(rh erga) — fafa ( Teer green ) Indian Standard BITUMEN EMULSION FOR ROADS ( CATIONIC TYPE ) — SPECIFICATION ( First Revision ) First Reprint MARCH 1997 Ics 75.140 PiV(ovR) SL. Me jot eo HoRIT® OF INDIA ‘nhar & WB) © bis 1995 BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002 Ostoier US ‘ Prive Geomp 4IS KET: 199 Indian Standard BITUMEN EMULSION FOR ROADS (CATIONIC TYPE ) — SPECIFICATION ( First Revision ) 1 scope This siandard covers the physical and chemical re- quirements of bitumen emulsions (cationic typ. forsoads 2 NORMATIVE REPERENCES ‘The following standards contain provisions which, through reference in the text, constitute provisions Of this standard, At the time of publication the editions indicated were valid. All standards are subject to revision and parties to agreement based on thisstandard are encouraged to investigate th possibility of applying the most recent edition of the standards listed below: 15 No Tite 13:1982 Paving bitumen (secondrevision) 269: 1989 Specification for 33 gra¢e ordinary Portland cement (ued: revision) 334: 1982 Glessary of terms relating to bitumen ond ta (sscond revision) 490: 1985. Tesi sieves 1201: 1978 Methods of testing tar and bituminous materials; sampling (fist revision) 1203: 1978 Methods for testing tar and bituminous materials — Deter- mination of penetration (first revision) 1203:1978 Methods for teiting tar and bituminous materials — Deter mination of eucit (fr revision) 1216:1978 Methods for testing tar_ and bituminous materials — Dete rmination ofsolubilityin carbon dis- uiphide oF tichloroeihyiene (rar revision) 3117:1965 _sSpeciicationtorbitunenemutsion for roads (anionic ype) TERMINOLOG SA. Forthe purpos piven in [S384 1982 and die following s ofthis stanvand, the definition apply 42 Cationic Emulsions An emulsions in which the cation of the emulsifier is at the interface with the bitumen particle; an emulsion in which the particles are positively charged and the aqueous phase is acidic, Breaking of these emulsions occurs by neutralization of charge. 4 MATERIALS 41 Any suitable grade of bitumen as_given in IS 73 : 1992 with or without addition of suitable ‘ux. may be sed. 4.2. Any emulsifying agent or any other ingredient, ‘which either quality-wise or quantity-wise, is likely. to elfect or harden the residue bitumen beyond the Iimis specified under $1 No. (is) of Table 1 shall snot be used. 5 TYPES Emulsified bitumen shall be ofthe following three types: a) Rapid Seicing ‘Type RS b) Medium Setting Type MS ©). Slow Setting Type ss. 6 REQUIREMENTS 64 Bitumen emulsion shatt be homogeneous. Within one year after manufactureit shall sow ne ondispersed Blaniataier Rough ag 6.2. The physivaland chemical requirements ofthe three types of emulsions shall comply with the requirements specified in Table 1. 7 SAMPLING 7 For the purpose of testing, the size of the sample and the sampling procedure from drums, varrels of bulk supply shall be as described in 15 1201 ; 1978 subject io the following: a) From Drums or Berreis ~ The content of ‘drura or barrel from which me sample fs be taken shall be thoroughly mised byIs ages 1995 rolling the cnatainer to ar fro for 3 pertog of 2 t0 3 minutes, suecessively in opposite direction, allowing ai least fhe revolutions. of the container in cach direction aad then up-ending the container through (wo revolutions first inone direction and then in Ihe opposite direction. From Bulk — Where practicable, bulk >) delivery of bitumen émulsion shall be agitated by forced circulation or air agita- tion, before sampling. ©) The sample of bitumen emulsion shall be drawn within 24 hours after delivery and tested within 7 days from the date of draw- ing, unless otherwise specified. ‘TAA Preparation of Samples Before carrying out anyof thetests, hesample shall be mixed by gentle shaking to ensbre uniformity. 72 If the single sample from a single run fails to falfilthe test requirements under 6,sample shall be drawn on the basis of 7.1 for testing in the same manrer. If these samples conform to requirement 06, he ot shall be accepted otherwise the ot shall ve rejected. 