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151 1201-1978 wes 120-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS ( First Revision ) Bitumen and Tar Product. Sectional Committee, BCDC 2 Chsimen Rapresting nor C. G. Swaumnara Cental Road Research Tastiute (CSIR), New ‘Bat Monte Sug. Gounass (Alero Swaminathan Sum NCA. Dt.X. Atruomo,” Hindgrtan Petroleum Corporation Ltd (Refinery ‘Division Bombay Suga. Maron ( Alurnate) Por G:M. ANAYAN Highways, & Rural Wor Department (PWD), SamA,K,Buartacuanvya National Tet House Caleutta Dnik.8. Bugrracaanyn Minbtey of Defence ( DCL) Shas. Ganovts (Alera) Cnr & Maracenon Ministry of Railways (RDSO) “Auranavy Grant & Maratconere Public Works Department, Punjab Roads Wing ( Menstry of Traayport) Aasaen Oi Co Le, Dighoi ‘Suman Cason (Alea) smn She ny Pee Coreraion Lt (Maing Har Soon Indio lena of Peon (CSIR ), De Dan SS Se aaa angle Ente MO seeomcia Chis Beach, Amy Headqucten seaatiy cana (Men) Suny R-R Baxons (Alemat) Marat Petrleum Corporation Lid (Marketing "Division ), Bombay (Contin on ose 2) (€ Copyri 1978 INDIAN STANDARDS INSTITUTION This publication is protected under the Indian Copyright 4:1 (XLV of 1957 ) and Teron whol or pW ay menace ih writen eran of he ‘ublaber thal be deemed tobe as infringement of copyright under the Said A 1S: 1201 -1978 to 151220 -1978 (Continued from page 1) Menbert Repesating Suet T. S. Kasmawurria Indian Oi Corporation Ltd (Refinery Division}, ‘Bombay, Sunt C, V. Rasswunsut( Allmete) Suet SB ous Tian Oi Corporation Ltd ( Marketing Division ), Bombay Sun Maseanin Panta Indian Roads Congres) ‘buat CG. Swaumarica ( Altra Suet MOR. Mata Tn Personal capacity, ( Cle Ganmen dia, Li, "Sammon Hlone, Veer Susatar "Surg, PB. No ‘STB Prebhedes, Bombay 400025 ) Sunt T. 5. Naver Ministry of Fetateu ‘Suna iP. Seanannanvan ( Almac) De AV. Rio ‘Nationa Buildings Organization Dak 'S, Rates (Alera) Resnmaxtanve Ministry of Defence (R&D Sr TK: Rov shale Tar Products ( 1895 ) Lid, Calcutta Shin: Dia Kn, Si General Pel Resear Lestiate (CSIR }, Dhanbad ‘Suat Anci Rawrt Cuoupntvny (dltnte Seaton” Sunvavon or Wonss Cental Public Works Department baz) ‘Sumenvon or Wonxs (DAZ) (Alurate) Swat St Sumstae ‘Drcetirate General of Supplies & Disposals Sm NSTiarnomsjan™”)—pharat_etrleum Corporation Lid (Ret nt NS Paswnaneajan i Peoteam ion foery 7 Divison), Bombay Sat. H. Sauna ( Alert) Swat Bs Ajrrna Say Director Genel, ISI ( Esafiio Mente) Dinecior (Civ Ene) Setar, Suny Jo. Mra Deputy Director ( Gir Engg )s ISI ‘Methods of Testing Tar and Bitumen Subcommittee, BCDC 2:2 Goneeer Paor C. G, Swauneariane Central Road Research Fomitute (CSIR ), New Dei Menbers, Por G.M. Axouvan Highways & Rural Works Department (PWD) "Tamil Nadw ShmJ.S. Base dia Insite of Ptcoleuin ( CSIR ), Debra Dux ‘Sine jc Nace at (Alternate) Sunt Ack Buarraciuava,” > National Test House, Caleutta “Sun K. D.Das ( Aleate) Snot G-C. Goseass ‘Amar Oil Co Ltd, Dighot ss Tam Crom ( Alea) Swat Bb. L. Raroon’ ‘aharat Petroleum Corporation rd (Refinery Bivslen), Bombay Suns C,H. Sana (Alene ae : 2 (Continued on page 3) 1S: 1201-1978 to 1S: 1220 -1978 ( Conia from poe 2) Mente Repeseing Baro H.K, Karoom Rngineerin-Chie's Branch, Army Headquarters a oto 7 ing of Opa (tt rae Suns M.R. Masa In peronal” capacity (Cle, Gammon India "Geno Hoe Vor Seti Mot FB. He Sia tote, Bian ots) Suma K.P, Noon ding "Gil \Gorporton Lad! (R&D Cente), Sunt G. Racuavexonan ‘Madras Refineries Liited, Matas ‘Sea Ve Vanowse (Alera Swau GV. Rawnawane “Hindustan, Petrsleum Corporation Lid. (Refinery Division) Bombay Sunt A.¥. Gurra (Alnat) Suu TK: Rov ‘Shalimar Tae Products (1995) Ld, Clsua Seignceiooe Excoan ‘Ministry of Transport and Shipping ( Roads Wing ) Is: Is: 1 1s: Is: Is: Is: 1s 18 1s 18 is Aeranpee A Ar 1: 121-1978 Dreruixarion or Waren Content (DEAN AND Srarx Merion ) e . +: 1212-1978 Deversunarion oF Loss on Hatin 1913-1978 Disrwiation Test... : : -1978 DeTuaMination oF MATTER Insoxvate 1 Benzene 1215-1978 Deverauation or Marrer INSOLUBLE iN TOLUENE 12161972 Demmmnarion or Souunusry aw Cannox Davi- 1217-1978 _Darzrutsation oF Miwerat Marran ( Ast) +S 12181978 Dereewmatton oF Puznots 1219-1978 Detexmxation or NAPHTHALENE $220-1978 Derensemazion oF Vouatiue Matren Conran ros SoreDuLes 4 201-1978 co 1280-1978, CONTENTS rao o 5 Suma nm 7 1202-1978. Devanumearin oF Spacirc Graviry and 208-1878 Duranuinario oF Peneraarion we 29 V204197@. Darsauinanox oF Resor or SepcxD Pact= mmuron Se os 1205-1978 Direnuanarion o¥ Sorrmano Pour “3 errr 1206 (Parr TE)-1978 Derenussation oF Viscosry: Paxr TL (Powe Kaur Vcore ee Paxr If1)-1978. Derenancariox oF Vicosry: Par IIL 1206 (Pan ountic Veen on e277 {12071978 DeremunaTion or Equivacous TaurenaroRe CEvT) Se 112081978 Derewamanion or Deomasry a {1205-1978 Devensmarion oF Fass Punt ano Foxe Pore 75 112104978. Fuoar Tesr a a7 137 Mi 45 1S: 1201 «1978 15:1220- 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS ( First Revision ) 0. FOREWORD 0.1 These Indian Standards ( First Revision ) were adopted by the Indian Standards Institution on 30 June 1978, after the drafts finalized by the Bitumen and Tar Products Sectional Committee had heen approved by the Civil Engineering Division Council. 0.2 A series of published Indian Standards cover tar, bitumen and bituminous materials. These standards require, amongst other require- ments, detailed testing of each of these products. At one stage, the vatious methods of tests relating to each product were included in che same standard. Since these specifications were prepared over a period of time, the methods of tests, prescribed for the determination of similar properties varied in procedure and equipment from one standard to another. Tt was, therefore, felt necessary to prepare a standard compilation of methods of test for tar and bitumen to simplify these test procedures and to pres. cribe, as far as possible, the same standard equipment for determining similar properties. 0.3 This seria of standards om snethods of tests was fit published i 1958, “However, during the course of tha period a number ofimprove: ‘ments have since been made in carrying out ef these methods of tex and accordingly, the compliation of methods of tet is now being reved to Bring pide” dications haven parcular provisions of repeatability and reproducibility limits specified under each test. Also, under methods of texts for determining the vicosty require, ments (IS 1206) additional methods of test have been includel Br the determination of absolute’ and kinematic viscosity under separate part ©4 The Sectional Comittee responsible for the preparation of these standards has taken into consideration the views of producers, consumers and cechnologists and has related the standard to the Inanuficering and irde_ pacers Tolowed athe county tn thie hell” Due weghage has “abo. been given to the need for international. co-ardimaton between standards prevaling in diferent countries of the world. Theae 5 1511201 - 1978 to 1S: 1220 - 1978 consierations have led the Sectional Committes to derive asistnce fom the standards and publentions of the following associations and committe Standardization of Tar Products Tests Committee, London Inmate of Petroleum, United Kingdom American Society for Testing Materials, Philadelphia 0.5 While preparing this compilation of methods af tests, simplification in the range and type of thermometer, condensers and’ receivers ued in ‘avious texts has Been kopt in view. "Accordingly, the committer hopes {hat this simplifcaton wa help the laboratories fo cqulp themselves with 2 complete range of apparatat for fstng tar and bitumen. Asa guide to ae Uborstones lata apparain rogue fo tating far and tame fieording to these standards nas been provided in Appendix A at the end. ‘The thermometer specified in this compilation are identifed in terms of designations according tothe Insitute of Petroleum or Amecian Society for Testing Materials and hence their equivalent 1P and ASTM desig- ratios are aio gen inthe Appendix. Correponding equivalent Indian Standard designtions covering there thermometers are also indicated. Te ESHoweves, important to note tht all thermometers used in thse tests olla s"Coninniey create fom she Nanal Pysal Labora: tory of India or any other institution authorized by the Government of India to sue such corticates 06 In reporting the rll ofa test or analysis made in accordance with these standards if the fal valu, observed or calculated isto be rounded Off ie shall be done in accordance with 1S: 21960". “Riles for rounding off rumerical values (ried). 6 ‘1S: 1201-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: SAMPLING ( First Revision ) 1. SCOPE, 1.1 This standard covers methods of sampling bitumen and tituminous Reta a their quid semisolid or sold sates supplied in any of the ) Cans or small containers, drums, barrels and bags; 'b) Solid materials in loose form; ¢) Rail tank wagon and road tank trucks/lorries; and, 4) Bulk storage tanks and other types of bulk storage. Nove —‘The provbionof this tadard shall applicable to bun emulin toy subject tomodieadon ies nthe relevant andar eis 2, PURPOSE. OF SAMPLING 2 Som hth a et vortions for visual and laboratory examination or for preservation for Fecord. The examination may be made to determine: -" Preservation fe a) the average quali of the material in the lot, b) the extent of variation ing quality, in the different portic she eaten of i quality inthe diferent portions ofthe ) conformity to the specified requirements, 3. TERMINOLOGY 3.0 For the purpose of this standard the following definitions shall aoply, $d Let The quantity of material of th tame composition fixed for inspec time, "Alot may cont of the whole or part of the 7 1S: 1201-1978, BAA. Formation of Lots 42) The lot shall be formed before sampling is undertakens 3b) The basic principle in forming the lots thatthe material in the lot » Tl be 2 homogeneous atoaible wih regard’ the quality Characters speelied; and ©) Care shall be taken to see that the material in a single lot comes from the same source/batch of manufacture ard as far a8 posible ‘fom raw material of identical origin. 3.2 Top Sample — A top sample is one taken at a level of one-sixth of the depth of the material below the top surface and in the centre of the container. 33 Middle Sample — A middle sample is me taken at a level of one- hhalf of the depti. of the material below the top surface in the centre of the ‘container. 3.4 Lower Sa A lower sample is one taken at a level of five-siths fof the depth of material below the top surface in the centre of the Nove ln th case of Boronia lind tanks ad ans of cma shape ‘top middie’ and lower" sample taken at levels corresponding to one-sixth, one halt td tivesiath of the depth of product in the tank are not representative,” In such ‘reumstancay samples shall be taken at levee Correrpending fone, ope a Sd Brealabs of tat volume. : : ‘ewe of cone-vofed tanks the sample may be drawn from as near eae er 3, Aveoce Samle A ous seas of posite ape se at cia oe pase caecum ay aa Sect seme seen te pane SF oer aS niece ar a cena nee ee ein ren ke ene ata eres, uly mad op by. coming eee eee oe eee tee $4 Samer Serif spot me oni by coming eee nate etanee eres tte sampled, pe ye See once CORTE te $2 all Level Semple Ths orn ty bron cod anoles cog pant sz rete pon cote drwcof Fel opening har sean acorn atch ae ey, bn ea 15: 1201 - 1978 4. SAMPLING APPARATUS 4.1 Bitumen Sampler — A strong metal vessel of about half litre capa city, the handle of which shall be attached by a means not adverse jected by hot bitumen (ste Fig. 1). 4.2 Sampling Thief or Tube Method — The sampling thief or tub: shall be either of glass or metal, to reach to within 3 mm of the bustom ¢ ‘the vessel and having a capacity of approximately half or one titre. 7 metal tube suitable for sampling 250 litre drums is illustrated in Fig. £ ‘The rings shall be soldered to opposite sides of the tube at the upper en: for convenience in holding it. “oe at {Alt dimensions in milimetes. Fie. 2. Sawrumo Tose Fro. 1 Brrumex Samper 15; 1201-1978 4.3 Ship Auger —of such diameter and length at to permit a core of fanvenien’ sg oe takon throughout the depth ofthe package of cake St illustrated in Fig. 3. - - Lae DRA Fic. Sup Avorn 4.4 Sampling Scoop — of such dimensions as to enable a core of conve- nent size to be taken throughout the depth of the package (see Fig. #). HAMMER HEAD FOR DRIVING WTO BARRELS, ‘moooUN “NS hanoce 22mmDIA Fro. 4 Sauetine Scoor 4.5 Knife or Spatula — provided with a strong, broad steel blade for use ‘with materials which are soft. 4.6 Hammer and Chisel — of any convenient size for use with samples which are hard enough to shatter. {$2 Rotel Sampler — mde of metal wih = handle and stopper (1 5). ssnall-mouth cans with cork ‘ease they shall be wide-mouth glass jars or bottles. samples of semi-solid and solid materials shal be friction-top cans. 10 1813201 -1978 os ‘i | noe meen + 22 oot [Nove—A tolerance of 18 percent i allowable on dimension in limetrr Fio, 5 Borrue Sauruzn ron Tank Cans 1811201 - 1978 1S 7h enc cone oe at a BT aan ea en gat peop EE Retr 6. SIZE OF SAMPLES 1 The sae ofp to be taken for eng shall be as lows 8) Liga Mail 1) From smal container, cans, drum and bares —~one lite fr each separate sample. Bree 2) From bul storage tanks and drums-—5 lise. °) Sami on Slit Maes 1) From barely, drums, cakes and powdered materi in bags — | to 2 kg for each separate sample. “a Geen 2) From blk minim of 5g compote or average sample 7, PROCEDURE AND SCALE OF SAMPLING s or Small Containers, Barrels, Drums and Bags Matrils—The number of packages to be sleted for sampling ftom the fot sal be in accordance! with fat I'and 2 of Fab, ‘The'sample packages shal be teleced at random, TABLE 1 SCALE OF SAMPLING (Clowes 7.11 end 71.2) No. or Coma a Snot Sora! Bo, Comune ‘ron Sue 1 1 2 15 2 6, 50 7 sly, 150 5 151 5 500 8 £01 ad above 8 TAA Gonpae aap Foe ah ty pags a Fe sampled tian ho esas etd i ie andar Seperate ca iii peacenne inher gen A 2 Te Tin] oar a cena pepe hs ly pe 18: 1201-1978 ackages shall be thoroughly mixed together and then the requisite Pecntky. far testing. shal be withdrawn. This shall be the cempoaite Rrple” An dential compote sample i required may ao be made oe arBing a reference sample under the joint seals of the purchaser and the {eller Ifthe composite sample passes in respect ofall the requirements of the specication, the bt may be considered to be in conformity to the requirements of the specification. 7.12. A sampling tube of convenient size shall be lowered into the package so that it touches the bottom, and a sample obtained by closing The top end of the tube with the thumb and withdrawing the tube, If the tube contains free water its contents shall be rejected and the tube again lowered into the package to such depth as to avoid the watt. ‘The tube shall then be withdrawn as before and its contents used to rinse the tube ‘and sample container and then discarded. The tube shall next be lowered Slowly as far as possible into the contents of the drum or can, without touching the water layer, if present, ‘The tube shall then be closed and withdrawn and the sample allowed to flow gently and without splashing {nto a sample container. 74.2 Semisoid or Solid Materials —The number of packaga to be selected for sampling from the lot shall be in accordance with col 1 and 2 ‘of Table 1. ‘The sample packages shall be selected at random. 7.A2A From each of the sample packages from the lot appropriate quantity shal be taken. For thi purpose an appropriate sampling syparat, Ei or device may be used which may involve use of hammer, chisel, knife or spatula, auger or a scoop. Ifthe material is held in small containers swith bung-bele too small to ineroduce the thie, the contents of the Sontaincr shail be mixed thoroughly by shaking and the requisite quastity SFsample shall be poured owt. Care shall be taken to ensure shat from tach container the material faken is fully representative and. preportional fo it contents. The material so taken from each of the sample containers Shall be tuoroughly mixed together or melted together if necessary to form @ combined ase of material rom which a slab ample for teing shall etaken, ‘This shall be called the composite sample. requiree a similar Componite sample may be taken for purpose of preservation for reference finder the joint seals of purchaser and the eller. ‘The composi sample Shall be required to past all the specified requirements in order ‘0 declare 2 lot to be ia conformity to the requirements ofthis specification. 7.2 From Rail Tank Wagon and Road Tank Tracks/Lorries 7.2.1 A careful obrervation of the condition of the material in regard to the presence of foam, sediment, or free water on top or at the bottom of the Material in the wagonjtruck sbal be made immeGately before saropl- ing, and, if such extraneous materials are present in measurable quantities 13 15: 1201-1978 their voiume shall be estimated and samples of each shall be taken and properly labelled. If possible, the foreign materials shall be removed and discarded before sampling. 72.2 Liquid bituminous materials shall, if practicable, be sampled before heating, but if heating w necesary, a no te shall he temperature exceed that required. for satisfactory’ sampling. Semsolid 6 sol Shtuminovs matetials shall be rendered fuld by heating. 7.2.3 When possible, thoroughly mix the material to be sampled by circulating for several hours before samples are taken. Collect the sample from the draw-off cock at the bottom of the tank in the bitumen sampler. When it is not posible to mix the contents of the tank, of when itis dcsired to ascertain if the contents of the tank are uniform, take samples by means of a bottle sampler by the method described in 7.3.1. Close the sample container immediately. 7.24 From each tank wagon/truck the requisite quantity of material shall be taken to. constitute the composite sample for testing. If the ‘composite sample is found to pass all the tests, the material in the tank ‘wagon [truck shall he covfsdered to be in conformity to the requirement of theipeication. If required an identical composite sample may be taken for reference. 73 From Balk Storage TSA Liquid Materials and Moterials Made Liguid by Heating —The inlet ‘and outlet to the storage tank shall be closed and a S-litre sample drawn from the top, middle and bottom contents. The sample may be. taken from drain cocks on the side of the tank if such are available, with the help of a sampler illustrated in Fig. 1 and when so taken, enough material shall bbe allowed to flow through the drain cocks and’ discarded to ensure a reprentative sample from the contents of the tank. | Otherwise samples may be taken by lowering into the material a suitable botde sampler, a ‘atisfuctory type of which is iustrated in Fig. 5. ‘The bottle or can shall be fitted with a stopper which shall be removed by a string or wire attac ed toit after it has been lowered to the proper depth. ‘The three samples, rom bulk storage may be tested separately for consistency in order (0 detect stratification. They may then be combined, thoroughly, mixed, fand a S-litre sample taken therefrom for other tests that may be required for determining average characteristics of the material. 