BRITISH STANDARD Physical testing of rubber — | Part A6: Method for determination \, ) compression set at ambient, eleva’ low temperatures : No COPYING WITHOUT NST PERMISSION EXCEFT AS PERMITTED BY COPYRIGHT LAW BS 903-A6: 1992 ISO 815:1991 Incorporating ‘Amendment No.1BS 903-A6:1992 Committees responsible for this British Standard ‘The preparation of this British Standard was entapsted by the Plastics and Rubber Standards Policy Committee (PRM/-) to Technical Committee PRM/22, ‘upon which the following bodies were represented: BP Chemicals Ltd. British Railways Board British Rubber Manufacturers’ Association Ltd, GAMBICA (BEAMA Ltd) Feet Maken ages Inattatn of Weer and Environmental anagem 6 Hisipeian Beer Sot? Bist Ansa Mingo Deteee TAPRA Technsogy Le SATRA Pontwens Teohonlogy Cente “This Bytsh Standard having Ivan prepazed under the Aircon ofthe Pasties and tuber tanned Paley Cormte,w publish tuner the author tp ‘Standards Board ad intoeflect on 15 May 192 ‘© st 02-1900 First published October 1887 ndments issued since publiontion = Seontedaion nsierioes Ame" ” ‘Third dition March 1968, ni Seal Fourheditinhtoy 1992 Amd. No. | Date toner 7976 March 1994 | Indicated by a sideline in the margin IB ncaa cea poe oe fee 2 SeeuersBS 903-A6:1992 Contents me Committees responsible, Inside front cover National foreword ‘Scope Normative referene: Principle 1 2 3 4 Apparatus 5 Test pieces 6 Test conditions 7 Procedure 8 9 Expression of results Precision ‘Test report ‘enstoz.1999BS 903-A6:1992 National foreword ‘This British Standard has been prepared under the direction of the Plastics and Rubber Standards Policy Committee. It is identical with 180 815 Rubber aaapeted or thermoplastic — Determination of covipression set at ambient, 7 aesconi tow temperatures, as amended by Technical Corrigendum 1 published | D tthe Invernational Organization for Standardization (SO). As 1SQ 8)9;.001 ty IM sporacdes ISO 1653 this Part las been revised to incorporate Bart AMO Telermination of eompression set under constant deflection at low te Pre ctendard specifies rather different methods for the determinati temperatures and at ambient or elevated temperatures Overy tnd gubsequent measurement for the low temperature test temperature, BS 903-A6:1969 and BS 903-A39:1980 “ee Other changes to the standard are pt ee ae rguitement for tubricaion ofthe ost piece ® aon ae ato tcl br mest a ic hike ae natn tymaiching of epecen rca thiknee ofthe et oe Menge are now iantifed as‘ypee Aan rathor than 2 and 1 oaectee Adcinenal nformstion, The sire the socondpacomseph of Addition apiguotn a to what porcedtage compression strain should be 1 applied if the rubber hardnes: RHI 16 information given in the fourth a ae pcs smlarlyanBigugirit regard toa baxdnes of 90 IRED. For dhe removal af doubt the fl tation is recommended 1 1) apply 25 % compression fotadbbers whose nominal hardness is equal toor less than 80IRHD, : 1 reedlin fe rers whose nominathardnssis eal \ 2) ar 1 an BT IRHD Bute than or equal to 89 TRHD sy enaly 10% eompreasion ara for rubbers whose nominal hardness \2 greater than 89/1De < * 6) x crosereterettes Inverguoyf ing? Correeponding British Standard % BS 903 Physical testing of rubber Part A86:1985 Temperatures, humidities ond times for Conditioning and testing of test pieces {dentieal Part A32"1988 General directions for achieving elevated pr subnormal temperatures for test purposes (denticad Part A38:1991 Methods for the determination of Tannsiens of test pieces and products for test purposes | (Udentical) 180 4661-1:1986 Part A36:1988 Preparation of somples and test Picoes " (dentical) 180 5725:1986, BS 5497 Precision of test methods 5 Part 1:1987 Guide for the determination of repeatability ‘and reproducibility for a siandard test method by {interlaboratory testsBS 903-A6:1992 ‘The Technical Committee has reviewed the provisions of ISO 1826:1981, towhich normative reference is made in the text, and has decided that they are aceeptable for use in conjunction with this standard. A British Standard related to 180 1826:1981 is BS 903-A19:1986. A British Standard related to ISO 468:1982 ry provisions of a contract. Users of British Standards are respon: ct application. Compliance with «British Standard doesat o from