin-based binders.2 Normative referencesThe following normative documents contain provisions which, through reference in this text, constitute provisions ofthis Technical Specification. For dated references, subsequent amendments to, or revisions of, any of thesepublicati
28、ons do not apply. However, parties to agreements based on this Technical Specification are encouraged toinvestigate the possibility of applying the most recent editions of the normative documents indicated below. Forundated references, the latest edition of the normative document referred to applies
29、. Members of ISO and IECmaintain registers of currently valid International Standards.ISO 565, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes ofopenings.ISO 2591-1, Test sieving Part 1: Methods using test sieves of woven wire cloth and perforated metal pla
30、te.ISO 14422:1999, Carbonaceous materials used in the production of aluminium Cold-ramming pastes Sampling.3PrincipleA test portion of the cold-ramming paste is digested under reflux with quinoline to dissolve the binder. The digestionmixture is poured on to a fine-aperture sieve, upon which the maj
31、ority of the aggregate thus retained is washed freeof residual binder with further portions of quinoline and then dried and weighed. The mixture and washings passingthrough the sieve are filtered through a filter pad and the very fine particles of aggregate thus recovered arelikewise washed, dried a
32、nd weighed.The content of the aggregate is determined from the total mass of the particles retained on the sieve and the filterpad, and the content of the quinoline-soluble matter is calculated by difference.The particle-size distribution of the solids retained on the fine-aperture sieve is determin
33、ed by test sieving.Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-ISO/TS 14423:1999(E)2 ISO 1999 All rights reserved4 Terms and definitionsFor the purposes of this Techn
34、ical Specification, the terms and definitions given in ISO 14422 and the followingapply.4.1effective binder contentproportion of the product soluble in quinoline, expressed as a percentage by mass5 ReagentsWARNING Refer to the reagent suppliers health and safety data sheets for the precautions which
35、 are tobe observed for the safe use of quinoline and dichloromethane.5.1 Quinoline, of purity at least 98 % by mass, freshly distilled, boiling between 235 C and 237 C at 101,36 kPa.5.2 Dichloromethane (methylene dichloride), of purity at least 98 % by mass.6 ApparatusOrdinary laboratory apparatus a
36、nd the following:6.1 Distillation flask, round-bottomed, of borosilicate glass, capacity 2 litres, having a ground-glass socket.6.2 Reflux air condenser, of effective length 550 mm, having a ground-glass cone by means of which it may befitted to the socket of the distillation flask (6.1).6.3 Electri
37、c heating mantle, capable of maintaining gentle boiling of the contents of the distillation flask (6.1)whilst under reflux.6.4 Nest of test sieves, 200 mm in diameter, conforming to ISO 565, of stainless-steel wire cloth, with nominalapertures of between 53 G6dm and 5 mm inclusive, with lid and rece
38、iver.NOTE Other nominal apertures recommended for inclusion are: 2 mm and 1 mm, 500 G6dm, 250 G6dm and 75 G6dm.6.5 Receiver test sieve, 200 mm in diameter, conforming to the requirements of ISO 565, of stainless-steel wirecloth, of 53 G6dm nominal aperture. Prepare by heating in the electric oven (6
39、.7) for 1 h at a temperature of110 C Gb1 5 C then allow to cool to ambient temperature in a desiccator and store in the desiccator until required foruse.6.6 Dish, of glass or porcelain, capable of fitting below the receiver test sieve (6.5) and collecting all the liquidswhich pass through.6.7 Electr
40、ic oven, of size sufficient to contain the receiver test sieve (6.5) and capable of being maintained at110 C Gb1 5C.6.8 Funnel, Hartley 3-piece or equivalent, having a disc diameter of 120 mm.6.9 Glass-fibre filter pads, of diameter 120 mm, with a retention of at least 98 % by mass for particles of
41、size1,2 G6dm.Drybyheatingfor1hat110CGb1 5 C then store in a desiccator until required for use.6.10 Mechanical sieve shaker, capable of accommodating the nest of sieves (6.4) with the lid and receiver, asdescribed in ISO 2591-1.Copyright International Organization for Standardization Provided by IHS
42、under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-ISO/TS 14423:1999(E) ISO 1999 All rights reserved 37 SamplingPrepare a representative laboratory sample of cold-ramming paste in accordance with ISO 14422.8 Preparation of test portionTake 100 g
43、Gb1 0,05 g from the laboratory sample (see clause 7) in accordance with 6.5.3 of ISO 14422:1999.9 Procedure9.1 Transfer the test portion quantitatively to the distillation flask (6.1). Add 1 litre of quinoline (5.1) and swirl thecontents of the flask to mix the test portion with the quinoline. Place
44、 the flask in the electric heating mantle (6.3)and fit the reflux air condenser (6.2) to the flask. Bring the contents of the flask to a steady boil and continue boilingunder reflux for 1 h.Switch off the electric heating mantle and allow the flask and its contents to cool to 50 C Gb1 5C. Weigh ther
45、eceiver test sieve (6.5) to the nearest 0,01 g then place it over the dish (6.6). Carefully transfer the hot contents ofthe flask as completely as possible to the sieve. Rinse the flask using successive 20 ml portions of quinoline at50 C Gb1 5 C until all the visible solids have been transferred to
46、the sieve. Wash the contents of the sieve withquinoline at 50 C Gb1 5 C until the washings passing through the sieve show no additional colour due to dissolvedbinder. Allow the quinoline to drain from the sieve contents then separate the test sieve and the dish.9.2 Transfer the contents of the dish
47、quantitatively to a container to await recovery of the solids by filtration.9.3 Replace the receiver test sieve over the dish and wash the aggregate on the sieve with 10 successive 100 mlportions of dichloromethane (5.2), allowing each portion of the solvent to drain off before adding the next. Afte
48、r thefinal wash, leave the sieve and its contents to drain for 1 h and discard the washings. Place the receiver test sievewith its contents in the oven (6.7) maintained at 110 C Gb1 5 C for 1 h, taking care that no boiling of residualdichloromethane occurs, leading to loss of solids.Remove the recei
49、ver test sieve with its contents and allow to cool to ambient temperature in a desiccator. Weighthe receiver test sieve and its contents to the nearest 0,01 g. Repeat the operations of heating, cooling andweighing until the difference between two consecutive weighings does not exceed 0,01 g.9.4 Weigh a dried filter pad (6.9) to the nearest 0,01 g. Assemble