7.3.2 Solid Materials in Loae Form — Mix the piece representing the total quantity on a clean hard aurface and proceed a follows: Place the broken down samples on a clean impervious surface, mix by shovelling and heap into a cone by depositing separate small quantities one fon top of the other, the cone being formed symmetrically throughout, with 4 1: 1201-1978 ee ipsa team wra ing erat, hr heat a fee ng hr, inde aout SU Gane Super ame in etic ponion thee of he cone ad sabe Cow tral geen a Sone i i aon the sabre fe om om edo ea eit, Form aoe coo eee ins solr wate ei a by pag i 8 at eats ppeiity antes a ot Bee Blethen cmon ong cage Nel pep peters ek rede peas Speen cr: ad argh ang torachate ay Rene Fir fone ae comply and et tel he oo remaing urge oro, eee Suk by fore guar ipa aera repay a a TO TT al ee ite 2B Sem eh a ire ee he somnatn mle S, Aeccmae selena pest te pera 8. PRECAUTIONS ee 1 nn, he etc! cmt on 82 ennng Scam ear peers ch sal be cher wk pole eepe peda nee arpa Soebroto Saleen 2p al nee int may be eee em epee Ren eer SEA spelen mail the than ato bean and tal ot bec or camp By yaoran of oe Cone Semone be poe a oil ge sal akan emt pe Se emp epryeeepnpon, Poy sling prac rte coor hr nea get Serer alte go " ) eae ee Tegner all dan aed dean oo SOROS GPRS tena sca ate Seca gr mater ted digs ed Sine ing oh samatng peat a tl bs nad age cg cE eo Ta EY cee Ang ing cod Fong ee a? eam Hes ele or by 18 1811201 - 1978 4) Daring sampling operations, the material being sampled shall be : Protected as Tatas pos ile from the effects of wind and weather, id the sample containers shall be closed immediatly ater the ample has been taken. ) The operator engaged in sampling shall have clean hands fre ftom ) Thy atonal (tiles ite the atteril Beng sampled). Clean gloves may be worn, but only when ‘cwental to. protect the Sperator fm some health ot other hazard. f) Liguid) materials in tanks and_othor bulk containers shall be Sampled by the appropriate mit! od described in this standard The sample shal’ Ye draws thgough dip hatches, manhole of ther opening giving direct and anconfined acces tothe bulk of Tiguia.” Sample alall not be drawn fom dip-pipes ot other fittings nor shall gauge gases or drain Stings be twed for sampl- ing purpones except where 4 special. ¢) The depth of any fee water shall be determined before sampling operations are commenced, to ens that no free water b included inthe sample 1) Tehore is any reason to suapeet that « sample ora set of samples ) Fray not be ely rpresentaives further sample or ae of amplt Seall’be taken’ “The necesity for taking second o ‘check Semple, or set ofsampley i frequendy duc ether to fallre. oF to Eyeing he prviuon of len apparatn gay Simplified i separate sampling apparatus, sample containers, a Sher equipment are retved and Kept soparate for difrent ‘lasses of products, whe the pobity of crror ia labelling may be" argely liminaiedif'eachtample i clearly marked. before the ext sample taken. All metal tampling gea shall be made of on-spark generating material Glass stoppers shall be ground to the neck of the Body. aps of cans shall be fied with washers of cork ot other Sng material Corks and voppers tall be ted or wired on 1) Rubber stoppers and corks shall not be used for closing any ves Containing samples of tar and bitu-nen- 1m) Care shall be taken to see that nothing in the mmpling procedure fends to contamination ofthe stock, fot example, by drt or other fntrancous matter picked up. by'a wet Dung” by fragments of or by other foreign matter and the sample-continers are portesty clean and dry beore filing 1) Ieis adviable to take more than one set of samples for check Purposes in cae of dapute, leakage or brealage in transit or for [ny other reatons ») Every posible precaution against fie hazard shall be taken when tampling famutable materia like cutback bicumen, et i 1S: 1201-1978 9. LABELLING, PACKING AND STORAGE OF SAMPLES AND. SAMPLE CONTAINERS. 9.1 Labelling — Sample containers shall bs labelled; gummed labels may be ured on gla surfers, but in general wird on label sual be Fabs saltbe pormaseny marked ia penel sword aie presre 3c exerted wo indent the paper, The folowing information ia ered Inn he pape wing information Shall be 2) Sample eeference number; b) Place at which sample was drawn; 6) Date of sampling; 4) Initials or other identification mark of sampling officer; ©) Grade of materials £) Quantity represented by sample; 8, Tank No acageNo-(andype), nae ft ot deaths ype, of ‘container from which sample was drawn aad type of sample (top, middle average, ete); and the 4) The name ofthe manufacturer, i known. 9.11 The above details shall also be recorded in a book kept separatel for the purpose. ares 9.2 Packing — Sample containers shall be sealed. properly w prevent tampering’ The ype of packing ued for samp which seer be transported depends largely on the means of conveyance. "Wooden ates oF strong. cardboard cartons are recommended for cans contain samples, “The space round the sample container shall be led wi material, uch a sew, dts when sch materials are used, the con oF stopper covered with’ a paper or viscose cap in order to prevent contamination of the sample on opening, oe 9.3 Storage — Samples of materials which may be affected by light or hea shall be stored ina cool, dark place, porioical amination shal be made leakage. 1b: 1202-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF SPECIFIC GRAVITY (First Revision) 1. SCOPE LA This standard covers the methods for the determination of specific gravity of asphalt, bitumen, bituminous products, road tar, coal tar, coal {ar pitch, creosote and anthracene oil, 2, TERMINOLOGY 2.0 For the purpose of this standard, the followng definition and those ‘sven in IS: 834-1965 shall apply. 2.1 Specific Gravity—{The ratio of the mass of a given volume of the psu to the" of an equal volume of water, the temperature of Doth being specie 2A If the temperature of the substance is /, and that of water is fg the specific gravity S, is denoted by St/ty;t, and fy shall be specified clearly. 21.2 The specific gravity of bitumens, fuxed native asphalt, road tars, coal tar pitch and blown bitumen shall be determined at 27°C and that of reatote ‘oil and anthracene coil at 38°C. and shall be exprested as specific. gravity 27°C/27°C or 38°C/38°C. 3. METHOD A ( PYKNOMETER METHOD) 341 This method covers the determination of specific gravity for semic solid bitumen road tars and ereotote and anthracene ei 3.2 Apparatus — Specific gravity bottles of $0 ml capacity shall be used. ‘One of the two types of specific gravity bottles, namely (a) the ordinary gpalagy pe pee gravy bse wid’a nec o'6 mim diameter (1 TA) a 1¢ wide-mouthed capillary type specific gravity bottle (Jee Fig, 1B) with a neck of 25 mm diameter shall be used. Glenary of eras eating to Bitumen and tar (aid), is \ & Fro. IA. Oxpnany 0,18. Wom-Movniao Gaonaany Ten aratany Were care GRAVITY cine GRavirY Seem oma ede wt Tes stay seed eet ue al bee ay Heat ll Ba otra we! 3.2.2 Constant Temperature Bath— A water bath having a depth greater than that of Pyknometer capable of being maintained within 0'2°C of the desired temperature. 3.23 Bath Thermemster — It shall conform to tne following requirements: Characteristic Requirement Range ow aC Graduations ore Immersi 65 mm Overall length 340 + 10 mm Stem diameter 55 t080 mm Bulb length 10 to 16 mm Bulb diameter Not larger than stem diameter Length of graduated portion 150 to 190 mm Longer lines at each 1°Gand °C Figured at each sc Scale + 026 33 Procedure — Cle and weigh the specie gravity botle to- Ser oeat the stoppet (Wh. Fil With frehly bled and. cooled Sized water and inert dhe stopper Gry. Keep the beetle up t0 its 20 neck for not lets than half an hour ina beaker of distilled water maintan- tdvava temperature of 27-04 O1°G or any other temperature at which specite gravity ls to be detained; wipe All surplus toitare fom the Trace with a clean, dry cloth and. weigh again (0). Alter weighing the bowte and water together (b) the bot shall be deed aga. 3.31 In the case of solide and seminolids, bring a amall amount of the material fo-4 fd condition by gentle spplicauon cf heat, care being {aken to prevent lom by evaporation. Wien the material ‘a auficienty uid, pour a quantity info the clean, dry speciic gravity bottle mentioned a3. toll at least hall” Slightly warm the bottle belore filing. Keep the material away from touching the sides above the final level of the botde and avoid the inclasion of ar bubbles, “The use of a smal funnel wil prevent contamination ofthe neck of the bottle. To permit excape of Entangled sir bubbles, allow the partly filled bore to stand for half an four ata mutable temperature, then cool tothe specified femperatire and ‘weigh with the stopper (6) 3.3.2 Fil the specific gravity botle containing the asphalt with freshly boiled tilled water placing the stopper loosely nthe specine gravity botde. “Do not allow any air bubble to remain in the specie gravity Bote Pls the more gravity bt in the waterbath and pri he stopper firmly in place. Allow the specific gravity bore to remain ia the water bath fora period of not les than 80 minut, "Remove the specie gravity bottle from the water bath, wipe all surplus moisture from the Seface with a clean dry cloth and wegh ic along withthe stopper. 4323 In te cae of igus ach econ and anthracene i the tle up to the brim and inser the stopper firmly." Keep the filled for not les than hal-an hour ins beaker of dialed water maintained at a temperature of 27-0 + 0°1°C, remove the bottle from the beaker, wipe ailsurps water ffom the muface with a clean, dry cloth and weigh aga. 2.4 Calealatlon —Calelate the specie graviey of the material at ) Specific gravity (solids and semiolids} ») Specific gravity a Bah oie where ‘@.= mass of the specific gravity bottle, b= mam of the specific gravity bottle filled with distilled water, ‘¢m mass of the specific gravity bottle about half filled with the material, a 1811202 - 1978 d= mass of the specific gravity bottle about half filled with the material and the feat with distilled water, and ¢ = mass of the specific gravity bottle completely filled with the material. 3.5 Report — Results ofthe test shall be expressed aa the ratio of mass of 2 given volume of the material at a temporature specified under 2.1.2 to the mas of the same volume of water at the same temperature. 3.6 Precision — With samples which are neither very volatile nor very viscous and using a pyknometer of at least 25 ml capacity, the results of duplicate tests should not differ by the following: Repeatability Reproducibility 0.002 9-005, 3.7 Precantions — When making the specific gravity determination, it is important that: 4) only freshly boited and cooted distilled water shall be used; ) at no time of weighing shall the temperature of the apparatus be » Showed vo exceed te apethed tempers pe 6) precautions shall be taken to prevent expansion and overflow of fhe contents resulting from the heat of the hand when wiping the surface of the apparatus, 4) all air bubbles shall be eliminated in filling the apparatus and inserting the stopper; ©) weighing ahall be done quickly after fling the apparatus and hal be accurate to Ol mg; and £) to prevent breakage of the apparatus when cleaning aftor a deter- ination has been made pon a very viscous of semitolid Inaterial, its advisable to warm it in an oven at a temperature hot above 100°C, until mort of the material is poured out nd thea to avab it with a piece of soft cloth or cotton waste. When fool, t may be finally rinsed with caibon disulphide, benzol or ther solvent and wiped clean. 4, METHOD B (BALANCE METHOD ) 4.1 This balance method of test is intended for the determination of the specific gravity of all bituminous materials sufficiently solid to be handled in fragments. 42 Apparatus 42.1 Balance Analytical 4.2.2 Thermometer —as given in Method A. 2 4.23 Balance Swaddle — A pan straddle of con beaker and permit determination of the weight (ae Fig. 2 Fig. 2 AxavyricaL, BaLaNor Equirren wir!) 4.24 Thread — A length of fine, waxed, silk thread, 4:25 Brass Mads ~ cubical, messing approximal® cage 43 Test Specimen — The test specimen shall be a off eauring Sppronnatcy 30 maton each elge, "Trop Toking seal oamgle ctthemnsal by gesle app Ing ete to preven los by evaporation, Sd pote suiciently tid into a 20/mm brast cubical mould tf Oe ee ee pene ems er bubbles. The hot material should slightly more thé, fle tnoulds and when col the excess Say be oo Remove te spornen fom the mod wie cota So 44 Procedure — Tare the balance frst witha pico” Sind salient long to rach fon he hoa on ee 23 35:1202- 1978 fo the rest. Attach the test specimen to the thread, 40 as to be suspended about 25 mm above the straddle from the hook on the pan support, and weigh to the nearcat O'l mg. Weigh the specimen, still suspended by thread, and completely immersed in freshly boiled and cooled distilled water at 27°0 + 0'I°C, to the nearest 0-1 mg, adhering air bubbles being first removed with a fine wire. 45 Galeatation— Calculate the specific gravity of the material ax Specific gravity = where @= mass of the dry specimen, and ‘b= mass of the specimen when immersed in distilled water. 4.6 Report — Report the specific gravity to the nearest 0-001 at 27°C 27°C. "The buoyancy/correction in this case is negligible. 4.7 Precision — The duplicate results shall not differ by more than the following: Size of Sample Repeatability Reproducibility 5g or larger 0-005, 0-007 ey 18; 1203-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF PENETRATION ( First Revision ) 1. SCOPE 1.1 This standard covers the method for the determination of i of asphaltic bitumen and fluxed native asphalt and blown type bitumen. 2. TERMINOLOGY 2.0 For the purpose of this standard, the following definition and those given in IS: $34-1965* shall apply. 2. Penetration —The penetration of a bituminous material is the distance in tenths of a millimetre that a standard necdle will penetrate vertically into a sample of the material under standard conditions o temperature, load and time. 3. APPARATUS 3.1 Container —A metal or glass eylindrical, flat bottom container o cementially the following dimensions shall be used: For penetrations below 225: Diameter, mm 55 Internal depth, mm 35 For penetrations between 225 and 350: Diameter, mm 0 Internal depth, mm 6 3.2 Needle — A straight, highly polished, cylindrical, hard steel rod, wit ‘conical and parallel portions co-axial, having the shape, dimensions an 41811203 - 1978 tolerances given in Fig. 1. “The needle is provided with a shank approxie mmacly 9 mm in dlameter into which it's inmovahy Beet ERS oe ‘hall be symmetrical and the point shall be “blunted” by grinding aes truncated cone SS All dimensions in milimetes. Fro. 1 Nexoue vor Payeraarion Test 3.3, Water Bath —A water bath preferably with a thermostat maintained ting, alg Containing, not les than {0 litres of water, the: sanpls Poing immersed to a depth of not les than 100 mam irom the top aed ‘{ybported on a perforated shelf not less than 50 mm from the beens the bath, S44 Transfer Dish — A small dish or tray, provided with some means Bch ensure a firm bearing and prevent the rocking of the coneaiver ent ShENCR pactty a will ensure complete immersion f the contaiaee dares the test, 33 Penetration Apparatus —Any apparatus which will allow the rang tyhenetate without appreciable fiction, and which is accurate, calibrated to yield results in tenths of millimetee shall be adopted $4 Thermometer — It shall conform to the following requirements: Characteristic Requirement Range Oto4ec Graduations 2c Immersion 65 mm Overall length 540 + 10 mam Stem diameter 55 t080 mm Bulb length 10 t0 16 mm. Bulb diameter Not larger than stem diameter Length of graduated portion 150 to 190 mm Longer lines at each 1°C and 5°C Figured at each 5c Seale £020 on 817 Time Device — For, hand Cining eee sath a tse a ste ence my be sued poh Seorspowilon ora os janed fe prov! be cach 6 Tie iaeeoat tah beste ot Machel oe penetnees hat tated gear oe AMENDMENT j) a + 1203-1978 MET! 11ND BITUMINDDS ZR TE DETERMINATIODUS. WEE Firs) CFO Revista Page 25, clause 32, line 1 Jor hard ie. = Subsite 6 (eves) contact with its image reflected | sutubly placed source light. he suring 42.22 Unlow otherwise sec wei eel ale al A oad Weighs oie nea, carer and ving we = Srimposed (th "Methods fortes tar and bituminowy 18+ 1203-1978 4.2.3 Note the reading of the dial or bring the pointer to zero. Release the needle and adjust the points, if necessary to measure the distance penetrated. Make at least three determinations at points on the surface Of the sample not less than 10 mm apart and not less than 10 mm from the side of the dish. After each test, return the sample and transfer dish to the water bath, and wash the necdle clean with benzene and dry. In the case of material of penetration greater than 225, three determinations fon each of two identical text specimens using a separate needle for each determination shall be made, leaving the needle in. the sample on completion of each determination to avoid disturbance of the specimen. 5. REPORT 5.1 Express the depth of penetration of the needle in tenths of millimetre. 5.2 The value of penetration reported shall be the mean of not les than, tree determinations whove values do not differ by more than the amount siven below: Penetration Maximum Difference Oto 49 2 50 to 149 4 150 t0 249 6 250 and above a 6. PRECISION 6.1 The duplicate results should not differ by more than the following: Penetration Repeatability Reproducibility Below 50 1 Unit 4 Unite Above 50 3 percent of their 8 percent of their 17, PRECAUTIONS 74 UF the sample contains extraneous mater, it shouldbe sewed through TSisieve 90 {wr 18: 460-1962") 1.2 To avoid overheating at the bottom of the container ute of an air ‘ven or sand hath is recommended. notrating into the sample, if there is any ney that determination shal be dncardd. eves (rea. 28 1S: 1204-19: Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF RESIDUE OF SPECIFIED PENETRATION ( First Revision ) 1. SCOPE 1.1 This standard covers the method for the determination of residue specified penetration of cutback bitumens, 2. TERMINOLOGY 20 For the purpose of this standard, the following definition and thy given in 18: $34-1965* shall apply. 2.1 Residue of Specified Penetration —It is the percentage by m of a residue obtained by heating bituminous material to the requit ‘temperature and having a specified standard penetration value. Alternatively, the determination of residue of specified penetratior ‘made at two stages, one giving a penetration higher than 100 and other lower than 100, and the result is obtained by interpolation, 3. APPARATUS, 3.1 Container — A flat-bottomed, cylindrical seamless tin dish 70 1 in diameter and 45 mm in depth 3.2 Heating Bath — A cast iron bath with the shape and dimensions shown in Fig. 1 permitting the immersion of the container to a dept! 32 mm through an opening I-6 mem larger in diameter than the conta Itshall be provided with three rivets or bolts so at to support the contal 6 mm above the hot plate. ‘The free air space between the sides of {antainer and of the air bath below the opening shall be not lew © "*Glowary of era relatng to bitumen and ta (rvs). 