legal obligations, immunity Summary of pages ‘This document comprises a front cover, an inside front cover, pages i (0 iv, pages 1 to 10, an inside back cover and a back cover. ‘This standard has been updated (see copyright date) and may have had amendments incorporated, This will be indicated in the amendment table on the inside front cover. pst o2-1099 itiISO 815:1991(K) 1Scope ‘This International Standard specifies methods for the determination of compression set characteristics ofvuleanized and thermoplastic rubbers at ambient, clovatod or low temperatures, ‘The methods are intended to measure the ability of rubbers ofhardness within the range 10 [RED to95 IRHD to retain their elastic properties at ‘specified temperatures after prolonged compression at constant strain (where possible 25 %) under one of the alternative sets of conditions described. For rubber of hardness greater than 80 [RHD, a lower compression strain is used: 15 % for a nominal hardness from 80 IRHD to 89 IRHD and 10 % for a nominal hardness from 90 [RHD to 95 IRED NOTE 1 When rubber fe held under compression, phyaicl or ‘hema ehanges ean our that prevent the rubber retrain to lus original dimonsions after release ofthe dofrming force, The ‘result sa set the mitt of which depends gn the tise and {eaperatuee of compression ae well aon the time and leaperature of resorery At elevated temperatures, chemical bocoms increasingly more important and lead Yo permanent sct which canbe monrared ty allowing test dard trperature. At low tompernren, cis, fe undertaken a the ta trp NOTB2_ Guidanoe for using the precision rvulfegiven in informative Annex Ac tr compression se isforatve Anans B 2 Normative references Kost 1s which, ‘The following standards eémtai through reference in this te ‘provisions of this International Sta e time of publication, the edi re valid, All standards are subj and parties to agreements based on this tional Standard ‘re encouraged to inves 16 possibility of applying the mogP recent editions of the standards indicated bolowi Members of IEC and 180 maintain segisers of currentiyvalid International Standards 180 468: fac8 roughness — Parameters, and gejeral res for specifying 33, Rubber — Standard temperatures, Fand times for the conditioning and testing of test pices. 180 1826:1981, Rubber, uleanized—Time-interval between vulcanization and testing — Specification. 180 $383:1985, Rubber — General directions for ‘achieving elevated or subnormal temperatures for test purposes. 180 4648:1991, Rubber, vulcanized or thermoplastic — Determination of dimensions of test pieces and produets for test purposes. ‘8 91021099 meee fener 180 4661-1:1986, Rubber, vuleanized Preparation of samples and test pieces — Part I: Physical tests. 180 6471:1983, Rubber, vulcanized — Determination of eryetaltsion effets under compression. rubber products — method a as Determination of standards A test piggS fl thickness is compressed at tiakdariferpetare toa doned ses hihi then malligined nstant for a specified time at a Fixed stand elevated temperature. The stain inroloneed and afler th eat plese as ben allowed er at landard tomporatue fore opecifed lth tet pee a apna 3 Principle 3.1 Ambient ai hw temperatures 3 piece of known thickness is compressed at indard temperature to a defined strain, which tant for a specified time at a fixed low temperature. The strain is released and. the test piece allowed to recover at this temperature. The thickness is measured at intervals after the release of the strain so that an assessment of compression set characteristics is obtained from a plot of recovery against time at the low temperature. 4 Apparatus 4.1 Compression apparatus, consisting of compression plates, steel spacers and clamping doviee. 