8 TRSIS Unless specified otherwise, tests shell be carried out as deseribed by methods referred to in Table 1. 9 MARKING 9.41 Each container shall be legibly and indelibly ‘marked with ihe following: 4) Indication of the source of manufacture, b) Month and year of manufacture; ©) Type; 4) Batch aumber; and e) Date of expiry. MLL BIS Certification Marking ‘The container may elso bo marked with the ‘Standard Mark. 9.LLL The wse of the Standard Mark is governed bythe provisions of Bureau of Indian Standards Act, 1986 and the Rules and Regulations made there- under. The details of conditions under which the licence for the use of the Standard Mark may be ‘granted to manufacturers or producers may be ob- tained from the Bureau of Indian Standards. Table 1 Physical and Chemical Requirements of Bitumen Emulsion (Cationie Type) (Clauses 42,6.2 and 8) st Characteristics Type of Emulsion Method of Test No r Reto RS Ms: s a o @ « ©) o 4) Residue on 6tmitror 005 0s 008 aAanexB IS Seve (percent by ms, $a) . 1) Viscosity Sayboll Furl Vissometes, Appenas A conde ofS S117 1965 ‘AtsiC - - 20400 Arse 50-400 0-400 = i) Caagulatioe of emulsion Nil Nil Ni Annex aclow enperaare iv) Storagestatility 1 1 1 AonesD after 20h, percentage, Mar 1) Pariclecharge Positive Positive Poste Annex E Wi) Cowingatilty snd water resistance ‘Ames ‘Coating dy sggregnie - Go0s - Coning aterspryirg = Fair = Conting wet ageregne = Fair = Contin, after spaying = Fair vil) Siatiiyto mising with cement - = 2 Amex {pereenage congletion) sii) Misi vith water Nit Na NI Anaesth i) Tete on rue Armed a) Residve by evaporation, co s ” escea lin b) Feseintion2s°cnvogssce 6-210 oor vo.210 6) Duetity 21°Clem, Ais 75 1S 75 {) Solutlty: Intiehowsetytene, 975 os 987 Mix Ts requrement shal be applic oly ade situations where the amiiew teperture i ble 15°C, ' 2ANNE Cc (Table 1) METHOD FOR DETERMINATION OF COAGULATION OF EMULSIONS AT LOW’ C-L APPARATUS Cll Glass Boiling Tube—150 mm Jong and 25 mm in internal diameter, provided with a cork cal hole 13 mm in diameter. (600-micion IS Sieve. and cent C12 Sieve 4.3 Beaker — Two, 6 ml capacity. C-La Water-tiuth — Thermostatically controlled, MATERIALS 1 Solution — A I-peremt solution of cettimide (a mixture of alkyltsimethy! ammonium bromide) in N/10 hydrochloric acid €-22 Solvents — Xylene andacetone. ¢-3 PROCEDURE C-AL Wash 600-micron JS Sieve with xylene, acetone and distilled water. Moisten thecleansieve with cetrimide. Pass some of the emulsions through the sieve and introduce 20 mi of sieved emulsion into the boiling tube. Bring the emulsion PERATURE, ing process stir slowly. Lower the temperature of water, byadding commen salt, 0-1 t0 -1.5°C so. that the temperature of the emulsion is reduced to °C. At PC discontinue stirring and transfer the tube to another beaker with a freezing mixture at 2 temperature of ~3 10 —4°C and allow the emul- sion to remain quiscent for 30 minutes. Remove the tube from the freezing mixture without disturbance and allow the vemperature of the content to rise spontencously to room temperature. Moisien the sicve with cetrimide and pass the emulsion through, the sieve. Wash the tute free from emulsion and other residue with ceirimide and pass the washings through the sieve, Tho coagulated bitumen, if any, vill be retained on the sieve, C4 REPORT Report the emulsion as ‘passed’ if no coagulation takes place, NOTE — Ifthe emulsions exposed to temperature below °C during storgearamsponatin the folowing addtional cestena all appy by plunging the ube intothe water at 30°Cand stir a) Subzero temperature —178°C emily with tte thermometer unit temperature oft) Freeang and shaving ele shall be repeated three te emulsion is constant. Remove the tube from tine warm water and plunge iatothe beaker containing ©) After the inde theenusonsha bean or iged water at the botiom of which crushed ice is honogeney. fetained by apiece of wire geuge. During the cool ANNEX D ( Table 1) METHOD OF DETERMINATION OF STORAGE STABILITY D-l APPARATUS D-LL Cylinders — Two 500-ml glass cylinders, vith pressed or moulded glass bases and cork or lass toppers, having an outside diameter of 50 + ‘5 mm and