29 15: 1204-1978 SECTION xx } 1 ines iin cs) or Hearne Bare ~—— Oe PCH Plate — Suitably mounted and heated cither electrically or by ~HbeaRh ofa gas flame, capable of maintaining the sample continuously at the euired Cemperatare, provided with an apparatoy, rach ay a Theortat or gurbprosure regulator 3.4 Thermometer — An opsn fa thermometer having the range for nus °C to ps 400°C shall conform to the following Tmmersion Temperature range ~6Cto + 400C Subdivision 2 Longer graduation lines at each 10°C Graduation numbered at each 20°C multiple of Scale error at any point up to 372°C ve when standardized shall not exceed 5 Needle — as specified under 3.2 of IS : 1203-1978*. Methods Tor eating Determination of penetration tar and Bituminous mater 30 18: 1208 1978. 3.6 Water Bath — as specified under 8.8 of 1S: 1203-1978°. 3.7 Penetration Apparatus — as specified under 3.5 of 1S: 1203-1978*, 4, PROCEDURE 4:1 Preparation of Sample AAA Thoroughly stir and agitate the material as received to ensure a comipicte mixture before the portion for testing is removed. Ifthe sample contains extraneous matter, it should be sieved through IS Sieve 30. 4.2 Weigh a 100-00 4 0:10 g sample of the material to be tested into the tared container, and place the container in the air bath in position to be heated. Support the thermometer in the sample equidistant from the sides of the container, with the bottom of the bulb neither more than 6 mam above nor touching the bottom of the container. Immerse the bulb completely in the sample and keep it immersed throughout the heating. Heat the sample as rapidly as possible, without foaming, to a temperature of 249°C ard during the evaporation ‘maintain the temperature between 249°C and 260°C. Stir the sample from time to time to prevent local overheating and, to maintain a homogeneous sample, flux in the sample all cakes of hardened bitumen which form at the sides of the container. 4.2.1 An experienced operator would be able to judge approximately tho consistency of the teadue be should obtain to secure the desired Penetration witen i i judged that the residue might show che required penetration, return to the container the bitamen on the thermométer Thich may be readily scraped off. “Remove the container from the ath, cool and weigh 43 Determine the penetration of the residue in accordance with 4.2 of IS: 1203-1978" with the exception that the container as specified in 3.1 in which the evaporation has been conducted, shall be used. 44 Frequently, it is necessary to make several trials before a residue of the required penetration is oblained. If is found to be of greater value than required, remove all water from the container and the surface of the sample, and repeat the heating and determination of penetration as before Ordinarily, a residue is considered as satisfactorily obtained when its penetration is 100, 4.4.1 When itis necessary to determine more precisely the percentage of residue having a penetration of 100, such as a percentage shall calculated by interpolation between percentages of two fesidues, onc having. a penetration greater and one having a penetration lower than 100. ‘*Metbods for waiting tr and bituminous materiale: Determination of penetration eels ye 80 and i ial: De pen 31 15; 1204-1978 5. REPORT 1 Calculate the percentage by weight ofthe origina simples and report Beh perentage reidue of 100 penetration, satng whether te pene teaion as actly determined for the sample teted or calculated. by interpolation. 6. PRECISION 6.1 Duplicate determinations by this method shall not differ from each i y, and not more other by more than 1-0 percent with the same operator, than 2°5 percent between different laboratories. 7. PRECAUTION stain types of eut back bitumens readily form sings of hard bitumen Be iuevsde Pe container Care shall be taken the this atrial Sarpltly Maxed into the sinple before the penetration of readue smn 15: 1205-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS; DETERMINATION OF SOFTENING POINT ( First Revision ) 1. SCOPE LA This standard covers the method for the determination of softening point of asphaltic bitumen and fluxed native asphalt, road tar, coal tas pitch and blown type bitumen, 2. TERMINOLOGY 2.0 For the purpose of this standard, the following definition and those given in IS : 834-1965* shall apply. 2.1 Softening Point — The temperature at which the substanc attains a articular degree of softening under specified condition of test. 3. APPARATUS 34 Ring and Ball Apparatus —A conveniont form of appacatus is illustrated in Fig. 1. 2 3.11 Stal Balis— two; cach 9°5 mm in diameter and weighing 350 4 0-05 g. 3.1.2 Brass Rings — twos the sings shall be tapered (see Fig. 2) and shall conform tothe fllowing dimaations, = P=4 ( ' Depth 64401 mm Inside diameter at bottom 159 tO mm Inside diameter at top 175 £01 mm, Outside diameter 206 + 01 mm *Glomary ofterms relating o bitumen and tar (ried). 33 18: 1205-1978 Fro 1 Asemy oF Apraratus ror DeTERMNaTion OF Sorrexisa Port ( Rixe axb Batt — Two Rinos ) For convenience in mounting the sings ina suppor ofthe type shown in Fig. I o'd, tne ouside diameter of the ting af the bottom may be Staller, but sal be no les shan 10 mm 3.1.3 Ball Guide — A convenient frm of ball centering guide. A recom- rngndid for of ball guide i lumeatd in Fog. 3 3.14 Supprt — Any means of supporting the rings may be used provid- ce tho falling conditions are observed: 3) The rings shall > ure af te supported in a horizontal postion with the upper @s Stan below the surface of the bath liqui « disesnce of exactly 25 snm between the boston ‘the top surface of the bottom plate of the apport 34 tatcen anne i eee All dimensions in millietes, All dimensions ia milinnetres. Fic. 2. Tarmren Reno 3. Batt Cenrerise Guioe ‘All dimensions in millet. Fie. 4 Rune Hoxper ©) The thermometer shall be suspended 0 that the b bulb is level withthe bostom of he rings, and with Woo ‘the rings, but net touching them, - a! 31-5 Thermomier—10 shall be of the mescuty-inglae filled, with the stem made of lead glas or other swig, fe ieee ‘Spitaved and enamdled at the back and. provided wean Sonal ee amber and glass ring at the top. "The bul shall be cyindsed a 35 t5: 1205 - 1978 suitable thermometric glass. The dimensions, tolerances and graduations of the thermometer shall be as [ollows: _ igh Tenpoce Tempe | -dowarc — socor00c Graduaon ateach 020 ose Longer inateach °C re — ve sc Temerdon, mes Toul Total Overt length 81810304 mm 370.0304 mm ees Seton Lengthofbul, Mer 910 4 _ Not larger than Not larger than Lr _ 60.70mm — 60%070mm Dinaace fim botom af 75 t090 mm 78080 mm parent — hove eos Jah — a heat reste lan veel oto than 8 rm in dame «eo TED i ih Th hath egal ‘be eahly bled dh Se eee eke tae ane ee ae er Ce a a alain hie rece ‘operation. 4. PROCEDURE .1 Preparation of Test Sample — Hest the material toa temperature tctwoen4a¢C and 100°C above it stening puny str un completely Mend and free frome bubbles 4nd water and Ste, if necaary, troupe TS Sion 80° (a 13: 460-1962°). Place th ngs’ prevouly eated toa tenporature Spproninating fo fiat of the molten atria on 4 metal Tine wih is bean coated wif mature of equal pats of glycerine sod “Speciication or test sieves ( ected). $6 18: 1205-1978 dextrine, and fill with sufficient melt to give an excess above the level of the ring when cooled. After cooling for 30 minutes in ain lel he material in the ring by removing the excess with a warmed, sharp ball 4.2. Materials of Softening Point Below 80°C — Assemble the apparatus with the rings, thermometer and ball guides in postion, aad Ai eee 1 a height af 90 mm above the upper surface ‘of the stags mith ene Boiled dtiled water at temperature of S°C., Malnals fe Meuse temperature of 5° for 15 minute ater which place ball aay Cooled to a temperature of 5°C, by means of een in Cok Par ate ‘Apply heat tothe bath and str the liquid so thatthe temperature sees slog to 30 5 0856 per sunt nl de matron 2 Slows the ball to pane WOU Tg” he rte ar eanens a shall not be averaged over the period ofthe test and any teri ahnn he fate of temperature rie does ot fall within the pecibed nt thet he frat three minutes shall be ejected. "Make the determination’ intiears 43 Materials of Softening Point Above 80°C — The procedure for materials of softening print above 80°C. is similar to Uae deste under 4.2\with the diférence that glycerine © wed ie plate CPrgee inthe bath and the sarting temperature of the test #350" Stale determination in duplicate 5. REPORT 5.1 Record for each ring and ball, the temperature shown by the thermo- ‘meter af the instant the sample surrounding the ball touche the bette: plate of the support, if any, or the bottom of the bath. 5.2 Report to the nearest 0'5°C the mean of the temperature recorded in duplicate determinations, without correction forthe emsegant Hog ae thermometer, as the softening point. "sen 6. PRECISION G1 Test results shall not differ from the mean by more 1 following: : a ing Point peor . Seeing city —— Racy 400 0 10 55 Gi to 80 ts 5s 81 10 100 ss = 101 to 120 2 7 121 to 40 30 re 37 35: 1205 - 1978 1, PRECAUTIONS: 71 Only feeshly boiled distilled water shall be used in the te Aue distilled water 3 used in the test, as other- WEG git bubbles may form on the specimen and affect the accuracy of the 1.2 The prescribed ra accuracy of real 73 A sheet of filter TELA theet of filter paper or thin amalgamated sheet, placed on the Roatan ec Bias Wesel and conveniently weighed would prevent the eater 8 tothe gat veucl, and considerable time and wouble in cleaning would thereby be'saveds te of heating shall be rigidly adhered to for ensuring 151 1206 ( Pare 1)-1971 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF VISCOSITY PART I INDUSTRIAL VISCOSITY ( First Revision ) |. SCOPE Ll This standard ( Part I) covers the methods for the determination of ‘iscosty of road tar and cutback bitumens. . TERMINOLOGY 10 For the purpose of this standard, the following defini given in IS: 394-1965" shall apply. 2 Industeial Viscosity — The property of a fuid by which it resists flow due to internal fiction, and one of the methods by whieh it is measured, is by determining the time taken by 50 cc of the material to flow from a cup through a specified orifice under standard conditions of test and at specified temperature. and those 3. METHOD A (VISCOMETER FITTED WITH 10mm CUP FOR ROAD TAR) 341 Apparatus BA1 Tar Viscomeler —consists essentially of a cup having a specified orice and valve; n water bath mourted on three lige having arable Sleeve forthe cup. a strrer, a shield anda receiver Cie Fig. 1). Th fsllowing ithe detaed description of the diferent pars and acresorics afta viscometer: 8) yp —known as the 10-mra cup, i constructed of hard brass tube fof the dimensions shown in Fig. 2 and Gvtod with an external Brass collar at the upper (open ) end of the cylinder to support” the "Gilonary of term relating to bitumen and tar (sed) 39 1511206 ( Part 1)- 1978 Fic. ‘Tax Vcore 1811206 (Pare 1)-197 No 105 4 PHOSPHOR BRONZE 1o.0co#.025 OSPHOR BRONZE SPHERE 12.70.05 DIA 0/10 cast {Alt dimensions in milimetrs, Fro, 2. 10-mm Tar Gur axp VaLvE cup in the sleove of the water bath. The bottom of the cup consis of a circular phosphor-bronz= plate screwed into the cylinder an ‘made conical to facilitate drainage of the tar after usc, It yrovided centrally with a perfectly cylindrical. phosphor-bronz {[Sojio cast) extension of the dintesions showat in Fig. 2. TE extension is drilled and polished internally to give a 10-m circular orifice. The upper rim of the orifice shall be perfect circular in order to pravide a seating for the valve. ‘The dimensions of orifice and jet shall be as follows: Diameter of the orifice 10-000 + 01025 mm Length of the jet 5-000 + 00025 mm 4 15 1206 ( Part I)-1978 1) alee sal ef dinension shown in Fi 2., Te serves to coe the ‘orice of the 10-mm cup and is a phosphor-bronze sphere gfe toa oct etal fo” The fod leeds ¢ itvelling peg-and at the upper cnd a hemisphere by which the walve i beldin the valve support ©) Hater bath — ade of copper shee is ylindical in shape, about 160 mm in diameter and 105 mm in depth. It may be heated electrically, care being taken that local heating is avoided. ‘The water bath is mounted on three equidistant legs which are riveted to the cylindrical wall of the bath and are of sufficient length to permit a 100-ml cylinder to be placed below the orifice of the cup. 4) Sleeve — to receive the cup and to hold it in position with an ‘easy sliding fit. It is a stout brass tube, 105 mm in height and 42 mm internal diameter, which is bronzed or soldered ‘ central hole cut in the bottom of the bath. er — consns of four vertical vanes, with the upper and lower Portions turned in opposite direceons, mounted. on a cylinder Athi slips on the sleeve with an eany aiding. The cylinder i Git sway been the vane to fellate heat tant rom the State in the bath tothe tar cup: vertical grooves ate provided on the inner surface of the cylinder to preven the water fm the bath from being carried into the tar cup, if the srring system be sed. 1) Curced shield — fixed to the upper edge of the cylinder and extends to within about 5 mm of the walls of the water bath. ‘This shield carries an insulated handle for rotating the stirrer, a support for 2 thermometer, and a swivelled support for the valve. The two ppositions of this valve support are respectively (a) well clear of fhe tar cup, and (b) extending over the tar cup t0 that the valve, ‘when resting on the support, hangs vertically over and 161 mm above the orifice of the tar cup. 8) Rectiver—a 100-ml_ graduated measuring cylinder _ with graduations at 20 ml, 25 ml and 75 ml capacities, having an Internal diameter of not more than 29 mm. 2 1h) Thermometers —two standard thermometers, one for the bath and another for the cup. Both the thermometers shall be of the same range, depending on the temperature at which the determination eS nutes “the thermemcters shall he of nercury in glass tue wi eylindrest iby and made of stable thetmmetet fs and shal conforin to the following eurtnent 2 1811206 (Part 1) -1978 Charactriti Low Medi High 2 wc — a7amEFC —-oIAE Graduations OC orc orc Immerion 65 mm Som 65 mm Overalllengh 40 10mm 3404 10mm $404 10 mm Sumdiameter 55%080mm 55i60mm 55%080mm Bulblengh 10016 mm 10 16mm 00 16 mn Bulb diameter «-—— Not largo than the tem daneter —-— Langenaf 1506 190mm 1501619 mm | 150 190m . 1°¢ 7 Uingrline "ands Cand Crean te Figuredatexch °C so sc Seale 020 #020 osc 5) A stop weteh or a sop clack or any ether timing device — eapabte of being read up to half a second. ’ mee 3.2 Procedure 3.21 Adjuat the tar viscometer so thatthe top fhe tar cup level Heat the water in the water bath tothe temperature apecied Re soe wae —rLFrr:C—~—r:—C—C—:__—=UiC“iSCCEs IErbait forthe Garnet af the ce thcsaens eueeatag, oughout foquent intervals or preferably, nent Eger a ae Satan agg traeaeess ee fod ist immersed when the laters wera, "U6 PRE Om the va SADUR tsa tree san: tt pad oan ered oe “8 1811206 (Part 1) -1978 of the specified temperature. Remove the thermometer and quickl Femove any exces of tr ao that the final level ison the contre linc of the Teveling peg when the valve in vertical postion. 3.2.6 Lift the valve and suspend it on the valve support. Star che stop veatch or the ine recording device when the reading in the eylinder 25 mil and stop it when it 75 ml, Note the time in seconds, 3.3 Report 33.1 Report the time in seconds taken by 50 ml of the tar to low out as the viscosity of the sample at the temperature specified for the tett. 3.3.2 State clearly whether the sample was dried or tested as received at the presence of water, particularly in quantitis les than one percent, hhaa a marked effect on the viscosity. Report the method of drying adopted. 3A Precision — The results of repeat determinations on portions of the tame sample shall fall within -b4 percent ofthe average of several readings, 3.5 Precautions 5A The working range ofthe instrument withthe 10-mm eup is uch that the time of efflux shall be between 10 and 140 seconde 35.2 The temperature of tet shall be appropriate to. emulate the condition specified under 35:1 and shall be a ulaple of 5°, not lower than 20°C" 3533 The tar cup is critical part of a viscometer and. speci precautions shall be. obscrved in i treatment and we. Any cleaning Proves shall be of gentle nature. Nonccorroding solves, such ay light {ar oll, fee from phenol ate recommended. rather than’ machanteal teas, auch at dusters, which are lable to cause abrasion of the meta ‘Specially atthe orice. It any material be wed for rubbing the int SP the cup, it shall not be such as may distintegrate in sey leaving Particles which may interfere with the fee ow ofthe sample through the ice. 3.54 The orifice of the tar cup shall be tested at Feequont intervals with a guuge having appropriate diameter 4, METHOD B ( VISCOMETER FITTED WITH 4-mm CUP FOR CUTBACK BITUMENS ) 441 Apparatus — The tar viscometer as specified in Method A shall be used with one modification, namely that the 4-mm cup shall be fitted instead of the 10-mm cup.’ The dimensions of orifice and jet shall be as follows: Diameter of the orifice 4000 4 0-025 mm Length of jet 5-000 4 0-025 mm 4 18: 1206 ( Pare) -1978 42 Procedure ~The procedure shall be the same as specified in Method A (we 3.2) except that the mm cup shall be fitted in tar viscometer instead of the 10-mm cup. 4.3 Precautions 43:1 The working range for the instrument with the 4-mm orifice is such that the time of efflux shall be betireen 20 and 200 seconds, 43.2 The temperature of test shall be appropriate to ensure the condition specified under 4.3.1 and shall be a suitable multiple of °C, not lower than 20°C. 5. REPORT BAL Report the visecsty of the sample at the specified temperature for. the {et the time in seconds nearest to whole number taken by 50 mal of the tar to flow out. 6. PRECISION 6.1 Results of duplicate tests should not differ by more than the following amount: Viscoiy Repeatability Reproducibility Below 20 5 Qs 2s 20 to 40 5 Qe TO percent of the S408 5 percent 10 percent of the of the ‘mean’ 48 18 : 1206 ( Part I1)-197 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF VISCOSITY PART I ABSOLUTE VISCOSITY ( First Revision ) 1. SCOPE LA This standard (Part II) covers the method for the determination + Absolute viscosity of bitumens and cut-backs by vacuum capillary visce ‘meters at any specified temperature. It is applicable to materials havir 2 viscosity range of 42 to 200 000 Poises. [Nome — The standard cover thee types of viscometers and any one of them can | wed fr determination of tovolute vaca. 2, TERMINOLOGY 2.0 For the purpose of this standard, the following definitioas and tho: given in IS: $34-1965* shall apply. 