DETERMINACAO DA PERCENTAGEM DE Ex Brisk BETUME DE MISTURAS BETUMINOSAS PARA ESPECIFICACAO PAVIMENTACAO, POR CENTRIFUGAGAO ASTM D2172-81 1 -PREAMBULO L.1-Este método de ensaio permite a determinagZo da quantidade de betume, por centrifugago, existente em misturas betuminosas. Os agregados obtidos através deste método podem ser, posteriormente, utilizados para andlise granulométrica. 1.2-Qs solventes a utilizar na extracgdo do betume sao: tricloractileno, 1.1.1 tricloroctano, cloreto de metileno ou benzeno. 1.3- A quantidade de betume na amostra & calculada por diferenga entre o peso total € os pesos do agregado extrafdo da dgua ¢ do filler cantidos no extractor. Q resultado ¢ expresso em percentagem ponderal, calculada em relagdo & mistura betuminosa sem agua, sendo designada por “percentagem de betume”. Quando o resultado, expresso em perventagem, é calculado em relago ao peso de agregado total, designa-se por “teor em betume”. NOTA: Os resultados obtidos neste ensaio podem ser afectados pela idade do material ensuiado, isto é, nas amosiras mais antigus hi uendncix para obtengio de percentagens de betume ligciramente mais haixas. Sao obtidos melhores resultados quando 0 ensaio € realizado sobre misturas recém-preparadas au sobre amostras de pavimentos recém- -executados, 2- APLICAGAO, 5 © mélodo descrito na presente ESPECIFICAGAO pode ser utilizado para o determinagio da percentagem de betume em misturas betuminosas a quente, para efeitos de controlo, aceitasio, i¢d0 periddica ou investigayio3+ APARELHOS E UTENSILIOS Estufa - Com capacidade para manter uma temperatura de 110°C + 5°C ‘Tahulcira - Com cerca de 30 cm de comprimento, 20 cm de largura e 2,5 cm de altura, Balanca - Com preciso de 0,01% do peso da amostra, no mfnimo. Manta eléctrica - De 700 W, com regulacdo continua ou com regulaco para poténcia baixa, média e alla Pmveta_graduada - Com capacidade de 1 0X) ov 2.000 ml. Provera graduada, com capacidade de 106 ml (opcional). Cadinho - Com capacidade de 125 ml. Excicador Extractor - Consistindo numa taga do tipo representado na Figura | ¢ num aparelho de centrifugacio no qual a taga giraré a velocidades controladas, variiveis até 3.600 cpm. A velocidade pode ser controlada manual ou autom: samente, com uma variagio preestabelecida. O extractor deve incluir também um recipiente para recolha do solvente extraido da taga e um dreno para a sua remogio. E conveniente que o aparelho possua um dispositivo anti- explosio ¢ que seja instalado sob uma chaminé ou num local com exaustor, para ventilagzo (hott). NOTA: Pode utilizar © um dispositive semelhante a0 da Figura, de maiores dimensoes. Filiros - Anelares, de feltro ou de papel. com us dimensties do hocal-da taga, NOTA: A norma ASTM prevé, opcionalmente, utilizago de filtros de papel, de baixo teor em cinzas, que, apds a extracgdo, sia qucimados. Esta especificagao nfo inclui o procedimento a tomar no caso de se ut ireste tipo de filtros.4- REAGENTES Solucio saturada de carhonaio de aménio, do tipo reagente (necessfrio apenas para a determinago da percentagem de filler no Lfquido extraido pelo métado da incineraeio). Benzeno (ver precaugdes a tomar, no parigrafo 5). Gloreto de metilena (ver precaugées a tomar, no pardgrafo 5). LLLiticloroctano (ver precaugGes a tomar, no parigrafo 5). ‘Trisloroctileno (ver precaugées a tomar, no pardgrafo 5). 5- PRECAUGOES Qs solventes mencionados no pardgrafo anterior devem ser utilizados sob uma “chaminé” de Protecgiio ou numa Grea bem ventilada com um bom exaustor, dado que todos eles siio t6xicos. 6- PREPARAGAO Da AMOSTRA Se a mistura nao esti suficientemente mole que a amostra seja separada com uma espétula ou uma colher, deve-se colocd-la num tabuleiro ¢ aquecer a 110 + 5°C, apenas até estar suficientemente trabalhivel. Separa-se a quantidade de matcrial necess4ria para a realizagfo do ensaio, com um valor’ minimo de cerca de 650 x, para misturas com maxima dimensio nominal do agregado igual a! 12,5 mm, NOTAS: 1. A massa do provete deve ser tanto muir quanto maior for a m&xima dimensio nominal do agregad. 2. Quando a massu do provete for excessiva, em relagio A capacidade do equipumento utilizado, @ provete deve ser ensaiado por partes ¢ os respectivos resultados tratados de mode aprupriady para 0 edlculo da percentagem de betume (vd. seegio 9)3. E necessdrio um provete suplementar para a determinagio da percentagem de gua na mistura. Este provete deve ser retirado imediatamente apés a separagao da amosira destinada a extracgio do betume. No caso de a amostra ter sido colocada na estufa a 110 + 5°C, até massa Constante, nfo € necessdria a determinayio do teor em 4gua da amostra. 7 - PERCENTAGEM DE AGUA Na MISTURA Determina-se a percentagem de gua na mistura de acordo com a Norma ASTM D1461, salvo se se estiver nas condigties da nota anterior A massa de Sgua contida (W2) na amostra destinada 3 extracgtio do betume & igual ao produto da massa total da amostra (W1) pela percentagem de 4gua na mistura, 8- TECNICA DE ENSAIO 8.1 - Determinur a massa de 4gua contida na amostra (vd. 6 e 7), caso seja necessirio 8.2 - Colocar a amostra (650 g a 2 5000 g) de mistura betuminosa) na taga. 8.3 - Cobrir a amostra com o solvente (vd. 4.2, 4.3, 4.4 €4,5) e esperaro tempo suficiente para que o Solvente “ desintegre” a amostra (miximo 1 hora). Colocar a taga no aparetho de centrifugagao, Secar 0 filtro, determinar a sua massa e coloci-lo sabre o bordo da tga. Colocar a tampa, fechar bem com um grampo ¢ colocur um recipiente sab 0 dreno, para recolha do Iiquido extrafdo. 