having S-mi graduations, hon glass tube D-12 Glass Pipette — A 6-ml sy pipette, ‘or 1 000-ml capacity, made of borosilicate glass. D-L5 Glass Rol 64 mum in diame! with flame polished ends, ‘cand 178 man in length. D.16 Oven — Thermostatically controlled, copable of maintaining temperature of 163 = 28°C. D2 PROCEDURE D2.1 Bring the bitumen emulsion to room temperature (21 to 27°C), Place a S00-ml repre- sentative sample in cach of the two glass cylinders. Stopper the cylinders and allow them tostand un- disturbed, at kaboratory air temperature (21 to 2FO), for 24 hours. Alter standing for this period, Temove approximately $5-mi from the top of the ‘emulsion by means of the pipette orsyphon without disturbing the rest, Thoroughly mix exch portion. 2.2 Weigh 5020.1 g of each sample sopsirately weighed S04 or 1 O00-ml glass beakers, ntowh beaker having previously heen weishol wit d fee D-LE). Adjust 122 ten ofthe own to 163 = 24°C. Then plece the be containing the rods snd sample i the oven hours. At the end of this pericd remove cach beaker and thoroughly stir the residue. Replace in the oven for I hour, hen reinove the beakers from the oven, allow 10 cool to room temperature, and ‘weigh, with the rods (see Note). NOTE—Careshal beteken prevent eso bitumen fiom thebesier through forming ce spateriay cr both. For this Feson, 1 O00 pl beakers e recommended. Also, the pla ingot uakers and emelsicn simples 23 colsorwaem oven Sno bringing the even and sample up toa temperaute of 1G8C roger is permsibe. If preterced, prelininary eaporatign of watery be accomplishes tycarecutneating recep. followed ty oven trentent at 162°C for 1.2.3 Afier removal of the sample, syphon off the next 390-ml (approximate) from each of te cylinders, Thoroughly mix the emulsion remaining in the cylinders and weist 1 ginto separate IS BSS 199 ‘weighed 600 oF 1 fm lass beakers. Determine the bituminous residue of these samples in accord ance with D-22, D3 CALCULATION Calculate the storage stabilityas the numerical df. ference between the average percentage of bituminous residue found in the two top samples and that found in the two tottom samples. D-t PRECISION D-4.1 Duplicate determinations by the same operaior shall not be considered suspect if the determined values differ by more than 0.5 percent. D-4.2 Reproducibility ‘The values reported by each of the two laboratories representing the arithmetic average of duplicate determinations shall not be considered suspect valuesif the reported values differ by more than 0.6 percent. ANNEX E (Table 1) METHOD FOR DETERMINATION OF PARTICLE CHARGE E-L APPARATUS E-L1 Current Source — A 12 V battery. E-L2 Rheostat—of 2 00 ohm capacity E-L3 Ammeter —of0.1 ampere capacity. +L Stainless Steet Plates — Two, 25 mm x 75 mmsize. E-LS Glass Container — of 500 ml capacity. E-2 PROCEDURE Take sufficient quantity of a representative sample of bitumen emulsion in the glass container, Im- merse two stainless steel plates 25 mm X 75 mm which are connected to 2 12 sols tttery circuit, through a switeh, a rkeostat and on ammeter, toa depth of 25 mm and markthe +Veand ~ Ve plates. Close the switch and adjust the rheostatso that the current in the ciccuit is more thand mA. Open the circuit after 30 minutes ard remove the plates. Gently wash the plates if necessary with distilled water to remove unbroken emulsion and then examine. E3 REPORTING An appreciable layer (continuous opaque film) of ‘deposited bitumen on the negative plate (cathode) witha relotively clean bitumen free positive plate (anode) indicates a cationic emulsion of positively ‘charged partictes. ANNEX F (Table 1) COATING ABILITY AND WAT Pot APPARAT s whole enamelled kitchen titre capacity, FLL Mixing Pan — 9 pan with handle, of approxinatel FAL2 Mixing Blade— A putty knife with a 30 mm % 90 mm steel blade with rounded corners, A254 mm kitchen mixing spoon may be used as an alter RESISTANCE F-L3 Sieves — Standard sieves ot 1y mm and 4.75 sym conforming io 1S 460: 1988. Flt Constant Head Water Spraying Apparatus — An apparatus for applying tap water in a spray under a constant head of 775 ma. The water shall issue