2:1 Absolute or Dynamic Viscosity of a Newtonian Liquid—Itis 2 internal friction, such that if a tangential force of one dyne (0-00001 N ‘acting on planes of unit area separated by unit distance of the liquid pre duces uni tangential vloity, the eg unit for the viscosity of the ligui 2.2 Newtonian Liquid —A liquid in which the shear stress is direct! Proportional to the rate of shear strain. ‘The constant ratio. of she: Stress to the rate of shear strain is called the coefficient of viscosity of tt liquid.” Tf this ratio is not constant then the liquid is non-Newtonian, 3. APPARATUS 3.1 Viscometers — Capillary type made of borosilicate glass, anneale Suitable for this tet are given Ia SLT to 33. : ‘Glossary of terme relating to bitumen and tar (raised). a 15 11206 ( Part 1) - 1978 3.11 Camon-Maming Vacuums Viscometer (Fig. 1) —‘The size, numbers] approximate bulb factors K, and viscosity ranges for the series of Cannon ‘Manning Vacuum Capillary Viscometer are a3 follows: Viscomatr ‘Approximate Calibration Factor Viacority Range Size No. ‘30 em Fig Vacuum Poses pers Poises Balb B Bulb 10 20 06 36 to 800 u Go 20 120 to 2400 2 200 60 360 to 8000 B 60-0 200 1200 to 24000 4 2000 60-0 3600 to 80000 For all viscometer sizes the volume of measuring bulb C is approxi ‘mately three times that of bulb B. ‘The viscosity ranges correspond to a filling time of 60 and 400 s for boch measuring bulbs. 3.1.2 Asphalt Institute Vacuum Viscometer ( Fig. 2)—The size numbers, approximate radii, approximate bulb factors Ky and viscosity ranges for the series of Asphalt Institute Vacuum Capillary Viscometer are as follows: Viscometer Capillary —_Appraximate Calibration Factor Viscosity Size No. Radius” —_K. 30cmFlg. Vacuum: Poise pers Range Potser em BulbB Bulb Bulb D 25 00125 2 1 07 42% 900 50 0-025 8 4 3 180 to 3200 1000-050, 32 16 10 600 to 12.800 200 0100 128 ot 40 2-400 to 52.000 400 © 0-200 500 2501609600 0 200.000 ‘This viscometer has measuring bulbs B, C and D located on the viscometer arm Af which isa precision bore glas capillary. The measure Ing bulbs are 2 em long capillary segments Separated by timing marks F, GH and L. 3.13 Modified Koppers Vacwm Viscomeer (Fig. 3) —"The size numbers approximate radii, approximate bulb factory and viscosity ranges for the series of Modified Koper: Vacuum Capillary Viscometer are a follows: Visomatr Capillary Approximate Calibration Factor Viaosity ‘iceNo. “Redir” —K-30.cm Hg Vacuum: Pose pers Range’ Poser, SubB BulbG BulbD 2 00252 1 07 42% 800 50 0-025 8 4 5 180% 3200 1000050 ooo 600 0 12800 200 100 12RD 2400 to, 52.000 400 0200 © 500,250 160-9600 10 200 000 * 150 1206 ( Part 11)..1978 To vac tl Fine Tae" \vAcuUM tupe -M. OVERFLOW suLa-O amo TMG ani H. sue-C SECOND TiMiNa HARK ~G FIRS TNC WARK =F carnuagy-K All dimension ia millimetres, Pio. 1 Caxwox-Manwtso Vacuunt CaPmisary Viscomeren 49 181 1206 (Part 11 )- 1978 ‘To vacuum oe suge=A vacuum 1use-M tyiRo timing MARK HL SECOND TIMING WARK- G fist TiMiNG MARK= All dimensions in milimete prcnaRy VISCOMBTER Fio.2 Asenacr Insrrrure Vacuuse CArmtal 50 1S: 1206(Part) 1978 To vacuum vacuum Tuge ~ M ‘GROUND _GLASS_JOWNT-N. FILLING TUBE ~ A, All dimensions in millimetres. Fic, 8 Moomm Korrers Vacuua Carttuany VeOMETER, ‘This viscometer consists of a Separate filling tube 4, 24 @ Precision Bees RN, capillary Vacuum tube ad These pai ate Ronee aa roe eee gas Jpiat M, having a 24/40 standard ou ing bulbs B, C, and D on the gles capilary set =! segments separcted by timing marks FG Hae “7 51 15: 1206 ( Part IL) 1978 ‘A viscometer holder can be made by deilling a 28-mm hole through the centre ofa No. II rubber stopper and setting the stopper between the hole and the edge. When placed in a S-cm diameter hole in the bath cover, it holds the viscometer in pla ce. 3.2 Thermometer — Ths thermometer shall be of mercury in glass tube ‘with cylindrical bulbs and made of suitable thermometer glass and shall Conform to the following requirements: Characteristic Lew Medium High Range O10 44°C S78 t0 82" 76 to 122°C Graduations 02°C. orc oc Immersion 65 mm 65 mm 65 mm Overall length 3404 10mm $40 + 10 mm 340 10mm Stemdiameter 55to80mm 55t080mm — $5to80mm Bulblengthh © -10to 16 m= 10 to 16 mm. 10t0 16 mm. Bulb diameter Notlarger than Not larger than Not larger than thestem dia- the stem die the stem dia- meter meter meter Length of gradu- 150 to 190 mm 150 to 190mm 150 to 190 mm. ated portion Longgrinesat Cand 8G Cand S*C 1°C and 5°C Figured at each 5°C se. sc Scale £02 £07C £020 3.3 Bath — A suitable bath for immersion of the viscometer so that the liquid revervoic or top of the capillary, whichever is uppermost is at least 20mm below the upper bath level, and with a provision for the visibility of the viscometer and the thermometer. Firm support for the viscometer Shall be provided. "The accuracy of the viscometer bath should be ty of the sample, provided the three determinations be within ++ 5 percent of their mean value, BALA If the valu their m: then record 1 of three determinations do not lie within + § percent of but the two higher values are within -- 5 percent of their mean the mean of the two higher values as test result, 3 35: 1208 - 1978 lal goin Sige nie Burr mail aa 5.3 Ia normal te is not obtinableon thtcesuccenive tet, report the Gucility a beng unobtainable under the conditne of tats 6. PRECISION 6.1 Test results shall not differ by more than the following: Repeatability 10 percent of the mean Reproducibility 20 percent of the mean 7. PRECAUTIONS 7.1 The plate upon which the mould is placed shall be perfectly at an: Tevet to that the bottom surface of the mud touches e roughodts 7.2 In filing the mould, care shall be taken not to disarrange the parts and thus distort the briquette and to ace that no air pocket shall be within the moulded sample." Se “ 15: 1209-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIAL DETERMINATION OF FLASH POINT AND FIRE POINT ( First Revision ) 1. SCOPE 1.1 This standard covers the methods for the determination of flash poi dnd fire point of asphaltic bitumen and fluxed native asphalt, cutbacl bitumen and blown type bitumen, 2, TERMINOLOGY 2,0 For ihe purpose of this standard, the following definitions and thos given in 15: 894-1965* shall apply. 2.1 Flash Point — The fash point of a material the lowest tempera it which the application of iestflame causes the vapours from the matcris Tmomentariy earch fire in the form of a flash under specified conditior of tet. 2.2 Fire Point —The fire point is the lowest temperature at which th ‘pplication of toxt flame causes the material to ignite and burn at lea far'5 + under specified conditions of tet. 3. METHOD A ( PENSKY-MARTENS — CLOSED ), FOR DETERMINATION OF FLASH POINT FOR BITUMEN OTHER THAN CUTBACK BITUMEN 3.1 Apparat ‘3.1 Pensky-Martens Closed Tester (see Fig. 1) consisting of th following major parts: 'a) Cy —made of brass, conforming to the dimensions given ‘Table 1. ‘The inside’ of the cup may bo, turned to a slight larger diameter above the filing mark and the ouside may 1 tapered above the flange, but the wall thickness at the upp *Glomary of term relating to bitumen and tar (revised). 7% 15 1209-1978 A—OiL-Cup -H — Revolving Sbuter — Heating Vee! J—Orifee c—stirer K— Gauge Dise D~Thermoseter L— Ling Hooks E—Ignition Burner ——_-M-—Optional Form of F— Plot Borner ‘Stirrer Operating 6 ~ Spring Handle Device Fro, 1 Pansxy-Manrens Crosep Taster 6 15; 1209-197 "FABLE 1 DIMENSIONAL REQUIREMENTS OF PENSKY-MARTENS TESTER (Gta 3.1. (0) se Doernowat Reguiemaners Min Niwmat Ma No. ao nm me 0 e » © @ 1) Teside darter below fling mark ws 8st fi) Ditierence between inside and ouside diameten = $0. $2 below ing mark i) ese height see 559 Te '8) Thicknes of bottom eM OM ‘Distance from rim to fling mark aes ae: i) Distance, lower surface ange to bottom of cup 2456 464 Se see aeglioee Teter peat Sera Tate taal Tae Hse ere sae a ce | Position of the lid on the cup and the cup itself in the stove. Be pecs aS et b) Lid—The lid, includi 1) stirring device, (2) cover pre » ee i eat a oe, a oe Same 1) Stirring device —The lid shall be equis with a stirrir Serie cg ude ge oa eee et eee cents ee cia cg at Gee hone tteeagaat tres ‘The amaller (upper) propeller shall have an overall diamet peng arto ond Posen eae ener ire tae to ae Tanetnelr sas Sy eee pee eee ois ae Poi, a ea laine pisces asec key hac ke gen n 1851209. 1978 2) Cone proper —"The cover proper (st Fig. 2) shall be of bras, and Shall have a rim projecting. downward. almost to the flange of the cup and ftsng the outside of the cup closely. ‘The thickness of the cover measured just nse the rim, sha belot lew than OB man and aot mere than 2 mn. "There thall be a proper locating device, engaging with a corre. Ponding locating device on the Bange of the cup. ‘There shall be four op ‘with the following dimensions: 4) Opening 4 isan area defined by arca of twoconcentric circles and the intersected lengths of two radii. ‘The radius of the Outer eircle shall be not less than 22°4 mm and not more than 246 mm. ‘The radius of the ianer circle shall be not Jess than 13:5 mm and not more than 142mm. The chord of the are of the outer circle shall be not less than 12-7 mm, and not more than 13:7 mm- Openings B and C are of equal areas, each of the same general form as opening 4, but of approximately half the (angular) width, The radii of the defining inner and outer Circles shall be within the limits specified for the radii of the two circles, arcs of which partly define opening A. ‘The chord ofthe outer arc for opening B or opening C shall be not lest than 4°8 mm and not more than 5°6 mm. ‘The sum of the areas of openings B and C shall be neither less than 75 percent, nor more than 100 percent of the area of opening 4. Openings B and C shall be equally distant from opening A and radii drawn through cach of their centres shall be at an angle of not less than 135° and not more than 140". ii) Openings 4, B and C need not conform exactly to the shape ‘of geometrical figures bounded by arcs of two concentric circles and intersected lengths of radii. Their boundaries should, however, fall on or between the lines indicated by the imiting values of the dimensional specification of the preceding text and of Fig. 2. iv) Opening D is a split tube to grip the thermometer collar, Tis contre is approximately 20 mm from the centre ofthe lid ‘and on a radius at an angle of not les than 50° and not more than 60" to a radius passing through the centre of opening C. Tt shall be set at an angle of not less than 10°, and not more than 15° to the perpendicular. Its height shall bbe such that, when a standard thermometer is in position, the bottom of the bulb shall be 35:6 to 40'6 mm below the 8 ings in the cover (s0 Fig. 2) 15: 1209-1978 = miimsmn 289 mn Sasimurn 24° un — ‘nin 155 mm I~ Raton 162 mm [K-—nininum 127 ma sims 167 om init 48 men *— Seu 56 mm $—spprox U— approximately 127 mm Angles pare equal ‘Bogle #— minimum 135° maximum 140° ee ae By ae Fro, 2 Cover vor Pexsxy-Manrens Ciosep Tesvsr 79 1811209 - 1978 level ofthe rim ofthe cup (which corresponds tothe Iower surface of the portion of the lid inside the rim ) 8) Sher —"The lid shall be equipped with a brass shutter, approximately 25 mm in thicknem, operating on the plane of the upper surface of the lid. The shutter shall be ab shapd Snd mounted that it rotates on the axit of the horizontal entre of the lid between the fwo stops, 3 placed that when ivone extreme postion, the openingy A Band C of the id are completely closed and when in the other extreme positon, these onfices are completely opened. 4) Flaneasporure device —The fame-expesure device shall have a tip with an opening 0-7 t0 0'8 mm in diameter. ‘The flame txponure device shall be equipped. with an operating tnechaniom which, when the shuiter i in the open postion, ‘epreses the tip to that the centre of the orifice is between the planes ofthe under and upper surfaces of the lid proper, At aipoint on a radius passing through the centro ofthe large? pening A and approximately 2°5 mm from the outer edge of the opening. A'piloe flame for automatic rlighting of the txportre fitioe should be provided. "A bead, muy in dic meter of suitable material, may be mounted on the lid 40 that Se of the testflame ean be regulated by comparison. The mechanism operating the shatter shoutd be ofthe spring type tnd constructed 20 that when at ret the shutter shall exacly lowe the three openings 4, 2 and C.. When operated the over extemoy the tree aponigy inthe, shal be ext open and the tp of the exposure tube shall be tally depresed Phe air bath is cleconcaly heated and gas is not available, an-oil burner shall be used to provide the testflame, the position of which shall correspond with that of the gas fame Previously specified. ©) Stove — Heeat shall be supplied to the cup by means of a properly aligned stove which is equivalent to an air bath. ‘This stove shall ‘consist of (1) an air bath, and (2) a top plate on which the ange of the cup rests. 1) ir beth — The air bath shall have a cylindrical interior, 41-3 to 42-2 mm in depth and a diameter not less than 3-mm and not more than 4mm greater than the outside diameter of the cup. ‘The air bath may be cither a lame-heated metal casting fof an electri-resistance element. If the heating element is a flame-heated metal casting, it shall be so designed and used that the temperature of the bottom and walls is approximately thesame. On this account should be not less than 6 mm in thickness. The casting 80 4 15: 1209-1978 shall be designed so that products of combustion of th: ame Cannot past'up and come in contact with the cup. Ifthe at bath Of the electevreatance type, it shall be constructed {thas all pars of the interior Mirage are heated equally ‘This necensittes an even distribution ofrestance wire t cover the bottom and walls, and a method of construction such that heat is given out from the whole core ofthe rxstance clement rather than directly from the see. “The result obtained withthe electrically heated iestrument shall agice with that obtained with gas-heated apparats with in''G'and 396 respectively, according fo whether the low or high range thermometer i wie. 2) Tip plate—The top platc shall be of metal. The total » Takes from th uppel surface ofthe plate tothe tion af the air both shall exceed the distance from the under mrface ifthe flange tothe bottom of te cup by not les than 1-6-mam Sind not more than 3 mm,” The top plate shall be mounted ‘rth am airgap betwoen ft and the air bath ‘The top plate May be stared othe ar bat by mea of hens and {pating-bishings. ‘The spaing-bishings sould be of proper iHickness to define the aingap which shall be not lex than Simm nor more than 48 min.” The spacine-bushing shall be rot more than 9'3 mm in diameter. ‘The thermometers conforming to the fllowing requirements shall be used: . se Tow Range High Range Range = 7 to + NOC 90 t0 370°C Graduation at each osc 20 Longer lines at each PC and 5°C 10°C and 20°C Figures at each 3c 20°C Immersion 57mm 57mm Overall length 200-4 10mm 280 + 10mm Length of graduated 1430 177mm 143 t0 177 mm portion Bulb shape Cylindrical Cylindrical Bulb diameter, Max + Not larger than stem diameter —» Stem diameter 55t080mm — 55 to 8) mm Distance, bottom of bulb 75 to 90 mm. 75 0 90mm. to lowest graduation Expansion chamber Required Required Top finish Ri Ring Scale error, Max, osc 1°C up t 260°C plus or minus 2°C above 260°C 81 18: 1209 - 1978 Either of the thermometers may be employed if the indicated reading {alls within 93 to 110°C. The thermometers shall be mounted securely it a thermometer collar so that the distance from the under side of the rim of the collar to the bottom of the bulb is 52 to 55 mm, ‘The thermometer collar shall have an outside diameter of 12°70 4 0°05 mm and a flange of 23 to 2°8 mm in thickness. The cement used to fasten the thermometer into the collar shall be of mich a nature that it will withstand the action of oil up to the highest temperature at which the thermometer is uted, A swelling shall be provir dded to ensure the location of the thermometer collar at the corzect point, 3.2 Procedure 3.21 Clean and dry all pacts of che cup and its accessories thorough before the test i started. Take particular care t avoid the presence of any solvent used to clean the apparatsa afters previo tert Fill the cup with the material to be tsted up tothe level indicated by the filling mark, Place he id on the eup and st the latter inthe stove. Take eare tha the locating devices are properly engaged. Trarre the thermometer, high or Joy rang, as required. 3.2.2 Light and adjust the test-flame so that itis of the size of a bead uf 4mm in diameter." Apply heat at such a rate that the temperature record- ‘ed by the thermometer increases between 5 to 6°C por minute. ‘Turn the stirer at a rate of approximately 60 revolutions per minute, Apply the testflame at each temperature reading which is a multiple of 1°C up to 104°C. For the temperature range above 104°C, apply the test- flame at cach temperature reading which isa multiple of 2°C, the first applic ation of the tert-lame being made at a temperature at least 17°C below the actusl fish point. Apply the testlame by operating the device controlling the shutter and test-flame burner so that the flame is lowered, in 0°5 soconds, left in its lowered position for one second, and quickly raised. {ots igh poston. “Discontinue the stirring during the application of the 3.3 Calculation 3.3.1 Observe and rocord the barometric pressure. 3.3.2 No corrections shall be made except in cate ot dispute, when the flash point figure shall be corrected according to the following rules: 1) For each 25 mm below 760 mm barometric reading, add 1°C to the fagh point; b) For each 25 mm above 760 mm barometric reading, subtract 1*C. from the fash point. 2 18: 1209-19 3.4 Report — Unles otherwise specified, normally the flash point shall {taken as the temperature read on the thermometer at the time of the flat application that catises a distinct fash in the interior of the cup. 3.5 Precision — The duplicate test results should not differ by more th the following: Flash Point Repcatabiity Reproducibility 104°C and below 35°C Above 104°C. asc 3.6 Precautions 3.6.1 The testflame will neither be larger than stipulated nor will it applisd more frequently than specified as the surface layer is liable to snuperheated. 3.6.2 The bluish halo that sometimes surrounds the test-lame shall n bbe confused with the true flash 4. METHOD B (PENSKY-MARTENS — CLOSED), FOR DETE] MINATION OF FLASH POINT FOR CUTBACK BITUMEN 4.1 Apparatus ALLA Plath Point Tesier — Pensky-Martens Closed Testor as describe under 3.1.1 except that the stirrer shall be mechanically operated to stir a downward direction at a speed of 70 to 80 rev/min. 41.2 Thermometer — Low range thermometer as specified in 3.1.1(d) 422 Procedure — Bring the material to be tested and the toster to a. tor perature of 17°C lower than the expected flash point. Completely fill t Air space between the cup and the interior of the air bath with water the temperature of the tester and material. Raise the temperature throug, fout the duration of the test at a rate of not less than 1°C and not more the V'S°C per minute, Proceed as described in 3.2.2 except that : a) rate of heating to be not less than 1°C and not more than 15° per minute, 1b) the rate of stirring to be 70-80 rev/min, and ©) the textflame to be applied at cach 05°C rise in temperature 4.3 Calealation and Report — Calculate and report the flash point « described under 3.3 and 34. 