8.4-Comegar a centrifuy ao devagur, wumentur yrudualmente a velocidade até a0 méximo de 3.600 rpm ou até que @ solvente deixe de currer pelo dreno. Deixur parar a méquina ¢ juntar 200 ml de solvente, repetinds o process, Utilizar um niimero de adigcs de 200 ml de solvente ado inferior 23. até que o liquido exteaida seja clara (cor de palha). Recolher @ Ifquido num capo graduado,8.5 - Remover 0 filtco ¢ secar a0 ar. Se se utilizar Milt * de feltro, devem-se escovar bem os produtos ‘minerais aderentes & sua superficie, para junto dos restantes agregados extraidos. Secaro filtro numa estufa, até massa constante, ¢ pesé-lo, Retirar euidadosamente todo 0 conteddo da taga para o tabuleiro previamente pesado, introduzi-lo ‘hum banho dc vapor e, depois ,secd-tos até massa constante numa estufa ou numa manta eléctrica, de 1104 5°C, e pesé-to. Se 0 solvente uilizado for o tricloroetileno ou 1.1.1. tricloroetano, 2 introdugao ne banho de vapor pode ser dispensads. A masse do agregado extraldo (W3) & igual A massa do agregada contido no tabuleiro mais 0 acréscimo da massa do filtro. NOTA: Dado que o agregado seco absorve humidade quando exposto aq ar himido, deve-se Pesaro apregado extraldo logo que este tiver arrefecido até uma temperature razofvel, apés a secagem, 8.6 - Determinar a quantidade de filler contido no liquide extrafdo pelo seguinte método: * Método de incineragio ~ Anotar 0 volume total do Uquido extraido. Dewerminar a massa de um cadinho. Agitar 0 extracto e deitar imediatamente cerca de 100 ml no cadinho. Secar num banho de vapor ou numa manta eld rica (deve-se usar sempre o banho de vapor quando o solvente for benzeno). Tacinerar 0 residuo aué ao rubro sombriv (500 a 600°C), deixar arrefecer e juntar 5 ml de solugdo saturada de carbonate de umGaio por cada grama de cinza, Deixat repousar 2 femperatura ambiente durante | hora, Secar na estufa a 100°C, até mussa constante, arrefecer hum excitador ¢ determinar a massa G. ~ Calculara massa de filler contida no volume total de liquide extraido (W4), através da seguinte expresso: W4=GVj/(V} - Vo) sendo: G - Massa de cinza (g) determinada nu ndimero anteriorV1 ~ Volume total do liquido (ml) V2_~ Volume de Iiquido apés extracgao da parte que foi incinerada (rl) 9- ResuLTapos 9.1-A percentagem de betume de uma mistura betumminosa € calculada pela seguinte f6rmula: (Wy, ~ W2) - (W3 + Wa) % betume = x 100 * Wi - Wa sendo: W) - Massa total da amostra W2 ~ Massa de agua na amostra (no caso de nfo se determinar 0 twor em égua da amostra tem- se W2 =0, depois de seca a amostra) W3 - Massa do agregado extraido Wa - Massa de filler contida no ltquido extrafdo (determinada em 8.6) 92-0 teor em betume pode ser calculada pela expressio: (Wy - Wa) - (W3 + Wa) © (%@)= x 100 Wa - W4na on, vith or va. nd. ugh sity acy sity sto are, ion the ito Ho the ure red ror for ™%s mn, SUM Designation: D 2172 - 93 i ‘ll Standard Test Methods for Quantitative Extraction of Bitumen From Bituminous Pav Mixtures’ “This standards ased unde the fied designation D 2172: the number immediately following he desiation ndcates the ear of ‘ontinal adoption on he ex f revision the ero ast revision. A number in parentheses indices the yer lst reaporval-A superset epsilon (indicates an editor change ce the last revision o eaporoval, This standard has ben approved for use be agencies ofthe Deparment of Defense. Consul the De) Indes of Specifications and Standards forthe specie war of nue which has ben adopted bythe Departmen of Defense 1. Scope LLL These test methods cover the quantitative determina- sion of bitumen in hot-mixed paving mixtures and pavement samples. Aggregate obtained by these test methods may be wed for sieve analysis using Test Method C117 and Test Method C 136, 1.2 The values stated in inch-pound units are to be rparded as the standard, The values given in parentheses are {or information only. 1.3 This standard does not purport to address all of the safety problems, if any. associated with its use. It is the responsibility of the user of this standard to establish appro- priate safety and health practices and determine the applica. bility of regulatory limitations prior to use. Specific hazards are given in Section 7. Note 1—The results obtained by these test methods may be affected by the age of the material tested, with older samples tending to yield sighly lover bitumen content, Best quantitative results are obtained ten the test is made on mixtures and pavements shortly afer theit preparation. It is difficult to remove all the asphalt when some lugreztes are used and some chlorides may remain within the mineral tmater affecting the measured asphalt content, 2, Referenced Documents 2.1 ASTM Standards: : C117 Test Method for Materials Finer Than 75-um (No. 200) Sieve in Mineral Aggregates by Washing? C128 Test Method for Specific Gravity and Absorption of Fine Aggregate? C136 Test Method for Sieve Analysis of Fine and Coarse Aggregates? €670 Practice for Preparing Precision and Bias State- ments for Test Methods for Construction Materials? D10 Test Method for Specific Gravity of Semi-Solid Bituminous Materials? 604 Specification for Diatomaceous Silica Pigment" D979 Practice for Sampling Bituminous Paving Mixtures? 1461 Test Method for Moisture or Volatile Distillates in Bituminous Paving Mixtures? "These test methods a€¢ under the juraiction of ASTM Commitee O-t on Rout and Paving Materials and are the dec ceipanuiliicy of Suisommtce '00125'0n analss af Bhurinous Mixtures, Current eiion approved Sept. 13,1993, Pablhed Novernbcr 1983 Onginall Dblahed ag D 317263 T, Lant previous edition D 2172 = 92 Sanna Bako ASTM Standard Vol O4 02 Nanaia Bak of ASTM Standards. Vol 08.03 “Anna! Brot of ASTM Standards Vol 06 03 1856 Test Method for Recovery of Asphalt from Solu- tion by Abson Method? D2ILI Test Methods for Specific Gravity of Halogenated Organic Solvents and Their Admixtures* 22 Federal Specifications: 0-T-620a (Int. Amd. 3) I,1,1-Trichloroethane, Technical, Inhibited Methyl Chloroform)® 0-T-634 (latest) Trichloroethylene, Technical® 3. Summary of Test Methods 3.1 The paving mixture is extracted with trichloroethyl- cine, 1,1,1-trichloroethane or methylene chloride using the extraction equipment applicable to the particular method The bitumen content is calculated by difference from the mass of the extracted aggregate, moisture content, and min- eral matter in the extract. The bitumen content is expressed as mass percent of moisture-free mixtures. 