5S: 1201-1978 to 18: 1220+ 1973 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS ( First Revision ) Bitumen and Tar Products Sectional Committee, BODC 2 Chairman Representing Pror C. G. SwaumvaTitan Central Read Research Inctitute (CSIR), New Delhi Members Suet ¥. C. Goxmarn ( Alternate to Prof G. G. Swaminathan } Sunt N. ADs. X. ALPHONSO Hindustan Petroleum Gorporation Ltd ( Refinery Division ), Burbay Suna. N, Maranun ( Alternate } Paor G. M.AxpAvaw Highways & Rural Works Department (PWD), “Famil Nadu Sunt A. K, BaatracHaryya National Test House, Calcutta Dr K. 8. Baarractarya Ministry of Defence ( DCI} Suet §, K. Ganoutt ( Alternate ) Cuewost & Meracturowt Ministey of Railways (RDSO ) Assistant CHEMIST & METALLURGIST ( Alternate ) Giucr Exomsen Public Works Department, Punjab Cier Excnvzer (Rone) Roads Wing ( Ministry of Transport ) Sui R, P, Sia ( Alternate ) Sua G. G. Goswant Assam Oil Go Ltd, Dighoi Sura Iswan Cuanpra ( Aliernate ) Sunt A. Y. Gupte Hindustan Petroleum _ Corporation Lid ( Marketing vision ), Bom Suez Einaat Since Indian Institute of Peteoleum ( CSIR }, Dehra Dua Sum J.3. Barr 1 Alerts) Bris H. K. Karoot Engincer-in-Chie(’s Branch, Army Headquarters Sari JK. Chas ( Alten} - . Sux D. Bharat Petroleum Corporation Lid ( Marketing Division ), Bombay Sunt R.R. Banoas (Allerncle ) (Continued on page 2} © Copyright 1978 BUREAU OF INDIAN STANDARDS in whole or in part by any means except with written permission of the This publication '8 protected under the /ndian Copyright Act (XLV of 1957) and publisher shall be deemed to be an infringement of copyright under the said Act.IS: 4201 «1978 to 15: 1220-1978 (Continsed from pege Members Representing SmarT. §. Keusnwawynins Indian Qil Corporation Ltd ( Refinery Division], Bombay Sua ©, V. Ramanuatny ( Aiternate ) viet Sumer S. BO Kuraene Indian Oil Corporation Ltd {Marketing Division }, Rembay: Smet Mauasin PRASAD Indian Reads Congress Paar CG, Swaaiwatian | Alternate } Sunt M, K, Mave Tn personal capacity (Clo Gammon India Lid, ‘Gammon House, Veer Saverkar Mera, PA. Sc. 8129, Probhederi, Mombay 400025 ) Sim TS, Naver Ministry of Petrolvume ‘Sawa ‘T. P. Svpratmanyax ( Altemate ) De AV Bxo "Notional Buildings Organization Da R. $. Ratna ( Atternoie) Reenesoxranvi Ministry of Defence (R&D } Sam T. K. Rov ‘Shalunar Far Products (1935 ) Ltd, Calcutta Six: Diise Kur Sa: iateal Fuel Research Institwie COSER ), Dhanbad ‘Sues Agu Kavrt Couprory ( Alternate ) Semox Suxvavon or Woxxa Central Public Works Department, (Daz Sunvevon of Wonss{ DAZ) ( Alteraia) SuavS, Suuorare Directorate General of Supplies & Disposals Swat S, P.Gupra ( Alterzaie) Sut N. §."ltavaganayas Bharat Petroleum Corporation Led (Refinery ‘Division }, Bombay Suna G, Hi, Sauzoa ( Alteruaie ) Sig D. Ajernta Stata, Director General, IST (Lxeffcio Menber ) Director (Civ Engg} Seareiary Suet JR. Menta Deputy Director ( Civ Engg ), 181 Methods of Testing Tar and Bitumen Subcommittee, BCDG 2:2 Concener Pro C. G, Swawiaraay Gentral Road Research Institute (CSUR }, New Dah Members Pror G. M. Axvavane Highways & Rucal Works Department (PWD } Tamil Nadu Sua J. 8. Ban Indian Institute of Petroleum (CSIR ], Dehra Disn ‘Sinai |.M. Nacwan.{ Attertate ) Sumy A. K, BuATTACIARY YA ational Tet Home, Gateutta ‘SuacK. D. Das ( Alternate) sna1G. G. Goswant Assam Oil Co Ltd, Dighoi Sunt Tawar CHranorn ( Alternate} . Saat B.B. L. Karcon Bharay Petcolewn Corporation Lid (Refinery 4 Division }, Bombay Sunt G. H. Sancna ( Atiernate Sunt G. H. Sanna ( } ( Comin en pge’3)1S: £201 - 1978 to 18 1 1220 21978 ( Continued from page 2) Members Representing Brig H.E, Karoon Engineer-in-Chicf's Branch, Army Headquarters Sunt B.S. Mannatnca ( Aternate) . Suet $. B, Kutkarnt indian Oi Corporation Ltd ( Marketing Division ), Bombay ‘Sumr M, R, MALra In personal capacity (Cfo Gammon india Ltd, Gammon House, Ver Savarkar Marg, P.B. No. $129, Prabhadent, Bombay 400025 Suri K, P. Nain Indian Gil Corporation Ltd (R & D Cemre), Varidabad Suet G, RacHavenpran Madras Refineries Limited, Matras ‘Suar'T. V. Varannse ( Alternate) Sum C. V, Rauaswany ‘Hindustan Petroleum Corporation Ltd (Refinery Division }, Bombay Sat A. Y. Guete ( Alienate ) Suet T. K. Ror Shalimar Tar Products ( 1995 ) Ltd, Celcutta Smmpanirsnina Eoowmen Ministry of Transport and Shipping (Roads Wing } OADS1S: 1201 . 1978 to. . 1S: 1220-1978 CONTENTS Forrworp a 1S: 1201-1978 Sampnine oo 18; 1202-1978 Determination or Srecirrc Graviry IS: 1203-1978 Dereatnation or PaneTRATION 18: 12904-1978 Dereaumation ov Resipor oF Spacrsep Pane- TRATION ood oy ae on IS: 1205-1978 Derermtwation or Sorrenine Post... - IS: 1206 (Part1)-1978 Determination oF Viscosity: PART I INDUSTRIAL Viscosity ... ane to 1S: 1206 ( Parr I] )-1978 Derersination or Viscosity: Part nn Apsotuts Viscosity on oe os IS; 1206 ( Pagr YIE)-1978 Dztexmination or Viscosiry ; Paar IIT Kinematic Viscosity ___ 15: 1207-1978 DETERMINATION o* Eguiviscous ‘TeMPERATURE (EVT) te o on oe 1S: 1208-1978 Determination ov Ductiniry we te TS: 1209-1978 Determination or Fiase Pot ap Fire Pom. IS: 1210-1978 Froar Tesr oe wa IS: 1221-1978 DerermixaTion or WATER Content (Dean AND Starx Mrtuop ) - IS; (212-1973 Derermination oF Loss on Heatina Dusrication Test LYTERMINATION CF MATTER INSOLUBLE IN Benzene Duversixation oF Marrer Insocurte in ToLuenr, Devermination or Sorunrry m Carson Discr- brane OM TRICHLOROETHYLENE ... TR. 1217-19738 Devekwination or MinerAt Matter ( Am) Uy: FR18-1978 DeteRMmNAtion oF Prenors 2 P216.1078 YS: 219.1978 Davcemenation or NAPHTHALENE 3S 22a 1G7R Nev anpix A ‘ATION OF VOLATILE Marten Contenr SSATUS SCHEDULES... 4 PAGE 19 25 29 33 39 47 37 65 71 75 87 91 97 103 hg 121 125 13] 133 37 Mi m51811201 - 1978 to 18: 1220 - 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS ( First Revision ) 0 FOREWORD @,1 These Indian Standards ( First Revision) were adopted by the Indian Standards Institution en 530 June 1978, after the drafts finalized by the Bitumen and Tar Products Sectional Committee had been 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 various methods of tesls relating to cach product were included in the same standard, Since these specifications were prepared over a period of time, the methods of tests, prescribed for the determination of similar propertics varicd in proccdure and cquipment from one standard to another. It was, thercfore, 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 series of standards on methods of tests was first published in 1958. However, during the course of this period a number of improve- ments have since been made in carrying out of these methods of tests and accordingly, the compilation of methods of tests is now being revised to bring it up-to-date. Modifications have, in particular, been made to the provisions of repeatability and reproducibility limits specified under each test. Also, under methods of tests for determining the viscosity require- ments (1S: 1206 ) additional methods of tests have been included for the determination of ‘absolute’ and ‘kinematic’ viscosity under separate parts. 0.4 The Sectional Cominittce responsible for the preparation of these standards has taken into consideration the views of producers, consumers and technologists and has related the standards ta the manufacturing and trade practices followed in the country in this field, Due weightage has also been given to the need for international co-ordination between standards prevailing in different countries of the world. These 51S 1201 - 1978 to 1S ; 1220 - 1978 considerations have led the Sectional Committee te derive assistance from the standards and publications of the following associations and committees: Standardization of Tar Products Tests Committee, London Institute of Petroleum, United Kingdom American Society for Testing Materials, Philadelphia 0,5 While preparing this compilation of methods of tests, simplification in the range and t ¢ of thermometers, condensers and receivers used in various tests has been kept in view. Accordingly, the committee hopes that this simplification wall help the laboratories to equip themselves with a ‘complete tange of apparatus for testing tar and bitumen. As a guide to the laboratories a list of apparatus required for testing tar and bitumen according to these standards has been provided in Appendix A at the end, ‘The thermometers specified in this compilation ate identified in terms of designations according to the Institute of Petroleum or American Society for Testing Materials and hence their equivalent IP and ASTM desig- nations are also given in the Appendix. Corresponding equivalent Indian Standard designations covering thesc thermometers are also indicated. It is, however, important to note that all thermometers used in these tests should bear a conformity certificate from the National Physical Labora- tory of India or any other institution authorized by the Government of India to issue such certificates. 0.6 In reporting the result of a test or analysis made in accordance with these standards, if the final value, observed or calculated is to be rounded ‘off, it shall be done in accordance with IS : 2-1960*. Rules for rounding off numerical values (revised ), 61S, 1201 - 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: SAMPLING ( First Revision ) 1. SCOPE A.l This standard covers methods of sampling bitumen and bituminous materials, in their liquid, semi-solid or solid states supplied in any of the following forms: a) Cans or small containers, drums, barrels and bags; h) Solid materials in Ioose: farm; c) Rail tank wagon and road tank trucks/lorries; and. d) Bulk storage tanks and other types of bulk storage. Nora — The provision of this standard shall be applicable to bitumén emulsions also, subject to modifications given in the relevant standards on emulsions. 2, PURPOSE OF SAMPLING 2.1 From a lot repretenting 3 part or the whole of the material offered for inspection, samples are taken for the purpose of securing representative portions fur visual and laboratory cxamination of for prescrvalion for record, ‘The examination may he made to determine: a) the average quality of the material in the lot, b) the extent of variation in quality in the different portions of the material, and c) conformity to the specified requirements. 3. TERMINOLOGY 3.0 For the purpose of this standard the following definitions shall aoply. 3.1 Lot —The quantity of material of the same composition offered for inspection at one time, A lot may consist of the whole or a part of the quantity ordered for.15: 1203 - 1978 BAL Formation of Lots a) The lot shall be formed before sampling is undertaken; b) The basic principic in forming the lot is that the material in the lut should be cs homogeneous as possible with regard to the quality characteristics specified; and c) Care shall be taken to see that the material in a single lot comes from the same source/batch of manufacture ard as far as possible from zaw material of identical origin. 3.2 Top Sample — A cup sample is one taken at a level of one-sixth of the depth of the material below the top surface and jn the centre of the container. 3.3 Middle Sample — A middle sample is one taken at_a level of one- half of the depti. of the material below the top surface in the centre of the container. 3.4 Lewer Sample — A lower sample iy one taken at a level of five-sixths of the depth of material below the top surface in the centre of the container. Nove 1 —In the case of horizontal sylindrical tanks and tanks of irregular shape, ‘top’, niddle’ and ower’ samples takes at levels corresponding to vacaixth, onchatt and ‘five sixths of the depth of product in the tank are not representative. In euch circumstances, samples shall be taken at levels corresponding to one-sixth, one-half, and five-sixths of that volume. Norte 2 — In the case of cone-roofed tanks the sample may be drawn from as near the centre as possible. 3.5 Average Sample — A true average or representative sample is such that its composition would be ths same as that of any part of the quantity sampled if the whole wore mixed to onsure homogencity. When the con- tents of the vessel are substantially homogeneous as shown by preliminary examination of top, lower and middle samples and the cross section of the vessel ig uniform, an average cample is usually made up by combining equal parts of samples drawn from levels at one-sixth, one-half and five- sixths of the depth of the liquid below the top surface. 3.6 Composite Sample — A composite sample is onc taken by combining represéntative samples of a product from a number of containers, that is, from packages, in proportion to the contents of cach of the containers sampled, 3.7 Pipeline Sample— A composite sample taken at the filling point in the delivery end cf the pipeline. 3.8 All Level Sample — This is obtained by submerging a closed sampler to a point as near as possible to the draw-off level, then opening the sampler and raising it at a constant rate such that it is nearly, but not quite, full as it emerges from the quid and has drawn in the sample liquid at all levels, 83821201. 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 adversely affected by hot bitumen ( see Fig. L ). 4.2 Sampling Thief or Tube Method — The sampling thief or tube shail be either of glass or metal, to reach to within 3 mm of the buitom of the vessel and having a capacity of approximately haif or one titre. A metal tube suitable for sampling 250 litre drums is illustrated in Fig. 2. The rings shall be soldered to opposite sides of the tube at the upper end for convenience in holding it. Fig, 1 Bitumen Samper All dimensions in millimetres. Fic. 2) SampLina TUBE1831201 - 1978 4.3 Ship Auger —of such diameter and length as to permit a core of convenient size to be taken throughout the depth of the package or cake'as illustrated in Fig. 3. DOYS Fic. 3 Samp AvozR 4.4 Sampling Scoop — of such dimensions as to enable a core of conve- nient size to be taken throughout the depth of the package (see Fig. 4). HAMMER HEAD FOR DAIVING WTO BARRELS Fig. 4 SAMPLING 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. od Bottle Sampler — made of metal with a handle and stopper (se ‘ig. 5). 5, SAMPLE CONTAINERS 5.1 Containers for the samples of liquid bituminous materials shall be small-mouth cans with cork-lined screw caps, except for emulsions, in which ease they shall be wide-mouth glass jars or bottles, Containers for the amples of semi-solid and sulid materials shall be friction-top cana. 101831201 - 1978 Nore —A tolerance of 10 percent is allowable on dimensions in millimewes, Fie. 5 Borrtz Samper yor TANK Cars oy181 1201 - 1978 5.2 The size of the sample container used shall be such that it is nearly filled by the sample taken, just enough free space, such as 5 to 10 percent of the capacity of the container being left to allow for expansion and to enable the contents to be mixed by shaking. 6, SIZE OF SAMPLES 6.1 The sizes of samples to be taken for testing shall-be a8 follows: a) Liquid Materials 1) From small containers, cans, drums and harrels — one litre for each separate sample, 2) From bulk storage tanks and drums — 5 litres. b) Semi-solid or Solid Materials 1) From barrels, drums, cakes and powdered materials in bags — ‘ 1 to 2 kg for each separate sample. 2) From bulk a minimum of 45 kg composite or average sample, 7. PROCEDURE AND SCALE OF SAMPLING 7.1 From Cans or Small Containers, Barrels, Drums and Bags WAL Liquid Materials —The number of packages to be aclected for sampling from the jot shall be in accordance with col | and 2 of Table 1. The sample packages shall be selected at random, —_—— TABLE 3. SCALE OF SAMPLING (Glauses 7.11 and 7.1.2) No. oF Contaiwens/ No. or Contarers} Bags in THe Lor BAGS To BE FOR SAMPLING 1 1 2 to 15 2 1%, 50 3 SL, 150 5 151 4, 500 8 301 and above 19 TAAL Composite sample From cach of the packages selected for sampling a small quantity of material shall be withdrawn with the help of a sampling tube in accordance with the procedure given in 7.1.1.2. ‘The quantity so withdrawn from each of the packages shall be fully representa- tive and proportional te its contents. The material withdrawn from all the 12181 1201 2 1978 ackages shall be thoroughly mixed together and then the requisite Tuantlly for testing shall “be withdrawn’ This shall be the composite sample. An identical composite sample if required may alsc be made for keeping as reference sample under the joint seals of the purchaser and the seller. Ifthe composite sample passes in respect of all the requirements of the specification the lot may be considered to be in conformity to rhe requirements of the specification. 7.1.1.2 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, Lf the tube contains free water its contents shall be rejected and the tube again lowered into the package to such a depth as to avoid the watur. The tube shail 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 ta flow gently and without splashing into a sample container. 7L.2 Semisolid or Solid Materials—'The number of packages to be selected for sampling from the lot shall be in accordance with col J and 2 of fable 1. Fhe sample packages shall be selected at random, 7.1.2.1 From each of the sample packages from the lot appropriate quantity shall be taken, For this purpote an appropriate sampling apparatus, aid or device may be used which may involve usc of hammer, chisel, knife or spatula, auger or a scoop. If gic material is held in small containers with a bung-hole too small to introduce the thief, the contents of the container shall be mixed thoroughly by shaking and the requisite quantity of sample shall be poured out. Care shall be taken to ensure that from each container the material taken is fully representative and proportional to its contents. The material so taken from cach of the sample containers shall be toroughly mixed together or melted together if necessary to form a combined mass of material from which a suitable sample for testing shall betaken. This shall be called the composite sample. If required a similar composite sample may be taken for purpose of preservation for reference under the joint seals of purchaser and the seller. The composite sample shall be required to pass ali the specified requirements in order to declare a lot to be in conformity to the requirements of this specification. 7.2 From Rail Tank Wagom and Road Tank Tracks/Lorries 7.21 A carcful observation of the condition of the matcrial in regard to the presence of foam, sediment, or free water on top or at the bottom of the material in the wagonjtruck shall be made immediately before sampl- ing, and, if such extraneous materials are present in measurable quantities 13IS: 1201- 1978 their volume 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, bo sampled before heating, but if heating is necessary, at no time shall the temperature exceed that required for satisfactory sampling. Semisolid or solid bituminous materials shall be rendered fluid by heating. 7.2.2 When possible, thoroughly mix the material to be sampied 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 possible to mix the contents of the tank, or when it is desired 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 all the tests, the material in the tank wagon truck shall be corlsidered to be in conformity to the requirement of the specification, If required an identical composite sample may be taken for reference. 7.3 From Bulk Storage 7.3.1 Liquid Materials and Materials Made Liquid by Heating — The inlet and outlet to the storage tank shall be closed and a 5-litre sample drawn from the top, middie and bottom contents. The sample may be taken from drain cocks on the side of the tank if such are available, with the hel of a sampler illustrated in Fig. | and when so taken, enough material shall be allowed to flow through the drain cocks and discarded to ensure a representative sample from the contents of the tank. Otherwise samples may be taken by lowering into the material a suitable bottle sampler, a satisfactory type of which is iliustrated in Fig. 5. The bottle or can shall be fitted with a stopper which shall be removed by a sting or wire attach- ed to it after it has been lowered to the proper depth. The three samples from bylk storage may be tested separately for consistency in order to detect stratification, They may then be combined, thoroughly, mixed, and a 5-litre sample taken thorefrom for other tests that may be required for determining average characteristics of the material, 7.3.2 Solid Materials in Loose Form — Mix the piece representing the total quantity on a clean hard surface and proceed as follows: Place the broken down samples on a clean impervious surface, mix by shovelling and heap into a conc by depositing separate small quantitics one on top of the other, the conc being formed symmetrically throughout, with 419: 1201 - 1978 its apex always in the same vertical line, Alternatively, shovel the material into a funnel having a short cylindrical stem about 51 mm in diameter. Support this funnel in a vertical position above the top of the cone, and raise it ( without lateral displacement) as the cone grows higher to allow the material to flow out gently and not fall from a height. Forma new cone twice in a similar way, flatten the third cone by pressing it with a metal sheet or any other suitable appliance, the Mattening being carried out symmetrically, thus giving a mass af approximately uniform thickness and diameter. Divide the sample at this stage in quarters by pressing through it a metal cross constructed from four arm or blades which meet at a common centre, held at right angles to each other by stays. Remove a pair of uppusite quatlas completly audagjeet them. Mix the iwo remaining quarters together thoroughly, reduce in bulk by further quartering, and Tepeat the procedure until a final sample of suitable quantity is left. The gross sample shall not be less than 25 kg from which shall be selected 1 to 1°5 kg of the composite sample for tests. If the composite sample satisfies all the specified tests, the material in the lot shall be declared to be in conformity to the specified requirements. & PRECAUTIONS 8.1 In addition to the general precautions given in 8.2 in sampling for certain tests there are special precautions, which shall be observed and those are prescribed under the relevant method of tests, It cannot be over emphasized that the most careful work in the laboratory or in oil measure- ment may be rendered uscless if care is not taken when drawing the samples upon which such work is based. 