4.1.1 Compression plates, comprising a pair of paraliel, flat, highly polished chromium-plate stee! or highly polished stainless-steel plates, between thie faces of which the test piece is compressed, ‘The finish of the eurface of the compression plates shall be not worse than 0,4 im Ry from the mea line of the profile (see ISO 468). Tho plates shall —be sulficiently rigid to ensure that, with a test piece under load, no compression plate shall bend by more than 0,01 mm; —be of sulficient size to ensure that the whole of the test piece, when compressed between the plates, remains within the area of the plates Steel plates with a diamoter of approximately 115 mm and with a thickness of 6,5 mmand 12,5 mm, respectively. are suggested. A typical apparatus is shown in Figure 1) BS , Mrs. Roma Rey, [SO EXCHANGE INDIA, 29/10/2009 0: nsed Copy: ISO 815:1991(B) TSO 815:1991 06) 4.1.2 Temperature measurement device For low-temperature tests, the plates shall incorporate means of measuring their temperature directly with an accuracy of + 0,5 °C. 4.1.8 Mild-steel spacers), to provide the required. ‘compression. The spacer(s) shall be of such size and shape that contact with the compressed test piece is avoided ‘The height of the spacer(s) shall be as follows: here more than one spacer is used in any one test, the heights shall match to within + 0,01 mm of the ‘mean, Spacer dimensions 94mm max. ‘Test piece type 9,3 mm min. S 4.8mm max 47 mm min, - When crystallization studies are to be made, itis “necessary to control the compression strain as “accurately as possible, and spacers of different heights are required. Tho height of the spacers shall ‘behosen so that the compression of the test piece is (5 = 1) % of the measured thickness of the test piece. ‘Acompression strain of 15% shall be used for hhartinesses between 80 IRHD and 89 IRHD. The height of the spacer(s) shall be as follows: ‘Spacerdimensions Test piece ty 10,7 mmm max. oe OO 5.4 mm max 5,3 mm min, ® ‘Acompression strain of 10 % shall be Wg8@ for hiardnesses above 90 IRHD@Phe height of the spsicer() shall be as follo Spacer dimer 14,30 mm 11,25 mm 5,10 mm mi 5,65 mm min. [NOTE Foe eytallization studies, in order to aciove the Meter aftompreeion needed tomeet the permitted tolerances SERA Ficeehetene threo ots of acer for type A and four sate Granacer for trp Have required, For inate, spacers of Peeps am o.38 minand 9.02 mm for type Aand apacernot {fa cm, Ae? ma, 478 om and 480 rm forte Ball pei taoee oF 0,00 an, would cover the eange adequately Where a range of spacers is not available, the use of slip gauges is recommended to obtain the correct ‘compressed height. Care shall be taken that, with ‘The tast niece in ite compressed state, the jiece type 4.1.4 Clamping device, For testing at standard or elevated temperatures, a simplp screw device is adequate. For testing at low temperatures, a quick-release device is required. ‘This may be either mechanical or pneymatic. 4.2 Oven or low-temperature cabinet, with the requirements specified capable of maintaining the and test pices at the test tempe! tolerance specified in 6.2. ‘The low-temperature abi refrigerated or may be Liquid nitrogen. 1 measured directly if ‘apparatus with an ‘The cabinet for low-telip ‘equipped so that itis possible to release the test mechanically by day ice or tare shail be pieces and jut subsequent measurements without ‘by use ofhand-holes and gloves or ditefiote: shall beveap: jaintaining its temperature will iasible variation while these c agg being carried out. vach a steady-state temperature depeiig on the type of oven or cabinet and the heat fall the compression apparatus. To obtain rable results in the cage of an elevated test temperature and a 24h duration of test, itis necessary to reach the steady-state temperature ‘within the specified tolerances in the interior of the test pieces at least after 3h. 4.3 Pair of tongs, for handling the test pieces. 4.4 Micrometer dial gauge (to measure the thickness of the test piece), having a flat cirewlar foot of 4 mm to 10 mm in diameter and a flat solid base plate (seo ISO 4648:1991, method A) exerting a pressure of 22 kPa +5 kPa, It shall be suitable for tise at the required test temperature and shall be ‘calibrated for measurements at that temperature, For comparative purposes, the same dimensions of the circular foot shall be used. 4.5 Timing device, with a precision of + 0.28 or + 1%, whichover is the less preciee. teISO 815:1991(0) Dimensions in mitinetres | BiRest pieces . “5a/Dimensions ‘The test pieces shall be one of two sizes, designated type Aand type 3. Ata pice shall be a eylindieal aise of 29 mms 0/5 mm and :12,5 mm £ 0,5 mm, teat pie shall boa eyliniealdise of (3 mm + 0,5 mm and 6.8m + 0,3 mm ‘© nst 02.1909 ‘¢ 1 Typical apparatus for the determination of compression set using type A test pleces ‘Those two types do not necessarily give the same values for compression set, and comparison of rosults obtained using test pieces of different sizes shall be avoided. ‘TYype‘A test pigcos are preferred for testing rubbers having lo ression cet, because of the ‘accuracy attainable using these larger test pieces. ‘Type B test pieces are proforred when itis required tocut test pieces from products. In this case, the test pieces shall be taken as near to the eentre of the product as possible, unless otherwise specifiedc) BSI jed Copy. 28, Uncontr 0/2008 O5:: Roma Roy, ISO EXCHANGE - INDIA, 29/ oy: Mrs. 180 815:1991(E) 5.2 Preparation 6.6 Conditioning, me test pisces shall be prepared by moulding each Samples ‘and test pieces shall be protected from he tet Pieverponsble. Preparation by euting light and hewt 's mutch as possible during the ise whenetty laminating not more than 3 discs is interval betwee ‘vuleanization and testins ‘permitted. Prepared test pieces shall be conditioned Cutting shall be performed in accordance with immediately before testing for a minim 180 4661-1) fof 3 hat one of the standard temperats ‘Laminated test pieces shall conform with the in 180 471. The same tempes Hamensions specified in 6.1 and shall be prepared by throughout any one testor series 0 jatninating dises or rubber cut from sheets without ‘be comparable ‘adhesives. Dises may be compressed by a few In the ease of erystallizat {ereent for Limin, eo that they stick vogether. "he ‘shall be decrystallized im Peretyarof des laminated to produce atest piece ty eal them in a um ited three. The total thickness shall ‘They shat then be ‘then be measured, temperature. ‘eat pieces propared by the different methods fs Teal ees pronase ive iferentremtisand 6 7OSE conditions Comparison of values sball be avoided. ‘NOTH Aienton i drawn to the asked effects af the degren NT rn nmpewnnion et vos nay be Reet #2 eof moulded test pce tobe repreventaiv of Tame nt hknessn of sets oF moulings e ‘When capping is a problem, the test piece shapescan Xe dmproved by cutting it in two stages: fret cut an esr at cea then tim i ote exact “Hor 72.8). Gimnsions with a second cutter , ac may used when stag ‘The use of test pi .ces prepared by laminating lization or plasticizer migration at specil The toca for contol of fiuebe products shall be test Yemperatures agreed between interested part a Teenperacare often 5.3 Measuremont of thickness | ‘The temperatures of test shall he one ofthe ‘The thickness shall be measured at degen Randal temperatures 23 °C+2*C or27 °C Porton ofthe et pice to the nearest The amigo ari fr tein at aint temperate, Tesing the micrometer dial gauge 4 She of the following temperatutes for 54 Number Sevated:temperature or low-temperature tes eepdvsual ent pieces sal bengal For, Plavated temperatures Low temperati Taw temperature tests each fest piece inh be Pa “c tested ina soparats clamp device (6-1-0. eet ni yum time between O41 aha eon a cd ei ig Ane ee sca eam cas ee a ‘evaluations intended to ‘comparable, the tests, 5 12542 bars craton ee efor thee 1042 Epo ‘imeinterval. + 11542 = 10042 For product tests, whenever possible, the time me ‘between vulcanization and testing shall not 2002 er 2 months ofthe date of receipt ofthe product 250 +2 by the purchaser (see ISO 1826).Special care shall be taken in interpreting reeults obtained at elevated temperatures. As oven temperatures are increased, the results become inereasingly dependent upon the thermal stability of the vuleanizate. At still higher temperatures, surface oxidation of the test piece makes a significant contribution to the observed compression set. There is no simple correlation between the compression set observed at elevated temperatures and that observed at room temperature 7 Procedure 71 Proparation of compression apparatus With the compression apparatus (4.1) at standard temperature carefully clean the operating surfaces Apply a thin coating of lubricant tothe faces ofthe compression plates (4.1.1) that will come into ntact with the test pivoes, The lubricant used Shall have no substantial nction on the rubber during the test and it shall be described inthe test