4. Significance and Use 4.1 All of these test methods can be used for quantitative determinations of bitumen in hot-mixed paving mixtures and pavement samples for specification acceptance, service evaluation, control, and research, Each method prescribes the solvent or solvents and any other reagents that can be used in the test method. Test Method D 1856 requires that Method A be used when asphalt is recovered from solution, 5. Apparatus 5.1 Oven, capable of maintaining the temperature at 230 + 9°F (110 * 5°C) 5.2 Pan, flat, 12 in. (305 mm) long, 8 in. (203 mm) wide, and 1 in. (25 mm) deep. 5.3 Balance, or balances having an.accuracy of at least 0.01 % of the sample mass. 5.4 Hot Plate, clectric, 100-W continuous or low, me- dium, and high settings. 5.5 Small-Mfouth Graduate, 1000 or 2000-mL capacity. Optional small-mouth graduate, 100-mL capacity 5.6 Ignition Dish, 125-mL. capacity. 5.7 Desiccator, 5.8 Analytical Balance. > tonal Rook of ASTM Standard. Vol 15.08 ‘ Ataluble Feom Standardeation Documents Order Desk, Bldg & Section ©. 200 Robins Ave. Phiadelbia, PA 19111-5084, Attn NPODS. 2096. Reagents 6.1 Purity of Reagens—t used in all tests. Unless ot that all reagents shall cont Reagent grade chemicals shall be herwise indicated. it is intended form to the specifications of the Committee on Analytical Reagents of the American Chem. ical Society.” where such specifications are available. Other ‘grades may be used. provided itis first ascertained that the Teagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination, 62 Ammonium Carbonate Solution—Saturated solution of reagent grade ammonium carbonate ((NH,)sCOs] 6.3 Methylene Chloride. technical grade. Caution-—see Section 7. 64 1.1.1-Trichloroethane, conforming to Federal Specifi- cation O-T-620a (Int. Amd, 3). Caution—see Section 7, 6.5 Trichloroethylene, technical grade, Type 1, Federal Specification O-T-634, latest revision. Caution—see Section 1. 7. Hazards 7.1 The solvents listed in Secti under a hood or with an effective well-ventilated area, since they are indicated in Table 1 ion 6 should be used only surface exhaust system in a € all toxic to some degree as 8. Sampling 8.1 Obtain samples in accordance with Practice D979, 8.2 Preparation of Test Specimens: 8.2.1 If the mixture is not sufficiently soft to separate with 2 spatula or trowel, place it in a large, flat pan and warm to 230 9°F (110 * 5°C) only until it can be handled or mixed, Split or quarter the material until the mass of material required for test is obtained, 8.2.2 The size of the test sample shall be governed by the nominal maximum aggregate size of the mixture and shall conform to the mass requirement shown in Table 2 (Note 2): Note 2—When the mass ofthe tests the equipment used (for a particular method} the test specimen may be ivded into suitable increments, tested, and the results appropristely combined for calculation of bitumen content (Section 12) pecimen exceeds the capacity of 8.2.3 In addition, a test specimen is required for the determination of moisture (Section 9) in the mixtures. Take this test specimen from the remaining sample of the mixture immediately afier obtaining the extraction test specimen, Note 3—Ifrecovery of bitumen from the solution obtained from the extraction testis not required, the entice test specimen may be dried to constant mass in an oven at a temperature of 230 2 OF (110 2 SC) rior 1 extraction instead of determining the moisture content (Section 5), 9. Moisture Content 9.1 Determine the moisture 8.2.2) in accordance usin; Method D 1461 content of the mixture (see B the procedure described in Test Reatom Chemclt, amenson Chen Sacer Spec hema! Sees. Washington. OC. Far wagesions a he ea Usted by the Amencan Chemical Sovety se nclar (Chomrah. BOM Lid Poole, Doser rd Nanumal Forman Rosie S10, ng of esgens net Standard fr atowamen and the Ced Sate Pharmaceneis US Pharmaceutical Convention. Ine, LUSREL ih 0 2172 TABLE 1 Solvent Tonenty - "Tene Waguea Aneage ie Wena Aver Selvent Concentration fn expose, __ ‘5.087 week pon etiyone chonae mo “Teenevoetnyene 109 istrereroetnane 350 * Threshold Umit Concentration Can wnitee et the Amencan Conferansy Governmental Hygienists, 1977 Vaes “ne TABLE 2. Size of Semple See ‘Nominal Maxima formic SzeSurdes, Seve Se Mirus ot Sry ee ain 1 ve, 1s Min 2 1a, 3 thin a 9.2 Calculate the mass of water, H. (12.1) in the extra tion test portion by multiplying mass percent water (9-1) ¢ the mass of the extraction test portion, #1, (12.1 TEST METHOD A 10. Apparatus 10.1 In addition to the apparatus listed in Section 5, th following apparatus is required for Test Method A: 10.1.1 Extraction Apparatus, consisting of a bowl approx mating that shown in Fig. | and an apparatus in which bowl may be revolved at controlled variable speeds vod 3600 r/min. The speed may be controlled manually of with! Preset speed control. The apparatus should be provided wit 8 container for catching the solvent thrown from the bow and a drain for removing the solvent. The apparatus prefed ably shall be provided with explosion-proof features ané installed iri a hood or an effective surface exhaust system i provide ventilation. Nore 4—Similar apparatus of larger size may be used 10.1.2 Filter Rings, felt or paper, to fit the sim of th bowl, Sao 10.1.3 Low-ash paper filter