44, Precision — Duplicate tts shall not difer by the limit, specifi 83 151 1209-1978 5. METHOD C ( PENSKY-MARTENS— OPEN), FOR DETER- ‘MINATION OF OPEN FLASH POINT AND FIRE POINT 5.1 Apparatus — The standard Pensky-Mactens Tester and thermometers a presrbod in Method A'( ve 3.1} shall be used with the following ‘odlications ‘The cover ofthe cup shall be replaced by a clip which encircles the uppers ofthe cupland carta the thermometer and test-ame, ‘The tie carrying the thermometer" shall have. is centre on & radius at approximately 9° to the adie passing through the point of tachment of the testlame, aad sall be of euch a heghe that when ake thermometer isin position, te bully shall be fa the vertical aie of tecup and 12 mm bclow sh filing line, ‘The tea-ame aball be fged atthe versal xs of he cup andin iva withthe upper ede of the cup. 5.2 Procedure 5.2.1 All parts ofthe cup and its accesories shall be thoroughly cleaned and dried before the test is started. Particular care shall be taken to remove all traces of solvent used to clean the apparatus. 5.2.2 The cup shall be filed with the material to be tested up to the level indicated by the filing mark. 5.2.3 The clip carrying the thermometer and test-lame shail be placed fon the cup and the latter set in the stove. Care shail be taken to have the locating devices properly engaged. The thermometer shall be inserted. If it is known that the material will lash above 104°C, higher range thermome- ter shall be used, Otherwise it is preferable to start with the lower range ‘thermometer and change if a temperature of 104 to 110°C is reached. 5.24 The testlame shall be lighted and adjusted so that it is ofthe size of bead 4 mm in diameter. 5.25 Heat shall be applied ar such a rate that the temperature record ed by the thermometer increases neither less than 5°C. nor more than 6" per minute. ‘The surface of the material shall be carefully observed during heating. 5.3 Report 5.3.1 Open Flash Point — The open flash point shall be taken as the temperature when aflaih first appears at any point on the surface of the material 5.3.2 Fire Point — The heating shall be continued until the oil ignites and continues to. burn for 5 seconds, ‘The temperature of the material, ‘when this occurs, 'shall be recorded the fire point. aw 18: 1209-191 54 Precision — The following criteria should be followed for the accep ability of test results Repeatability Reproducibility Flash point arc ee Fire point ec 1c 55 Precaution — Care shall be taken to shield the apparatus fro: ‘draughts 85 18: 1210-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: FLOAT TEST ( First Revision ) 1. SCOPE 1.1 This standard covers the float test for bituminous materials 2. APPARATUS, 241 Float — Made of aluminium or aluminium alloy and conforming to Fig. 1 and the following requirements: Min Normal Max Weight offloat, ¢ 3770979038410 Total height of float, min 340 350 360 Height of rim above lower 265 270 25 side of shoulder, mm ‘Thickness of shoulder, mm 13 4 1s Diameter of opening, mr 1-0 1 ug 2.2 Collar — made of brass and conforming to Fig. 1 and the following requirements: Min Normal Max Weight of collar, g 960 980 1000 Overall height of collar, mm 23 US 27 lediameter of bottom,mm 12721282 1292 Inside diameter at top, mm 965 © 970 975, 22.1 The top of the collar shall screw up tightly agains lower side of the shoulder. e a 87 181 1210-1978 j : Front la a $ sn0t0.0: A coutaacen) Weight of Float, 3790 « 0208 Weight of Callas, 980 = 0208 ‘Asembly of Apparat {ANI dimensions in millimetre, except where otherwit stated. Fro, 1 Froar Test Apranarus 23 Thermometer —Low softening point thermometer, graduated in ‘centigrade scale and conforming to the following requirements: Liquid Mercury Filling above liquid ‘Temperature range Subdivisions Longer graduation lines at each Graduations numbered at each multiple of| Immersion, mm 88 181 1210-1978 ‘Total lengen 378 to 384 mm Bulb length 9% 14mm Bulb diameter Not larger than stem diameter Stem diameter Distance of bottom of bulb to graduation line at 0°C Distance of top of thermometer ‘to graduation line at 80°C Expansion chamber to permit heating to at least ‘Top finish Seale error at any point not to + exceed 24 Bath—A water bath at least 185 mm. in intornal di ‘containing water at least 195 mm in depth. The height of the container above the surface of the water shall be at least 100 mm. 25 Calibration of Assembly —The ssombly of the apparatus and dimensions additional to those given above are illustrated i Fig. 1. The fssembled float and collar, withthe collar filled flush with the boom and weighed to a total weight of 53°2 g, shall foat upon water with the tim B5eE 13 mm above the surface of water. 3, PROCEDURE 3.1 Preparation of Sample — Place the brass collar with the smaller end ‘on a bras plate which has been previously coated with equal parts of gly- ering and dextrine. Melt completely a suitable quantity of residue from ‘cutback bitumen ( see 3.2.3 of IS : 1213-1978" ) or the material ite for solid bitumen at the lowest posible temperature to bring it to a sufficiently fluid condition for pouring. Stir thoroughly until itis homogeneous and free from air bubbles and then pour it into the collar in any convenient manner until slightly more than level with the top. BAA Asphalt and Asphalt Products —Cool the material to room temperature for 15 minutes, place in water maintained at 5°C for 5 minutes, and trim the material flush with the top of the collar by meane of a spatula or steel knife which hes been slightly heated. Place the collar and plate in the water bath maintained at 5 1° and leave them in this bath for not Jess than 15 minutes and not more than $0 minutes. ‘Methods for wating ta and bitussinoas materials: Distillation tet (fu rst). cy 1S: 1210 - 1978 3.1.2 Tor Products —- Immediately immerse tar products for 5 minutes in the water bath at 5°C and trim the material flush with the top of the collar by means of a spatula or steel knife which has beon slightly heated, Place the plate and collar in the water bath at 5°C and leave them in this bath for not less than 15 minutes and not more than 30 minutes. 3.22 Hoat the bath water to the temperature at which the tt ito be made. Maintain this temperature accurately without stirring and the temperature Shall at no ime throughost th test Be alowed to vary by more than O'5°C from the temperature specified, Determine the temperature by immersing the thermometer with the bottom of the bulb at a depth of 40 2 2 min below the water nirface. 3.3 Alice the matcral to be tested has boon kept in the ice water at 5°C ise not less than 15 minutes, nor more than 30 tainutes, remove tho collar with iw contents from the plate, sew into the aluminium float and [mere in water at 5°C for one minute.” Remove the water, if any, from the inside of the float and immediately fost the latter in the warm bath, raking sure that the collar ts tightly into the float, and that there is Zo seepage of water between the colar and float during the test 4, REPORT 41 Durnin, by mean of stop wath, the time in mond betncce cing the apparatun on the water and when the seater brea {Berman Mine mean of tie takes Indupiasdeteraiation sal be reported. 5. PRECAUTIONS 5.4 Precautions shall be taken to ensure that the collar fits tightly into the float and to sce that there is no sbepage of water between the collar and float during the test. spa 90 1S: 1211-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF WATER CONTENT (DEAN AND STARK METHOD ) ( First Revision ) 1. SCOPE 1.1 This standard covers the method for the determination of water content of asphalt bitumen and fluxed native asphale, crude coal tar, road tar, cutback bitumen, Digboi type cutback bitumen and creosote and anthracene oil. 2. TERMINOLOGY 2.0 For the purpose of this standard, the following definition and thote given in IS: 334-1965* shall apply. 21 Water Content —The quantity of water present in a material expressed as a percentage by mass of the material. 3. APPARATUS AND MATERIAT. 3.1 Flask — of 500 ml capacity ( see Fig. 1), made of heat resistant glass, Well annealed and as free as possible from striae and similar defects. The top of the neck shall be ground to form the socket of a ground glass joint. 3.A.A A metal flask may be used. 32 Condenser — made of heat resistant glass, well annealed and as free ‘8 pomible from striae and similar defects, with shape, dimensions and tolerances shown in Fig. 2. 3.3 Receiver— made of heat resistant glass, well annealed and at free 3 posible from striae and similar defects, provided with ground glass joints with the dimensions and tolerances as given in Table I consisting estentially of the upper chamber, side tube with ground glass joint leading to the flask and the graduated tube. Numbered graduation marks shall be carried \Glosary of terms eating to Bitumen and tar (rsd). a1 ws 121-1978 Fi, 1 Draw AN Sramc Assenamey 1s: 1211-1978 EXT 01a MiNv 18. oor ge {8 oat \ 25s 2535 —_ 2525 EXT DIA 30 #2— M7 300810 exr ov {uan?, STANDARD GROUND| GLASS JOINT. All dimensions in wilimetes. Fra, 2 Conoenser 93 1S: 1211-1978 right round the receiver tube, The graduation marks midway between the numbered marks be carried abgut halfway round tho tube and the other ‘marks shall be intermediate in length and shall project equally at each end, beyond the shortest graduation marks. fe "TABLE 1 DETAILS OF RECEIVERS (Glu 33) Garacrry or Gasoamon —Nuamenina ar Mamnent Rar To ‘Receiver Tnranvat,, ‘Every ‘Exxon : mharioe I” Geasuarion = 2 oLw2inoos OS mt son 10 10 10a 1m +005 Fig. Fio. $ 2ml Recaver (DEAN AND STARK Apparatus) * IS: 1211 -1978 SP PEAS OF SoNSENER S06KET. OF xc. Sais ont ext on 272 WNT DANS 108 ALL DIMENSIONS IV Mad Fi. 4 10-ml Receiver (DEAN AND STARK APPARATUS) 3.3.1 When a metal flask is used, the receiver of the type shown in Fig. 3 and 4 without the ground glass joint shall be used and care shall be taken, to provide an air-tight connection between the flask and the recciver. 3.4 A 100ml Graduated Cylinder 3.5 Heater — Any suitable gas bumer or electric heater may be used. ‘A gas ting burner with ports on the inside circumference, shall be used with the metal sil and shall be of such dimension that it may he moved up and down the vessel when testing materials that are likely to foam or solidity in the still. 95 15: 1211-1978 3.6 Solvent — Carrier liquid shall he any one of the following: 3.6.1 Blond of 20 percent by volume of industrial grade toluene and 80 percent by volume of industrial grade xylene 3.6.2 Petroleum or coal tar naphtha ( 18: 213-1968" ) free from water yielding not more than 5 percent distillate at 125°C and mot less than 20 percent at 160°C. 3.6.3 Petroleum spivit with a boiling range of 100 to 120°C. 4. PROCEDURE 4.1 Place about 100 g of the sample, accurately weighed, in the Bask and 4100 ml of solvent (se 3.6). Attach the ask to the Dean and Stark Condensing and collecting syste, and vat the ask at such a rate that the condensate falls from the end of the condenser at arate of two five drops peraccond. ‘Continue the dinillaton unt condensed water is no longer ‘sible in any part of the apparatus except the botcom of the graduated tube and intl fhe volume of water collected remains constant for a period ‘not lem than five minuter-Remove the persistont ring of condensed water inthe condenser tube any, by incrensing. the rats. of distillation. by few drops per second. Wash droplet of water which adhere. to the iower end of te condenser tube into the reeiver with slvent|earrer liquid tng the spray tube. Insert «loose plug cotton wool inthe top of the Condenser tube to prevant the condensation of atmospherie mowure in the condenser tube 5. REPORT 5.1 Report the results as water contont to the nearest 0:05 percent by Weight if2 ml receiver, has been used and to the nearest O'1 percent if the 10 ml receiver has been used with 100 ¢ of sample. 6. PRECISION 641 Duplicate determinations shall not differ by more than the following: Water Collected Repeatability Reproducibility Ot rOm Ol ml 02 ml 11 t0.25ml —O-l_ml or 2 percent of 0-2 ml or 10 percent ‘the mean whichever of the mean which- is greater ver is greater peafcation for coal based naphtha (ft rion) 96 1821212 -1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF LOSS ON HEATING ( First Revision ) 1. SCOPE 1.1 This standard covers the method for determination of loss on heating of asphaltic bitamens. 2. TERMINOLOGY 2.0 For the purpose of this standard, the following definition and those given in IS: $34-1965* shall apply. 2.1 Loss on Heating — The loss in weight (exclusive of water ) of oil of ‘3 bituminous material when heated to a standard temperature and under specified conditions. 3. APPARATUS 3.1 Oven —A double-walled chamber, rectangular in form, interior dimensions not being lew than 292 mm in height from the top of the hhoating clement to the top of the chamber and not les than 298 mm ia width and depth. The chamber is provided on one side with a tightly fitting hinged door containing a doubleglass window, at least 100 mm square, through which the thermometer may be read without opening the door.’ Ventilation of the oven is provided by means of either one round ‘ventthole in the top and one in the bottom of the oven, or one round vent: hhole near the top and one niear the bottom on each of the two sides of the oven, the diameter of each venthole being 12 to 16 mm. Heating of the oven is done Ly means of electricity and the temperature is maintainee within the limits specified! for the teat, 3.2 Perforated Metal Shelf — A perforated metal shelf approximatel: 250 mm in diameter; an alurainium shelf of the form and dimensions show! in Fig. 1, is recommended. ‘The shelf is placed in the centre of the ove! "Glomary oF trams relating to bitumen and tar (ried). 7 Bs: 1211-1978 11212-1978 . svith respect to all dimensions ofthe interior ofthe oven, ands suspended a Bye Gene lt nd poe wih chia moo oot we Put of t06 renin 3.3 Thermometer —A thermometer graduated in centigrade dogrees, ‘and conforming to the following requirements shall be used Liquid Mercury Filling above liquid [Nitrogen gas ‘Temperature range 155 to 170°C. Subdivisions osc Longer graduation lines at each 1°C Graduations numbered at °C, 155°C, 169°C and 170°C Immersion Total Total length 150 to 154 mm Bulb length 100 15 mm Bulb diameter Not larger than stem diameter Stem diameter 601070 mm Distance of bottom of bulb to ‘graduation line: AcOG. 38 to 38 mm Av 155°C. 70 to 80 mm Distance of top of thermometer 20 to 30 mm to graduation line at 170°C Top finish, Glass ring. Seale error at any point when 05°C standardized, Mat 3.3.1 The top of the contraction chamber shall be not more than 41 mm above the bottom of the bulb. 3.32 The expansion chamber shall permit heating the thermometer at ‘ast 25°C above the highest temperature on the scale. 333 At the i SEARS Ieg polos thether mometer shall be graduated ffom —1°C 394 The thermometer shall be 33 le shall be supported fom the shaft of the metal {2g vewial positon, approximately 20 mim inside the periphery of ‘shelf with the bottom of the bulb 6 mm above the shell c = of met swith Intereal de meeal OF las, cylindrical in shape with a flat bottom ameter 85 mm and internal depth 35 mm. 99 151 1292-1978 4. PROCEDURE 4.1 Stir and agitate thoroughly the material as received, warming, if necessary, to ensure a complete mixture before a portion is removed for the text. 4.2 Heat the container in an oven at 100 to LI weigh. Weigh into the container 50-0 0 to the nearest 0°01 g. \0°C for 30 minutes, cool and 5 g of the material correct, 43 Bring the oven to a temperature of 163 + 1°C and place the sample container in the revolving shelf near the circumference of in one of the oceates if the recommended shelf is used. Close the oven and rotate the shelf during the entire test at a rate of 5 t06 rev/smin, the temperature being maintained at 163 +b 1°C for 5h after the sample has been intro- duced and the oven has again reached the temperature. ‘The 5 hour period shall start when the temperature reaches 162°C. in no case shall the total time, during which the sample is in. the ‘oven, be more than 5 hours 15 minutes. ‘At the end of the specified Theating period, remove the containers, cool to room temperature and ‘weigh t0 001 g. 4.3.4 In ordinary circumstances, a number of samples having about the same degree of volatility may be tested at the same time, but samples varying greatly in volatility shall be tested separately. However, when extreme accuracy is required, only one material, that is, two containers shall be placed in the oven at one time. 44 When the penetration of the sample after heating isto be determined, imelt the residue in the container at the lowest postible temperature and thoroughly mix it by stirring, taking care to avoid incorporating air bubbles in the material, Pout the residue into the container specified under 3.1 of IS: 1203-1978" and from the pouring stag> follow the procedure as described under 4.1 of IS: 1203-1978 5. REPORTING 3.1 Report to the nearest 0°05 percent the mean percentage lost in weight for the duplicate determinations, correcting for water content, if ‘any. Report alto the water content, Methods for tenting tae and bituminous materia: Determination of penetration (fos retson 100 1S: 1212-1978 6. PRECISION 6.1 Results of duplicate tests shall not differ hy more than the following: Loss on Heating Repeatability iil pL tpeatability Reproducibility 0 005 or 02 O5t0 10 02 oF 10020 03 os Above 2-0 10 percent of mean 20 percent of mean Nore — In this cave the repeatability fgstes refer to the derences between duplicate determinations made stmultaneotaly'in the ‘ave ovens’ ueTenee? Bet 7. PRECAUTIONS 74 Conduct the loss on heating test in duplicate, 72 Determine the water content of the sample in accordance with the method for determination of water content specified in 1S: 1211-1978°, 17.8 I the sample contains water, tet it in that condition, 7A Reject the tests during which samples show evidence of loss by foaming. {Methods for epg tar and bituminow mater : (Beso snd ba ets (fon) a ee 11 18:1213-197, Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DISTILLATION TEST ( First Revision ) 3. SCOPE 1.1 This standard covers the methods for the distillation test for crude coo tar, road tar, cutback bitumen, Digboi type cutback bitumen and ereosot and anthracene oil 2. TERMINOLOGY 2.0 For the purpose of this standard, the following definition and those give in 18: 334-1965" shall apply. 2.1 Distillation — The process by which the more volatile constituent ‘are separated from the less volatile ones. 3. METHOD A ( FOR CUTBACK BITUMEN ) 3.1 Apparace: SAA Distillation Flask — 500 ml, side arm having dimensions 2s shows in Fig. L. BALA The distance from the centre of the side tube at the junetior of the neck to the top of the neck shall be 12 ++ I mm. 3.A.L2 The side tube shall slope downwards from the junction wiel neck so that the acute angle between the side tube and the neck is 75 +t 3. 