from the apparatus in a low velocity spray, F-L5 Thermometer — {tshall be of he mercury in-glass type nitrogen filled, with the stem made OfIss nia 199S ead glass or othr ft shalt be engraved and enamelled at the back and provided with an the top, The bulb shall be gjliadrical, made of suitable thermometric glass. The dimensions, tolerances and graduations of the thermometer shall be as follow Range = PC 0 80°C Gradvationateach 02°C Longer lines ateach °C Figures at each re Immersion, mm Total Overall length 378 10384 ma Length of graduated 24310279 mm. portion Length of bulb 9to14 mm Bulb diameter No larger than stem diameter Stem diameter 6010 7.0mm Distance from botiom of 75 10 90 mm bulb 00°C Scale error, Mae orc F-L6 Balance — Capable of weighing 1 000 g within +01 g FAL? Pipette —of 10 ml capacity 2 MATERIALS F.2.1 Aggregate — Standard limestone aggregate stall be s laboratory washed and air cooled aggregaie sraded to pass 19 mm sieve and retained 01 4.75 mm sieve F:2.2 Calcium Carbonate — Chemically pure precipitated (CaCOs) shall be used asa dust to be nixed with the stancard aggregate, 2.3 Water — Tap water of not over 250 ppm CxCOs hardness for spraying over the sample. 3 SAMPLE ‘The sample shall be representative of the bitumen emulsion to be tested. F- PROCEDURE FOR TEST WITH WET AGGREGATE, Fatt Carry out the est at 24 2 5.5°C. F-4.2 Weigh 460 gofthe airdried/graded limestone aggregates in the mixing pan. Fu43 Weigh 40 gof CxCOs dust in the mixing pan and “mis with the 460 g of aggregate for approxicautely one minute by means of a mixing Slate 15 obtain uaifoum film of dust on te 5. The total eight of aygreyare agguegete partic shall be 465 g. F-44 Pipette 9.3-ml of water to the eperegate and CaCO3 dust misture into the mixing pan and mix thoroughly to obtain uniform wetting. F-45 Weigh 35 g of bitumen emulsion into the aggregate in the pan and mix vigorously with the mixing blade for $ minutes by a back and forth motion ia an elliptical path of the mixing blade or spoon, Attheend of the mixing period, tt thepan and permit any excess emulsion not on the ‘aggregate to drain from the pan. F-46 Remove approximately one half of the mix ture from the pan and place it on absorbent paper ‘and evaluste the coating. F-4. Immediately spray the mixture remaining ia the panwith tap water from the constant head water spraying apparatus to cover the mixture. The dis- tance from the spray head to the sample shall be (205 + 75 mm). Then carefully pour off the water. Continue spraying and pouring off the water until the overflow water cums clear. Carefully drain off the water on the pan. Scoop the mixture from the mixing pan on toabsorbent paper for evaluation of coating retention in the washing test. F-4.8 Evaluate the mixture immediately by visual estimation 2s to the total agoregates surface area that is coated with bitumen. F-4.9 Reporttheevaluation by visual estimation of the coating of the aggregate surface area by bitumenafter themixture hasbeen surface air dried in the laboratory at room temperature, A fan may be used for drving if desired. F-$ REPORTING OF TEST RESULTS. FS. Evaluate and report the following informa- tion for tesis with both dry and wet ayeregates. F-5.2 At the end of the mixing period record the coating of the total aggregate surface area by the bitumen emulsion as “good” ‘fair or ‘poor where a rating of ‘gos! means fully coated by the bitumen emulsion excessive of pinholes and sharp edges of the aggregates, a rating of ‘air’ coating applies 10 the condition of an excess of coated area over un- coated area and a rating of ‘poor’ applies 10 the condition of anextess of uncoated area over coated area. F-53 Afversprayingwith water record the coating of the toial ageregate surface area by the bitumen as ‘good’, ‘ir or ‘poor, F-5.4 Comments about the resu be included in the evaluation, s of the test mayANNEX G (Table 1) STABILITY To MIXING WITH CEMENT Gu APPARATUS 1.1 Sieves — A 140 mm IS Sieve approximately 100 mm in diameter end 40 mm in height and 450-micron IS Sieve approximately 200 mm in diameter. 