rings may be used in place the felt filter ring (10.1.2). Such filter rings shall consist low ash filter paper stock 0.05 + 0.005 in. thick. Th nominal base wcight of the paper shall be 330 + 30 Ib for ream (500 sheets—25 by 38 in.). The ash content of th Paper should not exceed 0.2 % (approximately 0034 ring). IL. Procedure 11.1 Determine the moisture content of the material i accordance with Section 9, 11.2 Place a 650 to 2500-g test portion into a bowl. Annex Al for alternative procedures to those prescribe herein and in 11.5, 113 Cover the test portion in the bowl wi tichlorocthylene, 1.1.1-trichloroethane or methylene chk Fide and allow sufficient time for the solvent to disintegrate the test portion (not over Ih), Place the bow! containing the| test portion and the solvent in the extraction apparatus. D2}Gh 0 2172 te. by be [Note—See Table 3 for metric equivalents . FIG. 1 Extraction Unit Bowl (Test Method A) be Bj TABLE 3 Metric Equivalents for Figures a a % 032 Te 3 5 143 ri Me 048 ™ 4a 6 152 "a oss. he 55 em 155 ey % rr} 2 55 es 157 “ me 073 Pe 59 ev 153 o ” 095 2 6a 5 185 4 127 a 63 ™% 187 * 139 2a 72 5 207 % 19 3 7s cn 247 1 25 ™ - 95 0 254 x vA 206 4 102 10% 257 We 302 Pts 108 2 205 o We 357 5 wr “ 385 1M 38 sm 138 1% 37 We a x and determine the mass of the filter ring and fit it around the edge of the bowl, Clamp the cover on the bowl tightly and place a beaker under the drain to collect the extract. 11.4 Start the centrifuge revolving slowly and gradually increase the speed to a maximum of 3600 r/min or until solvent ceases to flow from the drain. Allow the machine to Sop, add 200 mL. of trichloroethylenc, 1,1,1-trichloroethane or methylene chloride and repeat the procedure. Use suffi- Gient 200-mL. solvent additions (not less than three) so that the extract is not darker than a light straw color. Collect the ‘extract and the washings in a suitable graduate. 115 Remove the filter ring from the bowl and dry in air. {felt filter rings are used, brush off mineral matier adhering \0 the surface of the ring and add to the extracted aggregate Dry the ring to constant mass in an oven at 230 © 9°F (110 * 5*C), Carefully remove all the contents of the bow! into a metal pan and dry on a steam bath and then, dry to constant ‘mass in an oven or on a hot plate at 230 + 9°F (110 + 5*C). If trichloroethylene or trichloroethane is used as the extrac. tion solvent, the preliminary drying on a steam bath may be omitted. The mass of the extracted aggregate, 1%, is equal 10 the mass of the aggregate in the pan plus the increase in mass of the filter rings. 15.1 Use the following alternative procedure when low: ash filter rings are used: Place the aggregate and filter rings in a clean metal pan, Dry as specified above, Carefully fold the dried filter ring and stand it on the aggregate. Burn the filter ring by igniting with a bunsen burner or match. Determine the mass of the extracted aggregate in the pan, Hyah Non. $—Sinve dry agseepate absorbs moisture when exposed (0 air containing moisture. determine the mass of the exteacied aggregate immediately after cooling to 2 suitable temperature. 11.6 Determine the amount of mineral matter in the extract by any of the following test methods: 1 Ashing Method: 1.1 Record the volume of the total extract in. the graduate (11.4). Determine the mass of an ignition dish Agitate the extract thoroughly and immediately measure approximately 100 mL. into the ignition dish, Evaporate to dryness on a steam bath or hot plate, except use a steam bath when the solvent is benzene. Ash residue at a dull red heat, (500 to 600°C), cool, and add 5 mL of saturated ammonium, carbonate solution per gram of ash. Digest at room temper- ature for | h. Dry in an oven at 100°C to constant mass, cool in a desiccator, and determine the mass 1.6.1.2 Calculate the mass of mineral matter in the total volume of extract, W, as follow: Wes GM, ~ Ya) 4 = volume after removing aliquot, mL. 11.6.2 Cenirifuge Method: 11.6.2.1 For this test method use any suitable high-speed (3000 g or higher) centrifuge of the continuous-flow type.* 11.6.2.2 Determine the mass of a clean empty centrifuge cup (or bowl) to 0.01 + 0.005 g and place in the centrifuge Position a container at the appropriate spout to catch the efMluent from the centrifuging operation. Transfer all of the extract (from Test Methods A, B, C, D, or E as appropriate) to an appropriate (feed) container suitably equipped with a feed control (valve or clamp, etc.). To ensure quantitative transfer of the extract to the feed container, the receptacle containing the extract should be washed several times with small amounts of clean solvent and the washings added to the feed container. Start the centrifuge and allow to reach 2 constant operational speed (for‘example, 9000 r/min for the SMM type and 20 000+ r/min for the Sharples type). Open the feed line and feed the extract into the centrifuge at a rate ~f 100 to 150 mL/min, After all the extract has passed crough the centrifuge, wash the feed mechanism (with -entrifuge still running) with several increments of clean solvent, allowing each increment to run through the ce Fuge until the eMMuent is essentially colorless. 