report (oe clause 10). NOTES For meet parent icons or foooaicone vie elisa deny of hon ae tonded tupritre wv cate bent Iffor any reason a lubricant is not used, this | ita i mentioned in the test report or the prod Secifieation 72 Thickness measurement Measure the thickness inthe centhof each test piece to the nearest 0,01 mm. es ah 7.3 Applying the compression’ y Blac the test osha ‘Hepa of plates together with ihe gee I 33)" “avoiding contact Fe ee En Reece henes the elamping device (4:1) o thht the platos are dean togethor usiornly WHET they are i contact with the spacer( the applied compression shall be approximately 2b,% of the original thickness of the test piece, For hifi: hardnerses, the applied i ipproximately 15 % or 10 % taining the test pieces into the central fon or low-temperature cabinet (4.2) operating at the test temperature (see 6.2) 7.4 Terminating the test in the case of elevated , temperatures 7.6.1 Aftor the required tost duration (see 6.1), ‘remove the compression apparatus from the oven Immediately loosen the bolts and transfer the test pilgoos quickly to a wooden bench. Leave thom to recover at standard temperature for 30 min-+3 min, and then measure their thickness. ISO 815:1991(E) 7.6.2 An alternative method of cooling may be used, in which the whole compression sot assembly is cooled to standard temperature within 30 min to 120 min, the test pieces are released, and after a further 30 min +3 min the a ismeasured. If this cooling method is used, ft shall be clearly stated in the test rehort. 16 Terminatingthe @athe case oftow temperature * 7.6.1 After the refged WBituratlon, release the as possible and 7.6.2 Insi 4, measure the thickness of the central portion of the test piece, to the nearest 0 ¢ time intervals beginning as 1 mm, {avy tag er loge ef he cei dovice and ending after 2, which makesit possible hickness against the logarithm of time (0/403, 1 min, 3 min, 10 min, 30 min and 2h are esti). Test pieces shall alwaysbe handled with Mans (4.3). After 2, remove the st piece rom fae inet. Internal examination ‘ut the test pieces into two pieces along a diameter; ‘Jo ifany internal defects, such aa gas bubbles, are Say) Hou tiscard the tessa 8 Expression of results 8.1 The compression set C, expressed as a percentage of the initial compression, is given by the formula hig hy Tiga, 1? where hg is the initial thickness, in millimetres, of the test piece, ‘Ay isthe thickness, in millimotres, ofthe test piece after recovery; hg is the height, in millimetres, of the spacer Report the result to the nearest 1% 8.2.No individual test result shall vary from the numerical value of the median compression set by tiore than 2 % or by more than 1/10th of the mean, whichever is higher. Ifit does, three more test pieces shall be tested and the median value of all results shall be reported, together with the number of test pieces tested, ‘pHsi 02-1999Fintho eae oflow-temperature testing, results 9.2.0 A type 1 precision was menmurad inthe TP- M crented foreach test piece by plotting on The time period for repentability and reaver with semilogarithmic scales, with the reproducibility is on a seale of dave {otal of 19 re searthiaicabscisea and the thickness laboratories participated in the 100 7 wor helnoar dinate. In tho Une range atthe and 12 labors orien participated sn the,~ 25°C test. process, en approximately straight Kine aca Fesult in most eases, which permits the 1.4 FeeeiRion Feiss ete ce valve ster eny desired °..1 The precision reels test Perey cearcatoaterooriersctioct tice sasiinte gen at jon set ) or by interpolation. (i00andin Table for come Teompression set values arecalculated — 9g s st 4 9.3.2 The precision result ary periods of 30 s and 30 min. a testing are given in Annes cision 9.3.3 The eymbols r, cof reaults, are defing sneral ion calculations to express repeatability odueibility were performed in accordance yMR. 9272. Consult this for precision wand nomenclature. Annex A gives ‘oh the use of repeatability and repeatability, speatability, in Bl 14 An interlaboratory test programme (TP) was din 1986 by the Laboratoire de Recherche ide Controle du Caoutchoue et des Plastiques E 7 {COP), Three materials (vuleanized rubber full description ofthe sample and te ‘were used: A = SBR, B = NBR, wate Test pieces wore distributed to all, 2) compound and eure details, where ‘and tested at 100°C and at— appropriate, '8) the method of preparation of test pieces from amples, for example whether moulded or cut; by test method: 1) a full reference to the test method used, ive. the number ofthis International Standard, Dy the typeof eat piece wed, Le, Aor Band 2 ettlon notic wae nminated, tne andthe 5) she nature of the lubricant, ‘Dwther dhe ast picea were ested seperately or a0 45 4 Q hat ) test details: lon cf roo tet Ith Iboratary temperature, di ‘Amedian compression 2) the temperature and time of conditioning si rer oe me : tbe compression 100, he cmon ye drain an temperate oe 3) chedigmoter of the ciel micrometer fot, fine at room temperature after removal from the snparatus. 6) details of any procedures not specified in p26 For testing at—26°C, thecompression etwas tH “international Standard; Fae ree{ 30 sand 30 min afer removal ofthe test d) tet resul rece from the apparatus, while the test piece was Ip the number of test pieces used, pee 28°°- 2 the iitial thickens hg of the test pieces, required,ISO 815:1991(E) recovery, if required, and, if required, the in 8) the thickness h, of the test pieces after 4 the median value of the comprescion sot idual test results, ‘Table 1—Type 1 preci 5) in the case of low-temperature tests, a graphical prosentation; ©) the date of the test. jon for compression set at = ‘Material Average ae o 4 c 103 2a » Pah 2 198 33 " A aa ar Fock vatons ee cy a6 38 [Type B test piece at 30 min ar c us 33 Fs as so B 24,4 - a7 32 A 449 hf M40 3 Pele values 30 | yaa 00-3 Tale Type 1 preidlogtrBompresin et at 286 Sat wins Tae Hasectl o ® ” ype A tet piece a0 308 A 133 so 16 c | 33 40 59 fl 108 wt 16 Poole values ee ee Type B test pioce ak 30 A , a 24 69 c Raye 6 B i 65 23 90 Proled values’ far =e Type A tam pte ab'S0 min q , 94 46 25 120 5 16,6 a 150 Me, 72 60 120 Pooled values 118 30.2 a5 140" Type B test piece at 30 min a A as a Py 120 B 116 30 8 170 © 6 26 we 140 Pooled values 08 a se [oo ‘onstce.1999‘Annex A Gnformative) Guidance for using precision results [AA The general procedure for Ware precision A Fula is a8 follows, with the ‘symbol |21~ ¥21 reat ing 2 postive difference oe two desigrtement values (Le. without regard to sign). tag Enter the appronriate Precio table (for As iever test parameter is Deve considered) at a hate walue (of the measured ‘parameter) nearest averatent” data average under Nronsideration. This tothe eve the applicable ™ (> "Rox (R) for use im the decision Proce hs with these rand ales following Aral repeatability statement ‘may be tsed t© take decisions: iat For an absolute different ‘The A race =, #2) between tn ee (value) St ena identical materi rect operation of the fest procedure, will test eabilty ron average not More ‘than once im twenty case. ih 3.2 For a percentage diferent, between two teat (value) averaees: Ty sa en 22/8) * 100 vpetwvcon two test values: found om nominally a cal material amples nee ‘nornval an Soa ie are Oe) Than once in twenty case ‘he percentage diflerence, a, ia ins Raa ae, aca wich mete ma teoke deisons make de atl lesen: Te Ad Foran ab cneen ee aiteeured tt and IAW Mea og ee orgect bons re on nomnl , vest R ) peoeeyoe, wil exceed the tabula farore than once in tWen} (AA Bor a percentage test (value) averaees The in-air) a8 ent ‘oravories using normal av carrect test PrOoceataeR® srominally identical sraterial samples, wil ulated petween two indepe reproduc yer ‘not mi ercbetween two sntage difference werages, found itAnnex B (informative) ISO 815:1991(E) Type 1 precision results for compression set at - 25 °C and 100°C without lubricant “Material Average. Senay j 4 romarIacnTTA'E Type A test piece at 30 min [Tope B test picce at $0 min Paar TT Type A test piece at 308 Type B test piece at 305 ne A 19,3 145 754 21,8 3 E Meine (oe eae \Type B test piééaat 30 min esBs ©) 80 Chiswick igh Roma Mendon wa aat, BSI — British Standards Institution ‘sts the independent national body responsible for preparer British Standards. 1 er i the Li sie on standards in rope and athe Fateritional level. Itis Freorporated by Royal Charter. 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