641.2 Metal Dish — A round-bottomed metal utencil of approximately 500-ml capacity. G-.3 Steel Rod — A.stecl rod with rounded ends 3mm in diameter, G-l.4 Balance — 250 g capacity accurate 10 0.1 g G-L5 Graduated Cylinder — of 109-mi capacity G-1.6 Shallow Pan — of 100 mm diameter and of about 50-ml capacity. G-1.7 Oven — A well-ventilated oven controlled at 110°C. G-2 MATERIAL G-2.1 Ordinary portland cement conforming to IS 269 : 1989, it shall be kept in sealed container and not exposed to atmosphere before use. G-3 PROCEDURE G-3,1 Make up the water content of the emulsion to 50 percent by adding extra water if necessary. Pass the cement through 150-micron IS Sieve and weigh 50g into the metai dish, Weigh the 1.40 mm 1S Sieve and shallow pan to nearest 0.1 (544). Add 100-m of ertulsion to the cement in the dish and stir the misture at once with the steel roe with 2 circular motion making about 60 revolutions per minute. At the end of one-minute miging period add 150-ml freshly toiled distilled water at room temperature and continue stirring for 3 minutes Maintain the ingredients at a temperature of ap- proximately 25°Curing mixing. Pour the mixture through the weighed 1.40 mm IS Sieve and rinse with distilled water. Place thesieve in the weighed ppan, heat in the oven at 110°C until dry to nearest 01 e(F#2) G-4 CALCULATION Coagulation value where HW, = massin g ofweighed sieve and pan, W, = massin gof the sieve and pan and the material retained on them, end mass in gofbinder in 100-mi of diluted deterrained according to Annex J G-5 REPORT Report the coagulation value as percentage to the nearest wiole numb G-6 PRECISION ‘The duplicate test results shall not differ ty more than the following: Cement Mixing Repeatabiliny Reproducibility ‘Mass, Percent Mass, Percent Mass. Percent 0102 02 os NOTE — Ordinary portant cenent conforming to 18269: 11989 sta beset (Table 1) . METHOD FOR DETERMINATION OF MISCIBILITY WITH WATER M-1 PROCEDURE, Graduallyadd 150-m distilled water, with constant stirring to 50-ml of emulsion in a 400-ml beaker at a temperature of 20 t0 30°C. Allow the mixture to stand for 2hoursand examine it for any appreciable ‘coagulation ofthe bitumen content of theemulsion.ANNEX J (Clevsex 6.2, G-4 and Table 1) METHOD YOR DEVERMINATION OF RESIDUE BYEVAYORATION Jet APPARATUS JUL Glass Beakers — low form of 1 000-mt ‘capacity made of borosilicate glass. J-1.2 Glass Rods — With flame polished 64 mm in diameter and 177.7 man in length. J-1.3 Bolance— of $00 g capacity and accurate to #01g. J-L4 Oven — Themmostatically controlled at a temperature of 163 + 28°C. 2 PROCEDURE Weigh 50 + 01 ¢ of thoroughly {nia cach of three beakers each of which has pre- viously been weighed with the gless rod. Place the beaker alongwith the rodin the oven at 163 + 28°C for? hours. Atthe end of this period remove each ‘beaker anu stir the residue thoroughly. Replace in the oven for another one howr then remove and cool at room temperature, weigh the beakers along with the rods 4-3 CALCULATION FAL Residue,percent = 24-2) 2 A sve where Be ‘A = mass of beaker, rofl and residue g; and B = /arDmass ofbeaker snd rod, ¢ J-32 Take theaverage of three values obtained for residue, percent. . J-4 TESTS ON RESIDUE 4-41 Penetration— Determine penetration on a sample of the residue in accordance with IS 1203 : 1978. J-42 Ductility — Determine the ductility on a representative portion ofthe residuein accordance with IS 1208 1978 J-43 Solubility in Trichloroethslene — Deter- mine the solubility in trichlorbethylene on a representative sample ofthe residue in secordanee with IS 1216:Contact Numbers LBII Team GSHP 1-5 1 Mr. Andrew Bogle + 9825008039 2 Louis Berger International Office Plot No. 184, 8 (02712) 35909, 35910 Gandhinagar ISPN- (02712)49977 i + 02717-24381 3 Mr. Mr. William J. Hucchinson R.E. C1 9525023566 (m) 2 02767-20729 4 Mr. Henry T. Osea RE. C2 + 9825005771 (m) 5 Mr.C.TF RECS QA os2sos246 " raverso ost! se ROR 2 9825015538 (R) 02622-26991 John Bentley R. E.C4 + 9825015528 (0) 02676-20139 7 RC. Daria RECS 8 Mr. Falgunsinh Jhala (office) + 9825015529 9 Mr. Sanjay Kumar Singh ARE C2 + 9825023543 10 Mr. V. K. Shriwastava + 9825023546