11,6.2.3 Allow the centrifuge to stop and remove the cup {or bowl). Clean the outside with fresh solvent, Allow the residual solvent to evaporate in a funnel’or steam hood and then dry the container in an oven controlled at 230 + 9°F (110 * 5'C). Cool the container and redetermine the mass immediately. The increase in mass is the mass of mineral matter, Ws, (12.1) in the extract 11.6.3 Folumetric Method: 11.6.3.1 Place the extract in a previously tared and calibrated ask. Place the flask in a controlled-iemperature bath controlled to 0.2°F (0.1°C), and allow to come to the temperature at which the flask was calibrated. When the "The Shares Supereentnfage and the SMM continuourfiow ceninfuge have toon ound stable forth test method, 02172 desired temperature has been reached, fill the Mash wig solvent which has been kept at the same temperature. Brin, the level of the liquid in the flask up to the neck, insert ht stopper, making sure the liquid overflows the capillary, ang remove from the bath. Wipe the flask dry, determine the ‘mass to the nearest 0.1 g, and record this mass as the mass of ask plus extract. See Annex A? for a volumetric teg method alternative procedure if a controlled-temperatur bath is not used as prescribed herein, 11.6.3.2 Calculate the volume of asphalt and fines in the extract as follows: volume of asphalt and fines in the extract, volume of the flask, mass of the contents of the flask, mass of the asphalt and fines in the extract = mass of the total samples minus the mass of the extracted aggregate, and specific gravity of the solvent determined to the nearest 0.001 in accordance with Test Methods Dau. 41.6.3.3 Calculate the mass of fines in the extract a follows: My = K (My - Gh) where = mass of fines in the extract, specific gravity of fines as determined in accordance with Test Method C 128, = specific gravity of asphalts as determined in accor. dance with Test Method D 70, = as given in 11.6.3, 12. Calculation of Bitumen Content 12.1 Calculate the percent bitumen in the test portion as follows: Bitumen content, where: Ww, Wy wy We mass of test portion, mass of water in the test portion, mass of the extracted mineral aggregate, and, mass of the mineral matter in the extract. Nore 6—When ashies filter rings are not used, add the increase in mass of the felt filter ring to H's Note 7—For paving mistuies in which tr is used as the binder. 2 ‘modification of Test Method A is given in Annex A3, TEST METHOD B 13. Apparatus 13.1 In addition to the apparatus listed in Section 5, the following apparatus is required for Test Method B: 13.1.1 Extraction Apparatus, similar to that shown in Fig. “LBL Glass Jar, cylindrical, plain, made of heat-e 212oy FIG. 2 Extraction Apparatus (Test Method 6) ‘stant glass. The jar shall be free of cracks, scratches, or ther evidence of flaws that might cause breakage during heating. 13.1.1.2 Cylindrical Afetal Frames, one ot two, The lower frame shall have legs of sufficient length to support the frame, including the apex of the metal cone and paper cone liner above the solvent level. When two frames are used, the Upper frame shall have legs of sufficient length to support the ‘metal cone and paper cone liner at or above the top rim of the lower frame. The legs of the upper frame shall fit securely in the top rim of the lower frame. A bail handle may be Provided on the inside of the top rim of each frame for convenient handling. The metal used in fabricating the frames shall be essentially inactive to the solvents used in the ‘est method, 13.1.1.3 Condenser, fabricated with a truncated hemi- spherical condensing surface and a truncated conical top. Other suitable geometric shapes may also be used provided they accomplish the condensing and flow functions in- ba D272 tended. The material used in fabricating the condenser shall be esseutially urtreuctive to water and te the solvent used and shall be provided with suitable water inlet and outlet 13.114 Filter Paper, medium-grade, lastfitering. The diameter of the paper shall be such that when folded in accordance with the directions given belo. it shall come pletely line the metal cones in the frames. 13.115 dsbestos-Coaed Wire Mesh. approximately 3 ‘mim thick for use as insulation between the glass jar and hot plate. 13.1.1.6 Electric Hot Plate, Thermostatically: Controlled, of ‘sufficient dimensions and heat capacity to permit refluxing of the solvent as described in 15.2.5 14. Preparation of Test Portion 14.1 Prepare a test portion for moisture determination and extraction in accordance with the procedure described in Section 8. 15. Procedure 15.1 Moisture—Determine the moisture content of the mixture (see 8.2) in accordance with the test_method described in Section 9. 15.2. Extraction 15.2.1 Dry and determine the mass of one sheet of filter Paper for each frame to be used. Fold each paper on its diameter, fold the ends over, and spread it open to form a proper size to fit inside the metal cones. 15.2.2 Determine the mass of each frame with its filter Paper liner to the nearest 0.5 g. Record the mass, identifying each frame by number. 15.2.3 Place the test portion in the frame or frames. two frames are used, distribute the test portion approximately equally between the two. The top of the test portion must be below the upper edge of the paper liner. Determine the mass of cach loaded frame separately to the nearest 0.5 g, Again, record the mass. 15.2.4 Use one of the solvents specified in 6.3, 6.4, or 65. Pour the solvent into the glass cylinder and place the bottom frame into it, The solvent level should be below the apex of the one in the (lower) frame. If two frames are used, place the upper frame in the lower frame, fitting its legs into the holes in the upper rim of the lowes frame. Note 8—Sulficent denatured ethyl alcohol may be poured over the {est portion(s} 10 we the filter paper 15.2.5 Place the thermal insulating pad on the hot plate and then the cylinder on the pad. Cover the condenser. Circulate a gentle steady stream of cool water through the condenser, Adjust the temperature of the hot plate so that the solvent will boil gently and a steady stream of condessed~ solvent flows into the cone. If necessary, adjust the tempera ture of the hot plate to maintain the solvent stream at a rate necessary to keep the test portions in the cone(s) completely covered with condensed solvent. Take care not to allow condensed solvent to overflow the filter cone(s). Continue the refluxing until the solvent flowing from the lower cone is light straw cotor (when viewed against a white background). At this point, turn off the hot plate and allow the apparatus to cool with the water running in the condenser. When boiling has ceased and the cylinder is cool enough to handle. turn off the condenser and remove from the cylinder. 