8.2 A sample shall not include material other than that to be sampled and shall not ‘become altered, for example by evaporation of volatile consti- tuents or by oxidation, in the process of sampling. The following precau- tions shall be observed in sampling: a) Official saraples shall be taken by, or under the immediate super- vision of a person of judgement, skill and experience in sampling. b) The sampling apparatus, including cords or other ancillary gear, and sample containers shall be dry and free fram any substance which will contaminate the product. c) The sampling. apparatus shall be filled and allowed to drain at Jeast twice before drawing the sample and the sample container shall be rinsed at least twice with the material obtained during the third or any subsequent filling of the sampling apparatus and shall be allowed to drain before being used to contain the actual sample. ‘This shall not apply when such filling, emptying, and rinsing are precluded by the sampling method being employed or by the nature of the material sampled. li1S: 1201 - 1978 a) During sampling operations, the material being sampled shall be protected as far as possible from the effects of wind and weather, aad the sample containers shall be closed immediately after the sample has been taken. e) The operator engaged in sampling shali have clean hands free from ') nh) = V3 m) n) P) any material ( unless it be the material being sampled). Clean gloves may be worn, but only when essential to protect the operator from some health ur other hacard, Liquid materials in tanks and other bulk containers shall be sampled. by the appropriate met!.od described in this standard. The sample shall be drawn through dip hatches, manholes, or other opening giving direct and unconfined access to the bulk of liquid. Samples shall not be drawn from dip-pipes or other fittings, nor shall gauge glasses or drain fittings be used for sampt- ing purposes except where so specified, ‘Vhe depth of any free water shall be determined before sampling operations are commenced, to ensurs that no free water is included in tke sample. If there is any reason to suspect that « iample or a set of samples may not be fully representative, a further sample or sct of samples shall be taken. The necessity for taking a second or ‘check’ sample, or set of samples, is frequently due either to failure or to. faulty labelling, The provision of clean apparatus is greatly simplified if separate sampling apparatus, sample containers, and other equipment are reserved and kept scparate for different classes of products, while the possibility of errors in labelling may by largely eliminated if cach sample is clearly marked before che next sample is taken. All metal sampling gear shall be made of non-spark generating materials. Glass stoppers shall be ground ty the neck of the body. Screw caps of cans shall be fitted with washers of cork or other oil-resist- ing materials. Corks and stoppers shall be tied or wired on. Rubber stoppers and corks shall not be ured for closing any vessel containing sauples of tar and bitu.nen. Care shall be taken to see that nothing in the sampling procedure Jeads to contamination of the stock, for example, by dirt or other extraneous matter picked up by a wet bung, by fragments of stoppers or by other forcign matter and the sample containers are perfectly clean and dry befure filling. It is advisable to take more than one set of samples for check Purposes in case of dispute, leakage or breakage in transit or for any other reasons. Every possible precaution against fire hazard shall be taken when sampling fammable materials like cutback bitumens, ete. 161S ¢ 1201 - 1978 9. LABELLING, PACKING AND STORAGE OF SAMPLES AND SAMPLE CONTAINERS 9.1 Labelling — Sample containers shall be labelled; gummed labels may be used on glass surfaces, but in general wired-on labels shall be preferred. Labels shall-be permanently marked. If a pencil is used, sufficient pressure shall be exerted to indent the paper. The following information shall be recorded on the label: a) Sample reference number; b) Place at which sample was drawn; ¢) Date of sampling; d) Initials or other identific ation mark of sampling officer; ¢) Grade of material; f) Quantity represented by sample; g) Tank No. package No. ( and type), name of rhe point of ttespatch; h) Type of container from which sample was drawn and type of sample ( top, middle average, etc ); and 3) The name of the manufacturer, if known, 9.1.1 The above details shall also be recorded in a book kept separately for the purpose. 9.2 Packing — Sample containers shall be sealed properly to prevent tampering. The type of packing used tor samples which are to be transported depends largely on the means of conveyance. Wooden cases or strong cardbeard cartuns are recommended for cans containi samples. The space round the sample container shall be filled with material, such as saw dust; when such materials are used, the cork or stopper shall be covered with a paper or viscose cap in order to prevent contamination of the sample on opening. 9.3 Storage — Samples of materials which may be affected by light or heat shall be stored in a cool, dark place, periodical examination shall be made for leakage.As in the Original Standard, this Page is Intentionally Left Blank18; 1202 - 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF SPECIFIC GRAVITY ( First Revision ) 1, SCOPE 1 This standard covers the methads for the determination of specific gravity of asphalt, bitumen, bituminous products, road tar, coal tar, coal tar pitch, creosote and anthracene oil. 2, TERMINOLOGY 2.0 For the purpose of this standard, the following definition and those Riven in TS + 334-1965* shall apply 2.1 Specific Gravity— The ratio of the mass of a given volume of the substance to the mass of an equal vulume of water, the temperature of both being specified. 2.1.1 Uf the temperature of the substance is 4, and that of water is fp the specific gravity S, is denoted by Sti/ta: 4, and , shall be specified clearly. 2.1.2 ‘Vhe specific gravity of bitument, Huxed native asphalt, road tara, coal tar pitch and blown bitursen shall be determined at 27°C and that of creosote oi! and anthracene oil at 38°C and shall be expressed as specific gravity 27°C/27°G or 38°C/38°C. 3, METHOD A ( PYKNOMETER METHOD ) 3.1 This method covers the determination of specific gravity for semi- solid bituinen cuad tars aad ercosite and anthracene oil. 3.2 Apparatus — Specific gravity bottles of 5U ml capacity shall be used. One of the two types of specific gravity bottles, namely (a) the ordinary capillary type specific gravity bottle with a neck of 6 mm diameter (se Fig. 14) and (b) the wide-routhed capillary type specific gravity bottle ( see Fig. 1B) with a neck of 25 mm diameter shall be used. ‘Glossary of terms relating to bitumen and tar ( revived). 1918+ 1202 - 1978 Fic. 1A Orpinary Fra. 1B Wis-Mouraxp GarrLLaRY TYPE Caruinany Tyre Specie GRAVITY Srxciric GRAVITY + Borrer Borrte 3.2.1 The ordinary specific gravity bottle shall be used for materials which remain absolutely finid st 27°C while the wide mouth capillary Pe shall be used for materials which remain semisolid or high viscous at 3.2.2 Constant Tonparature Bath— A watcc bath having a de th greater than that of Pyknometer capable of being maintained within 0°2°C of the desired temperature. 5.2.3 Bath Thermomater — It shall conform to the following requirements: Characteristic Requirement Range Oto 44°C Graduations Ore Immersion 65 mm Ovecrall length 340 + 10 mm Stem diameter 5°5 to 8°0 mm Bulb length 10 to 16 mm Bulb diameter Not larger than stem diameter Length of graduated portion 150 to 190 mm Langer tines at each 1°G and 5°G Figured at cach 5c Scale + O26 3.3 Procedure — Clean, dry and weigh the specific gravity bottle to- gether with the stopper (a). Fill it with freshly bailed and cooled distilled water and insert the stopper firmly. Keep the bottle up to its a2(8 1 1202 - 1978 neck for not less than half an hour in a beaker of distilled water maintain- ed ata temperature of 27-0 + O-I°C or any other temperature at which specific gravity ia to be determined; wipe all surplus moisture from the surface with a clean, dry cloth and weigh again (b). After weighing the battle and water together (bh) the bottle shall be dried again. 3.3.1 In the case of solids and semisolids, bring a small amount of the material to a fluid condition by gentle application of heat, care being taken to prevent loss by evaporation, When the material is sufficiently’ fluid, pour a quantity into the clean, dry specific gravity botle mentioned at 3.3 to fill at feast half Slightly warm the bottle before filling. Keep the material away from touching the sides above the final level of the bottle and ayoid the inclusion of atr bubbles. The use of a small funnel will prevent contamination of the neck of the bottle. To permit escape of entangled air bubbles, allow the partly filled bottle to stand for half an hour at a suitable temperature, then cool to the specified temperature and weigh with the stopper (c). 3.3.2 Fill the specific gravity bottle containing the asphalt with freshly boiled distilled water placing the stopper loosely in the specific gravity bottle, Do not allow any air bubble to remain in the specific gravity bottle. Place the specific gravity bottle in the water bath and press the stopper firmly in placc. Allow the specific gravity bottle to remain in the water bath for a period of not less than 30 minutes. Remove the specific gravity bottle from the water bath, wipe all surplus moisture from the surface with a clean dry cloth and weigh it along with the stopper. 3.3.3 In the case of liquids such as creosote and anthracene oil, fill the bottle up to the brim and insert the stopper firmly. Keep the filled bottle for ‘not less than halfan hour in a beaker of distilled water maintained at a temperature of 27-0 + 0°1°L, remove the bottle from the beaker, wi all surplus water from the surface with a clean, dry cloth and weigh again. 7 t Calculation — Calculate the specific gravity of the material as 3. a) Specific gravity ( solids and semisolids ) “& STE b) 5 ic gravity aa wict where a == mass of the specific gravity bottle, 6 = masa of the specific gravity bottle filled with distilled water, ¢ = mass of the specific gravity bottle about half filled with the material, 21181202 - 1978 d= mass of the specific gravity bottle about half filled with Ure material and the vost with distilled water, and ¢ = mass of the spacific gravity bottle completely filled with the material. 3.5 Report — Results of the test shall be expressed ag the ratio of muss of a given volume of the material at a temperature spacified under 2.1.2 to the mass of the same volume of water at the same temperature. 3.6 Presision — With samples which are neither very volatile nor very viscous and using a pyknometer of at least 25 ml capacity, the results of anplicate tests should not differ by the follawing: Repeatability Reproducibility 0-002 0-005 3.7 Precautions — When making the specific gravity determination, it is important that: a) only freshly boiled and cooled distilled water shall be uscd; b) at no time of weighing shall the temperature of the apparatus be allowed to exceed the specified temperature; c) precautions shall be taken to prevent expansion and over-fow of the contents resulting from the heat of the hand when wiping the surface of the apparatus; all air bubbles shall be climinated in filling the apparatus and inser ting the stopper; e) weighing shall be done quickly alter filling the apparatus and shall be accurate to 0° mg; and f) to prevent breakage of the apparatus when cleaning after a deter- mination has been made upon a very viscous. of semisolid material, it is advisable to warm it in an oven at a temperature not abeve 100°C, until most of the material is poured out and then to swab it with a piece of sett cloth or cotton waste. When cool, 2 may be finally rinsed with caibon disulphide, benzol or other solvent and wiped clean. d 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. 4.2 Apparatus 4.2.1 Balance Analytical 4.2.2 Thermometer —~ ax given in Method A. 2218: 1202 - 1978 4.2.3 Balance Straddie — A pan straddle of convenient size to support 4 beaker and permit determination of the weight of the specimén in water ( se Fig. 2). Fro. 2) ANALYTICAL Batance Eguiepen wri Pan STRADDLE 4,24 Thread ~~ A Icngth of fine, waxcd, silk thread, 4.2.5 Brass Moulds — cubical, measuring approximately 20 mm on cach edge. 4.3 Test Specimen — The test specimen shall be a cube of the material measuring approximately 20 mm on each edge, Prenare tie specimen by melting a smalt sample of the material by gende application of heat, tak- ing care to prevent loss by evaporation, and pouring the macerial when sufficiently fluid into a 20 mm brass cubical mould that has been treatud with a 1: ] mixture of glycerine and dextrin and placed on a brass plate previously so treated. T'ake precautions to prevent the inclusion of air bubbles. The hot material should be slightly more than that required to fill the mould, and when cool, the excess may be cut off with a hot spatula. Remove the specimen from the mould when cooled to room temperature. 4.4 Procedure — Tare the balance first with a piece of fine waxed silk thread sufficiently long to reach from the hook on one of the pan supports 23US: 1202- 1978 tothe rest. Attach the test specimen to the thread, #0 as to be suspended about 25 mim above the straddle from the heok on the pan Supports § ae weigh to the neareat O'l mg. Weigh the specimen, still suspended thread, and completely immersed in freshly boiled and cooled distilled water at 27-O-¢ 01°C, to the nearest Ol mg, adhering air bubbles being first removed with a fine wire. 4.5 Calculation — Calculate the specific gravity of the material aa follows: Specific gravity = 7 - where a = mass of the dry specimen, and 4 = nus of the specimen when immorsed 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 24AMENDMENT NO. 1) APRIL 1989 TO 1S: 1202 - 1978 METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS : DETERMINATION OF SPECIFIC GRAVITY ( First’ Revision ) ( Page 19, clause 3.2 ) — Insert the following after.3,2: “The stopper shall be provided with a bore I:0 to 2° mm in diameter, centrally located in reference to the vertical axis, The top surface of the Stopper shall be smoth and substandally plain and the lower surface shall be concave in order to aflow all air to escape through the bore. The height of the concave section shalt be 4:0 to 6°0 mm at the centre.’ CPCDC 6) Printed at Simoo Printing Press, Delhi, India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 penetration of asphaltic bituinen and fluxed native asphalt and blowa type bitumen. 2. TERMINOLOGY 20 For the purpose of this standard, the following definition and those given in IS : 334-1969* shall apply. 2.1 Penetration — The penctration of a bituminous material is the distance in tenths of o millimctre that a standard needle will penetrate vertically into a sample of the material under standard conditions of temperature, load and time, 3. APPARATUS 3.1 Container — A metal or glass cylindrical, flat bottom container of essentially the following dimensions shail be used: For penetrations Leluw 225: Diameter, mm 55 Internal depth, mm 35 For penetrations hetween 225 and 350; Diameter, mm 70 Internal depth, mm 45 3.2 Needle — A straight, highly polished, cylindrical, hard steel rod, with conical and parallel portions co-axial, having the shape, dimensions and *Glussary of terms cclating te bitunven and tas (revised). 25IS; 1203 - 1978 tolerances given in Fig. 1. ‘The needle is provided with a shank approxi- mately 3 mm in diameter inte which it is immovably fixed. The taper shall be symmetrical and the point shall be ‘blunted’ by grinding to a truncated cone, ONTO 1.62 Ba 0-08 10 0-99 OH O04 16 O08 “ All dimensions in millimetres. Fis. | Nerpie ror Panerration Test 3.3 Water Bath — A water bath preferably with a thermostat maintained at 25-0 + O-1°C containing not less than 10 litres of water, the sample being immersed to a depth of not less than 100 mm from the top and supported on a perforated shelf not less than 50 mm from the bottom of the bath, 3:4 Transfer Dish — A small dish or tray, provided with some means which ensure a firm bearing and prevent the rocking of the container, and of such capacity as will ensure complete immersion of the container during ic test. 3.5 Penetration Apparatus —Auy apparatus which will allow the needle to penetrate without appreciable friction, and which is accurately calibrated to yicld results in tenths of millimetre shall be adopted. 3.6 Thermometer — It shall conform to the following requirements: Characteristic Requirement Range 0 t044°C Graduations 02°C Innmersion, 65 mm Overall length 340 + 10 mm Stem diameter 55 to 80 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 cach 1°C and 5°C Figured at each sc Scale 40°2°C 26IS : 1203 - 1978 3.7. Time Device -For hand-operated penetrometers, any convenient timing device, such as electric timer, stop watch, or any cther spring actuated device may be used provided it is graduated 0-15 or Jess and is accurate to within +0°1 s for a 60-s interval. An andible seconds counter adjusted to provide ! beat cach, 0°33 may also be used. The time for a 1l-count interval shall be 5+01s, ‘Any automatic timing device attached to a penetrometer shall be accurately calibrated to provide the desired test interval within J. 0-1 a. 4. PROCEDURE 4.1 Preparation of Test Sample 4.1.1 Soften the material to a pouring consistency at a temperature not more than 60°C for tars and pitches and not more than 90°C for bitumens above the respective approximate softening point and stir it thoroughly until it is homogeneous and is free from air bubbles and water. Pour the melt into the container ta a depth at least 10 mm in excess of the expected penetration. Protect the sample from dust and ailow it to coo! in an atmosphere at a temperature between 15 to 30°C for 1} to 2h for 45 mm decp container and I to 13h when the container of 35 mm depth is used. Then place it along with the transfer dish in the water hath at 25:0 4+ 01°C! and allow it to remain for 1} to 2h and 1-to 14 h for 45 mm and 35 mm deep container respectively. 4.1.2 In the case of cutback bitumen and Digboi type cutback bitumcn, residue feft after distillation shall be used for the test. The procedure for handling the residue shall be in accordance with the method described under 3.2.4 of the distillation test (see IS: 1213-1978* ). 42 Testing 4.2.1 Unless otherwise specified, testing shall be carried out at 25°0 + 01°C. 4.2.2 Fill the transfer dish with water from the water bath toa depth suliicient to cover the container completely; place the sample in it and put it upon the stand of the penetratian apparatus. Adjust the needle (previously washed clean with benzene, carefully. dried, and loaded with the specified weight ) to make contact with the surface of the sample. 4.2.2.1 This may be accomplished by placing the needle point in contact with its image reflected by the surhaee of the material from a suitably placed source of light. 4.2.2.2 Unless otherwise specified, load the needle hoider with the weight required to make a total moving weight ( that is, the sum of the weights of the needle, carrier and superimposed weights) of 100 4 0°25 g. *Methods for testing tar and bituminous materials: Distillation test ( first revision }. 27IS: 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 Penctrated. 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 cach test, return the sample and transfer dish to the water bath, and wash the needle clean with benzene and dry. In the case of material of penetration greater than 225, three determinations on each of two identical test 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 nol less than three determinations whose values do not differ by more than the amvuni given below? Penetration Maximum Difference Oto 49 2 50 to 149 4 190 to 249 6 250 and above 3 6. PRECISION 6.1 The duplicate results should not differ by more than the following: Penetration Repeatability Reproducibility Below 50 1 Unit 4 Units Above 50 3 percent of their 8 percent of their Incan luean 7. PRECAUTIONS 7,1 If the sample contains extrancous matter, it should be sieved through IS Sieve 30 ( see 18: 460-1962" }. 4.2 To avoid overheating at the bottom of the container, use of an air- oven or sand bath is recommended. 7.3 While the needle is penetrating into the sample, if there is any movement of the container, that determination shall be discarded. *Specification fur test sieves ( revised }. 28AMENDMENT NO. 1 JULY 1989 TO IS : 1203-1978 METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS : DETERMINATION OF PENETRATION { First Revision ) ( Page 28, clause 4.23) — Insert the following new clause after a “4.2.4 For jgerminng the penetration ratio, testing shall also be carried out at 4°0° + 0°1° Nom — Fog test at 4°¢:, the total weight on the penetration needle shall be 200 £025 y aud the line uf pructrativa shall be 60 ( Page 28, clause 5.2) ~ Insert the following new clause after ‘.3 Determine the penetration ratio as under: . _ __ Pen, at 4°C.200 g.60's . Penetration ratio = Pen ar 2°C.100 ge 100 (BCDC 2) Printed at Simoo Printing Frese, Détni, India.AMENDMENT NO. 2 MARCIT 1989 To IS : 1203-1978 METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS : DETERMINATION OF PENETRATION ( First Revision ) { Page 25, clause 3,2, line 1) —— Substitute ‘stainless steel ( SS 316)’ for hard steel’. cecpe 6) Printed af Samco Printing Bross, Dalhi, India1S: 1204 - 1978 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 of specified penetration of cutback bitumens. 2. TERMINOLOGY 2.0 For the purpose of this standard, the following definition and those given in IS: 334-1965* shall apply. 2.1 Residue of Specitied Penetration — It is the percentage by mass of a residue obtained by heating a bituminous material to the required temperature and having a specified standard ponctration value, Alternatively, the determination of residue of specified penetration is made at two stages, one giving a penetration higher than 100 and the other lower than 100, and the result is obtained by interpolation. 3. APPARATUS 3.1 Container — A flat-bottomed, cylindrical seamless tin dish 70 mm in diameter and 45 mm in depth. 3.2 Heating Bath — A cast iron bath with the shape and dimensions as shown in Fig. 1 permitting the immersion of the container ta a depth of 32 mm through an opening 1’6 mm larger in diameter than the container. Itshall be provided with thre rivcts or bolts so as to support the container 6 mm above the hot plate. The free air space between the sides of the container and of the air bath below the opening shall be not less than 6 mm. "Glossary of terms relating to bitumen and tar ( revised }. 21S +1204 - 1978 SECTION Xx All dimensions in millimeues. Fic. | HEATING Bath 3.3 Hot Plate — Suitably mounted and heated cither clcctrically or by means of a gas flame, capable of maintaining the sample continuously at the required (cuperature, provided with an apparatus, such as a rheostat of gas prossuce regulator. 3.4 Thermometer — An open flash thermometer having the range from rainus 6°C to plus 100°C shall conform to the following: Immersion 23mm ‘Temperature range — 6°C to + 400°C Subdivision 2C Longer graduation lines at each 10°C Graduation numbered at each 20°C multiple of Scale error at any point up to 3726 re when standardized shall not excced 3.5 Needle — as specificd under 3.2 of IS ; 1203-1978", “Methods for testing tar and bituminous materials: Determination of penetration { fiat revision 5. 