3.4.2. Thermonder ~ of high dailaon, total immersion type, graduates in centigrade dogrcs ax specified, having a tange of 2't0 400°C ane ‘conforming to the following requicements Liquid Mercury Filling above liquid Nitrogen gas ‘Temperature range 210 400 “Glemary oft ating ten and tr (ie 103 191 1213-1978 All dimensions i millimetres, Fro, 1 Disritiation Fras Subdivision ‘Total length Stom diameter Bulb diameter Bulb length Distance of bottom of bulb to ‘graduation line at 0°C ‘Top finish Longer graduation Fines at each Graduations numbered at cach ‘multiple Immersion Seale error at any point up to '370°C shall not exceed. re 378 to 364 mm 6-0 to 70 mm [Not larger than stem diameter 10 to 15 mm 25 to. 45 mm Glass ring. sc 10 Total re 3.1.3 Condenser ( Water) — A250-mm__glass-jacketed condenser ( Fig. 2) with the dimensions and tolerances given below: ‘Length of jacket excluding the necks 250 kt S mm. Outside diameter of adapter of 234 1mm condenser tube Length of adapter 15 & Smm 108 18:1213-1978 Outside diameter of condenser 125 £05 mm tube proper Overall length of condenser tube 479 4: 25mm Tseuding adage 3.14 Adapter — of curved design ( se Fig. 2 ) having a heavy wall ( one millimetre ) and reinforced top glass, with an angle of approximacely 105° and with a diameter at the large end of approximately 18mm. ‘The outlet fend shall be ground to an angle of 45 5° with inside vertical. The small end shall have n diameter of not less than 5 mm. |--rhememeer eek ake epi tare Bihan) Rese TTT Fic. 2 Distiutarion Apparatus AsstMmiy 3.5 Shield — of galvanized iron, lined with 3-mm asbestos, fitted with transparent covered windows, of the form and dimensions shown in Tig. 3; used fo protect the flask from air currents ard to prevent radiation, ‘The cover ( top ) may be of transit board made in two parts, or it may be of ‘galvanized iron lined with 3-mm asbestos. 3.1.6 Crow Receivers — of 25 ml, $0 ml or 100 ml size and of dimensions and tolerances shown in Fig. 4 may be used. cell Rete Container — The container for the dalton ese shall 4350 g metal container approximately 76 mm in diameter snd 94 mm deep, provided with a lid. Ps 2 105 11 1213-1978 3-2 to: u7t2 129420 yet + a 3 Ts asta!" wis eats sotzit lec ELANGED OPENED CYLINDER TWO MICA WINDOWS MADE OF 28 HT ANGLE TO 2mm. ASBESTOS LINING eto RIVETED TO METAL dimensions in miimetres. Fie, 3. Sim oe ee ones Paha eS ils Lage rte fe ary cima mem hg ean So ih be ode el Sea ce oa ea he Tso a aes rca one on tae nis mt a "~“#iethods for testing tar and bituminous materials : Determination of water contest oS a ga 106 18112131978 ronaas al Fic. + Crow Rucnivers 100 mil, $0 ml axp 25 ml 3.2.1.1 Thoroughly stir and agitate the sample if necessary to ensure a complete mixture. B22 Assembly of Apparatus 9.2.2.1 Support the flask on a tripod or ring over two sheets of 1S 20 nesh wire gauze, 150 mm square (14 Fig. 2). Connect to the condenser tube by_a light cork joint. Insert the therinometer through a cork in the aeck of the flask with the bottom of the bulb € mm from the bottom of the Ala, the axis ofthe bulb of the flask through the centre of the neck being ‘vertical and the thermometer aligned on this axis, 32.2.2 The distance from the neck ofthe flask to the outlet end ofthe adapter shall be not more than 700 mm and not less than 600 mm. The ‘bumer should be protected from draughts by a suitable shield or chimney (se Fg. 3) 32.2.3 Adjust the adapter over the end of the condenser tube so a8 to {onduct the distillate into the receiver. During the dstilaion, cover close- Jy the top of the receiver witha piece of blotting paper or its equivalent, 107 1S: 1213-1978 Which shal bo cut soa tf the adapter ighty. Theadapter shall extend into the receiver at Teast 25 mm but not below the 100-mi mark 3.2.3 Distillation 32:34 Messe 200 ml of the material int the Mak, aumble the sppatatus and heat ao that the first drop comes ever in 5 fo 18 minut, Adjust the wate of dnillaton betwoen $0 to 70 drops per minute except {hat near the end ofthe distillation the heat input shal hot be 20 rapid so to result n'a temperature in exces of 300°C, 3.2.3.2 Should the sample foam, the distillation rate will have to be reduced, but the normal rate shall be resumed as soon as posible. Té ces foun pest, the dilation may be more ealy contolled by ‘applying the flame near the edge of the bulb and not at the centre. 3.2.3.3 Collect the distillate in the crow receivers and record the volume of distillate at all specified temperatures. Record also the volume of any separate water. When the maximum specified temperature of the test is indicated by the thermometer, discontinue the heating and drain into the reesiver any oil which may remain in the condenser tube. Measure by volume the residue and keep it for farther tests, B.2A Procedure for Handling Residue 3.2.4.1 When the temperature reaches 360°C, extinguish the flame and immediately (within, 30 seconds) pour the residue into the residue container, placing thns on its lid to prevent too rapid cocling at the bottom. 3.24.2 Allow the residue to cool in » position free from draughts to a temperature that is below its fuming point and at the same time suitable for pouring. 3.2.4.3 Stir the rosidue and pour into che raceptacles specified for testing for properties, such as penetration and softening point. 3.3 Report $3.1 daphalic Residue — Caleulate the percent residue to the nearest 01 R= [(200— TD) /200} x 100 where R = residue content, in volume percent; and TD = total distillate recovered to 360°C, in ml, 3.9.1.4 Report as the residue from dsillation to 360°C, pere volume by difference. a 108 1s: 1213-1978 3.32 Taal Distiller — Calculate the percent total distillate tothe nearest o-1 as follows: Tb percent = ( TD/200) x 100 33.24 Report as the total distillate to 360°C, volume percent, 3.3.3 Disillate Fractions 333. Determine the percentage by volume of the original sample by diitiing the ebserved volume {in millitres) of the fraction by 2. Report to the nearest 0" as volume percent as fellows: Up to 190°C Up to 225°C Up 1 2506 Upto 316°C. 5.3.8.2 Determine the percentages by volume of total ditillate by dividing the observel volurne in militres of the fraction by dhe maliitres serail to 360°C and taultiply by 100., Report to the nearest O'1 as the: ‘Eldlite: volume percent of total distillate to 360°C a9 follows Up to 190°C Up to 2256 Up to 260°C Upto 316°C 3.344 Where penetration, viscosity, of other tests have been carsid out report with reference to this method as well asto any other method used, (Eeample, “Penetration according 18: 1203-1970" of residue as. in 187 1215-1978"). 3.3.5 If the first fraction obtained contains water, note the volume ot water’ Deduct this form the volume of oll taken and correct all the Racine to 2 percentage based on the volums ofthe water-frce sample. 3.36 A convenient method for determining the volume of water is te transfer this fraction, after noting the volume, to a tube or cylinder graduated in Orl ml and to add about 15 t0 20 mi of benzol. This almos flay ays causes a clear separation between the oil and water, 3.3.7 Barometric presture correction as stipulated under 8 shall be applied where necessary. 3.4 Precision — Duplicate results shall not differ by more than the following : Repeatability Reproducibility 2 ml distillate 4 ml distillate FRicthods for tating tar and bitominous material: Determination of penetratio (nstncion). 109 1S: 1213-1978 Which shall be cut so as tofit the adapter tightly, ‘The adapter shall extend into the roceiver at least 25 mm but not below the 100-ml mark. 3.2.3 Distillation 3.2.3.1 Measure 200 ml of the material into the flask, assemble the apparatus and heat so that the first drop comes over in 5 0,15 minutes, Adjust the rate of distillation between 50 to 70 drops per minute except that near the ond of the distillation the heat input shall hot be so rapid a8 ‘0 result in a tomperature in excess of 360°C. 3.2.3.2 Should the sample foam, the distillation rate will have to be reduced, but the normal rate shall be resumed at soon as possible. It excess foaming persist, the distillation may be more easily controlled by applying the flame near the edge of the bulb and not at the centre. 3.2.3.3 Collect the distillate in the row receivers and record the volume of distillate at all specified temperatures. Record also the volume of any separate water. When the maximuma specified temperature of the test is indicatod by the thermometer, discontinue the heating and drain into the recsiver any oil which may remain in the condenser tube. Measure by volume the residue and keop it for farther test. 3.24 Procedure for Handling Residue 3.2.4.3 When the temperature reaches 360°C, extinguish the flame and immediately (within, 30 seconds} pour the residue into the residue container, placing this on its lid to prevent too rapid cooling at the bottom, 3.24.2 Allow the residue to cool in a posi ion free from draughts to a femperature that is below its fuming point and at the same time suitable for pouring. 3.2.4.3 Stir the residue and pour into che raceptacles specified for testing for properties, such as penetration and softening point. 3.3 Report 3.31 Asphalic Residue — Calculate the percent residue to the nearest 0'1 as follows R (200 — TD} /200} x 100 where R = residue content, in volume percent; and TD = total distillate recovered to 360°C, in ml, 3.3.14 Report as the residue ffom distillation to 360°C, percent volume by differenee. 108 15: 1213-1978 3.8.2 Total Distillate — Calculate the percent total OL as follows: late tothe nearest TD percent = ( TD]200) x 100 3.3.2.1 Report as the total distillate to 360°C, volume percent. 3.38 Distillate Fractions 35.3.1 Determine the percentage by volume of the origial sample by dividing the observed volume (in mililitres) of the fracton by 2. Report to the nearest OI as volume percent as follows Up to 190°C Up to 225°C Up to 260°C Upto 316°C 333.2 Determine the percontages by volume of total distillate by dividing the abserved volume in millitres ofthe fraction by the malilitres ecovered to 360°C and multiply by 100,” Report to the nearest OT as the Uisllte, volume percent of total distillate to 360°C as follows: Up to 190°C Up t0 225° Up (0 260°C Upto 316°C 3.3.4 Whore penetration, viscotty, or other tests have been carried out, report with reference to this method at wellas to any other mahod used” (Example "Penetration according “18: 1203-1978" of residue aa. in Is: iz1-1978"), 3.3.5 If the fret (raction obtained contains water, note the volume of water. Deduct this from the volume of oll taken and correct all the fractions to.a percentage based on the volume ofthe water-rce ample. 3.3.6 A convenient mothod for determining the volume of water is to transfer this fraction, after moting the volume, to a tube cr cylinder sgraduated in 0-1 ml and to add about 15 to 20 mi of benzol. This almost aly .ys causes a clear separation between the oil and water, 3.3.7 Barometeic pressure correction as stipulated under 8 applied where necessary. hall be 3.4 Precision — Duplicate results shall not differ by more than the Illowing: * Repeatability Reprodvibility 2 mil distillate 4 ml distillate “Methods for tesiog tar and bituminous materials: Determination of penetration nntnsion. 109 13-1978 3.5 Precaution — During the progress of distillation, the thermometer shall remain in its original position. No correction shall be made for the ‘emergent stem of the thermometer. 4. METHOD B (FOR ROAD TAR) 4.1 Apparatus 4.1.1 Distillation Flask — A flask with dimensions and tolerances a: given below shall be used: Distillation capacity, ml 750 Capacity of bulb, ml 975 4 20 Internal diaineter of neck between side 21 ‘aper and bull, mm Internal diameter of side tube, mm 85205 External diameter of side tube, mm 10205 Length of side tube, mm 1605 Radius of curvature at the bate 2 ‘of the neck, mm ‘Thickness of walls of bulb neck 10 to 15 ofsside tube, mm 4.11.41 The distance from the centre ofthe side tube of cach flask at the junction of the neck tthe top ofthe neck ahall be 75/49 mm. The distance from the centre of the side tube ofeach flask atthe junction with the neck to the liquid surface, when the flask is vertical and contains a quantity of liquid equal in volume to the dvlation capacity ofthe fas, Shall be 90-43 mm. may 4.1.2 Thermometer —same as for Method A { s¢ 3.1.2). 4.1.3 Air Condenser — made from a straight tube of good quality retistance glass, with one end finished square with the axis and the other end ground at an angle of 45° with the axis and conforming to the following dimensions: Tnternal diameter 20+ 1 mm Overall length {600 + 10 mam Wall thickness 10 to 15mm 4.1.3.1 The side arm of the flask shall extend at least 25 mm beyond the cork in the upper end of the condenser. 10 1:1213 -1978 AA Drought Screen — rectangular, made of 0711 mm Standard Wire Gauge sheet metal, with the dimensions shown in Fig. 3 and open a& top dnd bottom and complying with the following requiremen’: In each of the two narrow sides of the draught screen there shall be two circular holes, 25mm in diameter each, and situated a illustrated in Fig. 5. In each of the four sides of the draught fereen there shall be three holes with their centres 25 mm above the base of the draught screen, These hole shall occupy the pos tions asshown in Fig. 5. ‘The diameter ofeach of the holes centrally Situated in the longer sides shall be 25 mm and of the remaining ten holes 12 mm, Atthe middle of each of the wider sides a vertical slot with the dimensions as shown in Fig. 5 shall be cut downwards from the top of the sereea. ‘Ashect of hard asbestos of silica board. 6 mm in thickness and having a central circular hole 110 mm in diameter, shall be supported horizontally in the screen and shall fit closely to the sides of the aereen to ensure that hot gases from the wourer of heat do not come in contact with the sides of neck of the flask. The flask shall be placed. in position and presed down so as to close completely the Foe in the board. ‘The supports for this board may conveniently consist of triangular pieces of metal sheet fraly fixed to the screen Sti four comers. In one of the narrow side of the screen a door shall be provided, haaving the dimensions and position as shown in Fig. 5. Tn each of the narrow sides of the screen a mica window shall be placed centrally, with bottom of the wind level with the top of the asbestos she The dimensions and position of the windews shall be as shown in Fig. 5. 4.1.5 Crow Receiers — same as specified in Method A (se 3.1.6). 42 Procedure (LEER pean of he Sample —same as speed in Maso A 4.2.2 Assembly of Apparates — Set up the distillation flask complete with sherman, Sica and een he anaomncer sal he 98 fteed inthe ask that the bottom of the capillary i level with the lower de of the sde tube joint and the immersion mark ia level with the top ofthe cork. 42 Dislaion 4.2.3.1 Weigh 7500 + 0°5 g of the material into the weighed distill. ation flask, and assemble the apparatus, using the 25-ml receiver to collect the first fraction. Place this and the subsequent receivers so that the am sao =_— >| _ | “ie le ' — como || | om en oe a eee ee Tio, 5 Dravonr Scrssx — cond ometer indicates 200°C within 35 + 5 min from the start. Ce Vhon examining tars which are liable to froth on heating, it may Jn the maximum. specified. period 0035 25 mints. “Only in the withif, of such tars which froth excesively may the preliminary period o heativent, record the time taken to reach 200°C. Caley stil, adjust the flame so 5 mil of distillate collect in not less than 54 but not more thar a Ot ea ctiatlaton tate, which corresponds to 90 0° mnie pee 8 onl in shy recur any extend over 78 the wept tion and if the cullection of any 5 ml extends over less than aoe tha a¢ cast 165 but not more than 195 seconds. 7: OVE 49.3.4 Ifin any test, the conditions specified in 4.2.3.3 are not et, the Fe material. of th = 12 1811213 «1978 4.2.3.5 The specified distillation rate. corresponds approximately to 90 drops/min or 3 drope in each 2 ld be taken only as a guide. " Graduated receivers should be used for the collection of the dines Fite so that the time taken to coliect each 5 ml may be kept under close observation, 4.23.6 Make a rocord ofthese times throughout the test so that compli- ance with the distillation requirements may be subsequently checked 4.2.3.7 When the thermometer indicates 200°C, replace the 25-ml receiver by another receiver which has been warmod immediately before use, s0 that naphthalene is prevented from solidifying on it inner wall aed thus interfering with the checking of the distillation rate 4.25.8 Take the other fraction at 270°C and 300%C of at sich other temperatires as may be specified, in the 100ml receives, the etosktey being changed without interupting the distlaton 4.2.3.9 Extinguish the Bunton Hame immodiaely the highest specified temperature is reached. Include, im the Anal faction, eituiner a ics from the condenser within five minutes after the fame fe estingutie 4.2.3.0 Should solids tond to deposit during dstilation, warm the condenser so that such solids are collected in the fraction with ‘which *hey 423411 Ascer:ain the weight of the distillate to 200°C. in g, note the volume of the water and, assuming a density of 1-00 gil, second she ois frente rams ind the weight of the light ofl inthe faction up to 200°C by diflerence. Determine the weights of other fraction in he 42.3.12 In addition, note the volumes of the fractions ‘up to 200°C’ and ‘200 to 270°C and ‘reserve for use in connection with the deere, ration of phenols (see IS :1218-1978*). 4.2.3.3 Keep the flask with the cork and the thermometer in Position for one hour after the flame has been extinguisied, Then weigh be fask and cesiduc, after which mix the contents of the flask. thoroughty by shaking. Pour out half. Again shaue the remainder and dete softening point by the method ilustrated in 1S: 1205-19761, 43 Report Carry out the stilton tt and report the szarat fesults and the average as percentage by weight on the sample, “ears? ‘the time in seconds for each 5 ml of ‘distillate. . . Methods for wating tr and hituminows material: Determination of shen (first revision ). oa! oo eltfcthsforteing tar and bituminos materials: Determination of softening point ns 1811213 1978 4.3.1 Barometric pressure correction as stipulated under 8 shall be applied where necessary. cision —The ean of two, souls conducted by the ae to Peer Raia net Mier ome" mean ofthe two raul ia Bod laboratory by more than the following: *) mores 1 percent mn 3 amaoee rofl ®) Sumaant) Set ln ratte 9 Sees) 5, METHOD € (FOR CRUDE COAL TAR) 5 Apparstee S14 Disljon Flask — same a8 specie in Metbod B (4 AA). 512 Theron same a speed in Method A (3.4.2). 513 Air Gndawe— same a specie in MetiodB (1 4.43). SAA Mast Heating ath (Se Fig. 6) — The bath sal contain fle oy ‘melting below 70°C in such quantity that when, the botom ofthe Haskin’ mu from the bottom of the bath, the level of the mo About 13min below the rim of the bath a lange Central, : Tare of Four Pit or Similar Device to Retain Flange 1 Theo Fg aad ow sr ota Ove Pace, "Al dimensions in milimetes. Dimensions in misime. Fro, 6 Meta Hearino Bars .L.S Crow Rececers — same as specified in Method A (ser 3.1.6). 4 81 1213-1 52 Procedure 5.2.1 Prparation of Sale — same a8 specified in Method A (03.2: 5.2.2 Auumbly of Apparatus —Set up the ditilaion flask az Method 8 (ie 422). p22 Sete btm afte Aa ont ino fame Hat fusible metal to a temperature slightly higher han ie mekenn pein Jmmerse the faa centrally in the bath the botiom of We EEL Boag least'5 mm above the bottom ofthe bath 5.2 Disillaion— Take 250 ml of the material and carry out ¢ gation seaily a the rate of 9 mlm and ithoat mepsag distillation, collect oll fractions separately in the graduated rereine: a) Up to210°C b) 210 to 230°C. ©) 230 to 270°C. 4) 270 to 300°C ) 300°C to the stage of pitch 5.2.3.1 Should solide tend to d condenser so that such solids are col ‘come over. 5.3 Report osit during the distillation, warm tk ted in the fraction with which the acts afta of anthracene and cool the fractions to 19°54 03°C." Reg, Fhe, omperature, with occasional stirring, till solide seaaraie out ci A hours, whichever is lex, and report the rest of this observation oc te, Poneentage of oil draining out of each fraction in whieh solide make, appearance. 