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इंटरनेट मानक Disclosure to Promote the Right To Information Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public. “जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न’ 5 तरफ” Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru “The Right to Information, The Right to Live” “Step Out From the Old to the New” IS 10512 (2003): Method for Determination of Wax Content in Bitumen [PCD 6: Bitumen Tar and their Products] “!ान $ एक न’ भारत का +नम-ण” Satyanarayan Gangaram Pitroda ““IInnvveenntt aa NNeeww IInnddiiaa UUssiinngg KKnnoowwlleeddggee”” “!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै” Bhartṛhari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 10512:2003 Indian Standard METHOD FOR DETERMINATION OF WAX CONTENT IN BITUMEN—SPECIFICATION (First Revision) ICS 75.140 GBIS2003 BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002 J(/niimy 2003 Price Group 4 .,. ‘,,. Bitumen Tar and Their Products Sectional Committee, PCD6 FOREWORD This Indian Standard (First Revision) wasadopted bytheBureau ofIndian Standards, afterthe draft finalized by the Bitumen Tar and Their Products Sectional Committee hadbeenapproved bythe Petroleum, Coal and Related Products Division Council. This standard waspublished in 1983,which waslargely basedonUOP46-64. Sincethepresent method ishaving the following disadvantages theCommittee decidedtorevisethestandardtoalignthe samewith DIN 52015:1980 ‘Determination of paraffin wax content inbitumen’ inorder to over come the disadvantages: a) The method isnot specific to‘Paraffin waxcontent’ onlybutspecifiesthewaxcontent which includes wax and micro-crystalline wax, b) The method does not mention the purity of ‘fullers earth’, c) There isno mention of ‘Reproducibility’ inthe method, d) Fullers earth having the particle sizewithin the range 10-35p, isnot available indigenously, e) There isno mention about the availability of fullers earth, f) The sieves required to check theparticle size offullers earth arenot available indigenously, and g) The wax content value varies with the quality of fullers earth. The composition ofthe Committee responsible for formulation ofthis standard isgiven inAnnex A. Inreporting the results of atest or analysis made inaccordance with this standard, ifthe final value, observed or calculated, isto berounded off, itshallbedone inaccordance with IS2: 1960‘Rulesforrounding off numerical values (revised)’. -– 4!.. ,:-- 1S 10512:2003 Indian Standard METHOD FOR DETERMINATION OF WAX CONTENT IN BITUMEN—SPECIFICATION (First Revision) 1SCOPE 4.2 Steam Bath This standardprescribes amethod usedfordetermining 4.3 Heating Cabinet (Oven), fortemperature at least the paraffin wax content of bitumen. The method is 150”C. applicable to bitumens having paraffin wax with 4.4 Bunsen Burner melting point above 25”C. NOTE—Paraffhr waxes include only those hydrocarbons 4.5 Thermometers, having leastcount atleast0.5°C. crystal1izinginanether/ethanolmixtureattemperaturesdown 4.6 Distillation Flask, as shown inFig. 1,fitted with to–20”C,obtainedbyaspecifiedprocessandhavingamelting pointofabove25°C. cork stopper. 2REFERENCE 4.7 Sheet Metal Guard Ring, ofabout 18mm inside diameter and about 65mm outside diameter. The following standard contains provisions which through reference inthistext, constitutes provisions of 4.8 Cooling Bath, as shown inFig. 2. this standard. At the time of publication the edition 4.9 Test Tubes, as shown in Fig. 2, fitted with spout indicated was valid. All standards are subject to andbored cork stopper. revisions and parties to agreements based on this standard are encouraged to investigate the possibility 4.10 Funnel, asshown inFig. 2. of applying the most recent edition of the standard 4.11 Erlenmeyer Flask, 100mlcapacity, fitted with a indicated below: bored cork stopper (tobeused asdistillation receiver) IS No. Title (seeFig. 3). 