3018 : 1204-1978 3.6 Water Bath — as specified under 3.3 of 15: 1203-1970". 3.7 Penetration Apparatus — as specified under 3.5 of IS; 1203-1978*. 4, PROCEDURE 4.1 Preparation of Sample 4.1.1 Thoroughly stir and agitate the material as received td ensure a complete mixturc before the portion for testing is remmoved. _ If the-sample contains extrancous matter, it should be sieved through IS Sieve 30. 4.2 Weigh a 100-00 + 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 mm 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 and 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 homogencous sample, flux in the sample all cakes of hardened bitumen which form at the sides of the container. 4.2.2 An experienced operator would be able to judge approximately the consistency of the residue he should obtain to secure the desired penetration when it is judged that the residue might show the required penetration, return to the container the bitumen on the thermometer which may be readily scraped off. Remove the container from the airbath, cool and weigh. 4.3 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 cvaporation has becn conducted, shall be uscd. 44 Frequently, it is necessary to make several trials before a residue of the required penetration is obtained. If it is found to be of greater value than sequired, remove all water from the container and the surface of the sample, and repeat the heating and determination of penctration as before, Ordinarily, a residue is considered as satisfactorily obtained when its penetration is 100. 4.4.1 When it is necessary to determine more precisely the percentage of residue having a penetration of 100, such as a percentage shall be calculated by interpolation between percentages of two residues, one having a penetration greater and one having a penetration lower than 100. ¥Methods for (esting tar and bituminous materials: Determination of penctration (fist revision ). 31IS : 1204 - 1978 5. REPORT 5.1 Calculate the percentage by weight of the original samples and report it ac the percentage residue of 100 penetration, stating whether the pene- tration was actually determined for the sample tested or calculated by interpolation, 6, PRECISION 6.1 Duplicate determinations by this method shall not differ from each other by morc than 1-0 percent with the same operator, and not more than 2°5 percent between different laboratories. 7. PRECAUTION 7.1 Certain types of cut back bitumens readily form rings of hard bitumen at the side of the container. Care shall be taken that this material is completely fluxed into the sample before the penetration of residue is determined.18: 1205-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF SOFTENING POINT { First Revision ) 1. SCOPE 1.1 This standard covers the method for the determination of softcning point of asphaltic bitumen and fluxed native asphalt, road tar, coal tar pitch and blown type bitumen. 2. TERMINOLOGY 2.0 For the purpose of this standard, the following definition and those given in IS : 334-1965* shalt apply. 2.1 Softening Point — The temperature at which the substance: attains a particular degree of softuning under specified condition of test. 3. APPARATUS 3.1 Ring and Ball Apparatus —A convenient form of apparatus is illustrated in Fig. 1. BAA Steel Balls-— two; each 95 mm in diameter and weighing 3:50 + 0-05 g. 31.2 Brass Rings — two; the rings shall be tapered { see Fig. 2) and shall conform to the following dimoasions: Depth 6440-1 mm Inside diameter at bottom 15°99 + Ol mm Inside diameter at top 17-5 + 0-1 mm Outside diameter 20°6 + Ol mm *Glowary of tcrms relating te bituincn and tac (revised). 3318: 1205 - 1978 ERMINATION OF ‘two Ranas ) Fic. 1 AsieMptxy oF Arraratus ror D Sorteninc Por (Rung anp Bact For convenience in mounting the rings in a support of the type shown in Fig, 1 to 4, the outside diameter of the ring at the bottom may be smaficr, but shall be not less than 19-0 mm. SL.3 Ball Guide — A convenient torm of ball centering guide. A recoin- niended form of ball guide is iustrated in Fig, 3. 3.1.4 Support — Any micaus of supporting the cings may be used provid- ed the following conditions are observed: a) ‘Che rings shall be supported in a horizontal position with the upper surfaces of the rings 50 mm below the surface of the bath liquid re shath be a distance of exactly 23 inm between the bottom rings and the top surlace of the bottom plate of the support, if any, ur the Lottorn of the bath. 341S: 1205 - 1978 THIS DIAMETER To Be SLIGHTLY (APPROX 0-OSae) LANGER THAN 95 19 ALLOW PLAGING AND CENTERING $5 STEEL OAL 24 WALL WITH 116 RECESS FOR HOLOMNG aING LL protstons eater THREE EQUALLY SPACED = 4:8 DIA HOLES BEIMEEN rt 7 cach wa Wako ul at 20-4to4 Hs ‘All dimensions in millimetres. All dimensions in millimetres, Fie. 2. Tapzrep Rinc Fic. 3. Bate Centertna Guine AU dimensions in millimetres. Tic. 4 Runs Howwen c) The thermometer shail be suspended so that the bottom of the bulb is level with the bottom of the rings, and within 10 mm of the rings, but nct touching them. BLS Thermometer —Tt shall be of the ameicury-i-gls type, nitrogen filled, with the stem made of lead glass or other suitable glass. Tt shal! be engraved and enamelled at the back and provided wilh an cxpausion chamber and glass ring at the top. The bulb shall be cylindrical, made of 35IS; 1205 - 1978 suitable thermometric glass. Tho dimensions, tolerances and graduations of the thermometer shall be as follows: Low High Tamperaturs. Temperatere Range —2°C to 80°C 30 to 200°C Graduation at cach O20 0520 Longer lines ateach re vc Figured at each 2C SC Immersion, mm Total Total Overall Jength 378 to 384 mm. 378 to 384 mm Length of graduated 243 to 279 mm 243 to 279 mm portion Length of bulb, Max 9 to It 9 to 14 mm Not larger than Not larger than stem diamater stem diameter Stem diameter 6-0 to 7-0 mm 60 to 7-0 mm Distance from bottom of 75 to 90 mm 75 to 90.mm bulb to 0°C Scale error, Max #£02°C +0-3°C 3.1.6 Bath — a heat resistance glass vesscl not less than 85 mm in diame- ter and 120 nuu de dept, The bath liquid shall be freshly boiled with distilled water when testing maierials having softening points below 80°C, and pure glycerine for materials having softening points above 80°C, 3.1.7 Stirrers — manual or mechanical, which operates smoothly to ensure uniform heat distribution at all times throughout the bath. The etirrers shall be ao placed that the moulds are not disturbed when the stirrer is in operation, 4, PROCEDURE 4.1 Preparation of Test Sample — Heat the material to a temperature between 75°C and 109°C above its softening point, stir until it is completely fluid and free from air bubbles and water, and filter, if necessary, through IS Sieve 30 (see 1S: 460-1962"), Place the sings, previously heated to a temperature approximating to that of the molten material, on a metal plate which has been coated with a mixture of equal parts of glyccrine and ecification for test sieves { revised ). 36IS: 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 ait, level the material in the ring by removing the excess with a warmed, sharp knife, 4.2 Materials of Softening Point Below 80°C — Assembie the apparatus with the rings, thermometer and ball guides‘in position, and fill the bath to a height of 50 mm above the upper surface of the rings with freshly boiled distilled water at a temperature of 5°C. Maintain the bath at a temperature of 5°C for 15 minutes after which place a ball, previously cooled to a temperature of 5°C, by means of forceps in each ball guide. Apply heat to the bath and stir the liquid so that the temperature rises at a uniform rate of 5-0 + 0°5°C per minute until the material softens and. allows the ball to pass through the ring. The rate of temperature rise shall not be avcraged over the period of the test, and any test in which the rate of temperature rise docs not fall within the specified limits after the firet three minutes shall be rejected. Make the determination in duplicate, 4.3 Materials of Softening Point Above 80°C — The procedure for materials of softening point above 80°C is similar to that described under 4.2 with the difference that glycerine is used in place of water in the bath and the starting temperature of the tcst is 35°C, Make the determination in duplicate. 5. REPORT 5.1 Record for each ring and ball, the temperature shown by the thermo- meter at the instant the sample surrounding the ball touches the botturn 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 for the emergent stem of the thermometer, as the softening point. G. PRECISION G1 Test results shall not differ from the mean by more than the following: Softening Point Repeatability Reproducibility °C °c °C 40 to 60 10 5S fl to 80 15 55 81 to 100 20 55 102 to 120 25 55 121 to 140 3-0 oy 371S : 1205 - 1978 7, PRECAUTIONS 7.1 Gnly freshly boiled distilled water shall be used in the test, as other- wise air ubbles may form on the specimen and affect the accuracy of the results, 7.2 The prescribed rate of heating shall be rigidly adhered to for ensuring accuracy of results. 73 A sheet of filter paper or thin amalgamated sheet, placed on the bottom of the glass vessel and conveniently weighed would prevent the material from sticking to the glass vessel, and considerable time and trouble in cleaning would thereby be saved. 38181 1206 ( Part I) - 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF VISCOSITY PART | INDUSTRIAL VISCOSITY ( First Revision } 1, SCOPE 1A This standard ( Part 1} covers the methods for the determination of viscosity of road tar and cutback bitumens. 2, TERMINOLOGY 2.0 For the purpose of this standard, the following definition and those given in 3S : 334-1965* shall apply. 2.1 Industrial Viscosity — The property of a fluid by which it resists flow due to’ internal friction, and one of the methods by which 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 specificd temperature. 3. METHOD A (VISCOMETER FITTED WITH 10-mm CUP FOR ROAD TAR) 3.4 Apparatus BAL Tar Viscometer — consists essentially of a cup having a specified orifice and valve; a water bath mounted on three legs having a suitable sleeve for the cup, a stirrer, a shield and a receiver (see Fig. 1). The foliowing is the detailed description of the different parts and accessories of tar viscometer: a) Cup— known asthe 10-mm cup, is constructed of hard brass tubs of the dimensions shown in Fig. 2 and Gtted with an external brass collar at the upper (open) ond of the cylinder to support the Glossary of terms relating to bitumen and tar ( revised ). 91521206 ( Part 1) - 1978 VALVE SUPPORTED tN “UP” POSITION INSULATED MANDLE Fic. 1 Tar ViscomzTer18: 1206 ( Part 1) - 1978 HARD BRASS TUBE ooo t-025 IGGC0.0a5 HOSPHOR BRONZE SPHERE 12-70 2-05 DIA eoflo Cast All dimensions in millimetres. Fro. 2. 10-mm Tar Cur anp VaLve cup in the sleeve of the water hath. The bottom of the cup consists of a circular phosphor-bronzc plate screwed into the cylinder and made conical to facilitate drainage of the tar after use. It is provided centrally with a perfectly cylindrical, Phosphor brome (90/10 cast ) extension of the dimensions shown in Fig. 2. The extension is drilled and polished internally to give « 10-mun circular orifice. The upper rim of the ofifice shall be perfectly circular in order to provide 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 +: 0-025 mm 411811206 ( Part 1) - 1978 b) Valre— shall be of dimensions shown in Fig. 2. It scrves to close the orifice of the 10smm cup and is a phosphor-bronze sphere attached ta a monel metal rod. The rod is provided with a levalling peg and at the upper end a hemisphere by which the valve is held in the valve support. ) Water bath — made of copper sheet, is cylindrical in shape, about 160 mm in diameter and 105 mm in depth. It may be heated electrically, care being taken that local heating is avaided, The water bath ig 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. d) Sleve— to Teceive the cup and to hold it in position with an easy sliding fit. Ie is a stout brass tube, 105 mm in height and 42 mm internal diameter, which is bronzed or soldered into a central huls cut in the bottom of the bath, ¢ Stirrer — consists of four vertical vanes, with the upper and lower portions turned in opposite directions, mounted on a cylinder which slips on the slecve with an casy sliding fit. The cylinder is cut away between the vanes to facilitate heat transfer from the water in the bath to the tar cup; vertical grooves are provided-on the inner surface of the cylinder to prevent the water in the bath from being carried into the tar cup, if the stirring system be raised. f Curved shield — fixed to the upper edge of the cylinder and extends te within about 5 mm of the walls of the water bath. This shield carries an insulated handle for rotating the stirrer, a support for a thermometer, anda swivelled support for the valve. ‘The two positions of this valve support are respectively (a) well clear of the tar cup, and (b) extending over the tar cup so that the valve, when resting on the support, hangs vertically over and 16-1 mm above the orifics of the tar cup. g) Receiver—a 100-ml_ graduated measuring cylinder with graduatinas at 20 iul, 23 al and 73 ml capacitics, having an internal diameter of not more than 29 mm. h Thermometers — two standard thermometers, one for the bath and another for the cup. Both the thermometers shall be of the same vange, depending on the temperature at which the determination fe being mate The thermaniclers shall be of mercury in glass tube with cvlindrical bulbs and made of suitable thermometer lass and shall conform to the following requirements:15 5 1206 ( Pare 1) - 1978 Characteristic Low Medium High Range 0 to 4°U 378 to BEC 76 to 1B2U Graduations oz 02°C 02°C Immersion 65 mm 45 mm 65 mm Overall length 340 + 10 mm 340 + 1d mm 340 + 10 mm Stem diameter S5toFOmm $510 80 mm 55 to 8-0 mm Bulb length 10 to 16 mm 10 to 16 mm 10 to 16 mm Bulb diameter <——— Not larger than the stem diameter ———> Length of 150 to 190mm 150 ta 190 mm ~—150 to 190 mm graduated portion Longer lines 1°C and 5°C: 1°C and 5°C I’C and S°C at each Figured at each SC sc SG Seale + 02°C £02°C +O5C j) A stop wateh of a stop clack or any other timing device — capable of being read up to half a second. 3.2 Procedure 3.2.1 Adjust the tar viscometer so that the top of the tar cup is level. Heat the water in the water bath to the teraperature specified for the test and maintain it within + 0°1°C of the specified temperature throughout its bulk for the duration of the test, the stirrer being genuy rotated at freqnent intervals nr, preferably, continnariely. 3.2.2 Clean the tar cup orifice of the viscometer with 4 suitable solvent and dry thoroughly. 3.2.3 Warm and stir the material under examination to 20°C above the temperature specified for the test, and cool, while continuing the stirring. When the temperature has fallen to slightly above the specified temper- ature, pour the tar mto the tar cup until the levelling peg on the yalve rod is just immersed when the latter is-vertieal_ 3.2.4 Pour imto the graduated receiver 20 ml of mineral oil, or a one percent by weight solution of soft soap, and place it under the orifice of the tar cup. 3.2.5 Place a second standard thermometer in the tar and stir the Jaster until the temperature is within + 0°1°C of the specified temperature. When this temperature has been reached, suspend the thermometer co- axially with the cnp and with its bulh approximately at the geometric contre of the tar. Allow the ateembled apparatus to stand [or five minutes during which period the thermometer reading shall remain within 0-05°C 4318 +1206 (Part 1) - 1978 af the specified temparature. Remove the thermameter and quickly vemove:any excess of tar so that the final level ison the centre line of the levelling peg when the valve is in vertical position, 3.2.6 Lift the valve and suspend it on the valve support. Start the stop watch or the time recording device when the reading in the cylinder is 25 ml and stop it when it is 75 mL. Note the time in seconds. 3.3 Report 9.3.1 Report the time in seconds taken by 50 ml of the tar to flow out as the viscosity of the sample at the tampsfature specified for the test. 3.3.2 State clearly whether the sample was dried or tested as received. as the presence of water, particularly in quantities less than one percent, has a marked efferr on the visensity. Reporr the method of drying adopted. 3.4 Precision — The results of repeat determinations on portions of the same sample shall fall within +4 percent of the average of several readings. 3.5 Precautions 3.5.1 The working range of the instrument with the 10-mm cup is such that the time of efflux shall be between !0 and 140 seconds. 3.5.2 The temperature of test shall be appropriate to emulate the condizion specified under 3.5.1 and shall be a multiple of 5°C, not lower than . 3.5.3 The tar cup is a critical part of a viscometer and special precautions shall be observed in its treatment and use. Any cleaning process shall be of gentle nature, Non-corroding solvents, such as light tar oils, free from phenols, are recommended rather than mechanical means, such as dusters, which are liable to cause abrasion of the metal, especially at the orifice. Tfany material bo-uscd for rubbing the intcrior of the cup, it shall not be such as may distintegrate in use, leaving particles which may interfere with the free flow of the sample through the orifice. 3.5.4 The orifice of the tar cup shall be tested at frequent intervals with a gauge having appropriate diameters. 4, METHOD B ( VISCOMETER FITTED WITH 4-mm CUP FOR CUTBACK BITUMENS ) 4.1 Apparatus — ‘I'he 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 dtmensiéns of orifice and jet shallbe as follows: Diameter of the orifice 4000 + 0-025 mm Length of jet 5-000 -£ 0°025 mm 4IS: 1206 ( Part 1) - 1978 4.2 Procedure — The procedure shall be the same as specified in Method A (see 3.2) except that the 4mm cup shall be fitted in tar viscometer instead of the 10-mm cup. 4.3 Precautions 4.3.1 The working range for the instrument with the 4-mm orifice is such that the time of efflux shall be between 20 and 200 scconds, 4.3.2 The temperature of test shall be appropriate to ensure the condition specified under 4.3.1 and shall be a suitable multiple of 5°C, not lower than 20°C, 5. REPORT 5.1 Report the visecsity of the s.mple at the specified temperature for the test, the time in seconds nearest to whole number taken by 50 ml of the tar to flow out. 6, PRECISION 6.1 Results of duplicate tests should not differ by more than the iollowing amount: Viscosity Repeatabilily Reproducibility Below 20 ¢ 25 Qs 20 to 40 s 258 10 percent of the inant > 405 5 percent 10 percent of the of the mean mean 45As in the Original Standard, this Page is Intentionally Left Blank1S + 1206 ( Part I) - 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF VISCOSITY PART it ABSOLUTE VISCOSITY ( First Revision ) 1. SCOPE LA This standard (Part II) covers the method for the determination of absolute viscosity of bitumens and cut-backs by vacuum capillary visco- meters at any specified temperature. It is applicable to materials having a viscosity range of 42 to 200 000 Poisus, ‘Nore — The standard covers three types of viscometers and any one of them can be used for determination of absolute viscosity. 2, TERMINOLOGY 2.0 For the purpose of this standard, the following definitions and those given in I$ : 334-1965" shall apply. 2.1 Absolute or Dynamic Viscosity of a Newtouian Liquid — It is an internal friction, such that if a tangential force of one dync (0:00001 N ) acting on planes of unit area separated by unit distance of the liquid pro- duces unit tangential velocity, the cgs unit for the viscosity of the liquid is 1 Poise. 2.2 Newtonian Liquid — A liquid in which the shear stress is directly proportional to the rate of shear strain, The constant ratio of shear stress to the rate of shear strain is called the coefficient of viscosity of the liquid. If this ratio is not constant then the liquid is non-Newtonian, 3. APPARATUS 3.1 Viscometers — Capillary type made of borosilicate glass, annealed suitable for this test are given in BLE to 3.1.3. *Clossary of terms relating to bitumen and tas (renired 4718: 1206 ( Part 11) - 1978 3.1.1 Cannon-Manring Vacuums Viscometer ( Fig. 1) — The size numbers} imate bulb fuctors K, and viseusily ranges for the series of Cannon- Manning Vacuum Capillary Viscometer are as follows: Viscometer Approximate Calibration Factor Viscosity Range Size No. 30 cm Hg Vacuum Poises pers Poises (ren Bulb B Bulb 10 20 06 36 to 800 u G0 20 120 to 2400 12 200 60 360 to 8000 13, 60-0 20-0 1200 to 24000 “4 200-0. 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 both measuring bulbs. 3.1.2 Asphalt Institute Vacuum Viscometer ( Fig. 2) —'The size numbers, approximate radii, approximate bulb factors K, and viscosity rangcs for the series of Asphalt Institute Vacuum Capillary Viscometer sure as fellows: Viscometer Capillary Approximate Calibration Factor Viscosity Size No. Radius. ~—-K. 30. cmElg. Pacuum: Poise pers Range ‘Poises om BulbB BulbG BulbD 25 0-012 5 2 1 O7 42 to 800 50 0025, 8 4 3 180 to 3200 100 0-050 32 16 10 600 to 12800 200 0-100 128 6+ 40 2400 to 52000 400 0-200 800 250 160 9 600 to 200 000 This viscometer has measuring bulbs B, @ and D located on the viscometer arm M which is a precision bore glass capillary. The measur- ing bulbs are 2 cm long capillary segments separated by timing marks F, G, Hand L. 3.1.3 Modified Koppers Vacuum Viscometer (Fig. 3)—The size numbers approximate radii, approximate bulb factors K, and viscosity ranges for the series of Modified Koppers Vacuum Capillary Viscometer are as follows: Viscometer Capillary Approximate Calibration Factor Viscosity SizeNo. Radius -K. 30 com Hg. Vacuum: Poise pers Range Poises cm coe Bulb B BulbG Bulb D 25 00125 2 i O7 42 to 800 50 0-025. 8 4 3 180to 3200 100 0050 32 16 10 600 to 12800 200 0-100 198 64 40 2400 to 52.000 400 0-200 500 250 160 9 600 to 200 000 48TS¢ 1206 ( Part 11) -1978 TO VACUUM FILLING Tupe-A VACUUM TUBE -M OVERFLOW BuLE-O THIRD TIMING MARK -~H 230-260 Bula: C SECOND TIMING MARK -G FIRST TIMING MARK —F CAPILLARY ~ Fitl LINE-E Alll dimensions in millimetres. Fie, 1 Canyon-Manaing VAGUUM CAPILLARY VISCOMETER 491821206 { Paxe 11} - 1978 1G vacuum FILLING tug -A VACUUM TUBE ~M. SOURTH TIMING MARK ~ L 230-260 THIRD TIMING MARK ~H SECOND TIMING MARK - G EARS) TIMING MARKS F Fila Line - E All dimensions in millimetres. Fia. 2) ASPHALT INSTITUTE VACUUM CAPILLARY VISCOMETER 5018 1 1206 ( Pare IT ) - 1978 TO VACUUM VACUUM TUBE ~ M. GROUND GLASS JOINT -N. FILLING TUBE ~ A FOURTH TIMING MARK ~ L FIRST TIMING MARK ~F File LINE — E Ail dimensions in millimetres. Fic. 3° Moorrrep Kovrers Vacuum Capittary Viscomerer This viscometer consists of a separate filling tube 4, and a precision bore glass capillary vacuum tube M. These two parts are joined by borosilicate ground glass joint V, having a 24/40 standard tapor. The measuring bulbs B, G, and D on the glass capillary are 2 cm capillary segments soparated by timing marks F, G, Hand L. 51IS: 1206 ( Part If) - 1978 A viscometer holder can be made by drilling a 28-mm hole through the centre ofa No. 11 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 place. 