333 Barometric presture correction at stipulated under 7 shall be applied where necessary. & METHOD D (FOR GREOSOTE AND ANTHRACENE O11.) 6.1 Apparatus $:11 Divivion Flask — A ask with dimensions and tolerances as given below shall be used: om wa Distillation capacity 150 mi Capacity of bulb 1 at 5 181 1213 «1978 Internal diameter of neck 18 4 1mm ‘between side, taper and bulb Internal diameter of side tube 50405 mm External diameter of side tube 7-0 4 05 mm Length of side tube 1204 4mm Radius of curvature at the base of 10mm ‘ack Thickness of walls of bulb, nock, 08 to 1-2 mm fide tube 6.1.2 Thermometer — sine a8 specified in Method A (1 32.2). 6.13 Air Condenser — same a specifica in Method B (se 4.1.8) 6.14 Drought Seen — same a8 specified in Method B (ote 42). 6.15 Rectvers — same a8 specified in Method A (se 3.6). 6.2 Procedare 6.2.1 Prepratio of Sample — same as specified in Method A (se 32.1). 6.2.2 Anembly of Apporas— saroe a specified in Method B (se 422). 623 Distillation 6.23.1 Thoroughly mix the sample a prepared under 6.2 2sovmitak,” Weigh 100105 got nntte ely ino ae weed digtlation flask and star the ivlation, wing the naked flame of the Sumner, Continue the distilation at the fate of 50-3 09 ml per minute Hitoe any rengon the distillation rate falls outside the specified mis at amy ime after the frst 9 inl of distilte have collected and before the Binal Specied temperature ir roached, discard the tet andl start another test on a ‘btther portion of the materia 6.2.3.2 Te specific distilation rate corresponds approximately t0 90 ropa por minute or three dropr in each two seconds, but this should only te taken asa guide, Graduated receivers should preferably be used for the ealecton ofthe isiatein order thatthe rate fm millittes per minute nny be kept rnder clos observation. 6.2.3.3 Change the receiver at each specified temperature (1 6.3) without stopping the distillation, Extinguish the lame sehen the thermo- Jneter reaches the highest spectied temperature, and include in the final faton theo with dite he idea win Be wnt afr therlamne has beon extingushoa.” Should solide tend to deposit during U Ailton, warm the condemer so that such solids are collected in the fraction with which they come over. 6.2.34 During. the progres of dlatilation, che thermomccer shall remain init original positon, No correction’ shall be made for the ‘imargent stem of the thermometer ne 1811213 -19 6.3.1 Report the cumul ing ranges of temperatures: 0 to 210°C. 010.2356 Oto 315°C 0 t0 255°C. 6.3.2 Also, report the weight of the residue 6.3.3 If the first fraction contains water, determine theamount of wat Deduct this amount from the weight of oil taken for the test, and report the fractions at percentage by weight based on the weight ofthe water ive weights of fractions obtained at the follo 6.34 A convenient method for determining the amount of wate i tranafr ths faction, aftr weighing, toa tube of eyinder gradu Ol and to add 191020 malo bene. thi amt aways Sons cle separation Between theo and water and asnuming a dens of 1.00 the weight of water can be calculated. : ae aphid Bugmeri, prere comecton ax apulated under 8 sha 7. PRECISION 7A The duplicate results shall not differ by mote than the following Repeatability Reproducibility Up to 2300 16g 358 Up to 280 to 315°C. 15g 34g ‘Total distillate 178 17g ‘8, BAROMETRIC PRESSURE CORRECTION Bal Ifthe barometric pressure during the period of test remains within FER of 700 5 mm, no correction new be applied othe specie di lation temperatures. If the pressure is beyond that range, apply the fol ing correction to the specified temperatures: Correction for temperature in degrees centigrade = 0-000 12 (760— P) (4-42: where f= corrected barometric presure during test, and 4m specified temperature in degrecs centigrade, nr 15: 1214 - 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF MATTER INSOLUBLE IN BENZENE ( First Revision ) 1. SCOPE. 11 This standard covers the method for the determination of matter insoluble in benzene for creosote and anthracene oil. 2. APPARATUS 21 Beaker — of 200-ml capacity. 2.2 Sintered Glass Crucible — of porosity No. 4. 2.3 Filter Papers —two, cach about 150 mm in diameter, grade Whatman No, 5 of its equivalent. 23.1 Filtering Funnel and Botle 3. REAGENT 3.1 Benzene — ordinary, conforming to 1S: 534-1965*. 4. PROCEDURE 4:1 Weigh accurately a minimum of 50 g of the well-mixed material into a conical flask and dissolve it by warming on a water bath in four times its volume of benzene, the flask being loosely covered. Filter the solution through either: ‘) the sintered glass crucible, oF ) the filter papers. 411 Method Using Sintered Glass Cruible—Dry the crucible at a temperature of 100 4. 2°C and weigh accurately when cool. Decant the solution through the dried and weighed crucible. "Speifcation for benzene (sind). ng 151 1214-1978 ‘Transfer any insoluble residue to the crucible by means of additional benzene, and wash the filter paper with benzene until afew drops of the ferate yield no residue on evaporation. Dry the crucible at a temper= ature of 100 42°C until itis of constant mass; allow it to. cool ina Aesiceator, and weigh correct to 01 mg. 4.41.2 Method Using Fer Papr— Counterpoted double filter paper shall bbe ued. For counterpoting, heat the two Biter papers to a tamperatare Of 100 42°C and resuce them to equal weight by removing the apex tthe heavier filter paper after folding. For filtering, use the ecu pipet {tsi the originally beaver paper so tha the separated material w eaiged by the inner paper yet both of them are equally subjected to any acon trerted by the of and benzene. Dry the Ber papers ata temperature of {oo 2°C ntl they are of constant weight, allow them to cool na desiceator and weigh correct to Ol mg. 5. CALCULATION 5.1 Caleulate and express the results as percentage by mass of the material as follows: Benzene insoluble, percent = 274 x 100 where A= mass of crucible or filter paper, B= mass of crucible + insoluble matter, and (C= mass of sample taken. 6. REPORT 61 Report the percentage insoluble in benzene to the nearest 0-1 percent. 7, PRECISION 7A The duplicate results should not differ by more than the following: Repeatability Reproducibility 1-0 percent 2°2 percent 8. PRECAUTION 8.1 The tolvent benzene is extremely inflammable. Handling of bensene shall be carried out away from any source of heat or flames. 129 a ————————— ee 3S: 3215-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF MATTER INSOLUBLE IN TOLUENE ( First Revision ) 1, SCOPE 1.1 This standard covers the methods for the determination of matter ‘naoluble in toluene for road tar and pitch. 2. METHOD A (FOR SOFT GRADE PITCH) 2.1 Apparatus 21.1 Beaker — of 200-ml capacity. BAZ Sintered Class Crucible — of porosity No. 4. 2.1.3 Filter Papers—two, each about 150 mm in diameter, grade Whatman No. 5 or ity equivalent. 23.1 Filtering funnel and bottle 2.1.4 Water Bath— maintained to constant temperature of 95 ++ 5*C, Glycerine may be used in place of water for temperature 95°C and above. 21S A 100-ml Graducted Cylinder 2.2 Reagent 2.24 Tolume— nitration grade, conforming to 18 : 587-1967, 2.3 Procedure 234 nonin 2 tetra 2 he orgy mid ea ee a ah tema at Geotail TRE A" MA ane as Ie Singha bae ac dager alc op aa eae ett so as SENET ag fot oe 0 ste “*Speidcation for tluene, pure, nitration grade (fist rision). a 1811215- 1978, 2.3.1.1 Method wing ler paprs— Counterpoised double filter shall bo used. For counierpobing, heat the two fiter papers to a tempe: ature of 106 + 2°C and reduce them to equal weight by removing the pet ofthe heavier paper after folding. For filtering, use the uncut paper inside the originally heavier paper, s0 that scparated' material is retained by the inner papes, yet both of them are equally subjected to. any. action exerted by dolicne. Wash the residue by repeated decantation, with toluene heated 995 + 5°C until $00 ml of toluene have been used in all Transfer the residue to the filter paper and continue the washing wi altogether 500 ml of hot toluene have been used. Dry the residue in an ven ata temperature of 100 2G unl ti of constant weight. 23:2 Method wing sintered slats crucible —Dry the crucible at a temperature of 100 4:20 and weigh accurately whan cool. Decant the toluene solution through the erveible using gente suction to seit Altre tion and avoiding. the transfer of the sediment. Wash repeatedly by dlecantation until 300 ml of toluene have been used. Transfer the sediment in the beaker to the crucible and continue washing ‘until 500 ml of toluene have in all been sed. Dry the reidue in an oven at a temperse ture of 100 sb 2°C until it's of constant weight, 2.3.2 Preserve the residue crucible for ash determination (see TS? 1217-1978"). 24 Calealation—Calevlate and express the result as percentage mass ofthe material taken for dh tet as fllows: - 7 Tnsoluble matter in olvene, 109 w, percent by mass ah either case with the filter paper or sintered where W, = mass of the dry material in g, and W, = mass of insoluble matter in g. 3. METHOD B (FOR SOFT MEDIUM, HARD MEDIUM AND HARD PITCH GRADES) 3.1 Procedure 3.1 Treat about one gram of the material, finely divided, if possible, and accurately weighed, with 100 ml of toluene at the laboratory temperature, in the manner described under 2.31. 3.1.2 Treat the residue in the beaker in exactly the same manner as described in 2.3.1 with a further 100 ml. of toluene at laboratory. temperature, ‘Then treat it with three successive quantities, each of “Methods for ‘eving tar and bituminout materials: Determination of mineral matter (ah) (ja rnin) 122 1811215 -1978 100 ml, of toluene at 95 45°C in exactly the same manner as described in 2.8.1 except that each setling period. during which the beaker i standing in the water bath need only be of five minutes. 3.1.8 Transfer the residue to the filter paper or sintered glass crucible ‘and continue the washing until a further 500 mal of hot toluene have been Used. Dry the residue in an oven at a temperature of 100 + 2°C until it is of constant mass. ALA Preserve the residue with the filter paper for ash determination (ste TS: 1217-1978"). 32 Caleulation — Calculate and express the result as percentage by mass of the material taken forthe test as tollows: Insoluble matter in toluene, yy, percent by mass = yy x 100K where Wy dry mass ofthe material, and 17, = mass of insoluble matter. 4. REPORT 4.1 Report the percentage insoluble in toluene to the nearest O'l percent. 5, PRECISION 5A The duplicate test results should not differ by more than the following: Repeatability Reproducibility 0°5 pereent 10 percent 6. PRECAUTION 6.1 The solvent toluene is extremely inflammable. Handling of toluene shall be carried out away from any source of heat or flames. Methods for ating tar and bituminour materials: Determination of mineral matter (ash) Got rien) 123 AMENDMENT NO, 1 APRIL 1984 To IS : 1216-1978 METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS : DETERMINATION OF SOLUBILITY IN CARBON DISULPHIDE OR ‘TRICHLOROETHYLENE, ( First Revision ) Alterations ( Peg 125, tle) — Substitute the following forthe existing ile: ‘Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS : DETERMINATION OF SOLUBILITY IN CARBON DISULPHIDE, CARBON TETRACHLORIDE OR TRICHLOROETHYLENE ( First Revision Y (Page 126, clause 2.6 formula) — Substitute the following for the 3g formula: “Matter soluble in carbon disulphide, yy carbon tetrachloride, or tichloroethye =—1>Ms_ x 199+ lene, percent . ( Page 128, clause 3.5, formula )— Substitute the following for the exiting formula: ‘Matter soluble in carbon disulphide, carbon tetrachloride or trichloror thy lene, pereent by weight Wi—Wy 100 Wet * 10) «sap Addenda (Page 125, clause LA, line 2)— Add the following after the word “carbon disulphide": “carbon tetrachloride (Page 125, cause 22:2)—Add the folowing new clause after 22:2 : «2.2.3 Carbon tetrachloride-technical grade, conformingto IS : 718 1977 (Page 125, footnote with ‘f° mark) — Add the following new foot note after the exiiting foot-notes: « Specification for carbon tetrachloride (second rviion).” (Page 126, clause 2.5, lines 3, 11 and 13) — Add the following afte the word *trichloroethylene » * or carbon tetrachloride” (Page 126, clause 2.6, line 2) —~ Add the following after the wor “ trichloroethylene * or carbon tetrachloride” (Page 126, clawe 2.6.1, ine 2)—Add the following after th word 'trichloroethylene " “or carbon tetrachloride * (Page 127, clause 2.7, informal table, frst column, heading) — Add th following after the word * trichloroethylene': “or carbon tetrachloride” (Page 128, clause 34, lines 6 and 10) — Add the following after th word ‘trichloroethylene “or carbon tetrachloride * (Poge 128, cause 3.6, lire 2)— Add the following after the wort “ trichloroethylene " “or carbon tetrachloride’ (wane 2) 182 1216-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF SOLUBILITY IN CARBON DISULPHIDE OR TRICHLOROETHYLENE ( First Revision ) 1. SCOPE L.A This standard covers the methods for the determination of solubility in carbon disulphide or tichlororthylene for asphaltic bitumen and native asphalt 2. METHOD A (FOR ASPHALTIC BITUMEN) 2.1 Apparatus BLA Gooch Crucible 2.2 Conical Glass Flask— of 200-ro capacity 2.2 Solvent 22.1 Cerbon Disulphide —redinilled grade, conforming to 1S : 717-1969*, 22.2 Tricloroetiplene — conforming to 1S: 245-1970. 2.3 Preparation of the Material — {f th> material contains water, heat it to a temperature not exceeding 130°C until the water has been removed, seine comanth, whey eee doing xing. Peon ths operaon 2.4 Preparation of Gooch Gracible — Insert shefiter tube inthe stopper of the filtering fuk, set the Gooch crucible in the Ger tube, and connect the flask to the suction pump. Fill the crucible with some of the suspen tion of asbestos ia the water, allow it to settle partly in the crucible and “= Sperifcation or enon dialphide eecal (Su ii) {Specification fr tichloroethpene echnical (seed atin) 125 1811216 -1978 Sf150°C. "Cool the crucible in the desceato, weigh and renee eae Ay Ber tube supported in the cleans dey ering fee 2-41 Inthe determination, the asbestos apparently absorbs irreversibly 4 zmall amount of soluble bitumen (usually I to 3 rele of ele hich is not removed by a subsequent washing with sohee. yatbes of asbestos used, therelire, shall be kept aah ensure reproducible result. ight in the specified limits to 2.5 Procedure — Weigh about 2 g of the dry material correct to the nearest OOO1 g into a 200-ml conical flask and add 100 ml of cate disulphide or trichloroethylene. Stir the contents of the flask, and then allow it to stand, loosely corked, for a period of one hours Filter ire Contents of the flask through the Gooch crucible prepared ay decried under 24 which has been weighed to the nearest O0OI g.. Molten tee gibestos pad with carbon disulphide before commencing’ filtration, ard filter at a rate of not more than two drops per second at Bee gi trichlorocthylene until a filtrate is obtained which is not discelee oy Allow the crucible to dry in air for 30 minutes, after which place it i ay gyen at 100 to 110°G for one hour. “Allow the crucible te coud aa a desiccator and then weigh. 26 Calculation and Report — Calculate the matter soluble in carbon disulphide or trichlorocthylene as follows: ‘Matter soluble in carbon disulphide oF trichloroethylene, percent where Wi = weight in g of dry sample taken for the test, and W,— weight in g of insoluble material retained in the Gooch crucible, 2.6.1 Report the result obtained in 2.6 to the nearest 0-05 percent as the matter soluble in carbon disulphide or trichlorocthylene of the dey material, 126 18: 1216 -1978 2.7 Precision —Test results shall not differ from the mean by more than the following ‘Metter Soluble in Carbon Repeatability Reproiucibility Disulphide or Trchloroethylone Below 98 percent 05, 10 98 to 100 percent or oz 3, METHOD B (FOR NATIVE ASPHALTS ) 3.1 Apparat 3.141 Glass Top Funnel — approximately 100 mm in diameter the stem fiwed with a tap and the top ground flat 3.1.2 Glass Plate — to cover the funnel, about 120 mm in diameter, witha hole of about 16 mim diameter in the centre. 3.1.3 Claus Fumnel—sinaller than that described, under 3.12, with it stem pasting through cork placed in the hole in the gts plate the lower end of the stem teaching approximately halfway ows the tap finnet A Filler Papers — tw, Whatman No. 5 or equivalent filter papers, 162 mim in Qtr, Sad ws nals oboe Sha at AMELIE ounterposed and folded togsther as shown ia Fig. (paren cue Fic. 1 Foupep Fintan Parer 3.22 Solvent and Material 3.2.1 Carbon Disulphide — redistilled, conforming to 1S : 717-1969. 3.2.2 Camen!—itable for sealing the glass plate to the funncl. Tk say be peopred wit 10" gat Bsns’ 30 cher oath faa Be ehyerine PY * Speciation far aon pide, eit i). 127 1511216 - 1978 3.3 Preparation of Sample — If the sample contains water, heat a I portion at a temperature not exceeding 130°C, the material being co tantly stirred when possible, until the rate of low in weight of the sample doce not exceed 0'1'g during a 15-minute period of heating. 3.3.1 Ifthe loss in weight on drying exceeds 0-1 percent, determine water content of another sample of the material in accordance with 1S: 1211-1978 3A Procedure — Dry the two filter papers (st# 3.14) in an oven at 100 to 110°C, cool in a desiceator, counterpoise, fold together as illustrated in Fig. 1 and place in the tap funnel. Weigh about 2-g of the dry material, as prepared in 2.3, correct to the nearest 0-001 g in the filter papers and Soctze the cover to the funnel by meant of the eement. Now add carljon disulphide or crichloroethylene through the small funnel until the filter paper is about half filled, and then allow it to stand for 30 minutes. Draw the solution off through the tap. Place a watch glast on the small funnel to ‘minimize evaporation. Close the tap and introduce a further quantity of carbon disulphide or trichtoroethylene through the small funnel and again draw the solution off after 30 minutes. Repeat this procedure until the solvent draw off is no longer discoloured. When the filtration is completed, remove the cover and allovr the filter papers to dry in air for 30 minutes before placing them in a ventilated ait oven at 100 to 110°C for one hour. ‘Next place the filter papers in a desiccator and when cool, weigh the inner filter paper and contents, using the outer filter paper as a counterpoise. 3.5 Calculation — Calculate the solubility of the dry material as follows: ‘Matter soluble in earbon tc io eee = (agg 18) aul, where Wi = mass in g of the dry sample taken for the test W, = mass in g of recovered insoluble matter; and W = water content of sample, if determined. 346 Report — Report the reult obtained in 3.5 to the nearest 008 peresnt ethe matter soluble in carbon dnulphide or teichorocthytene, 3.7 Precision — Test results shall not differ from the mean by me the following: Repeatability 05 Reproducibility os Methods fr teing ta ar! Dituminous mateiak: Determination of water copteat (Dean and Sark soethod} (fat rin Je 128 1S: 1216-1978 4.7.4 Those preconfigured not include any allowance for diferences due to variations in sampl 4 mancauTON rg ee i al tm fhe ni ett a ae Se eee cess tomentsoreee 4.2 The vapours of carbon disulphide are toxic and adequate ventilation shall be provided. 