23ih 2172 15.2.6 Remove the frame assembly from the cylinder. Allow to dry in air (hood) and dry to constant mass in an oven at 230 + 9°F (110 + 5°C) (see Note 5). 15.2.7 Transfer the extract quantitatively to the graduated cylinder (5.5) and determine mineral matter in the extract in accordance with 11.6.1. Alternatively, mineral matter in the extract may be determined by the method described in 11.6.2 of 11.6.3, In this case. it is not necessary to transfer the extract from the extraction cylinder to a graduated cylinder. The extract may be transferred directly from the extraction (1.6.2.2) cylinder to the centrifuge feed container 16. Calculation of Bitumen Content 16.1 Calculate the percent bitumen in the test portion in accordance with the procedure described in Section 12, ‘TEST METHOD C 17. Apparatus 17.1 In addition to the apparatus listed in Section 5, the EXTRACTION KETTLE Stanoano ze-ot ALUMINUM UTENSIL oe ARF ‘TROWS oF Fins Fins staccenco ou attennare sorrou CONDENSING LID C FLANGE suPPORTS Fruren cuoT™ fescierl a [ J extraction aasKer FIG. 3 Extraction Apparatus (Test Method C) 214h wore STENCIL CLOTH FILTER 2000! 185 MESH BASKET consreu D272 SOUDENSINE Lip FINS TO 86 V2" 50. mit Wa" soucine Snecen ES inatve@nicte Bowes Lh Femme ome Vecavee’ SF Stee Nove—See Taole 3 for meine equivalents, FIG. 4 Extractor Unit (Test Method C) fotlowing is required for Test Method C: 17.1. Extraction Apparatus, consisting of a container, condenser lid, and stand. Suitable types are shown in Figs. 3 and 4; however, other extractors of differing shapes may also be used successfully. A standard 26-qt (25-L) aluminum cooking utensil has been found to be suitable. The important features regardless of shape are that the exiraciors have snug-fitting lids, be of sufficiently large size to accommodate the required test portion, and include cooling fins arranged 80 a5 1o provide for efficient refluxing, "7.1.2 Basket, for test portion as shown in Fig. 3 of one designed for use with an extractor of different shape. 1.1.3 Filter Clorh.® of approximately 185 mesh, placed over the No. 4 screen and shaped to cover the inside of the basket completely to ensure retention of all aggregate sizes greater than the cloth mesh during extraction. 18. Preparation of Test Portions 18.1. Prepare test portions for moisture determination and * A I6XX Swiss Stencil Cloth sala fom the Alls Silk Sercen Supa Co, 113) Sisautce Ave. Chiasn IL 6!” 1 ssh fr tht pope 215ah extraction in accordance with the procedure deveribed in Section 8, 19. Procedure 19.1 Moisture—Determine the moisture content of the mixture (see 8.2) in accordance with the test method described in Section 9. 19.2 Extraction: 19.2.1 Determine the mass of the sample (3500 to 10 000 2) in the red basket assembly to the nearest | g and plac the extractor. Pour 1150 to 1250 mL of trichloroethylene, 1,1,1-trichloroethane, or methylene chloride (Section 6) over the test portion. Fit the extractor lid tightly in place and allow water to circulate freely in the top. Apply heat from. either a gas burner or an electric hot plate. 19.2.2 Reflux the sample 1.5 to 3h until all bitumen is extracted from the aggregate. Shut down the extractor after 1.5 hand inspect the test portion. Mix the test portion with a trowel and continue extraction to completion. Nore 9—The test portion is completely extracted when. upon spection, no discoloration is found on the aggregate oF on the surface Fa trowel that has thoroughly mised the text portion, 19.2.3 Remove the basket with the test portion, dry in air and then to constant mass on a hot plate or in an oven at 230 + 9°F (110 * 5°C), 19.2.4 Drain the extract from the extractor and wash clean, with fresh solvent. Combine the extract and the washings in a graduated cylinder. 19.2.5 Determine the mass of mineral matier in the extract in accordance with the test method described in U.6.1, 11.6.2, oF 11 20. Calculation of Bitumen Content 20.1 Calculate the percent bitumen in the test portion in accordance with the procedure described in Section 12. Nore—See Table 3 for mete eaunakenis FIG. 5 Extractor Unit (Test Method 0) 02172 TEST METHOD ty 21. Apparatus 21.1 In aduition to the apparatus fisted in Scott 5. following apparatus is required for Test Method D: 7 ALLA Extraction apparatus. Fig. 3. consisting of ay extraction Kettle of metal or borosilicate glass. fitted wig” perforated basket and a condenser top. The underside of condenser shall be covered with numerous rounded knobs, distribute the condensed solvent uniformly over the surge of the sample. The suspension of the basket shall be arn to support the basket Ys in. (12.7 mm) above the bottom of the kettle, for immersion of test portion in the solvent, ang least 3 in. (76.5 mm) above the bottom of the ketle fr refluxing (see Note 4) 21.1.2 Cloth Filter Sack the basket. with an elastic hem for lining 22. Preparation of Test Portions 22.1. Prepare test portions for moisture determination ang extraction in accordance with the procedure described ig Section 8. 23. Procedure 23.1 Moisture—Determine the moisture content of the mixtures (see 8.2) in accordance with the test method described in Section 9. 