3.2 Thermometer — The thermometer shall be of mercury in glass tube with cylindrical bulbs and made of suitable thermometer glass and-shall conform to the following requirements: Chavacteristic Tow Medium High Range 0 te 44°C 37-8 tn 82°C 76 to 1220 Graduations o2c 02°C 0-20 Immersion 65 mm 65 mm 65 mm Overalliength 340 + 10 mm 340 + 10 mm 340 £10 mm Stem diameter 5°5 to 8-0 mm 55 to 80 mm 5-5 to 8-0 rm Bulb length 10 to 16 mm 10 to 16 mm 10 to 16 mm Bulb diameter Not larger than —Not larger than Not larger than the stem dia- the stem dia- the stem dia- macter meter motor Length of gradu 150 to 190 mm 150 to 190 yam 150 to 190 mm ated portion Longer lines at 1°. and 5°C VC and 5°C: °C and 53°C each Figured at each = 53°C aC 7c Scale -£ 0" +£o2C + OLE 3.3 Bath — A suitable bath for immersion of the viscometer so that the Liquid reservoir or top of the capillary, whichever is uppermost is at least 20 mm below the upper bath level, and with a provision for the visibility of the viscometer and the thermometer. Firm aupport for the viscometer shall be provided. The accuracy of the viscometer bath should be + 0:1°C over the entire length of the viscometer or frora viscometer to viscometer in the various bath positions. 3.4 Vacuum System —A vacuum system capable of maintaining a vacuum to within -0-09 cm of the desired level up to and including 30 em of mercury. Ce such sstem is shown in Fig. 4. The glass tubing of 695 mm diameter and all glass joints should be completely aictight and a0 loss of vacuum should be permitted till the experiment ison. A vacuum or aspirator pump is suitable for dhe vacuum source. 3.5 Timing Device — A stop watch or stop clock capable of boing read up te halt a second. 52TS: 1206 ( Part 11) - 1978 GiASS OPEN-FNN MERCURY MANOMETER 10 VISCOMETER BOROSILICATE GLASS STOPCOCKS CARTESIAN MANOSTAI (OPTIONAL) BLEEO VALVE 10 vaCUuLM PUMP I-LITRE SURGE TANK 1- LITRE SURGE TANK Note — All tubing is of glass with 6°35 mm OD. Fic, 4 Suaorsren Vacuum System FoR VACUUM CAPILLARY VISCOMETERS 4. CALIBRATION OF VISCOMETERS 4.1 Reference Material — Any liquid of known viscosity may be used for calibration purposes. 4.2 Calibration — Charge a clean-dry viscometer by pouring the refer- ence material to within + 2 mm of fill line E (Fig. 1, 2 and 3). Place 53IS: 1206 ( Part YE) - 1978 the-charged viscometer in the viscometer bath maintained within -+0-1°C at the calibration temperature. Establish a 30 + 0°05 cm vacuum in the vacuum system and connect it to the viscometer with valve closed in the Une leading to the viscometer. After the viscometer has been in the bath for 30 + 5 minutes, start the flow of liquid in the viscometer by opening the stup cock in the line leading to the vacuum system. Measure to within 0'5 3 the time required for the leading edge of the meniscus to pass between timing marks F and G, Also measure to within 0-5 s the time required for the lead- ing edge of the meniscus to pass between, timing marks Gand H. Calculate the calibration factor X for each bulb as follows: vr key where K — viscometer bulb calibration factor polses/s at 30-0 em Hg, ¥ = absolute viscosity of reference material at calibration tem- perature in poises, ani ¢ = flow time in seconds, Repeat the calibration procedure using the same viscosity standard or another reference material. Record the average calibration constant K. 5. PROCEDURE 5.1 Preparation of the Sample — Heat the sample to a temperature not more than 60°Q for the tars and pitches and not more than 90°C for Ditumens above their respective approsimate softcning point temperature respectively until it has become sufficiently fluid to pour. Transfer about 20 ml into a suitable container and maintain it tu a temperature of 135 4 55°C sticring occasionally to prevent local overheating and allow the entrapped air to escape. SAL] Charge the viscometer by pouring the prepared sample to within + 2 mm of fill line Place the charged viscometer in an oven or bath maintained at 135 £ 5°5°C for a period of 10 -+ 2 min w allow large air bubbles to escape. 52 Testing — Maintain the bath at the test temperature within + 01°C, Place the charged viscometer vertically in the waterbath with the help of a holder so that the uppermost timing mark is at least 2 cm below the surface of che bath liquid. Establish 3 vacuum of 30 + 0°05 ¢m of mercury in the vacuum system and connect it to the viscometer with the valve closcd. After the viscometer has remained in the bath for 30 4- 5 min open the valve and allow the asphalt tv flow into the viscometer. Measure tu with- in + 05s the time required fur the leading edge of the meniscus to pass between successive pairs of timing marks. Upon completion of the test, 541S: 1206 (Part Il) - 1978 remove the viscometer from the bath and place it in an inverted position in an oven maintained at 135 + 5°C until asphalt is deained off thoroughly fram the viscometer. Clean the viscometer thoroughly by rinsing several times with an appropriate solvent comple Dry the tube by passing a slow stream of filrered dry air throngh the capillary for 2 minutes. Periodi- cally clean the instrument with chromic acid to remove organic deposits. Rinse thoroughly with distilled water and acetone and dty with clean air. 6. CALCULATION 6,1 Calculate and report the absolute viscosity to three significant figures, by the following equation: ‘Viscosity Poises a=» At where K = selected calibration factor, in poise per second; and. t = flow time, in seconds. 6.2 Always report the test temperature and vacuum with the viscosity test results, For example, viscosity at 60°C, 30 cmHg Vacuum in poises. 7, PRECISION 7.1 The duplicate test rcsults should not differ by more than the following: Repeatability Reproducibility ? percent of their mean 10 percent of their mean 55As in the Original Standard, this Page is Intentionally Left Blank1S : 1206 ( Part II) - 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF VISCOSITY PART SI] KINEMATIC VISCOSITY ( First Revision } 1. SCOPE 2.1 This standard (Part III) covers the method for the determination of kinematic viscosity of paving grade and cut-back bitumens and distillation. residues of cut-backs. It is applicable to the materials having a viscosity range -of 30-100 000 cSt. 2. TERMINOLOGY 2.0 For the purpose of this standard, the following definitions and those given in IS : 334-1965* shall apply. 2.1 Absolute or Dynamic Viscosity of a Newtonian Liquid —- It is an internal friction such that, if a tangential force of one dync ( 0:00001 N ) xeting on planes of unit area separated by unit distance of the liquid pro- duces unit tangential velocity, the cgs unit of the viscosity for the liquid is 1 Poise. 2.2 Density — Iv is the mass per unit volume, the cgs unit of density is g/cm? and the ST unit of density is 1 kg/m*. 2.3 Kinematic Viscosity of a Newtonian Liquid — It may be defined as the quotient of the absolute or dynamic viscosity divided by the density of the Tiguid under test; both at the same temperature. The cgs unit of kinematic viscosity is the stoke which has the dimensions square centimetre persecond. For petroleum products the kinernatic viscosity is generally expressed in centistokes (cSt) which is 1/100th of a stoke. 2.4 Newtonian Liquid — A liquid in which the shear stress is directly proportional to the rate of shear strain. The constant ratio of shear stress to the rate of shear strain is called the cocflicient viscosity of the liquid. If this ratio is not constant then the liquid is non-Newtonian. "Gloncary of terme relating to bitumen and tar ( reised). 5718: 1206 ( Part II1)~ 1978 3. APPARATUS 3.1 Viscometers — The capillary type of viscometer of borosilicate glass annealed snitable for the test are as given in 3.1.1 and 3.1.2. 3.1.1 Cannon-Fenske Viscometer for Opaque Liquids — Detailed drawings of the reverse-flow Cannon-Fenske viscometer are given in Fig. 1. The size, dimensions, approximate constant, kinematic viscosity range, capillary diameter and bulb, volumes shall be as given in Table 1. ———— ee TABLE 1 DIMENSIONS OF CANNON-FENSKE OPAQUE VISCOMETER FOR ‘RANSPARENT LIQUIDS OPAQUE AND T! Size APPROXI- Kivewaric = Insioz Dia Insine Dia Voiume = VoLUmE. No. MATE ‘Viscostry or Tune, or Tune, © Bur2s4, = Bune Constant, RANoz, R NanvG, Cann J Dil St/s ‘oSr mm Tunes ml (5%) (2%) A, FanpK (5%) rom (£5%) 150 0-035 21095 O78 32 ZL Ww 200 Or 6 to 100 1-02 a2 21 uM 300 025 15 to 200 1-26 34 at uN 350 O5 30 to 500 148 a4 zt u 400 12 72 ta 1200 1:88 a4 ay iN 490 25 150 to 2 500 220 37 at NW 500 a 480 to 8 000 a0 40 21 n 600 20 ¥ 200 ta 20.000 4-00 aT zt 3 3.1.2 BS U-Tube Modified Reverse Flow Viscometer —The viscometer shall be made of clear borosilicate or other heat resistant glass free from visible defects, All glass tubing used in the construction of a single viscometer shall be of the same composition and the finished instrument shall be thoroughly annealed, ‘The design and dimensions of the viscometer are given in Fig. 2 and Table 2, . TABLE 2_ DIMENSIONS AND VISCOSITY RANGES OF BS U-TUBE MODIFIED REVERSE FLOW VISCOMETER FOR OPAQUE LIQUID Size Approximate = Viscomry = Insie Dna Lenore Insp Dra Votuwee No. — Constant Rance, orTus R or tHe ATE, F = Burne cSt/s St mm Tox R annG ml (2%) 9 mm 4 o1 6-100 4-26 185 5 o3 19-300 164 185 6 10 60-1 000 224 185 7 30 180-3 000 293 185 ga 10 600-10 000 +00 185, 9 30 1800-36 000 BS 185 10 100 6000-100000 7:70 210 1 300 18.000-300000 10-00 210 58IS: 1206 ( Part I) - 1978 All dimensions in millimetres. Fig. 1 Cannon-Fenskr OPAQue VisCoMETER FOR Opaque AND TRANSPARENT Liguins 581S: 1206 ( Part IME) - 1978 25 N-22 275 STOPPER F MATERIAL ly — 4 CAPACITY 1mt \SHZE_ 170 9 ONLY All dimensions in millimetres. Fic, 2 BS/LP/RE U-luse Revers FLow ViSCOMETER: FOR Opague Liguips 3.2 Bath —A suitable bath for immersion of the viscometer so that the liquid reacrvoir or top of the capillary whichever is uppermost is at least 20 mm below the upper bath lev, Provision shall be there for visibility of the viscometer and the thermometer. The efficiency of the stirring and the balance between heat losses and heat input shall be such that the temperature of the bath mcdium is maintained at 4 0°1°C! over the entire length of the viscometer. 3.3 Thermometers — The thermometers shall be of mercury in glass tube with cylindrica’ bulls and made of suitable thermometer glass and shall conform to the following requirements: Characteristic Low Medium High Range Oto 44°C 378 to 82°C 76 to 122°C Graduations O23 o2C 02°C Immersion 63 mm 65 mm 65 mm 60TS: 1206 ( Part MIL) - 1978 Characteristic Law Medium High Overall length © 340410mm = =—340-£ 10 mm 340 4+ 10 mm Stem diameter 55 to FO mm. 55 to 8-0 mm 5:5 to 80mm Bulb length 10 te 16 mm 10 to 16 mm 10 to 16 mm Bulb diameter —- Not larger than ‘Not larger than Not larger than the stem the stem the stem diameter diameter diameter Length of gra- 150 to 190 nm 150 to 190 mm 150 to 190 mm duated portion Longer lines at 1°C. and 5°C. PGand 5°C 1°C and 5°C each, figured at each Scale Orc AGOLG OG 3.4 Timing Device —Any timing device such as stop-watch or stop- clock expable of being read up to 0°53. 4, CALIBRATION OF VISCOMETER 4.1 Reference Material — Any liquid of known viscosity may be used for calibration purposes. 4.2 Calibration — Charge the clean dry viscometer by pouring the reference material. Place the charged viseameter in the viscometer bath matitained at calibration temperature within + GHC, Allow the charged. viscometer to remain in the bath long enough to reach the tcst temperature. Measure to within 01s the time required for the leading edge of the meniscus to pass from the first timing mark to the sccond. Calculate the viscometer constant C, as fallaws: gc Ca L where V = viseosi di centistokes for dhe stasdard liquid, and f= efftix time it seconds. 4.3 If the viscomuter is used at a lwcation other than the calibrating ishoratory the constant @ should be correrted for the diffrence in the acceleration of gravity ‘7 at the tye locations as fullewst C, = fw OC a where G4 = calibration constant in the testing laboratory, Cy = calibration constant in the cahbration laboratory, 618: 12065 (Part Ul) - 1978 $2 -— acceleration of gravity at the testing laboratoty, and 1 = acceleration of gravity at the calibration laboratory. 5. PREPARATION OF SAMPLE 5.1 Procedure for Cat-Back Bimumens and Oil Distillates — Open the sample container and mix the sample thoroughly by stirring for 303 taking care to avoid entrapped air. For too viscous samples, heat the sealed container in a bath or oven maintained at about 60°C. Pour immediately 20 ml into a clean dry container having a capacity of about 30 ml and seal the container immediately. 5.2 Procedure for Kitumens — Heat the sample to a temperature not more than 60°C for tars and pitches and not more than 90°G for bitumens above the corresponding approximate softening point temperature rex pectively until it attains pouring consistency, Stir it thoroughly and transfer approximately 20 ml in a 80 ml container. Local over-heating and entrapped air should be avoided. &. PROCEDURE 6.1 Procedure for Canuon-Fenske Viscometer 6.1.1 To charge the Cannon-Fenske viscometer invest the viscometer and apply suction to the tube Z, immersing tube W in the liquid sample. Draw liquid through tube NV filling bulbs 2 to fill mark G, wipe excess sample off tube WV and inyert the viscometer to its normal position. Align the viscometer vertically in the bath. Visual observation is sufficient. How- ever, it can be done mare accurately and quickly by suspending a plumb bulb in the tube £, Allow the viscometer to remain in the constant temperature bath for a sufficient timc to cnsure that the sample reaches temperature cquilibrium. Tt takes about 20 min at 38°C, 25 min at 100°C and 30 min at 135°C. When the test temperature is reached, remove the stopper in the tubes ¥ and £ respectively and allow the sample to flow by gravity. Measure to the nearest Ola the time required for the leading edge of the meniscus to pass frum ming mark E to timing mark FL Tf this efflune time is levs than fis, select a viscometer of smaller capillary diameter and repeat the operation. 6.1.2 Upon complctiun of the test, clean the viscometer thoroughly by several rinsings with an appropriate solvent completely miscible with the sample, followed by a completely volatile solvent, Dry the tube by passing a slow stream of filtered dried ate through the capillary for 2 amin or until last trace of solvent is removed. 62IS + 1206 ( Part M1) - 1978 6.2 Procedure for BS U-Tube Modified Reverse Flow Viscometer 6.2.1 Mount the BS U-tube viscometer in the constant temperature bath keeping tubs L vertical, Pour sample through tube W to a point just above filling mark G, allow the sample to flow freely through capillary ‘R, taking care that the liquid column remains unbroken until the lower mark H and then arrest its low by closing the timing tube with a cork or rubber stopper in tubc L. Add more liquid, if necessary to ‘bring the upper meniscus’ slightly above mark G. After allowing the sample to attain bath temperature and any air bubble to rise to the surface (usually about 20-30 min is required ), gently loosen the stogper allowing the sample to flow until it is approximately at the lower filling mark if and press back the stopper to arrest flow. Remove the excess sample above filling mark G by inserting the special pipette until itz cork rests on top of the tube W and apply gentle suction until air is dawn through, The upper meniscus shall coincide with mark G. Allow the viscometer to remain in the constant temperature bath for a sufficient fime to ensure that the sample reaches temparature equilibrium. It takes about 20 min at 38°C, 25 min at 100°C and 30 min at 135°C, Remove the stopper in the tube Wand L respectively and allow the sample to flow by gravity. Measure to the nearest 0°! s the time required for the leading edge of the meniscus to pass from timing mark E to timing mark #, If this efflux time is less than 60s, select a viscometer of smaller capillary diameter and repeat the operation, 6.2.2 Upon completion of the test, clean the viscometer thoroughly by several mixing with an appropriate solvent completely miscible with the sample followed by a completely volatile solvent. Dry the tube by passing slow stream of filtered dry air through the capillary until the last trace of solvent is removed. 7, CALCULATION FL Calculate the kinematic viscosity up to thrve significant figures with the help of following equation: Kinematic viscosity cSt = Ct where C = calibration constant of the viscometer in ccntistokes per second, and. t= cflux time in seconds. 8. REPORT 8.1 Report always the test iemperature aiong with the results as follows: Kinematic viscosity at 60°C = tx St G3IS: 1206 ( Part Ill) - 1978 9. PRECISION 9.1 The duplicate test results should not differ by more than the values given in Table 3. TABLE 3 PRECISION OF TEST RESULTS = MATERIAL REPEATABILITY REPRODUCIBILITY 0. w@ (2) @) % of Mean i) Asphaltic bitumen at PB “350 Hi) Gutback bitamens at ore a) Below 3.900 cSt 1s 3 b) 3000 406 000 cSt 20 29 €) Above 6000 cSt ay 10-0 64181 1207 - 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF EQUIVISCOUS TEMPERATURE (EVT) ( First Revision ) 1, SCOPE 1.1 This standard covers the method for the determination of equiviscous temperature (EVT) of road tar. 2, TERMINOLOGY 2.0 For the purpore of this standard, the following definition and those given in IS: 3341965" shall apply. 2.1 Equiviscous Temperature — That temperature in degrees centi- grade at which the viscosity of the tar or pitch is 50 seconds as measured by standard tar viscometer specified in IS: 1206 ( Part T)-1978t. 3. APPARATUS 3.1 The tar viscometer anc accessories as specified under 3.1.1 of TS: $206 ( Part I )-1978} shall be used. 4. PROCEDURE 4.1 ‘The viecosity at any specified temperature preferably a multiple of 5°C shall be determined in the same manner as specified in Method A: Determination of viscosity of rvad tars [see 15; 1206 ( Part I )-1978f } shall be followed. 5, CALCULATION 5.1 Determine the viscosity of the road tar by Method A of IS: 1206 ( Part [)-1978f using the 10-mm tar cup at the given temperature. “Glossary of terms relating to bitumen-and lar (rnvsed). Methods for testing tar and bituminous materials: Determination of viscosity: Part 1 Industrial viseasity (first revision ). 651S: 1207 - 1978 5.1.1 From the viscosity so determined and the temperature of test, calculate the EVT from T'able 1, which shows the corrections to be applied for the temperature of test to give the EVT when the viscosity has been determined using the 10-mm cup. Example: For a tar having a viscosity of 106 seconds at 30°C, the correction is given in the row against 100 and col 6 as being + 4:3. ‘Therefore, its EVT shall be 34°3°C. TABLE 1 CORRECTION IN CENTIGRADE DEGREES TO BE APPLIED TO ‘TEMPERATURES OF TEST TO GIVE EVT OF TARS OF KNOWN VISCOSITY DETERMINED BY USING THE SPECIFIED 10-mm CUP (Giauses 5.1.1, 5.4.2 and 5.2) Visco 0 1 2 3 4 5 6 7 8 9 Serv N CoanzcTion W °C Seoows - 10 104 -87 -62 -77 -69 ~65 -61 20 57 ~45 43 -38 -35 33 30 ~w1 —E3 22 -20 -19 -17 =15 40 -h4 -b2 —rh -C9 —08 -06 -05 -04 -03 0 +90 $0 $02 FO3 405 FOG $07 FOR 409 60 HEL $b? FPS $b FES FPG FET FEF 418 79 +20 $21 422 422 423 424 425 89 +PR 49R £29 430 450 431 431 90 $34 FS $35 496 496 437 497 +26 493 +39 100 440 440 $41 FEL $42 G42 $43 443 444 444 NO $45 446 446 447 447 448 448 449 449 +50 1200 450 ASL PSL $2 482 $52 483 458 454 454 13000 $55 495 455 456 $50 497 497 $57 458 458 140 $59 459 460 460 +60 46! 461 F461 462 +62 5.1.2 If the viscosity obtained is below 33 seconds or above 75 seconds, ascertain the approximate EVT from Tabie 1. Repeat the determination of the viscosity at the centigrade temperature, nearest to the approximate EVT, which is a multiple of 5. From the viscosity obtained in this repeat determination and the temperature of this test, calculate EVT from ‘able 1. 5.1.2.1 The results of repeat determinations on portiona of the same tar sample shall fall within 4 02°C of the average of several readings. 6615: 1207-1978 The following example illustrates the procedure when a retest is necessary: A tar tested at 35°C is found to have a viscosity of 99 seconds, which is outside the permissible range of 33 to 75 seconds. Table 1 Bives a correction of + 35°C to be applied, making the EVT approximately 38°5°C:. The determination of the viscosity is, there- fore, repeated at the temperature newrest to 365°C which is a multiple of 5, that is at 40°C. At this temperature the viscosity is found to be $8 seconds. From Table |, it is found that a correc- tion of ~1-7°C: is to be applied to the temperature of test, ‘The EVT is, therefure (40 — 1:7 °C = 30-3°C. 5.2 Method for Determining Trae EVT — The EVT determined a9 described in 5,1 may differ from the true EVT. In the case of tars of EVT at or above 17'5°C, the EVT determined according to the method des- eribed may differ from the true EVI by an amount in general not exceed- ing 10 percent of the difference between the temperature of test and the EVT. If it be required to know the true EVT, the viscosity shall be determined at two temperatures, differing by at least 5°C but not more than 10°C_and such that the viscosities are within the range of 25 to 100 seconds, The value of the EVT is calculated for cach temprrature of test by reference to Table |. Ifthe two values are not identical, the true EVT shall be calculated by means of the following farmula: Tene EVT = nag x (T-T) i (4 — where T, and Tz = values of the EVT calculated from the two test temperatures, and. d; and dg = respective corrections applied to the tempera- tures of test to give the EVT. Gare shall be taken with the signs for d, and dy: if the ternperature of the test be above the EVT, the correction shall be negative. If the same value be obtained, it represents the true EVT. 5.3 Approximate Relationship Between EVT and Viscosity 5.3.1 The EVT-Viscosity chart (se Fig. 1) shows the approximate relationship ranging between EVT and viscosity at various temperatures from 20 to 60°C. ‘To obtain trom a given EVT the equivalent viscosity in seconds at any one of the test temperatures shown, a straight-edge shall be laid at right angles across the seale and the rcading made on the appro- priate viscosity scale, 5,3.2 Since viscosities within 10 to [40 seconds only may legitimately be determined cn the tar viscometer described in Method A of 6718: 1207- EMT 0, 19 15 20 2s 30 45— 50 55 1978 VISCOSITY VISCOSITY AT 30°C = ssec —30 35 40 aT 20°C —50 viscosity 60 70 16068 4008 —s000 aoog 1000 Fra. 1 aT 38°¢ —sosec ro —80 VISCOSITY aT as'c — 202 ms ~*° viscosity —40 AT 50C 30 VISCOSITY 7 20sec ATEOT 10 ~1090 —40 a ~iosee “0 a = = =100 m4 h— 120 68 EVT-Viscosrry Renationsuip Cuart18; 1207 - 1978 1S ; 1206 ( Part I }-1978* figures outside these limits given in the chart are meant to be used for the purpose of rough comparison and not for accurate evaluation. 