129 18: 1217-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF MINERAL MATTER ( ASH ) ( First Revision ) 1, SCOPE A.A This standard covers the method for determination of mineral matter (ash ) for crude coal tar, piteh and other bituminous products. 2, APPARATUS 2.1 A porcelain or silica erucible of 30 ml capacity. 3, PROCEDURE 31 Thoroughly clean and dry the crucible in an oven. Cool ad. eigh (fom aims? a te thoroughly ed voir a he ercible and weigh (8). "Heat the crucible gently on s hot plate gradual IScrceing the pb fe femve volaide mais wifvout low. Beamer due to violent cbulltion, Finally, heat the crvible in a mole furnace. at a emperatare high enough to complete the incineration, Cocl to 100°C dnd place it n'a desiccator and weigh. Repeat cooling and weighing, Ul) a constant weight is recorded (¢). 4. CALCULATION 4.1 Calculate the percantage of ash content on the weight ofthe tar taken fn moanturesfice basis fellowa! Percentage ofash content =f 8 x 100 where 4 = mass of crucible in g, b= mam of crucible and moisture free sumple in g, and ¢ = mass of erucible and ash in g Ist 18: 1218-1978, Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF PHENOLS ( First Revision ) 1. SCOPE 1.1 This standard covers the method for the determination of phenols for road tar. 2. EXTRACTION 2.1 The phenols shall be extracted by a solution of sodium hydroxide and the extract shall be boiled to remove neutral oils and basos, ‘The phenols shall then be liberated by the addition of hydrochloric acid conforming to analytical reagent grade of 1S: 265-1962" and their volume shall be 3. APPARATUS. 3.1 Phenols Flask — of glass, conical, with ¢ long graduated neck and of the shape, dimensions and tolerances as shown in Fig. 1 and as given below Capacity 200 10 mt Maximum permissible error on eapacity: £01 ml ‘corresponding to any graduation mark Maximum permissible dfferenve between £01 ml the errors at any two graduation marks 3.2 A Beaker of Suitable Size 3.3 Separating Funnel Stoppered 3A Any Suitable Thermometer — covering a range of 40 t» 70°C. "Speciation for hydrocbleie acl (seced) 33 15 11218-1978 ‘At least 25mm Min, 125mm Not to exceed tH Max. 150mm Fic. 1 Paxxous Frask 4. REAGENTS 4.1 Sodium Hydroxide Solutien—10 percent m/m clear aqueous solution 42 Hydrochloric Acid Concentrated — conforming to analytical reagent grade of IS : 265-1962" *Specienion for bydvochloric ae (nd). 1m 11218 -1978 4.3 Sodium Chloride — dry powdered. 44 Methyl Orange Indicator —0'1 g of methyl orange dissolved in 100 ml of warm distilled water. 5, PROCEDURE 5 Warm, ifnccenary, the oil ditiling eo 270°Cin the distillation tet se Meso Bot 18 21-1278) un empl Hou, nd trae he ale ‘of te ell to a Roppered separating funnel of appropriate capacity, Rinse Te recetvers dm tehich the disilltes were tranerred with a equal volume fof'a clear aqueous 10 percent ( by mass) solution of sadium hydroxide, Previously heated to between 40°C and 70°C, and add to the oil in the Eeparating funnel, “Agitate the contents of the funnel vigorously for five minutes, and then allow i to stand. 5.2 Mr ic has setled, run the alkaline layer into a beaker, Agitate the Upper layer for five minutes witha further quantity of hot sodium hydro Nlde solition, equal tone quartee” off the volume. ofthe dstllate hich is being wasted, and with further succesive quantities of the hot fouluns hydrosie solution, each equal in volume-to the last, until all the Phenols have been removed, Dating the wathing proces, keep the con {ents of the fare in a liquid condition, immersing the funnel, it necesary Fi Nearm water af 40 t0 70°C 52.1 The complete removal of phenols can be ascertained by slightly aciddving the last washing with concentrated hydrochloric acid conforming to analytical reagent grade of 187265 - 1962} and examining for separated phenols, A large exciss of sodium hydroxide shall be avoided, but some Uxces shovld be maintained. Ara ough guide, 25 ml of sodium hydroxide selution ofthe strength indicated may be taken a suflcient to remove about 5 ral of phenols. 52.2 Reservethe tar diaillate ater removal of phenols forthe determi tion of naphthalene (see 15: 1219-1970). 53 Collect the alkali extracts, including any portion acidified, for the Bitpon of teting, “Make se chat he combiged wings ae alae Bol vigorously for 20 nue using fragments of porus or other suitable rt_ material to prevent bit oly and i the extract i clear, transer direct to the phenols ak. 5.3.1 If it be expected that the tar coutains 3} percent or miore of phenols, the boiled ‘washings (after filtration through last, wool i bos for eng tar an bituminous materials: Distillation tet (fa vin {Speciation for hydreeore acid (ied Methods for toting (stressor) 1S: 1218-1978 necesary) shall be divided abgue evenly between twn phenols flasks, the subsequent specified procedure being carried out on the contents of each flask and the volumes of phenol recoverrd being totalled. 5A If the solution ia not clear, filter it through glass wool, previously ‘moistened with saturated aqueous sodium chloride solution;” collect the filtrate in the phenols flask, wath the glass wool with 25 ml of saturated sodium chloride solution and add to the filtered soda washings. Add methyl orange indicator solution, followed by concentrated hydrochloric acid until after vigorous shaking together of the two layers, the methyl orange just indicates distinct acidity. During the addition of the hydro- Ghar ac, cool the contents of the Aask by immersing the flask from time to time in cold water. ‘5.5 Add just sufficient powdered sodium chloride to saturate the aqueous layer, and to leave a few particles undissolved. Bring the phenols into the graduated portion of the flask by adding saturated sodium chloride solution. Allow it to stand, preferably overnight, and then read the volume of phenols 6. CALCULATION AND REPORT 6.1 Calculate and report the percentage by volume of the phenols in the original sample of tar taken for distillation as under: Percentage phenol = -*. x 100 where volume of phenol in ml, and = volume of original sample of tar taken in ml. 6.1.1 The phenols ag determined always contain water which has not been derived from the distillate examined, 6.1.2 When the percentage of phenols is required by mass, assume the density of phenols t9 be 1-04 g/ml, and caleulate accordingly. 11219-1971 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF NAPHTHALENE ( First Revision ) 1. SCOPE 1.1 This standard covers the method for the determin: in road tar. 1.2 This determination is necessary only in respect of the naphthalea deposited at 15°5°C from solution in the total distillate up to 270°C, 2, PROCESS 21 ‘The distillation fraction of tar distilling up to 270°C left after th removal of phenols i cooled to 155 05°C andthe solid separated an weighes 3. APPARATUS 3.1 Crystallizing-Point Apparatus — as described under 5.1. 3.2 Buchner Funnel and Flask 3.3 Hand Screw Press 3.4 Thermometer 3.5 Blotting Paper 3.6 A Filter Pump 4. PROCEDURE, 4.1 Collect the distillate recovered up ta 270°C according to Method B IS: 1218-1978, This shall be. wathed free from phenols ( see IS: 1218 1978t ). Cool the residue to 155 + 055°C and maintain it with occasions Sticcing’ within these limita of temperature for two hours. Napthaten crystallizes out, 42 Transfor the cooled material to a cold Buchner funnel fisted with rapid filter paper, and rapidly remove as much oil as possible using « flte ion of naphthalen (eos for tet {Methods for tesing tar and bituminous mate im tet (fs resin) 1s: Determination of phenale (fe 137 38: 1219-1978 Pret ia a hand rude maphthalehe hewecn sheets of blotting paper and gain pres sepa, PEN: Rewove the oily margins of thee, aa eae Bie separately," Conduct the operations, starting (het sheee a 7 fo{he Buchner funnel tothe preliminary presing, with eee rapidity. $e AteiRh the preeed naphthalene and calulate the percentage by weight in the onginal tar 44 Determine the “corrected wet crystallizi thalene by the method described in 5. 5: CORRECTED WET CRYSTALLIZING-POINT 3:1 Apparatus — A crystalisiag-point apparatus of the shape, dimen- Hos aad tolerances given in Fig. Ty consisthig of the followings Siphny Otte Class Test Tabe — which serves ag an aie jacket, shall be Fee ea ead shots or similar loading materia Te b eeig ee Position, TOWRA whieh the inner tube, ay deserved in SA. west Position, yinasdint! Glass Tet Tube — approximately 25 ym in diame, closed Ins atens and reihich cates a titer in the forn of a loop alga eee aisafiem are a standard thermometer (se 5.1.4) phoced ‘centrally within Fer afube and the glass toop and the otter ob aac Ee being about Fraga fom the bottom ofthe inner tube. ‘The cork eis aoa rpg oh mark on the thermometer is level with the top of tesa Se Gitte Rath — a sles beaker of 1000 mi eapacty and 150 cam in Heighewwth es love of the liquid at least as high arden the sumple in the inner tu S44 Theronaer— with the following dimensions and characters Point’ of the pressed naph- Range 65 to 90°C Graduation at each ore Longer lines at each. 08°C and 10°C Pully figured at each 2c Tnmersion 100 mm ‘Maximum overall length 400 mm ‘Maximum length of main scale 215 mm Maximum bulb length 12 mn Maximum distance from bottom of bulb te 28 top of contraction chamioes, Limit ot accuracy 0056 porantateral for Test — While the diference betwean the erytaliinge i and of naphthalsne containing asc see ¢ lowering’of the crystalizing int reise ee —r—rCis Is :1219- 1978 LATER TER AS ‘snmner, 3103656 1009 mv EAN q i 25 | io [ares cuss 108 0 6 | 4 AOADING MATERIAL co Lowes -coome ath 1 where ehervite ted Al dincter rent wlernee on Simenion excep ihe nena Ai ination in mimes Fig, | Crysratuizine-Powst — AsseMaLy oF APPARATUS 181 1219 - 1978 should contain two percent + more of water, i shall be examined at feecived, If the sample shoul contain a amaller percentage of water, O'S ml of water shall be placw’ a the inner tube ofthe crysaliing post Spparaun before the sample trodsood ss described under 5.3. if the testis caried out in the pres 22 of two percent or more of wate, the Sidiion of 185°C: to the ober dlcrytalisng point gives tcrytalliing- Point ofthe material onthe basi 33 Procedare — Place abou. 40 g of the material for tex in a losly oppered conical ask which ax been orarmed ina boling water bath to 'HESG. ‘Mie the content thoroughly” and pour about 40 into the eatmed inner tbe ofthe erystlizing-print apparatus. Place the tube in Itejacket and assemble the apparaten as shown fn Fig. 1-wich the bath Ge BC below the expected ryuallving point Do tot heat the water during the subsequent operations Take the bath thermometer readings at intervals of hal'a minute seing when the temperature has fallen f 81°C. Suir the content of the inner tube continuously. 5A Results 54.1 The cxynallising-point corresponds to the firs five conscutive reatings during which the Temperature remains constant wikin 05°C: Sapercoling may occur, in which case the ve readings may be observa ffir the temperature rise." Atemperatare rac of °C shall be regarded a the masini allowable 342 Tra constant temperatre within 005°C i sot obtained over Sve readings, take tie nal tondings commencing withthe fiat of two succor sive rentings within 03+. Plt the readings on graph paper” againat time interval, and deaw a straight line tole ernly between tie fra and Second, and Betwcen the ith and thesixth of the six point just mentioned Produce the line backwards unt i iaterece the earlier portion of the 5.5 Report 5.5.1 Report the constant temperature within OSC. (we SAUL) ofthe point o interaction as found in BA2, atthe ceyatalizingeposnt 5.52 Report as corrected wet crystalzing point the valve obtained afer adding OBC so the observed cralizing pean 5.55 The corocted wet crytalizing-pont shall be not laver than. 70°C. Fit found to be below °C, the ication i thatthe Temoval of the txceative oil ax preseribed in 42 has not been caried out aattfuctorly and the determination has to be repeated. 6. PRECISION 6.1 The duplicate results shall not differ by more than the following: Repeatability ore Reproducibility 08 140 18: 1220. 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF VOLATILE MATTER CONTENT ( First Revision ) 1, SCOPE LA ‘This standard covers the method for the determination of volatile matter content of coal tar pitch. 2. APPARATUS 24 Platinum Crucible— complying with the following requirement (Gee Fig. 1): External diameter at base 240 4.05 mm External diameter at top 340 £025 mm External height 350.05 mm Volume to brim 270-405 mb Weight R0E10g 21 The crucible shail be provided with a closely fitting lid, grooved tc receive the rim of the crucible and having a central hole 2 mam in 4 shown in Fig. 1. =I] mm /35-0mm £05 — 240mm £05 Fro. 4 Puamum Cavers AND Lip un 1S: 1220-1978 2.2 Meker Burner — having a diameter of 31 mm at the to diameter being 30mm manianams nT OF STM AE the Cp, the lame 2.3 Water Manometer — connected bj ‘supply entering the burner, Deh Eh 24 Three-Arm Crucible Support — with silica points (see Fig.2). = All dimensions in millinetes, Fro, 2 Tunes-Anw Crvciste Scerort wir Sitica Poms 2.5 Retort Stand and Clamp — to hold the three-arm crucible support (se: Fig. 3), so arranged that when in position, the bottom of the crucible 310 mm above the burner, the eructble being completely enveloped by 142 18112201978 Fig. 8 Asseunty oF APPARATUS ght Screen — consisting of a semi-cylindrical metal reter and sufficiently high for the purpose. 4.1 Assemble the apparatus as illustrated in Fig, 3 with theuilica point fnolding the crucible as near the rim as practicable. Spread a small quan tity of powdered pure potassium chromate over the bottom of the crucible Light the burner, taking care that the gas is lit with the flame fully aerated Slowly increase the gas pressure at the burner until incipient fusion of th: 43 1S: 1220-1978 potassium chromate is apparent. ‘The final manometer reading shall be oted at corresponding to the gat presiure to be used in the test on the pitch, The lid of the crucible shail not be used during the trials. 4.2 Clean the crucible, dey and weigh without the lid. Weigh into the ratte g ofthe ly ded sme and past pont a ete wrth the de” Refight the burner andy if ncecsary, readjust the gas Dressire uit the manometer reading the same ax that noted nthe pe Fininary til. Place the burner in foition ander the ervelile and, afer three minutes, during which the manometer reading shall be kept costa, txtinguish the flames Cool dhe erveble and weigh without the lid The fon i mas shall be the volatile matter in the amount of sample taken for the test Calculate the peveentage of volatile matter by ma inthe tot Samp taken forthe ea 4.3 If the method has been properly performed, any deposit on the lid at the end of the experiment will be due to decomposition of the volatile ter. “If there be any evidence that molten pitch has spurted on Co the lid, the test shall be disearded and a feesh determination made. 5. PRECISION 5:1 The duplicate result shall not differ by more than the following: Repeatability 09 Reproducibility 38 ry 181201 -1978 © 18:1220-1978 APPENDIX A (Clause 0.5) APPARATUS SCHEDULES Apparatus Parpuse Water bath: 4) Constant temperature Gene 1) For temperatures beeen S°C 0 ? Boa Too Hot plate do Stop wate lock © any ther do Ting deviee ‘Analytical balance, seasiveness up bo ‘001 mg ven, up to 180°C ao Specie gravity bole: PDnany, 8 mm dla neck, Determination of speci gravity Bom apa by Wide puted, 29 mm dia : Se Bal apacly container dik: : “Sasimm dep, 55 mmdia Determination of penetration ar 2 - Joss on heating: ») 45 mm dexp, 70 mm dia Determination of psneration Transfer sh to Standard needle Determination of penetration — residue of specified penetration Penetration apparates — tain dish, 4 mm deep, 70 mn Detcrination of ride of #0 . dia fae ie fied penetration ig and bal apparacn Determination of softening point Mechanical ser &o us Ts: 1201-1978 to IS: 1220-1978 Apparatus Viscometer fitted with 10mm and ‘4-mm cups and other access Cannon Manning Vacuum Capillary “Viscometer Asphalt Institute Vacuum Capillary Modified Koppers Vacuum Capillary Viscometer ‘Vacuura System HIVAG Pump Cannon-Fenske viscometer for opa- ‘que and transparent liquids BS-U-Tube modified reverse flow viscometer for opaque liquids Ductitity moulds ‘Testing machine Posky-Mustens ( closed and open ) ‘ester Float cup and its assemblies Flask, 500 ml capacity Condenser Receivers: a) 2 mleapacity 'b) 10 ml eapacity ©) 25 ml capacity 100 ml graduated cylinder Distillation fas a) 150 ml capacity 1b) 500 ml capacity ©) 750 ml capacity Water condenser Adapter Purpose Determination of viscosity and EVT Determination of absolute viscosity do Determination of kinematic. visco- sity do Duetility test Ductility test Determination of flash and fire ‘point Float test Determination of water content do do do do “ctermination of water content ‘and mineral matter Distillation test do do do do 46 Apparatus Shield Crow receivers: a) 25 ml capacity ) $0 ml capacity ©) 100 mal capacity. Residue metal containers Draught screen Beaker, 200 ml capacity Sintered glass crucible Filter paper, filtering funnel and bottle Gooch crucible Flask, 200 ml capacity Glass plate Glas tap finned Glass fined Filter paper Air condenser Phenols flask Crystallizing-point apparatus Puchner funnel and fask Hand screw press Blotting paper Piatinum crucible Meker burner Water manometer Threcarm crvible support retort, stand and clamp ae Draught sereen 1S: 1202 «19° to 18:1220- 19: Purpose Distillation test do do do. ao do Determination of matter insol in benzene and. insoluble toluene do do do do Solubility in carbon disulphi crinascipee ce do do do Determination of mineral matter and distillation test Determination of phenols Determination of naphthalene do do do Determination of volati content, matter do do do do 7 181 1201-1978 ‘o 15 11220-1978 Thrmoreier: Mthod of Tes STPTC IP ASTM Nearest je Desig IS Designation ration 8) Determination of “—" IP8G "SM TH/PI-3 of, specific gravity, 18: 2480-1973" etration ») Determination of — — ASTM SM TH/PI- residue of specified NC-E2 16 oF 17 at netration 18 :2480-1973° ©) Betrmination of — TLowtange and — ASTM: SM TH[PI-4 of font test. 150.62 15: 2480-1973 2) Tigh range — = ASTM. SM THPI-6 of 16C-62 IS: 2480-19759 4) Determination of viscosity: 1) Low range — ec — SM THPI3 of 1S: 2480-1973% 2) Medium range — IPSC = — SM TI/PI-4 of 15: 2480-1973" 3) High range — IPC |= — SM THPI-6 of 1S: 2480-1973* ©) Determination of flashpoint and fire point: 1) Low range — sc = sMTIPI4 of 15 :2400-1973* 2) High range — IPisc — SM TI/PI-16 of 17 of 18:2480-1973* {) Determination of — — ASTM SM TI/PL8 los on heating 130-62 of 1s: 2480-1973* 2) Distillation test — ec — SM TYPEIG of IT of 1s: 2480-1973* h) Determination of T7C 9 — — SM TYPr-23 naphthalene of TS: 4825-1968 i) Determination of — IP 8C. SM TIPL3 of ductility TS : 2480-1978 peeiention fo aid stem general purposes gla thermometers (fi isin). ‘Speciation fr laboratory and reference thermometer 48

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