23.2: Exiraction 23.2.1 Insert a filter sack in the extraction basket and determine the mass with the tare pan to determine the total tare weight. Place the test portion (Note 2) in the filter sack and determine the total mass. Calculate the mass of the tex portion. 23.2.2 Attach the suspension rod to the loaded basket and set the assembly into the extraction kettle. Pour appro mately 600 mL of solvent (6.2, 6.3. or 6.4) over the test portion. Set the condenser cover in place on the keitle Provide a flow of cold water through the condenser lid. Raise lla: 0 ee. 216 SMBRAR TAISS SAS SPAS MWqh vate ahrough the upper hole of the suspension rod. Place the boiling which might wash fines over sides of basket. 23.2.3 Continue heating with the test portion in immer- sion position for 15 to 30 min and then raise the basket to refluxing level. Increase the heat and maintain active boiling until solvent dripping from the basket appears light straw color when viewed against a white background. If a stainless steel Kettle is used, lift out the basket and the condenser cover assembly for examination of the solvent, 23.2.4 Remove the extractor from the hot plate and allow to. cool for several minutes. Lift out the basket and condenser assembly. Cover the kettle, remove the filter sack, distribute its contents onto the tared pan in which the mass of the test portion was originally determined. Place the filter sack on top of the recovered aggregate. Dry on a steam bath and then in an oven at 230 + 9°F (110 + 5°C) to constant mass. Transfer the extraction to a 1000-mL graduate. Wash the extractor clean with solvent and add the washings to the ves 23.2.5 Determine the mineral matter in the extract in accordance with any of the procedures in 11.6. 24. Calculation of Bitumen Content 24.1 Calculate the percent bitumen in the test portion in accordance with the procedure described in Section 12, ‘TEST METHOD E 25. Apparatus 25.1 In addition to the apparatus listed in Section 5, the following apparatus is required for Test Method E: 25.1.1 Vacuum Extractor. complete with the vacuum pump, gasket, rubber tubing. filer paper, support plate, and funnel ring, similar to that shown in Fig. 6 25.1.2 Filter Paper, medium-grade. fast-filtering, 330 mm in diameter. 25:43 Stainless Steel Beaker, having a capacity of 9 qt 65). 25.1.4 Erlenmeyer Flasks, 10 mL each. 45.1.5 Graduate, glass, having a capacity of 500 mL. 25.1.6 Wash Boule, plastic. having a capacity of $00 mL. 25.1.7 Dial Theemometer. having a range from 50 10 180°F (10 to 82°C), 25.1.8 Mixing Spaon, 12 in. (305 mm) long. 25.1.9 Spatula. 9 in. (229 mm) long. 25.1.10 Suff Brisiled Brush, 1 in, (25 mm) wide, 25.1.11 Erlenmeyer Flask. glass, having a capacity of 1000 mt. 251.12 Warch Glass, having a 4-in. (102-mm) diameter. 25.1413 Metal Tongs. 6 t0 8 in. (152 to 203 mm) long, Nore 10—Use apparatus and matenals listed under 25.111. 38.112, 28.143, and 26.1.2 only with paving mixtures hard 10 Titer. as in Method EL slass, two, having a capacity of 26. Reagents and Materials 26.1 Diatomaceous Silica Filtering ud conforming to 27 Type 8 of Specification b 60: Zed lt Ueto, be 26.3 Methylene Chloride. 27. Preparation of Test Portions 27.1 Prepare test portions for moisture determination and extraction in accordance with the procedure described in Section 8, 28. Procedure 28.1 Moisture—Determine the moisture content of the mixture (see 8.2) in accordance with the test_ method described in Section 9, 28.2 Extraction 28.2.1 Place the extraction test portion into the tared stainless steel beaker and determine the mass, 28.2.2 If the test portion is above 130°F (54°C), allow it to cool to @ temperature less than 130°F (54°C). When suffi. ciently cool, pour 200 mL of denatured alcohol over the specimen. Add approximately 700 mL of methylene chloride and stir until the asphalt is visually in solution. Nore 11—Ifequipment is available. an ultrasonic cleaning tank may be used instead of the beaker (28.2.1) and the bitumen brought into Solution (28.2.2) in the cleaning apparatus, TEST METHOD E41 28.2.3 Place a dry tared filter paper on the vacuum extractor, taking care to center the filter, and tighten the wing ‘huts finger tight, 28.24 Stan the vacuum pump and decamt the solvent from the beaker into the extractor. taking care not to transfer the agg‘egate from the beaker to the extractor. Stop the vacuum when all solvent has been removed. 28.2.5 “Add another 700 mL of methylene chloride to the sample container and stir. 28.2.6 Repeat 28.2.4 and 28.2.5 until the solution is a light straw color and the aggregate is visually clean. Afier the last wash, gently pour the entire sample into the extractor and thoroughly rinse all aggregate particles from the sample container. Carefully spread the aggregate evenly over the filter. 28.2.7 Operate the vacuum pump for a few minutes after the last wash to aid in drying the test portion. Scrape the aggregate away from the side of the funnel ring toward the center of the filter to avoid loss when the ring is removed. Remove the ring and brush the clinging aggregate into the drying pan. Then pick up the filter paper and aggregate by holding the paper on opposite sides and raising it straight up, Place the test portion in the tared pan and brush the clinging aggregate from the filter into the pan - 28.2.8 Dry the extracted aggregate and filter to a constant mass in an oven at 230 * 9°F (110 + 5°C) 28.2.9 Determine the mass of the filter and aggregate in the pan and record. Subtract the mass of the filter and pan to determine the mass of the extracted aggregate. 