6. REPORT 6,1 The report of the EVT shall be the temperature in degrees centigrade at which. the viscosity is 50 seconds as measured by the standard tar viscometer. 7, PRECISION 7.L The EVY determination made by different operators should not differ by more than the following: Repeatability Reproducibitity oan orc “Mcthods for testing tar and bituminous materials: Determination of viscotity: Past I Industrial viseosity (first revision }. 69As in the Original Standard, this Page is Intentionally Left Blank18s 1203 - 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF DUCTILITY ( First Revision ) 1. SCOPE 1.1 This standard covers the method of determination of ductility of distilla- tion residue of cutback bitumen, blown type bitumen and other bituminous products. 2, TERMINOLOGY 2.0 For the purpose of this standard the following definition and those given in IS: 334-1965* shall apply, 2.1 Ductility — The ductility of a bituminous material is measured by the distance in centimetres to which it will elongate before breaking when a briquette specimen of the material of the form described under 3.1 are pulled apart at a specified speed and at a specified temperature. 3. APPARATUS 3.1 Mould — made of brass with the shape, dimensions and tolerances as shown in Fig. 1. The ends } and 6’ are known as clips, and the parts ¢ and a’ as sides of the mould. The dimensions of the mould shall be such that when properly assembled, it will form a briquette specimen having the following dimensions: ‘Total length 730 405mm Distance between clips 30-0 + 0-3 mm Width at mouth of clip 200402 mm Width at minimum cross- 10°0 + O01 mm section ( half way between clips ) Thickness throughout 10°0 + Ol mm Hoseary of terma relating to bitumen and tar ( revised }. 71U.N All dimensions in millimetres. Fie, 1 Mourn rar Ductiry Tssr 3.2 Water Bath — A bath preferably with a thermostat maintained within & 0°1°C! of the specified, test temperature, containing not less than 10 litres of water, the specimen being immersed to a depth of not less than 100 mm and supported.on a perforated shelf not less than 50 mm from the bottom of the Bach. 3.3 Testing Machine — For pulling the briquette of bituminous material apart, any apparatus may be used which.s so constructed that the specimen will be continuously immersed in water as specificd under 4.3 while the two clips are pulled apart horizontally with minimum vibrations at a uni- form speed, as specified and with suitable arrangement for stirring the water for attaining uniformity in temperature. 3.4 Thermometer — conforming to the following equirements: Characteristic Requirement Range Oto 40°C Graduations o2C Tramersion 65 mm Overall length 340 + 10mm Stem diameter 55 to 80 mm Bulb icugth 10 to 16 mm Bulb diameter Not larger than stem diameter Length of graduated portion. 150 to 190 mm Longer lines at cach IC and 5°C Figured at tach 5G Scale + 02°C 7215 1208 - 1978 4. PROCEDURE 4.1 Unless otherwise specified, the test shall be conducted at a temperature of 27-0 4. 05°C and at a rate of pull of 50°0 + 2:5 mm/min. 4,11 When a low vemmperature ductility test is desired, the test shall be mare at a temperature of 40 +0°5°C and at a rate of pull of 100405 mm/min. 4.2 Completely melt the bituminous material to be tested to a temperature of 75 t 100°C above the approximately softening point until it becomes thoroughily fluid. Assemble the mould on a brass plate and im order to prevent the material under test from sticking, thoroughly coat the surface of the plate and interior surfaces of the sides of the mould ( g and a in Fig. 1) with a mixture of qual parts of glycerine and dextrine. In filling, pour the material in a thin stream back and forth from end to end of the mould until it is more than level full. Leave it to cool at the room tempe- rature for 30 to 40 min, and then place in a water bath maintained at the specified temperature for 30 min after which cut off the excess bitumen by means of a hot, straight-edged putty knife or spatula so that the mould shall be just level full. 4.3 Testing — Place the brass plate and mould with briquette specimen, in the water bath and keep at the specified temperature for about 85 to 95 minutes, Then remove the briquette from the plate, detach the side pieces, and test the briquette immediately. 4.3.1 Attach the rings at cach end of the clips to the pins or hooks in the cesting machine and puil the two clips apart horizontally at a uniform specd as specified until the briquette ruptures. Mcasure the distance in centime- tres through which che clips have been pulicd to produce rupture. While the test is being made, make sure that the water in the tank of the testing machine covers the specimen both above and below it by at least 25 mm and is maintained continuously within 4.0:5°C of the specified temperature. 5. REPORT 5.1 A normal test is one in which the material between the two clips pulls out to a point or to a thread and rupture occurs where the cross-sectional areais aminimum. Report the average of three normal tests as the ductili- ty of the sample, provided the three determinations be within 4. 5 percent of their mean value. 5.1.1 If the value of three determinations do not lie within 4- 5 percent of their mean but the two higher values are within + 5 percent of their mean then record the mcan of the two higher values as test result. 733S: 1208 - 1978 5.2 If the bituminous material comes in contact with the surface of the water or the bottom of the bath, the test shall not be considered normal. Adjust the specific gravity of the water in the bath by the addition of either methyl alcohol or sodium chloride so that the bituminous material does not cither come to the surface of the. water, or tnuch the bottom of the bath at any time during the test. 5.3 Ifa normal test is not obtainable on three successive tests, report the ductility as bcing unobtainable under the conditions of test, 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 flat and level so that the bottom surface of the mould touches it throughout, 7.2, Yn filling the mould, care shall be taken not ta disarrange the parts and thus distort the briquette and to see that no air pocket shall be within the moulded sample. 7418 ; 1203 - 1978 Indian Standard METHODS: FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF FLASH POINT AND FIRE POINT ( First Revision } 1. SCOPE 1 This standard covers the methods for the determination of flash point and fire point of asphaltic bitumen and fluxed native asphalt, cutback bitumen and blown type bitwocn, 2, TERMINOLOGY 2.0 For the purposc of this standard, the following definitions and those given in IS: 334-1965* shall apply. 2.1 Flash Point — ‘Ihc Hash point of a material is the lowest temperature at which the application of ssst flame causcs the vapours from the matcrial momentarily catch fire in the form of a flash under specified conditions test. 2.2 Fire Point — The fire point is the lowest temperature at which the application of test flame causes the material to ignite and burn at least for 5.5 under specified conditions of test. 3. METHOD A ( PENSKY-MARTENS — CLOSED ), FOR DETERMINATION OF FLASH POINT FOR BITUMEN OTHER TEAN CUTBACK BITUMEN 3.1 Apparatus 3.1.1 Pensky-Martens Closed Tester (see Fig. 1) consisting of the following major parts: a) Cup— made of brass, conforming to the dimensions given in Table 1. ‘The inside of the cup may be turned to a slightly larger diameter above the filling mark and the outside may be tapered above the flange, but the wall thickness at the upper Glossary of terms relating to bitumen-and tar (revisel ), 1818 + 1200 - 1978 A— Oil-Cup H — Revolving Shutter 8 — Heating Vessel F—Orifice © ~Stirrer K— Gauge Die D~Thermomerer 2 Lifting Hooks £ + Ignition Burner M-— Optional Form of F—Pilot Burner Sticter Operating G. - Spring Handle Device Fic. 1 Psnsny-Maxruns Cuosep TasTer 161S 1209 - 1978 TABLE 1 DIMENSIONAL REQUIREMENTS OF PENSKY-MARTENS [ Chawse 3.1.3 (0) 3 Su Drwemonat. Regoneeants Min == Normal = Max No. mm mn mo w (2) () (4) (5) i) Thside diameter below filling mark 495 8 Sri fi) Differenee between inside and outside diameters 30 au a4 delow filling mark iii) Inside height 546 559 572, iv) Thickness of bottom 18 24 30 v) Distance from rim to filling mark ahs 28 222 vi) Distance, lower curface flange to bottom of cup 45-2 456 460 edge shall be not less than one millimetre. The flange should be approximately Mmm in width and approximately 3 mm in thickness. It shall be equipped with devices for locating the osition of the lid on the cup and the cup itself in the stove. A dle, attached permanently to the flange of the cup, is a desirable accessory. b} Lid— The lid, including (1) stirring device, (2) cover proper, (3) shutter, and (4) flame-cxposure device, shall satisfy the following requirements: 1) Stirring device —-The lid shall be equipped with a stirting device consisting of a vertical stocl shaft, neither lesa than 25 mm nor more than 3 mm in diameter, mounted in the centre of the cup, and carrying two two-bladed brass pro- pellers. The blades of both propellers shail be approximately 8 mm wide and shall be set at an angle of approximately 45°, The smaller ( upper ) propetler shall have an overall diameter of approximately 20 mm. ‘The larger (lower } propeller shall have an overall diameter between 32 and 44mm. The thick- ness of the propeller blades shall be neither less than 1-2 mm nor anore than 2-0 mm. The collars oa which the propeller blades are mounted shall have horizontal and vertical di- mensions not greater than 10 mm. The plane of the centre of the upper propeller shall be 10 mm below the level of the rim of the cup. The plane of the contre of the lower prapoller shall be 51 mm below the level of the rim of the cup. The level of the rim of the cup is in effect the level of the plane part of the portion of the under surface of the rim. 77481 1209-1978 2) Cover proper ~The cover proper ( see Fig. 2) shall be of brass, and shall have avim projecting downward almost to the flange of the cup and fitting the outside of the cup closely. The thickness of the rover measured just inside the rim, shall be not less than 08 mm and not more than 2mm. There shall be a proper locating device, engaging with a corres: ponding locating device on the flange of the cup, ‘Vere shall be four openings in the cover (see Fig. 2) with the following dimensions: i) Opening 4 is an area defined by arcs of twoconcentric circles and the intersected lengths of two radii. The radius of the outer circle shall be not less than 22:4 mm and not more than 246 mm, The radius of the inner circle shall be not less than 13°5 mm and not more than 142mm, The chord of the are of the outer cirele shall be not less than 127 mm and not more than 13-7 mm. if Openings B and C are of equal arcas, each of the sare general form as opening A, 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 twa circles, arcs of which partly define opening 4. The chord of the outer arc for opening B or opening C shall be not less 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 A, Openings B and C shall be equally distant from opening A and radii drawn through each of their centres shall beat an angle of not less than 135° and not more than 140°, iii) Openings A, 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 limiting values of the dimensional spccification of the preceding text and of Fig. 2. iv) Opening D is a split tube to grip the thermometer collar. Its contre is approximately 20 mm from the centre of the lid and on a radius at an angle of not less than 50” and not more than 60° to a radius passing through the centre of opening C, It shall-be set at an angle of not less than 10°, and not more than 15° to the perpendicular. Its height shall be such that, when a standard thermometer is in position, the bottom of the bulb shall be 35°6 to 40°6 mm below the 781S: 1209 - 1978 H — minimum 23-9 mm maximum 246 mm 3 minimum 13-5 mm meaimum 14-2 mm W— minimum 12-7 mm maximum 13°7 mm N= minimum 48 mm maximum 56 mn S— approximately 19-0 mm U — approximately 127 mm Angles p are equal Angle r— minimum 135° maximum 140" t Ate Oe > ” or ” ise Fic, 2. Cover ror Pensky-Marress Crosep Trsrer 7918 +1209 «1978 level of the rim of the cup ( which corresponds to the lower surface of the portion of the lid inside the rim ). 3) Sautter—The lid shall be equipped with a brass shutter, approximately 2-5 mm in thickness, operating on the plane of the upper surface of the lid. The shutter shall be ao shaped and mounted that it rotates on the axis of the horizontal centre of the lid between the two stops, so placed that when in one extreme position, the openings A, B and G of the lid are completely closed and when in the other extreme position, these orifices are completely opened, 4) Flame-exposure device — The flame-exposure device shall have a tip with an opening 0°7 to 0-8 mm in diameter. The flame- exposure device shall be equipped with an operating mechanism which, when the shutter is in the open position, depresses the tip so that the centre of the orifice is between the planes of the under and upper surfaces of the lid proper, at a point on a radius passing through the centre of the larger opening A and approximately 2°5 mm from the euter edge of the opening. A pilot flame for automatic relighting of the exposure flame should be provided. A bead, 4 mm in dia- meter of suitable material, may be mounted on the lid so that size -of the test-flame can be regutated by comparison. The mechanism operating the shutter should be of the spring type and constructed so that when ut rest the shutter-shall exactly close the three openings A, B and C. When operated to the other extreme, the three openings in the lid shall be exactl: open and the tip of the exposure tube shall be tully depressed. If the air bath is electrically heated and gas is not available, an oil burner shall be used to provide the test-flame, the position of which shall correspond with that of the gas flaine previously specified. c) Stove — Heat shall be supplied to the cup by means of a properly aligned stove which is cquivalent to an air bath. ‘This stove shall consist of (1) an air bath, and (2) a top plate on which the flange of the cup rests. 1) At bath — ‘Lhe air bath shail have a cylindrical interior, 41-3 to 42-2 mm in depth and a diameter not less than 3 mm and not more than 4 mm greater than the outside diameter of the cup. The aic bath may be cithor a lame-heated metal casting or an clectric-resistance element. It 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 it should be not less than 6 mm in thickness, The casting 80IS s 1209 - 1978 shall be designed so that products of combustion of the dame cannot pass up and come in contact with the cup. If the air bath is of the electric-resistance type, it shall be Constructed so that all parts of the interior surfuce are heated equally. This necessitates an even distribution of resistance wire to cover the bottom and walls, and a method of construction such that heat is given out from the whole core of the resistance clement rather than directly from the wire. The result obtained with the electrically heated instrument shall agree with that obtained with gas-heated apparatus with- in 1°C and 3°C respectively, according to whether the low or high range thermometer is used, Top plate—The top plate shall be of metal. The total distance frum the upper surface of the plate to the bottom of the air bath shall exceed the distance from the under surface of the flange to the bottom of the cup by not less than 1-6 mim and not more than 3mm. The top plate shall be mounted with an air-gap between it and the air bath. The top plate may be attached to the air bath by means of three screwa and spacing-bushings. The spacing-bushings s!.ould be of propor thickness to define the air-gap which shall be not less than 3mm nor more than 48 mm. The spacing-bushings shall be not more than 9°5 mm in diameter. x ad) The thermometers conforming to the following requirements shall be used: Low Range High Range Range — 7 to + 110°C 90 to 370°C Graduation at each osc 2G Longer lines at each 1G and 5°C 10°C. and 20°C Figures at each rc 20°C: Immersion 57 mm 57 mm Overall length 260 + 10 mm 200 + 10 mm Length of graduated 143 to 177 mm 143 to 177 mm portion Bulb shape Cylindrical Cylindrical Bulb diameter, Max < Not larger than stem diameter > Stem diameter 5:5 to 80 mm 5'5 to 8:0 mm Distance, bottom of bulb 75 to 9G mm 75 to 90 mm to lowest graduation Expansion chamber Required Required. ‘Top finish Ring Ring Scale error, Max, osc 1°C up to 260°C plus or minus 2°C above 260°C:IS; 1209 - 1978 Either of the thermometers may be employed if the indicated reading falls within 93 te 110°C. The thermometers shall be mounted securely in 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 55mm, The thermometer collar shall have an outside diameter of 12°70 + 0°05 mm and a flange of 2:3 to. 2‘8 mm in thickness. The cement used to fasten the thermometer into the collar shall be of such a nature that it will withstand the action of oi! up to the highest temperature at which the thermometer js used. A swelling shall be provi- ded to ensure the Incation of the thermometer collar at the correct point. 3.2 Procedure 3.2.1 Clean and dry all parts of the cup and its accessories thoroughly before the test is started, ‘Take particular care to avoid the presence. of any solvent used to clean the apparatus alter a previous test, "ill the cup with the matcrial to be tested up to the level indicated by the filling mark. Place the lid om the cup and sct the latter inthe stove, Take care that the locating devices are properly engaged. Insert the thermometer, high oy low range, as required. 3.2.2 Light and adjust the test-flame so that it is 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 per minute. Turn the stirrer at a rate of approximately 60 revolutions per minute. Apply the test-flame at each temperature reading which is a multiple of 1°C upto 104°C. For the temperature range above 104°C, apply the test- ame at each temperature reading which isa multiple of 2°C, the first applic: ation of the test-Aame being made at a temperature at least 17°C below the actual flash point. Apply the test-flame by operating the device controlling the shutter and test-flame burner so that the flame is lowered in 0-5 seconds, left in its lowered position for one second, and quickly raised to its high position. Discontinue the stirring during the application of the test-flame. 3.3 Calculation 3.8.1 Observe and record the barometric pressure, 3.5.2 No corrections shall be made except in case or dispute, when the flash point figure shall be corrected according to the following rules: a) For cach 25 mm below 760 mm barometric reading, add 1°C to the flash point; b) For cach 25 mm above 760 mm barometric reading, subtract 1°C from the flash point. 82 ’19: 1209 - 1978 3.4 Report — Unless otherwise specified, normally the flash point shall be taken as the temperature read on the thermometer at the time of the flame application that causes a distinct flash in the interior of the cup. 3.5 Preci: —- The duplicate test results should not differ by more than the following: Flash Point Repeatability Reproducibility 404°C and below 2°0 35°C Above 104°C ao°G BG 3.6 Precautions 3.6.1 The test flame will neither be larger than stipulated nor will it be applicd more frequently than specified as the surface layer is liable to be superheated. 3.6.2 The bluish halo that sometimes surrounds the test-flame shall not be confused with the true flash. 4, METHOD B ( PENSKY-MARTENS — CLOSED ), FOR DETER- MINATION OF FLASH POINT FOR CUTBACK BIFUMEN 4.1 Apparatus 4.1.1 Flash Point Taster - Pensky-Martens Closed Testor as described under 3st except that the stirrer shall be mechanically operated to stir in a downward direction at a specd of 70 to 80 rev/min. 4.1.2 Thermometer — Low range thermometer as specified in 3.1.1(d). 4.2 Procedure — Bring the material to be tested and the tester to a tem- perature of 17°C lower than the expected flash point. Completely fill the air space between the cup and the interior of the air bath with water at the temperature of the tester and material. Raise the temperature through- out the duration of the test at a-rate of not less than I°C and not more than 15°C per mimite. Proceed as described in 3.2.2 except that: a) rate of heating to be not less than 1°G and not more than 1°5°C per minute, ‘b) the rate of stirring to be 70-80 rev/min, and c) the cest-flame to be applied at each 0°5°C rise in temperature, 4.3 Calcolation and Report — Calculate and report the flash point as described under 3.3 and 3.4, 44 Precision — Duplicate tests shall not differ by the limits specified in 3.5. 83IS 1 1209 - 1978 5. METHOD CG ( PENSKY-MARTENS—OPEN), FOR DETER- MINATION OF OPEN FLASH POINT AND FIRE POINT 5.1 Apparatus — The standard Pensky-Martens Tester and thermometers as prescribed in Method A (se 3.1.1) shall be used with the following modifications: The cover of the cup shall be replaced by a clip which encircles the upper rim of the cup and carries the thermometer and test-flame. The tube carrying the thermometer shall have its centre on a radius at approximately 90° to the radius passing through the point of attachment of the test-Hame, and shall be of such a height that when the thermometer is in position, its bulb shall be in the vertical axis of the cup and 12 mm below the filling line. The test-flame shall be fixed at the vertical axis uf the cup and in level with the upper edge of the cup. 5.2 Procedure 5.2.1 All parts of the cup and its accessories shall be thoroughly cleaned and dried before the testis started. Particular care shall be taken to rcmmove all traces of solvent used to clean the apparatus. 5.2.2 The cup shall be filled with the material to be tested up to the level indicated by the filling mark. 5.2.3 The clip carrying the thermomater and test-flame shall be placed on the cup and the latter sct in the stove. Care shall he taken to have the locating devices properly cngaged, The thermometer shall be inserted. If it is known that the material will flash ahove 104°C, higher range thermome- ter shall be used. Otherwise, it is preferable to start with the lower range thermometer and change if's temperature of [04 to 110°C is reached. 5.2.4 The test-flame shall be lighted and adjusted so that it is of the size of a bead 4 mm in diameter. 5.2.5 Heat shall be applied at such a rate that the temperature record- ed by the thermometer increascs neither less than 5°G nor more than 6°C per minute. The surface of the material shall be carefully observed during heating. 