334:2002 Glossary of terms relating to 4.12 Test Tube, fitted with ground socket and awash bitumen and tar (third revision) bottle head fitted with ground cone (see Fig. 4). 3 TERMINOLOGY 4.13 Filtering Flask, 500 ml capacity. Forthe purpose of this standard, the definitions given 4.14 Vacuum Pump in IS334 shall apply. 4.15 Evaporating Dish 4 APPARATUS NOTE— Theapparatusfordeterminingtheparatlh waxcontent isavailable with M/s Petrotest Instruments GmbH &Co KG, 4.1 Balance, readable and accurate to+ 0.5 mg. Ludwig-Erhard-Ring 13,D-15827,Dahlewitz. 16*10 30 Alldimensionsinmillimetres. FIG. 1 DISTILLATIONFLASK 1 . 7.- 1 IS 10512:2003 OPENING CONNECTOR FOR FILTER FIASK 2200 , OPENING FOR INSERTION OF WRBO N DIOXIDE \/-&.. 1 OPENING FOR INSERTION OF THERMOMETER / Alldimensionsinmillimetres. FIG.2 COOLINGBATH 2 -, *L,..-. 7- IS 10512:2003 GUARD RING ICE WATER r- ! FIG.3 SCHEMATICDIAGRAMOFDISTILLATIONARRANGEMENT TEST TUBE FlllED WITH TEST TUBE SPOUT AND FITTED WITH BORED CORK II WASH BOTTLE STOPPER :: ~’ n < * FILTRATION FIG.4 SCHEMATICDIAGRA MOFFILTRATIONARRANGEMENT 3 ..,,. IS 10512:2003 5 REAGENTS solid carbon dioxide to get sample temperature of –20 * 0.5”C. A low temperature bath may be used. 5.1 Anhydrous Diethyl Ether, referred to in this Transfer 20+ 1ml of anether/ethanol mixture (asthe standard asether. washing liquid), prepared in a 1:1 ratio, in the test tube fitted with the wash bottle head and cool it in 5.2 Ethanol, Absolute the cooling bath to–20 +0.5 “C. 5.3 Reagent Grade Acetone 6.4 Keepthesampletemperature –20 *0.5 ‘Cconstant 5.4 Petroleum spirit having the following untilfiltration iscomplete. Placetheround filter paper characteristics: inthe funnel standing inthe cooling bath and connect it to the filter flask. Quickly transfer the slurry of a) Density at 15“C,g/ml : 0.690-0.705 crystals produced at–20 + 0.5°C to the filter. Rinse b) Boiling range: thetesttubewiththecooled washing liquid. Re-adjust I) Initial boiling point, ‘C ,A4in : 65 the temperature ofthe washing liquid to–20 * 0.5 ‘C 2) Collected volume of distillate, : 90 anduseitagainforrinsingthecrystalslurry inthefilter. about upto 90 ‘C, percent by Distribute thewashing liquid asuniformly aspossible volume between thethree washing operations. 3) Drying point, ‘C, Mm : 95 6.5 Support the filtration by agentle suction process c) Aniline point, ‘C : 59t061 during which thevacuum pressure shallnot fall below 6 PROCEDURE 5kPa(50mbar). Assoonasnomorefiltrateisdropping through, disconnect the filter assembly with vacuum 6.1 Melt the bitumen sample, pour 25 + 1g into the pump, liftoffthefilterusingthepincers and place itin distillation flask andweigh tothe nearest 10mg(MA). the funnel situated over the evaporating dish, which Heat the distillation flask with a 150mm high flame, has been previously weighed to-the nearest 0.5 mg. that hasjust ceased to be luminous, insuch awaythat Dissolve ‘the crude par~ffin residue by carefully the first distillate drop isproduced within 3to 5 min. spraying heated petroleum spirit over it. Dissolve in The guard ring, loosely fitted on the distillation flask, thesameway anyparaffin that may beadhering tothe shallpreventpossibleburning ofthecorkstopper. Take thermometer orto the test tube. Evaporate the mixed care that the vapours produced during distillation are filtrates in the evaporating dish over the steam bath. largely condensed. For this purpose, the distillation To prevent the liquid creeping over the rim, carry out receiver, weighed tothe nearest 10mg, intowhich the the evaporation inaweak air ornitrogen stream. Dry lowerbentendoftheoutlettubeprojectstoitsfulllength the residue for 15+ 1min at 125* 5‘C inthe heating (see Fig.3), shallbe immersed asfaraspossible intoa cabinet and then allow it to COOLAs soon as the mixture of finely reduced iceand water. There shall, previously purified paraffin waxes have cooled down however, still be a field of vision to allow the rate of but