5.3 Report 5.31 Open Flash Boint — The open flash point shall be taken as the temperature when a flash first appears at any point on the surface of the material. 3.3.2 Fire Point — The beating 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 as the fire point. 84+181 1209 - 1978 5.4 Precision — The following criteria should be followed for the accept- ability of test results : Repeatability Reproducibility Flash point ac nc Fire point eC 4c 5.8 Precaution — Care shall be taken to shield the apparatus from draughts. 85As in the Original Standard, this Page is Intentionally Left Blank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 2.1 Float — Made of aluminium or aluminium alloy and conforming to Fig. 1 and the following requirements: Min Normat Weight of float, ¢ 37°70 37°90 Total height of float, mm 340 35°0 Height of rim above lower 265 27-0 side of shoulder, mm. Thickness of shoulder, mun 13 V4 Diamcter of opening, mm 110 1b Max 38°10 360 275 13 112 2.2 Collar — made of brass and conforming to Fig. 1 and the following requirements: Min Normal Weight of collar, g 9°60 9°80 Overall height of collar, mm 22:3 22-5 Inside diameter of bottom, mm 12:72 12-82 Inside diameter ‘at top, mm 9°65 9-70 Max 10°00 22-7 12-92 9°75, 2.2.1 The top of the collar shail’screw up tightly against lower side of the shoulder. 871811210 - 1978 Thermometer- Foat otdath — Teeter 5 2 worese} z FLOAT (al) N ” = 3 pe std THREAD 2 2 Bw7OLO-Os & va @ rdotoug she | & 7 FF . Fe Se 3 22-5202 b4045-1 T — nora o=r |e i2*824t010 COLLAR (Br) Weight of Float, 37°90 + 0-20 Weight of Collar, 9-80 0-70 g Amembly of Apparatus All dimensions in millimetres, except where otherwise stated, Fic, | Froar Test Apparatus 2.3 Thermometer — Low softening point thermometer, graduated in centigrade scale and conforming to the following requirements: Liquid Mercury Filling above liquid Nitrogen gas Temperature range —2 to 80°C: Subdivisions O20 Longer graduation lines at each °C Graduations numbered at each 2°C multiple of Immersion, mm Total $8Total lengtt: Bulb length Bulb diameter Stem diameter 18+ 1210 - 1978 378 to 384 am 9 to ltmm Not larger than stem diameter 6'0 to 7-0 mm Distance of bottom of bulb to 75 to 90 mm graduation line at 0°C Distance of top of thermometer 30 ta 44 mm to graduation line at 80°C Expansion chamber to permit 150°C heating to at least Top finish Glass ring Scale error at any point not to 0-2°C. exceed 2.4 Bath — A water bath at least 185 mm_ in interaal diameter and containing watcr at least 185 mm indepth. The height of the container above the surface of the water shall be at least 100 mm. 2.5 Calibration of Asserably — The assembly of the apparatus and dimensions additional to those given above are illustrated in Fig.1. The assembled float and collar, with the collar filled flush with the bottom and weighed to a total weight of 53-2 g, shall float upon water with the rim 85 + 1°5 mm above the surface of water. 3. PROCEDURE 3.1 Preparation of Sample — Place the brass collar with the smaller end on a brass plate which has been previously coated with equal parts of gly- cerine and dextrine, Melt completely a suitable quantity of residue from cutback bitumen ( see 3.2.3.3 of IS : 1213-1978" ) or the material itself for solid bitumen at the lowest possible temperature to bring it to a sufficiently fluid condition for pouring. Stic thoroughly until it is 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. B.LA 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 means of a spatula or steel knife which has been’ slightly heated. Place the collar and plate in the water bath maintained at 5 3 1°C and leave them in this bath for not less than 15 minutes and not more than 30 minutes. ‘Methods for testing tar and bituminous materials: Distillation test ( frst revision). 8918: 1210 - 1978 3.1.2 Tar 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 bas been 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. 3.2 Heat the bath water to the temperature at which the test isto be made. Maintain this temperature accurately without stirring and the temperature shall at no time throughout the test be allowed to vary by more than 0°5°C from the temperature specified. Determine the temperature by immening the thermometer with the bottom of the bulb at a depth of 40 + 2 mm below the water surface, 3.3 After the material to be tested has been kept in the ice water at 5°C for not less than 15 minutes, nor more than 30 minutes, remove the collar with its contents from the plate, screw into the aluminium float and immerse in water at 5°C for one minute, Remove the water, if any, from the inside of the float and immediately float the latter in the warm bath, making sure that the collar fits tightly into the float, and that there is Ro seepage of water between the collar and float during the test. 4. REPORT 4.1 Determine, by meaus of a stop watch, the time in seconds between placing the apparatus on the water and. when the water hreaks through the material. The mean of time taken in duplicate determination shall be reported. 5, PRECAUTIONS 5:1 Precautions shall be taken to ensure that the collar fits tightly into the float and to see that there is no seepage of water between the collar and float during the test. 90IS; 1211-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF WATER CONTENT (DEAN AND STARK METHOD ) ( First Revision) 1. SCOPE LAL This standard covers the method fur the determination of water content of asphalt bitumen and fluxed native asphalt, 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 those given in IS: 334-1965* shall apply. 2.1 Water Content — The quantity of water present in a material expressed a3 a percentage by mass of the material. 3. APPARATUS AND MATERIAL 3.4 Flask — of 500 ml capacity ( sae Fig. |), 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-secket of a ground glass joint. 3.1.2 A metal flask may be used. 3.2 Condenser — made of heat resistant glass, well annealed and as free as possible 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 as free 34 possible from striae and similar defects, provided with ground glass joints with the dimensions and tolerances as given in Table ] consisting essentially of the upper chamber, side tube with ground glass joint Jcading to the flask and the graduated tube. Numbered graduation marks shall be carried *Glossary of terms relating to bitumen and tar ( revised ). on1S: 1211-1978 RECEIVER Fro. 1 Draw AND STARK ASSEMBLY 9219; 1211-1978 EXT DIA nun 16 EXT BIA {an 7? MAK & EXT DIA 3042 EXT QA fan, So0s10 STANDARD GROUND GLASS JOINT. All dimensions in millimetres. Fro, 2. Convensen 931S; E211 - 1976 right round the receiver tuhe. The graduation marks midway between the numbered marks be carried about half way round the tube and the other marks shall be intermediate in length and shall project equally at each end beyond the shortest graduation marks. rn TABLE 1 DETAILS OF RECEIVERS ( Clauss 3.3) Garaciry of GRADUATION NUMBERING A Maxmum Rur 70 RECEIVER IN INTERVAL, Eveny Exron ml at 20°C mil GaapuaTion ml 2 0-1 to 2 in 0-08 0-5 ml 0-02 Fig. 3 10 1 to 10inot ml 20:06 Fig. 4 oe on Fie. 3 2-ml Reorivan (DgAN Anp STARK APPARATUS ) 94Ws: 1211-1978 CONE OF GROUND cz, ONT AT END OF CONDENSER SOCKET OF GROUND rE GLASS SOUT T TOT cron area EXT DIA latt INT DIAS + O05 ALL DIMENSIONS i MAE Fra. 4 10-ml Reeniver (Dzax ann Stare Apparatus) 3.3.1 When a metal flask is used, the receiver of the type shown in Fig, 3 and 4 without the ground giass joint shall be used and care shall be taken to provide an air-tight connection between the flask and the receiver. 3.4 A100-ml Graduated Cylinder 9.5 Heater —- Any suitable gas burner or electric heater may be used. A gas ring burner with ports on the inside circumference, shall be used with the metal still and shail 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1921211 - 1978 3.6 Solveut — Carrier liquid shall be any one of the following: 3.6.1 Blend 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 ( 1S: 213-1968* ) free from water yielding not more than 5 percent distillate at 125°C and not less than 20 percent at 160°C. 3.6.3 Petroleum spirit with a boiling range of 100 to 120°C, 4. PROCEDURE 4.1 Place about 100 g of the sample, accurately weighed, in the flask and add 100 mi of solvent ( see 3.6). Attach the flask to the Dean and Stark condensing and collecting system, and heat the flask at such a rate that the condensate falla from the end of the condenser at a rate of two to five drops per second. Continue the distillation until condensed water is no longer visible in any part of the apparatus except the bottom of the graduated tube and until the volume of water collected remains constant for a period not less than five minutes. Remove the persistent ring of condensed water in the condenser tube, if any, by increasing the ratc of distillation by aYfew drops per second. Wash droplets of water which adhcre to the lower end of the condenser tube into the receiver with solvent/carrier liquid using the spray tube. Insert a loose plug of cotton wool in the top of the condenser tule to prevent the condensation of atmospheric moisture in the condenser tube. 5. REPORT 5.1 Report the results as water concent to the nearest 0-05 percent by weight if 2 ml receiver, has been used and to the nearest "1 percent if the 10 ml receiver has been used with 100 g of sample. 6 PRECISION 6.1 Duplicate determinations shall not differ by more than the following: Water Collected Repeatability Reproducibility 0 to 1-0 mi Ot ml 0-2 ml I-L to 25 ml Ql ml ar percent of — 0-2 mL-or 10 percent the mean whichever of the mean which- is greater aver is greater ation for coa) based naphtha { first revision ). 961S: 1212-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF LOSS ON HEATING ( First Revision ) 1, SCOPE 1. This standard covers the method for detersnination of loss on heating of asphaltic bitumens. 2. TERMINOLOGY 2.0 For the purpose of this standard, the following definition and those given in IS : 334.1965* shall apply. 2.1 Loss om Heating — The loss in weight (cxclusive of water } of oil of @ bituminous matccial 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 less than 292 mm in height from the top of the heating clement to the top of the chamber and not less than 298 mm in, width and depth. The chamber is provided on one side with a tightly fitting hinged door containing a double-glass window, at least 100 mm square, through which the thermometer may be rcad without opening the door. Ventilation of tic oven is provided by means of either one round yent-hole in the top and one ia the bottom of the oven, or one round vent- hole near the top and one near the bottom on each of the twa sides of the oven, the diameter of cach vent-hole being 12 to 16 mm. Heating of the oven is done by means of electricity and the temperature is maintained within the limits specified far the test. 3.2 Perforated Metal Shelf — A perforated metal shelf approximately 250 mm in diameter; an aluminium shelf of the form and dimensions shown, in Fig. 1, is recommended. The shelf is placed in the centre of the oven sary of terms relating to bitumen and tar ( revised }. 9718: 1212 ~ 1578 POSITION OF S@MPLE CONTAINERS bd Io 3 LLL RE ML. 5 SECTION XX All dimensions in millimetres, ALUMINIIM SHELF FOR Toss oN Heating Tast lee 1365 SQ) Fro. t 98181 1212 . 1978 with respect tv all dimeusiuns of the interior of the oven, and is suspended by a vertical shaft and provided with mechanical means for rotation at the ate of 5 to 6 rev/min. 3.3 Thermometer — A thermometer graduated in centigrade degrees, and conforming to the following requirements shall be used: Liquid Mercury Filling above liquid Nitrogen gas ‘Temperature range 155 to 170°C Subdivisions asec Longer graduation lines at each re Graduations numbered at Immersion Total length Bulb length Bulb diameter Stem diameter Distance of bottom of bulb to graduation line: Atorc At 155°C Distance of top of thermometer to graduation line at 170°C Top finish Scale error at any point when 0°C, 155°C, 163°C and 170°C Total 150 to 154 mm 10 to 15 mm Not larger than stem diameter 60 to 70 mm 33 to 38 mm 70 to 80 mm 20 to 30 mm Glas ring o5°C standardized, Max 3.3.1 The top of the contraction chamber hall be not more than 41 mm above the bottom of the bulb. 3.3.2 The expansion chamber shall permit heating the thermometer at least 25°C above the highest temperature on the scale. 3.3.3 At the ice point, thether mometer shall be graduated from —1°C to +1°C in 0-5°C divisions. 3.3.4 The thermometer shall be supported from the shaft of the metal shelf in a vertical position, approximately 20 mm inside the periphery of the shelf with the hottom of the bulb 6 mm above the shelf. 3.4 Container —of metal or glass, cylindrical in shape with a flat bottom and with internal diameter 55 mm and internal depth 35 mun. 9918; 1212 - 1978 4. PROCEDURE 4.1 Stir and agitate thoroughly the material as received, warming, if necessary, ta ensure a complete mixture before a portion is removed for the test. 4.2, Heat the container in an oven at 100 to [10°C for 30 minutes, cool and weigh. Weigh into the container 500+ 0°5 g of the matezial correct to the nearest 0°01 g. 4.3 Bring the oven to a temperature of 163 + 1°C and place the sample container in the revolving shelf near the circumference or in onc of the recesses if the recumumended shelf is used. Close the oven aud rotate te shelf during the entire test at a rate of 5 to 6 rev/min, the temperature being maintained at 163 + 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 and in no case shall the total time, during which the sample is in the aven, be more than 5 hours 15 minutes, At the end of the specified heating period, remove the containers, cool to room temperature and weigh to OO1 g. 4.3.1 In ordinary circumstances, a number of samples having about the same degree of volatility may be tested at the same time, but sampics varying greatly in volatility shali 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 is to be determined, melt the residue in the container at the lowest possible temperature and thoroughly mix it by stirring, taking care to avoid incorporating air bubbles in the material. Pour 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 5.1 Report to the nearest 0°05 percent the mean percentage loss in weight for the duplicate determinations, correcting for water content, if any, Report also the water content, "Methods for testing tar and bituminous materia’s: Determination of penctration (Arst revision }. 10018: 1212. 1978 6, PRECISION 6.1 Results of duplicate tests shall not differ by more than the following: Loss on Heating Repeatability Reproducibility percent 0 to05 Ol Oz OS to [0 o8 Oe 1-0 to 20 03 O68 Above 2:0 10 percent of mean 20 percent of mean Nore—In this case the repeatability figures refer to the differences between duplicate detcrninatiuns made sitmultansously in the sauic oven. 7. PRECAUTIONS 71 Conduct Uc loss on heating test in duplicate. 7.2 Determine the water content of the sample in accordance with the method for determination of water content specified in 1S : 1211-1978*. 7.3 If the sample contains water, test it in that condition. 7A Reject the tests during which samples show evidence of loss by foaming. Methods for testing tar and bituminous materials: Determination of water content (Dean and Stark method) (first sevision ), 101As in the Original Standard, this Page is Intentionally Left BlankIS : 1213-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DISTILLATION TEST ( First Revision) i. SCOPE 1.1 This standard covers the methods for the distillation test for crude coal tar, road tar, cuthack bitumen, Digboi type cutback bitumen and creosote and anthracene oil. 2. TERMINOLOGY 2.0 For the purpose of this standard, the following definition and those given in IS : 334-1965* shall apply. 2.1 Distillation — The process by which the more volatile constituents are separated from the less volatile oncs. 3. METHOD A ( FOR CUTBACK BITUMEN ) 3.1 Apparatus 3.1.1 Distillation Flask — 500 ml, side arm having dimensions as shown in Fig. 1. 3.1.1.1 The distance from the centre of the side tube at the junction of the neck to the top of the neck shall be 12 + 1 mm. 3.1.1.2 The side tube shall slope downwards from the junction with neck so that the acute angle between the side tube and the neck is 75 + 3°. 3.4.2 Thermometer — of high distillation, total immersion type, graduated in centigrade degrees as specified, having a range of —2 to 400°C and conforming to the following requirements: Liquid Mercury Filling above liquid Nitrogen gas Temperature range —2 to 400°C *Glowary of terms relating to bitumen and tar ( revised }. 103181 1243-1978 et —— 351 10 i : s poe eo-5 19 WBS 2.0678 THICK WALL All dimensions in millimetres. Fig. 1 Disrinration Frask Subdivision Total length, Stem diameter Bulb diameter Balls length Distance of bottom of bulb to graduation line at 0°C Top finish Longer graduation lines at cach Graduations numbered at each multiple Immersion Scale error at any point up to 370°C shall not exceed rc 378 to 384 mm 69 to 70mm Not larger than stem diameter 10 15 mm 25 to 45 mm Glass ring sc 1e°c Total rc 3.1.3 Condenser ( Water) —— A250-snm glass:jacketed condenser (see Fig 2) with the dimensions and tolerances given below: Length of Jacket excluding the necks Outside diameter of adapter of condenser tube Length: of adapter 104 250 + 5 mm 23 + mm 75- Simm18: 1213 - 1978 Outside diameter of condenser 125 +05 mm tube proper Overall length of condenser tube 475 + 25mm including adapter BAA Adopter — of cucved design ( see Fig. 2 ) having a heavy wall ( one millimetre ) and reinforced top glass, with an angle of approximately 105° and with a diameter at the large end of approximately 18mm. ‘The outlet end shall be ground to an angle of 45 + 5° with inside vertical. The small end shall have a diameter of not less than 5 mm. Water jackena_} EN contre ptapter 2 Wol ira pane” 254mm (1 in) WEEE Fie. 2. Distirarion Apparatus ASSEMBLY 3.1.5 Shield — of galvanized iron, lined with 3.mm asbestos, fitted with transparent covered windows, of the form and dimensions shown in Tig. 3; used to protect the flask from air currents ard to prevent radiation. The cover { top ) may be of transit hoard made in two parts, or it may be of galvanized iran lined with 3-mm asbestos. 3.1.6 Grow Receivers — of 25 mi, 50 ml or 100 ml size and of dimensions and tolerances shown in Fig. 4 may be used. 3.1.7 Residue Container — The container for the distillation residue shall be a 250 g metal container approximately 76mm in diameter and 54 mm deep, provided with a lid. 1051S: 1253 «1978 — 14843 tapta 300 1-0 pestos —— COVER IN TWO PARTS a-2to-3 ugte2 “ 12-34 2-9 yt a) = | FLANGED OPEN-END CYLINOER MADE OF 22 § WG GI WITH Bro RiGHT ANGLE TO 3 mm_ ASBESTOS LINING THE SLOT RIVETED TO METAL All dimensions in millimetres. Fig, 3) SHIELD 3.2 Procedure 3.21 Preparation of the Sample -— Distil a known volume of the thoroughly mixed sample from the distillation flask with the condenser, until water ceases to come over. Separate the water from the oil and return the oil to the distillation residue when the residue has cooled to 40°C. This proce- dure shall be adopted only if the water content of the material, as determi- ned according to 15: 1211-1978 is in excess of 0-5 percent. ‘Methods for testing tar and bituminous materials: Determination of water content { Dean and Stark method ) {frst revision ). 10618 5 1213 - 1978 rmaes —l Fro, + Crow Receivers 100 ml, 50 ml anp 25 ml 3.2.1.1 Thoroughly stir and agitate the sample if necessary to ensure a complete mixture. G22 Assembly of Apparatus 3.2.2.1 Support the flask on a tripod or ring over two sheets of IS 20 mesh wire gauze, 150 mm square (see Fig. 2}, Connect to the condenser tube by a light cork joint. Insert the thermometer through a cork in the neck of the flask with the bottom of the bulb € mm from the bottom of the flask, the axis of the bulb of the flask through the centre of the neck being vertical and the therraumeter aligned os this axis. 3.2.2.2 The distance from the neck of the flask to the outlet end of the adapter shall be not more than 700 mm and not Irss than 600 mm. The burner should be protected from draughts by a suitable shield or chimney ( see Fig. 3). 3.2.2.3 Adjust the adapter over the end of the condenser tube so as to conduct the distillate into the receiver. During the distillation, cover close- ly the top of the receiver with a piece of blotting paper or its equivalent, 107IS: 1213 - 1978 which shall be cut so as to fit the adapter tightly. The adapter shall extend into the receiver 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, asremble the apparatus and heat so that the first drop comes over in 5 to 15 minutes. Adjust the rate of distillation between 50 ta 70 drops per minute except that near the ond of the distillation the heat input shall nat be so rapid as to result in a temperature 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 as soon as possible. If escess foaming persists, the distillation may be more easily controlicd by applying the fame 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 ail 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 receiver any oil which may remain in the condenser tube. Measure by volume the residue and keep it for further tests. 3.24 Procedure for Handting Residue 3.2.4.1, When the temperature reaches 360°C, extinguish the dame and immediately (within 30 seconds) pour the residue into the residue container, placing this an its lid to prevent too rapid cooling at the bottom. 3.2.4.2 Allow the residue to cool in a position free frum draughts to a tempcraiure that is below its fuming point and at the same time suitable for pouring. 3.2.4.3 Stir the residue and pour into the receptacles specified for testing for properties, such as penetration and softening point. 3.3 Report 3.5.4 Asphallic Residue — Calculate the percent residue to the nearest 0-1 as follows: R-=[(200— TD) {200} x 100 where A = residue content, in volume percent; and. TD = total distillate recovered to 360°C, in ml, 3.3.1.4 Report as the residue from distillation to 360°C, percent volume by difference. 10819 ; 1213-1978 3.3.2 Total Distillate — Calculate the percent total distillate to the nearest 0:1 as follows: TD percent = ( TD/200) x 109 3.3.2.1 Report as the total distillate to 360°C, volume percent. 3.3.3 Distitlate Fractions 3.3.3.8 Determine the percentage by volume of the original sample by dividing the observed volume (in millilitres) of the fraction by 2. Report to the nearest 0°l as volume percent as follows: Up to 190°C Up to 225°C, Up to 260°C Up to 316°C 3.3.3.2 Determine the percentages by volume of total distillate by dividing the observed volume in millilitres of the fraction by the millilitres recovered to 360°C and multiply by 100. Report to the nearest 0'1 as the distillate, volume percent of total distillate to 360°C as follows: Up to 190°C Up to 225°C Up to 260°C Up to 316°C: 3.3.4 Where penetration, viscosity, or other tests have been carticd out, report with reference to this method as well as to any other method used. (@xample ‘Penetration according IS: 1203-1978" of residue as in IS: 1213-1978"). 3.3.5 If the first fraction obtained contains water, note the volume of water. Deduct this from the volume of oil taken and correct all the fractions to a percentage based on the volums of the water-frce sample 3.3.6 A convenient methed for determining the volume of water i3 to transfer this fraction, after noting the volume, to a tube or cylinder graduated in 0-1 ml and te add about 15 to 20 ml of benzol, ‘This almost alw cys causes a clear scparation between the oil and water. 3.3.7 Barometric pressure correction as stipulated under B shall be applied where necessary. 3.4 Precision — Duplicate results shall not differ by more than the followings Repeatability Reproda ibilily 2 mi distillate 4 ml distillate Methods for testing tar and bituminous materials: Determination of penctration (fast revision ). 10918: 1213 - 1978 3.5 Precaution — During the progress of distillation, the thermometer shall remain in ita original position. -No correction shall bo made for the comergent stem of the thermometer, 4, METHOD RB (FOR ROAD TAR) 4.1 Apparatus 4.1.1 Distillation Flask — A flask with dimensions and tolerances as given below shall be used: Distillation capacity, ml 750 Capacity of bulb, ml 975 + 20 Internal diameter of neck between side 2841 taper and bulb, mm Internal diameter of side tube, mim B5 409 External diameter of side tube, mm 110 +05 Length of side tube, mm 160 +5 Radius of curvature at the base 12 of the neck, mm Thickness of walls of bulb neck 10 to 15 of side tube, mm 4.1.1.1 The distance from the centre of the side tube of cach flask at the junction of the neck to the top of the neck shall be 75 + 3 mm. The distance from the centre of the side tube of each flask at the junction with the neck to the liquid surface, when the flask is vertical and contains a quantity of Liquid equal in volume to the distillation capacity of the flask, shall be 90 + 3 mm. 4.1.2 Thermometer —aame as for Method A { see 3.1.2). 4.1.3 Air Condenser — made from a straight tube of good quality resistance 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: Internal diameter 204 1mm Overall length 600 + 10 mm Wall thickness 1:0 to 1-5 mm 4.1.3.1 ‘The side arm of the flask shall extend at least 25 mm beyond the cork in the upper ond of the condenser. 1101S: 1213 - 1978 41,4 Draught Screen — rectangular, made of 0'711 mm Standard Wire Gauge sheet metal, with the dimensions shown in Fig. 5 and open at top and bottom and complying with the following requirements: in cach of the two narrow sides of the draught screen there shall be two circular holes, 25 mm in diameter each, and situated as illustrated in Fig. 5. In each of the four sides of the draught acrocr there shall be three holes with their centrcs 25 mm above the basc of the draught scrccu. Those holes shall occupy the posi- tions as shown 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. At the middle of cach of the wider sides a vertical slot with the dimensions as shown in Fig. 5 shali be cut downwards from the top of the-screen. A sheet of hard asbestos of silica board, G mm in thickness and having a central circular hole 110 mm in diameter, shall be supported horizontally in the screen and shail fit closely to the sides of the sereen to ensure that hot gases from the source of heat do not come in contact with the sides of neck of the flask, The flask shall be placed in position and pressed down so as to close completely the le in the board. “The supports for this board anay conveniently consist of triangular picces of mctal sheet firmly fixcd to the screen at its four corners. In one of the narrow side of the screen a door shall be provided, laving the dimensions and position as shown in Fig. 5. In cach of the narrow sides of the screen a mica window shall be placed centrally, with bottom of the window level with the top of the asbestos shelf ‘The dimensions and position of the windows shall be as shown in Fig. 5. 4.1.5 Crow Receivers — same as specified in Method A ( see 3.1.6 ). 4.2 Procedure A420 Preparation of the Sample — sarc as spccificd in Mcthod A (see 3.2.1). 4.2.2 Assembly of Apparatus — Set up the distillation flask complete with thermometer, air condenser and receiver. The thermometer shall be so fitted in the flask that the bottom of the capillary is level with the lower edge of the side tube joint and the immersion mark is level with the top of the cork. 4.2.3 Distillation 4.2.3.1 Weigh 750°0 + 0-4 g of the material into the weighed distill~ ation flask, and astemble the apparatus, using the 25-ml receiver to collect the first fraction, Placc this and the subsequent receivers so that the1S: 1213 - 1978 pen BRS mes — fe-— 208mm2§ — c-rmm, ~ |_——MICA WINDOW iy seers 3OARD A 1508 50 ASAELTOS mints t | ~ wa ann] 4 se dae | | xp Seg [| fof i. S 2omm DIA ‘ ‘eam DIA Fic. 5 Dravcut Screen condensate will flow down the sides. Apply heat at such a rate that the thermometer indicates 200°C within 35 + 5 min from the start, 4.2.3.2 When examining tars which are liable to froth on heating, it may be found that the temperature cannot be brought satisfactorily to 200°C within the maximum specificd period of 35 -- 5 minutes. Only in the testing of such tars which froth excessively may the preliminary period of heating be oxtended and then only just sufficiently for the purpose. Insuch an event, record the time taken to reach 200°C. 4.2.3.3 As soon as oil commences to distil, adjust the flame so that 5 ml of distillate collect in not less than 54 but not morc than 66 seconds. Maintain this distillation rate, which corresponds to 5:0 + 0:5 ml/min throughout the remainder of the distillation except that the collee- tion of the first 5 ml in any receiver may extend over 75 5 asthe upper limit, and ifthe collection of any > ml extends over less than 94 or more than’ 66s, the collection of 18 ml, including that 5 ml portion, shall extend over at least 165 but not more than 195 seconds. 4.2.3.4 Ifin any test, the conditions specified in 4.2.3.3 are not met, the test shall be discarded and another test carried out with a further portion of the material. Hz18; 1213 - 1978 42.3.5 The specified distillation rate corresponds approximately to 90 drops/min or 3 drops in each 2 #, but this should be taken only asa ide. Graduated reecivers should be used for the collection of the distil- fate so that the time taken to collect cach 5 ml may be kept under close observation. 4.2.3.6 Make a record of these 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 warmed immediately before use, so that naphthalene is prevented from solidifying on its inner wall and thus interfering with the checking of the distillation rate 4.2.3.8 Take the other fractions at 270°C and 300°C or at such other temperatures as may he specified, in the 100-ml receivers, the receivers being changed without interrupting the distillation. 4.2.3.9 Extinguish the Bunsen flame immediately the highest specified temperature is reached. Include, in the final fraction, oil which drains from the condenser within five minutes after the flame is extinguished. 4.2.3.10 Should solids tend to deposit during distillation, warm the condenser so that such solids are collected in the fraction with which they come over. 4,2,3.11 Ascer:ain the weight of the distillate to 200°C in g, note the volume of the watcr and, assuming a density of 1-00 g/ml, record the weight of water in grams. Find the weight of the light oil in the fraction up to 200°C by difference. Determine the weights of other fractions in the same manner. 4,2,3,12 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 determi- nation of phenols { see IS : 1218-1978" ). 4.2.313 Keep the flask with the cork and the thermometer in position for one hour after the flame has been extinguisted. Then weigh *he flask and residue, after which mix the contents of the flask thoroughly by shaking. Pour out half. Again shai the remainder and determine softening point by the method illustrated in TS: 1205-1978¢. 4.3 Report — Carry out the distillation test and report the separate results and the average as percentage by weight on the sample, Report the time in seconds for each 5 ml of distillate. pe Methods for testing tar and bituminous materials: Determination of phenols (first revision ). cates testing tar and bituminous materials: Determination of softening point ist revision ). 1131811213 ~ 1978 4.3.1 Barometric pressure correction as stipulated under 8 shall be applied where necessary. 44 Precision—The mean of two results conducted by the same laboratory should not differ from the mean of the two results in 2nd laboratory by more than the following: a) 200-270°C: 1:0 percent m/m b) 270-300°C 1-0 percent m/m ¢) Sum of (a) and (b) 1-5 percent mim ) Softening point of the 2c residue f &B) 4, METHOD C (FOR CRUDE COAL TAR) 3.1 Apparatus SAL Distillation Flask —~ same as specified in Method B ( see 4.1.1). 5.1.2 Thermometer same as specified in Method A {see 9.2.2). 5.1.3 Air Condenser — same as specified in Method B ( see 4.1.3). 5.1.4 Metal Heating Bath (See Fig. 6) ~The bath shall contain fusible alloy meiting below 70°C in such quantity that when the bottom of the flask is 5 nm from the bottum of the bath, the level of the molten metal is about 15 mm below the rim of the bath, A, As Three or Four Ping or Similar Device to Retain Flange Central, if Flange and Bowl are not in One Piece. All dimensions in millimetres. Dimensions in minima. Fic. 6 Metat Heatixe Bare $1.5 Crow Receivers —~ same as specified in Method A ( see 3.1.6). 1141832213 - 1978 5.2 Procedure 5.2.1 Preparation of Sample — same as specified in Method A (see 3.2.1). 5.2.2 Assembly of Apparaius —Set up the distillation flask as in Method B ( see 4.2.2). 5.2.2.1 Srnoke the bottom of the flask over a luminous flame. Heat the fusible metal to a temperature slightly higher than its melting point and immerse the flask centrally in the bath, the bottom of the flask being at least 5 mm abave the bottom of the hath. 5.2.3. Distillation —Take 250 ml of the material and carry out the distillation steadily at the rate of 5 ml/min and, without interrupting the distillation, collcct oil fractions separatcly in the graduated receiver as follows: a) Up to-210°C b) 210 to 230°C c) 230 to 270°C d) 270 to 300°C e) 300°C to the stage of pitch 5.2.3.1 Should solids tend to deposit during che distillation, warm the condenser ¢o that such solids are collected in the fraction with which they come over. 5.3 Report 5.3.1 Record the final temperature of distillation reached in the test. 5.3.2 Note and report the volume and appearance of each fraction. Determine and report the specific gravity of cach fraction at 27°C, Nucleate fractions (a) to (d) with a sinall crystal of naphthalene and fraction (c) with a small crystal of anthracene and cool the fractions to 155 + 05°C. Keep at this temperature, with occasional stirring, till solids separate out or for 4 hours, whichever is less, and report the result of this observation and the percentage of oil draining out ef cach fraction in which solids make an appearance. 5.3.3 Barometric pressure correction as stipulated under 7 shall be applicd where necessary. 6. METHOD D ( FOR CREOSOTE AND ANTHRACENE OIL ) 6.1 Apparatus 6.A.1 Distillation Flask — A flask with dimensions and tolerances as given below shall be used: Distillation capacity 150 mt Capacity of bulb 195 4 7 ml BS$81 1213 - 1978 Internal diameter of neck 18 + Imm between side, taper and bulb Internal diameter of side tube 50405 mm External diameter of side tube 70 + 05 mm Length of side tube 120 + 4mm Radius of curvature at the base of 10mm neck ‘Thickness of walls of bulb, neck, 0°8 to 1-2 mm side tube 6.1.2 Thermometer — same as specified in Method A ( ser 3.1.2 ). 6.1.3. Air Condenser — same aa specified in Method B ( see 4.1.3). 6.1.4 Drought Screen — same as specified in Method B ( ses 4.1.4). 6.1.5 Receivers — same as specified in Method A ( see 3.1.6). 6.2 Procedure 6.2.1 Preparation of Sample — same as specified in Mcthod A ( see 3.2.1). 6.2.2 Assembly of Apparatus — same as specified in Method B ( see 4.2.2). 6.2.3 Distillation 6.2.3.1 Thoroughly mix the sample as prepared under 6.2.1 in a 250-ml flask. Weigh 100 + 0-5 g of the mixture directly into the weighed distillation flask and start the distillation, using the naked flame of the burner. Continue the distillation at the rate of SO + 0-5 ml per minute. If tor any reason the distillation rate falls outside the specified kmits at any time after the first 5 ml of distillate have collected and before the final specified temperature is reached, discard the test and start another test on a further portion of the material, 6.2.3.2 The specified distillation rate corresponds approximately to 90 drops per minute or three drops in each two seconds, but this should only be taken asa guide. Graduated receivers should preferably be used for the collection of the distillate in order that the rate in millilitres per minute may be kept under close obscrvation, 6.2.9.9 Change the .cceive: at cach specified vemperature (sce 6.3) without stopping the distillation, Extinguish the flame when the thermo- meter reaches the highest specified temperature, and include in the final fraction the oil which drains from the condenser within five minutcs after the fame has beau extinguished, Should solids tend to deposit during the distillation, warm the condenser so that such solids are collected in the fraction with which they come over. 6.2.3.4 During the progress of distillation, the thermomecer shall remain in its original position. No correction shall be made for the emergent stem of the Uiermometer, 1161831213 - 1978 6.3 Report 6.3.1 Report the cumulative weights of fractions obtained at the follow- ing ranges of temperatures: 0 to 210°C 0 to 235°C 0 to 315°C: © to 355°C 6.3.2 Also, report the weight of the residue 6.3.3 If the first fraction contains water, determine the amount of water. Deduct this amount from the weight of oil taken for the test, and report all the Gractions @s percentage by weight bascd on the weight of the water-frce material. 6.3.4 A convenient method for determining the amount of water is to transfer this fraction, after weighing, to a tube of cylinder graduated in O'1 ml and to add 13 to 20 ml of benzol. This almost always causes a clear separation between the oil and water, and assuming a density of 1-00 g/ml, the weight of water can be calculated. 6.3.5 Barometric pressure correction as stipulated. under 8 shall be applied where necessary. 7. PRECISION 7.1 The duplicate results shall not differ by more than the following: Repeatability Reproducibility Up to 230°C 16g d5g Up to 230 to 315°C bsg 349 Total distillate 7g 17g 8, BAROMETRIC PRESSURE CORRECTION 8.1 Ifthe barometric pressure during the period of test remains within the range of 760 + 5 mm, no correction need be applied to the specified distil- lation temperatures. If the pressure is beyond that range, apply the follow- ing correction to the specified temperatures: Correction for temperature in degrees centigrade = 0-000 12 ( 760 — P) (44 273) where = corrected barometric pressure during test, and = specified temperature in degrees centigrade, WN?As in the Original Standard, this Page is Intentionally Left BlankIS: 1214 - 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF MATTER INSOLUBLE IN BENZENE ( First Revision ) 1. SCOPE 1.1 This standard covers the method for the determination of matter insoluble in benzene for creosote and anthracene oil. 2, APPARATUS 2.1 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 or its equivalent. 2.3.1 Filtering Funnel and Bottle 3. REAGENT 3.1 Benzene — ordinary, conforming to IS : 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 cither: a) the sintered glass crucible, or b) the filter papers. 4.1.1 Method Using Siniered Glass Crucible -—Dry the crucible at a temperature of 100 + 2°C and weigh accurately when cool. Decant the solution through the dried and weighed crucible. *Specification for benzene ( revised ). 11g1S3 1214-1978 Transfer any insoluble residue to the crucible by means of additional benzene, and wash the filter paper with benzene until a few drops of the filerate yield no residue on evaporation. Dry the crucible at a temper- ature of 100 + 2°C until it is of constant mass; allow it to cool in a desiccator, and weigh correct to 0] mg. 4.1.2 Method Using Filter Paper— Counterpoised double filter papers shall be used. Tor counterpoising, heat the two filter papers to a temperature of 100 + 2°C and reduce them to equal weight by removing the apex of the heavier filter paper after folding. For filtering, use the uncut paper inside the originally heavier Paper so that the separated material is retained by the inner paper, yct both of them are equally subjected to any action exerted by the oil and benzene. Dry the filter papers at a temperature of 100 4 2°C until they are of constant weight, allow them to caol in a desiccator and weigh correct to 0'1 mg. 5, CALCULATION 5.1 Calculate 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 6.1 Report the percentage insoluble in benzene to the nearest 0-1 percent. 7, PRECISION 7.1 The duplicate results should not differ by more than the following: Repeatability Reproducibility 10 percent 22 percent 8, PRECAUTION 8.1 The solvent benzene is extremely inflammable. Handling of benzene shall be carried out away from any source of heat or flames, 1201S1 1215 - 1976 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 insoluble in toluene for road tar and pitch. 2, METHOD A (FOR SOFT GRADE PITCH ) 2.1 Apparatus 2.1. Beaker — of 200-ml capacity. 2.1.2 Sintered Glass Cracible —~ of porosity No. 4. 24.3 Filter Papers—-two, each about 150 mm in diameter, grade n, No. 5 or its equivalenc. 2ASA Filtering funnel and bottle 2.1.4 Water Baih— maintained to constant temperature of 95 + 5°C. Glycerine may be used in place of water for temperature 95°C and above. 2.1.5 A 100-m! Graduated Cylinder 2.2 Reagent 2.2.1 Toluene — nitration grade, conforming to IS ; 537-1967". 2.3 Procedure 2.3.1 Warm in a 200-mnl beaker about 2g of the thoroughly mixed material, accurately weighed, on a_water bath, and intimately mix with 100 ml of hot toluene at 95 — S°C. After settling for 20 minutes with the beaker standing on the water bath, docant the supernatant liquid cautiously, avoiding disturbance of the sediment, through cither (a) the filter papers, or (b) the sintercd glass crucible. Specification for toluene, pure, nitration grade {first revision). 42){82 1215-1978 2.3.1.1 Method using filter papers— Counterpoised double filter papers shall be used. Tor counterpoising, heat the two filter papers to a tempc- rature of 100 + 2°C and reduce them to equal weight by removing the apex of the heavier paper after folding, For filtering, usc the uncut paper inside the originally heavier paper, so that scparated material is retained by the-‘inner paper, yet both of them are equally subjected to any action exerted by toluene. Wash the residue by repeated decantation with toluene heated to 95 ~++ 5°C until 300 ml of toluene have been used in all. Transfer the residue to the filter paper and continue the washing until altogether 500 ml of hot toluene have been used. Dry the residue in an oven at a temperature of 100 + 2°C until it is of constant weight. 2.3.1.2 Method using sintered glass cructble— Dry the crucible at a temperature of 100 -. 2°C and weigh accurately when cool. Decant the toluene solution through the crucible using gentle suction to assist filtra~ tion and avoiding the transfer of the sediment. Wash repeatedly by decantation 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 used. Dry the residue in an oven at a tempera- ture of 100 + 2°C until it is of constant weight. 2.3.2 Preserve the residue in either case with the filter paper or sintered crucible for ash determination ( see IS : 1217-1978" ). 2.4 Galculation — Calculate and express the result as percentage by mars of the matcrial taken for the test as follows: Insoluble matter in toluene, 100 W, percert by mass =—7 $ a wherc 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 3.1.1 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 2.3.1. 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 *Mcthods for testing tar and bituminous materials: Determination of mineral matter (ash ) (first revision ), 122181 1215 - 1978 100 ml, of toluene at 95 4. 5°C! in exactly the same manner as described in 2.3.1 except that each settling period during which the beaker is standing in the water bath need only be of five minutes. 3.1.3 Transfer the residue to the filter paper or sintered glass crucible and continue the washing until a further 500 ml 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. 3.1.4 Preserve the residue with the filter paper for ash determination (see IS : 1217-1978). 3:2 Calculation — Calculate and express the result as percentage by mass of the material taken for the test as follows: Insoluble matter in toluene, Wy percent by mass “WL x 100g ‘2 where W, = dry mass of the material, and W, = mass of insoluble matter. 4, REPORT 4,1 Report the percentage insoluble in toluene to the nearest 0°1 percent. 5, PRECISION 5.1 The duplicate test results should not differ by more than the following: Repeatability Reproducibility O'S percent 10 percent 6. PRECAUTION 6.1 The solvent toluene is extremely inflammable. Handling of toluene shalt be carried out away from any source of heat or lames. Methods for testing tar and bituminous materials; Determination of mincral maticr (asia) (first eavision ). 123As in the Original Standard, this Page is Intentionally Left Blank1811216 - 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF SOLUBILITY IN CARBON DISULPHIDE OR TRICHLOROETHYLENE ( First Revision ) 1. SCOPE 1.1 This standard covers the methods for the determination of solubility in carbon -disulphide or trichloroethylene for asphaltic bitumens and native asphalts. 2. METHOD A (FOR ASPHALTIC BITUMEN ) 2.1 Apparatus 2.1.1 Goock Crucible 2.1.2 Conical Glass Flask — of 200-ml capacity. 2.2 Solvent 2.2.4 Carbon Disulphide— redistilled grade, conforming to IS : 717-1969". 2.2.2 Tricklowetiplene — conforming tu TS : 245-1970t. 2.3 Preparation of the Material — If th> material contains water, heat it to a temperature not exceeding 130°C unti] the water has been removed, stirring constantly, when possible, during heating. Perform this operation as expeditiously as possible. 2.4 Preparation of Gooch Grucible — [nsert the filter tube in the stopper of the filtering flask, set the Gooch crucible in the filter tube, and connect the flask to the suction pump. Fill the erucible with some of the suspen. sion of asbestos i the water, allow it to settle partly in the crucible and Specification for carbon disnlphide, technical (firtf revisien } Specification for trichloroethylene, technical ( secend revision ). 