have not quite solidified, add 15ml of acetone. distillation to be checked. Adjust this rate so that a drop falls from the end of the outlet tube into the 6.6 Dissolvetheparaflin waxes bygently heating and distillationreceiverapproximately e verysecond. When carefully swirling the evaporation dish. Make up any no more drops are produced over a period of 10 s, acetone lostbyevaporation. Cooltheacetonelparaffln continue heating for afurther 1minwith acompletely waxsolutioninawaterbathto 15* 0.5‘Candseparate non-luminous flameuntiltheflaskglowsred. Complete by filtering the paraffin waxes. Then wash the thedistillation inamaximum of 15min. Donottransfer evaporating dish,thethermometer andthefilter several thecondensate leftintheoutlettubeafterdistillation to timeswithacetone brought to 15* 0.5 ‘C from awash the distillation receiver. Mix the distillate thoroughly bottle. The total volume of washing liquid shall be bygently warming itwhilst atthe sametime carefully 30l 1ml. Dissolvetheparaffin waxes purified inthis swirling the receiver. way,bycarefilly sprayingthemwithheated petroleum spirit and collect them again in the evaporating dish 6.2 After cooling, weigh thedistillate contained inthe already used. Then evaporate the collected liquid ina receiver tothe nearest 10mg (MJ. Depending onthe weak air flow ornitrogen stream over the steam bath. expected paraffh wax content, weigh to the nearest 2 to4g+5mg (mass Mc)ofthewarm distillate intothe 6.7 Dry the crystallized paraflln waxes obtained, at test tube (provided with spout). If the paraflln wax 125* 5 “Cfor 15* 1min inthe heating cabinet and content cannot beestimated inadvance, aninitialmass aftercoolinginthedesiccatorweighthemtothenearest of approximately 3g isrecommended. 0.5mg(MJ. This finalmassshallbebetween 50and 100mg. Otherwise, reject this result and repeat the 6.3 Dissolve the initial mass of distillate in25* 1ml test with an appropriately changed initial mass of the of ether and add 25 * 1ml of ethanol. Close the test samedistillate (Mc). tubewithastopper fittedwithathermometer extending down intotheliquidandplacethetesttubeinthecooling 6.8 Determine thesolidification point ofparaffin wax bath. Cool the bath liquid by adding finely reduced onthe rotating thermometer. 4 IS 10512:2003 7 CALCULATION all the three values and repeat the test on two further testportions. 7.1 For each test portion, calculate the paraffin wax content, expressed asapercentage by mass,using the 7.4 Express the paraffh wax content asa percentage following equation: bymass;rounded tothe nearest 0.1. (MBxA’Q 8PRECAUTION paraffin wax, percent~= ~MAXMc) x 100 Never evaporate petroleum spiritonnaked flame oron where ahotplate. Steam bath shduld invariably beused. MA = initial massofbitumen, ing; 9 PRECISION MB = mass ofdistillate received, ing; Mc = initialmassofdistillate taken upfortest, ing; 9.1 Repeatability and IfWo resultsareobtainedbyoneandthesameoperator MD = final mass ofparaffin wax, ing. under repeatability conditions, they are considered to 7.2 Ifthevalues measured forbothtestportions donot beacceptableandinaccordancewiththespecifications differ bymore than 0.3percent bymass,determine the of this standard ifthey do not differ by more than 0.3 mean of the two values. Otherwise, carry out a percent bymass. determination on athird test portion of 25 g and take the mean ofthe two values being the closesttogether. 9.2Reproducibility These values, however, shall not differ by more than If two single and independent results are obtained in 0.3 percent by mass. If the first two values are twodifferentlaboratoriesundercomparable conditions, equidistant from the third, specify thethird value. theyareconsidered tobeacceptable andinaccordance 7.3 If it isnot possible to obtain a mean value from with the specifications of this standard if they do not thesethree valuesunderthespecifiedconditions,reject differ bymore than 1.0percent by mass. 5