125,IS: 1216 -1978 apply a light suction to draw off the water, leaving a firm mat of asbestos in the crucible. Add more suspended asbestos and repeat the process until a mat weighing 0°5 + 0-1 g is built up after drying. Wash the asbestos mat_thoroughly with water and dry in the oven at a temperature of 150°C, Cool the crucible in the desiccator, weigh and replace it in the dry filter tube supported in the clean, dry filtering flask. 2.4.4 Inthe determination, the asbestos apparently absorbs, irreversibly a small amount of soluble bitumen (usually 1 to 5 mg/g of asbestos ) which is sot removed by a subsequent washing with solvent. The weight of ashestag used, therefore, shall be kept within the specified limits to ensure reproducible results. 2.5 Procedure — Weigh about 2 g of the dry material correct to the nearest 0-001 g into a 200-ml conical flask and add 100 ml of carbon divulphide or trichloroethylene. Stir the contents of the flask, and then allow it to stand, looscly corked, for a period of one hour. Filter the contents of the flask through the Gooch crucible prepared as described under 2.4 which has been weighed to the nearest 0-001 g. Moisten the asbestos pad with carbon disulphide before commencing filtration, and filter at a rate of not more than two drops per second at first, ‘The filtrate shall be quite clear. Transfer the insoluble matter remaining in the flask te the crucible by washing out the flask with a stecam of carbon disulphide or trichloroethylene from a wash bottle. Wash the material retained in the crucible with successive small amounts of carbon disulphide or trichlorocthylene until a filtrate is obtained which is not discoloured. Allow the crucible to dry in air for 30 minutes, after which place it in an aven at 100 to 110°C for ong hour. Allow the crucible to cool in a desiccator and then weigh. 2.6 Calculation and Report — Calculate the matter soluble in carbon disulphide or crichloroethylene as follows: Matter soluble in carbon disulphide or trichloroethylene, percent = ME) 100 1 where WW, = 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 tichlorecthylcuc of the dry material. 12618 : 1216 - 1978 2.7 Precision — Test results shall not differ from the mean by more than the following: Matter Soluble in Carboa Repeatability Reproducibility Disulphide or Trichtoroethslene Below 98 percent oS 10 98 to 100 percent O-1 02 3. METHOD 8 (FOR NATIVE ASPHALTS) 3.1 Apparatus 3.1.1 Glass Tap Funnel — approximately 100 mm in diameter, the stem fitted with o tap and the top ground flat 3.1.2 Glass Plate — te coves the funnel, about 120 min in diameter, with a hole of about 16 mm diameter in the centre. 3.1.3 Glass Funnei — smaller than that described under 3.1.1, with its stem passing through a cork placed in the hole in the glass plate, the Jower end of the stem reaching approximately half-way down the tap funnel. 3.1.4 Filter Papers— two, Whatman No..5 or equivalent filter papers, 185 mm in diameter, dried in a suitable oven, cooled in a desiccator, counterpoised and folded together as shown in Fig. 1. [Po PAPER CLD ke Fic. 1 Forpep Firtar Parrr 3.2 Solvent and Materia] 3.2.1 Carbon Disulphide — redistilled, conforming to IS : 717-1969*. 3.2.2 Cement — suitable for sealing the glass plate to the funnel. It umay be prepared with 10 g of gelatin, 80 ml of water and 20 g of glycerine. ~~ sSpeciticas ‘ation for carbon disulphide, technical ( firs? revisfon ). 127IS: 1216 - 1976 3.3 Preparation of Sample — If the sample contaias water, heat a 100g portion at a temperature not exceeding 130°C, the material being cons- tantly stirred when possible, until the rate of loss in weight of the sample foes not exceed U'l g during 2 15-minute period of heating. 3.3, Ifthe loss in weight on drying exceeds "1 percent, determine the water content of another sample of the material in a¢cordance with IS: 1211-1978". 3.4 Procedure — Dry the two filter papers (see 3.1.4) in an oven at 100 to 110°C, enol in a desiceator, counterpnise, 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 secure the cover to the funnel by means of the cement. Now add carbon disulphide or trichloroethylene 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 glass on the small funnel to minimige evaporation. Close the tap and introduce a further quantity of carbon disulphide or trichlorocthylene through the small funnel and again draw the solution off after 30 minutes. Repeat this procedure until the solvent drawn off is no longer discoloured. When the filtration is completed, remove the cover and allow the filter papers to dry in air for 30 minutes before placing them in a ventilated air 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 Caleulation — Calculate the solubility of the dry material as follows: Matter soluble in carborr disulphide or trichioroethylene, W, WW, 100 i =(o = = percent by weight { Wi x 100) x Jor TW, where 1, = mass in g of the dry sample taken for the test; W, = mass in g of recovered insoluble matter; and WW’, = water content of sample, determined. 3.6 Report — Report the result obtained in 3.5 to the nearest 0-05 percent as the matter soluble in carbon disulphide or trichlorocthylene, 3.7 Precision — Test results shall not differ from the mean by more than the following: Repeatability 05 Reproducibility 05 * Methods for testing tar anv bituminous materials: Detecmination of water content (Dean and Stark method } (first revision ). 1281S L216 - 1978 3.7.1 These precision figures do not include any allowance for differences due to variations in samples. 4. PRECAUTIONS 4.1 The handiing of carbon disulphide shall be carried out away from flames or other sources of heat as the solvent is extremely inflammable and the vapour is liable to ignite spontancously on contact with a hot surface. 4,2 The vapours of carbon disulphide are toxic and adequate ventilation shall be provided, 129As in the Original Standard, this Page is Intentionally Left Blank1S: 1217 - 1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF MINERAL MATTER ( ASH ) t First Revision } L, SCOPE LI This standard covers the method for determination of mineral matter (ash ) for crude coal tar, pitch and other bituminous products. 2, APPARATUS 2.1 A porcelain or silica crucible of 30 ml capacity. 3. PROCEDURE 3.1 Thoroughly clean and dry the crucible in an oven. Cool and weigh (a). Transfer about 2 g of the thoroughly mixed separated tar into the crucible and weigh (6). Heat the crucible gently on a hot plate gradually increasing the hpat to rcmave volatile matter without loss of cunteut due to violent cbullition, Finally, heat the crucible in a mule furnace at a temperature high enough to complete the incineration. Goal ta 100°C: and place it in a desiccator and weigh, Repeat cooling and weighing till a constant weight is recorded (¢). 4. CALCULATION 41 Calculate the porcentuge of ash content on the weight of the tar taken on moisture-free basis us follows: Percentage of ash content = -; x 100 where a = mass of crucible in g, b= mass of crucible aud moisture free sample in g, and ¢ == mass of cricible: and ash in g. 131As in the Original Standard, this Page is Intentionally Left BlankAMENDMENT NO. 1 JULY 1991 tO IS 1217 : 1978 METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS : DETERMINATION OF MINERAL MATTER ( ASH ) { First Revision ) { Page 131, clause 2.1, line 1) — Delete the words ‘porcelain or’. ( Page 131, clause 3,1 ) — Insert the following matter at the end: “Take 10g of powdered sample (passing through 600 micron IS sieve ) and treat with about 100 ml of toluene at 65 to 70°C for 15 minutes. Filter through filter paper No. 40 (ashless). Wash the residue with hot toluene (65 to 70°C ) till filtrate becomes of straw colour. Dry the residue and finally ignite in a muffle furnace at 900+ 10°C for coal tar products or at 700+ 10°C for petroleum products till constant mass is obtained.” (PONG 6) ned at Sifico Femting Press, Delhi. indiaIS: 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 sliall be extracted by a solution of sodium hydroxide and the extract shall be boiled to remove neutral oils and bases. The phenols shall then be liberated by the addition of hydrochloric acid conforming to analytical reagent grade of IS: 265-1962* and their volume shall be measured. 3. APPARATUS 3.1 Phenols Flask — of glass, conical, with ¢ lomg graduated neck and of the shape, dimensions and tolurances as shywn in Vig. | and as given below Capacity 200 + 10 mt Maximum permissiite error on capacity A: OF ml corresponding to any graduation mark Maximum permissible differen @ hetween & Olanal the errors at any two graduation marks 3.2 A Beaker of Suitable Size 3.3 Separating Funnel Stoppered 3.4 Any Suicahle Thermometer — covering a range of 40 t 70°C. *Speesheation for hydrochlorie seid ( rertved J. 133181 1218-1978 c} At least 25mm Min. 123mm Not to exceed Max. 150mm 19cm 4, REAGENTS 4.1 Sodium Hydroxide Solution— 10 percent m/m clear aqueous solution. 4.2 Hydrochloric Acid Concentrated — conforming to analytical reagent grade of IS : 265-1962*. ‘Specification for hydrochloric acid ( revised ). 1341S : 1218 «1978 4.3 Sedium Chloride — dry powdered. 4.4 Methyl Orange Indicator — 011 g of methyl orange dissolved in 100 ml of watm distilled water. 5, PROCEDURE 5.1 Warm, if necessary, the oil distilling to 270°C in tlc distillation test see Method 8 of IS; 1213-1978*), until completely liquid, and transfer the whole of the oil to a stoppered separating funnel of appropriate capacity. Rime the receivers from which the distillates were transferred with an equal volume of a clear aqueous 10 percent (by mass} solution of sodium hydroxide, previously heated to between 40°C and 70°C, and add to the oil in the separating funnel. Agitate the contents of the funnel vigorously for five minntes, and then allow it to stand. 5.2 Alter it bas settled, run the alkaline layer into a beaker. Agitate the upper layer for five minutes with a further quantity of hot sodium hydro- xide solution, equat to one quarter of the volume of the distillate which is beg washed, and with further successive quantities of the hot sodium hydvovide solution, cach equal in volumerto the last, until all the phenols have been removed, During the washing proceds, keep the con- tents of the funnel in a liquid condition, immersing the funnel, if necessary in warm water at 40 to 70°C. 5.2.1 The complete removal of phenols can be ascertained by slightly acidifying the last washing with concentrated hydrochloric acid conforming ty analytical reagent grade of IS; 265 - 1962+ and examining for separated phenuls. A Jarge excess of sodium hydroxide shall be avoided, but some excess should be maintained. As a rough guide, 25 ml of sodium hydroxide solution of the strength indicated may be taken as sufficient to remove about 5 ml of phenols. 5.2.2 Reservathe tar distillate after removal of phenols for the determina- tion of naphthalene ( see TS: 1219-1978f ). 5.3 Collect the alkali extracts, including any portion acidified, for the purpose of testing. Make sure that the combined washings arc alkaline. Boil vigorously for 20 minutes, using fragments of porous or other suitable inert material ta prevent bumping. Cool, and if the extract is clear, transfer direct to the phenols flask. 5.3.1 Tf it be expected that the tar contains 3} percent or more of phenols, the boiled washings (after filtration through glass wooly if * Methods for testing tar and bituminous materials : Distillation vest (first revision }, {Specification for hydrochtoric acid ( revased ). (pitetheds for testing tar and bituminous materials: Determination of naphthalene ist revision). 1351S: 1218 -1978 necessary} shall be divided about evenly betwcen two phenols flasks, the subsequent specified procedure being carried out on the contents of each flask and the volumes of phenols recovered being totalled 5.4 If the solution is not clear, filter it through glass wool, previously moistened with saturated aqucous sodium chloride solution; collect the filtrate in the phenols flask, wash the glass wool with 25 ml of saturated sodium chloride -solution and add to the filtered soda washings. Add methyl orange indicator solution, follawed by concentrated hydrochloric acid until after vigorous shaking together of the two layers, thc methyl orange just indicates distinct acidity. Duriag the addition of the hydro- chloric ‘acid, cool the contents of the flask 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 a= volume of phenol in mi, and & = volume of original sample of car taken in ml. 61,2 The phenols as 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 to be 1:04 g/ml, and calculate accordingly. 1363S: 1219-1978 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 determination of naphthalene in road tar. 12 This determination ia necessary only in respect of the naphthalene deposited ut 15°5°C from solution in the total distillate up to 270°C. 2, PROCESS 2.1 The distillation fraction of tar distilling up to 270°C left after the removal of phenols is cooled to 15-5 -L 0'5°C and the solid separated and weighed. 3. APPARATUS 3.1 Crystallizing-Point Apparatus — as doscribod under 5.1. 3.2 Buchner Funnel and Flask 3.3 Hand Serew Press 3.4 Thermometer 3.5 Blotting Paper 3.6 A Filter Pump 4, PROCEDURE AL Collect the distillate recovered up to 270°C according t» Method B of S$: 1213-1978*. This shall be washed free from phenols ( see IS: 1218- 1978+ }. Gool the residue to 15°5 + O-5°C and maintain it with occasional stirring within these limits of temperature for two hours. Naplithalene erystallizcs out. 4.2 Transter the couled matcrial to a cold Buchner funnel fitted with a rapid filter paper, and rapidly remove as much oil as possible using a filter * Methods for testing tar and bituminous materiala: Distillation test (first revision }. {Methods for testing tac and bitarinour materiale! Determination of phencl (frat revision ) 13718: 1219 - 1978 pump. Place the crude naphthalene: hetwean sheets of blotting paper and press in ahatd screw pres. Remove the oily margins of the cake, and again press separately. Conduct the operations, starting with the transfer to the Buchner {funnel to the preliminary pressing, with utmost rapidity. 4.3 Weigh the pressed naphthalene and calculate.the percentage by weight in the original tar. 4.4 Detormine the ‘core thalene by the method de: cd wet crystallizing-point’ of the pressed naph- rihed in 5. 5. CORRECTED WET CRYSTALLIZING-POINT 5.1 Apparatus — A crystallizing-point apparatus of the shape, dimen- sions and tolerances given in Vig. 1, consisting of the following. 5.1.1 Outer Glass Test Tube — which serves as an air jacket, shail be weighed with fea shots or similar loading material. It_is provided with a cork through which the inner tube, as described in 5.1.2, is held in Position, . 5.12 Tuner Glass Test Tube — approximately 25 mm in diameter, cload by means of a cork which carries a stirrer in the form of a loop of glass with a glass stem and a standard thermometer ( see SL ) placed centrally within the tube and the glass loop and the bottom of the bulb being about 10 mm from the bottom of the inner tube. The cork is so fixed that the immersion mark on the thermometer is level with the top of the cork. 5.1.3 Cooling Bath — a glass beaker of 1 000 ml capacity attd 150 mm in height with the of the liquid at least as high as the level of the sample in the inner tut: 5.1.4 Thermometer — with the following dimensions and characteristics! Range 65 to 90°C: Graduation at cach od Longer lincs at each 05°C and 10°C Fully figured at cavh 2c Immersion 100 mm Maximum overall length 400 mm Maximum length of main scale 215 mm Maximum bulb length 2mm Maximum distance from bottom of bulb to 25 mm tep of contraction chamber Limit of accuracy 005°C 5.2 Material for Test — While the difference between the crystallizing- point of dry naphthalene and of naphthalene containing a small amount of water is appreciable, the lowering of the crystallizing-point ceases when a mininnim of two percent of water is present. Therefore, if the samples 13818: 1219- 1978 THERMOMETER AS SPEED STRRER, 3703-56 IMMERSION MARK INNER GLASS TEST TUBE O00 mi BEAKER: rr 4 1c GLASS LOOP 16 6 OER ALL mw L LOADING MATERIAL t io { 150, OUTER GLASS TEST TUBE COOUNG BATH ~100 p | 5 percent tolerance on dimensions except where otherwise stated, All diameter dimensions are external. All dimensions in millimetees, 1 CGaystatutzinc-Pornr — AssemB.y OF APPARATUS 139IS: L209 - £978 should contain two percent or more of water, it shall be examined as received. If the sample should contain a smaller percentage of water, O° mi of water shall be placed in the inner tube of the crystallizing-point apparatus before the sample is introduced as described under 5.3. If the test iy carried out in the presence of two percent or more of water, the addition of 0-85°C to the observed crystallizing-point gives the crystallizing point of the material on the dry basis. 5.3 Procedure — Place about 40 g of the material for test in a loosely stoppered conical flask which has been warmed in a boiling water bath to 85°C, Mix the contents thoroughly and pour about 20g into the warmed inner tube of the erystallizing-point apparatus. Place the tabe in its jacket aud assemble the apparatus as shown in Fig. 1 with the bath 6 to 8°C below the expected crystallizing-point. Do not heat the water during the subscquent operations. Take the bath thermometer readings at intervals of half a minute, starting when the temperature has fallen ¢o 81°C. Stir the contents of the inner tube continuvusly. 5.4 Results $.4.1 The crystallizing-point corresponds to the first five consecutive readings during which the temperature remains constant within 0°05°C:. Supercooliag may occur, in which case the five readings may be ebsirved after the temperature rise. A temperature rise of 1°C shall bo regarded as the maximum allowuble. 3.4.2 Ifa coustant temperature within 005°C is not obtained over five readings, take six final readings commencing with the first of two succes- sive readings within 0-05°C, Plot the readiags on graph paper against time intervals, and draw a straight line to lic evenly between the first and second, and between the fifth and the sixth of the six points just mentioned. Produce the line backwards until it intersects the earher portion of the curve. 5.5 Report 5.5.1 Report the constant temperature within 05°C ( see 5.4.1) or the point of intersection as found in 5.4.2, as the crystallizing-puint, 5.5.2 Report as corrected wet crystallizing-point the value obtained after adding 0-85°C. to the observed crystallizing-point. 5.5.3 The corrected wet crystallizing-point shail be not lawer than 70°C. If it is found to be below 70°C, the indication is that the removal of the excessive oil as prescribed in 4.2 has not bean carried out aalisfuctorily anc the determination has to be repeated 6. PRECISION 6.4 The duplicate results shall not differ by more than che fullowing: Repeatability one Reproducibility oe 14019 ; 1220-1978 Indian Standard METHODS FOR TESTING TAR AND BITUMINOUS MATERIALS: DETERMINATION OF VOLATILE MATTER CONTENT ( First Revision ) 1, SCOPE 1.1 This standard covers the method for the determination of volatile matter content of coal tar pitch. 2. APPARATUS 241 Placioum Crucible — complying with the following requirements (see Fig. 1): Eaternal diameter at base 240 40-5 min External diameter at top 340 £ 0-25 mm External height 35-0 05 mm Volume to brim 27-0 4: 05 ml Weight 2204106 2.1.1 The crucible shall be provided with a closely fitting hd, grooved tu receive the rim of the crucible and having a central hole 2 mm in diameter, as shown in Fig. 1. 34-00mm mT 2mm 35-Omm 40:5 1$-34-0mm £05 Fie. 1) Pratinom Oxvorrs ann Liv 14]1S: 1220 - 1978 2.2. Meker Burner — having a diameter of 31 mm at the top, the flame diameter being 3U mm maximum. 23 Water Manometer —connsoted by means of a T-piece with the gar supply entcring the burner, 24 Three-Arm Crucible Support — with silica points (see Fig. 2). S BIA M5 ROD SCREWED M6 Imm 1D AND 4mm OD, BRONZE TUBES. TO BE BRAZEO INTO AING AND OLAMETRICALLY SLOTTED oo DA J Ea 2 Ola mg ROD SLICK PONT All dimensions in millimetres. Fis. 20 Tawes-Ana Cruciste Surrorr witt Sturca Porrs 2.5 Retort Stand and Clamp — to hold the three-arm crucible support (see Fig. 3), so arranged that when in position, the bottom of the crucible js 10 mm above the burner, the: crucible being completely enveloped by the flames. 14218 : 1220 - 1978 Fic. 3. -Assempty OF APPARATUS. 2.6 Standard Draught Sereen — consisting of a semi-cylindrical metal sheet, 300 mm in diameter and sufficiently high for the purpose. 3, REAGENT 3.1 Potassium Chromate — pure powdered potassium chromate, 4. PROCEDURE 41 Assemble the apparatus as illustrated in Fig. 3 with thasilica points holding the crucible as near the rim as practicable. Spread a sma!l 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 acrated. Slowly increase the gas pressure at the burner until incipient fusion of the 14318s 1220 - 1978 potassium chromate is apparent. The final manometer reading shall be nated as cotresponding to the gas pressure to be used in the test on the piteh. The lid of the crucible shall not be used during the trials. 4.2 Clean the crucible, dey and weigh without the lid. Weigh into the crucible 1 g of the finely divided sample and place in position as before with the lid. Religtit the burner and, if necessary, readjust the gas pressure until the manometer reading is the same as that noted in the pre- liminary trial, Place the burner in position under the crucible and, after three minutes, during which the manometer reading shall be kept constant, extinguish the flame. Cool the crucible and weigh without dhe lid, The loss in mass shall bi the volatile matter in the amount of sample taken for the test, Caleulate the percentage of volatile matter by mass in the total sample taken for the test. 4.3 If the method has been properly performed, any deposit on the tid at the end of the experiment will be due to decomposition of the volatile matter. If there be any evidence that molten pitch has spurted on to the Viel, the test shall be discarded and a fresh determination made. 5. PRECISION 3. Tie duplicate results shatl not differ by more than the following: Repeatability oS Reproducibility 38 14418 : 1201 - 1978 te IS : 1220 - 1978 APPENDIX A { Clause 0.8) APPARATUS SCHEDULES Apparatus Water bath: a) Constant temperature b) For temperatures between 35°C. and 100°C Hot place Stop watch or clock or any other timing device Analytical balance, sensitivencss up to Ol mg Oven, up to 180°C Specific gravity boctes: a) Ordinary, 6 mm dia neck, 50 ml capacity la) Wide mouthed, 25 mm dia hack, 50 ml capacity Container dish a} 35mm dup, 95 mm dia b) 45 mm deep, 70 mm dia ‘Transfer dish Standard needle Penetration apparatus Container dish, 45 mm deep, 70 mrt dia King and ball

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