28.2.10 Transfer the extract to the graduated cylinder (5.5) and determine the mineral matter in the exteact in accordance with the test method deseribed in 11.6.1, Alter: te 110. manutacured ty Johse-Manuile bas Ken found wratacton forhb v 2172 SA6°Grooee top 12" 10x U4" eoprene “0 ring. 3/8" ott a win weeuum 9896 Sea Fates Seiiea te Eircien 122! PLAN—Tonk 20 gage sheet metel 12 316" dio — Fitter Support t soae Slope 8"ing 174 SS stoss end point enteoct_J Pube Sint ‘ge0e be = F|-peain, volved PLAN ~ Funnel Ring, Berlorated Filter Suppart ‘Tonk ond Funnel Ring ore febricated trom sheet aluminum Funnel Ring Support 4 DETAIL~ Ring seol, with Fiiter Support ond Funnel emer Ring'in place. ELEVATION Tont, Filter Support, Funnel Ring ore—The deta, mensions and materiale show have been fous saistactory. Madiicalons are perms, proved can be demonstrated tal performance te equipment is nol adversely afected FIG. 6 Vacuum Extractor (Test Method E) natively, mineral matter in the extract may be determined in accordance with the test method described in 11.6.2 or 11.6.3. In this case, it is not necessary to transfer the extract, to the graduated cylinder. The extract may be transferred directly from the extractor to the centrifuge feed container (1.6.22). Nore 12—Sections 28.2.10 and 28.2.16 may be omitted when this test method is used only for conteol of paving minture bitumen content uring construction (plant contra) 218 TEST METHOD E-ll 28.2.11 To extract a slow-filtering paving mixture eff ciently. prepare the test portion as in 28.2.1 and 28.2.2. 28.2.12 Place a dry tared filter paper on the vacuum extractor, taking care to center the filter, and tighten the wing nuts finger tight 28.2.13 Weigh 50 g of oven-dried diatomaceous silica filtering aid into a 100-mL Erlenmeyer ask and add $00 mL.ietit run until the pad formed by the diatomaceous silica B08 face ry and begins to crack slight F5g2.15 Place the watch glass in the extractor and gently gar the solvent from the test portion over it. Remove it with ‘and wash with the wash bottle, Add the rest of the ple and proceed as in 28.2.4 through 28.2.9. Subtract the of the drying pan, filter paper, and diatomaceous silica the total mass to determine the (dry) mass of aggregate. 982.16 Determine the amount of mineral matter in the in accordance with the procedure described in 58.210 (see Note 12). 14g, Calculation of Bitumen’ Content (Applicable to Both Method E-I and Method E-11) 29.1 Calculate the percent bitumen in the test portion in accordance with the procedure described in Section 12. (30. Precision and Bias 30.1 Mixtures with Aggregate Water Absorption Capaci- ties of Less than 1.25 % (Note 13) hh p22 ot me ee on 194 henge INS, Awa cements eal sees mmtely in suspension : 0 ACIS ACO, ARN srg Immediately pour the diatomaceous silica and ides elol ACME ACTS. AC-20, AR-ZOO0, ARAN. and 2 © over the Filter, Start the vacuom vary ARUN, Gralaions consistently hd 3 nomiaal marcus secon ethylene chloride over the filter. Start th PEM size wf at must “sn, stone. Walee absorption eapuelis sere coms tently below 1.28% Nore 14—A statistical evaluation showed no difference in precision between various solvents. Therefore the precision statement for cach test ‘method includes data obtained using any of the following solvents: benzene, tichloroethane,trichloroethylene, methylene chloride, 30.2 Mixtures with Aggregate Water Absorption Capaci- ties Greater than 1.25 and Less than 2.5 %: 30.2.1 The precision and bias statements for aggregates with these properties are currently being developed, 30.3 Mixtures with Aggregate Water Absorption Capaci- ties Greater than 2.5 % (Notes 14 and 15), Acceptable Standard Range of Two ton, % Test Resuls, %, Test and Type Index (ers Single-operator precision Method A (centrifuge) oss 156 Method B (reflux) 020 ast Mattilaboratory precision Method A (centrifuge) oss 186 Method B (reflux) 031 088 ‘These numbers represent, respectively, the (1s) and (4255) limits as described in Practice C 676. Accepiable Note 15—These precision statements are based on 1 material Standard, Range of Two (agsregate water absorption capacity preter that 25%, 7 replicas and Deviation. Tes Results laboratories. A gradation with Yein. maximuc site stone was used Test and Type Index cay (dsp Nore 16—The precision and bias statement for asphalt content of ‘Sagh-opertor precision (Note 15) mixtures having aggrepate with absorption greater than 23% was Method A (centrifuge) 02 059 developed using the test results from 5 laboratories, This is less than the Method B, C. and D (reflux) 019 0s 10 laboratories recommended by ASTM. Method (vacuum) ox 039 Mlilaboratory precision (Note 15) Method A (centiuge) on 062 Method 8, C, and D (reftux) 023 0.65 Method E (vacuum) . 022 059 4iThese numbers eepeesent, respectively the (15%) and (623%) limits ‘AASHTO Materials Reference Laboratory (AMRL} National Institute of ‘as descrbed in Practice C 670, ‘Standards and Technology (NISTI. Gathersburg, MD X ANNEXES: (Mandatory Information) AI. Test Method A Alternative Procedure ALI tn 11.2 place a 650 to 2500-g test portion in a bow! that has been previously dried to a constant mass with the Alter ting AL In 11.5 instead of removing the filter ring from the A2t Instead of using a controlled-temperature bath as Prescribed in 1.6.3.1, measure the temperature of the 29 bowl and drying in air. dry the bow! with the filter ring to a Constant mass under an infrared lamp or in an oven at 230 + STF (110 + 5°) A2, Test Method A (Volumetric Method) Alternative Procedure extract and make necessary corrections to the volume of the Mask and density of asphalt and the solventMh o 2172 |A3. Test Method A Modification for Determination of Tar A3.1 Cover the test portion in the bowl with erystal-free eosote and place the bow! for 1h on a hot plate or in an ywen maintained at 240°F (116°C). Proceed in accordance vith [1.3 and 11.4 except use two 200-mL additions of -osote previously heated to 240°F (116°C). Treat the test sortion in the bowl with three 200-mL additions of richloroethylene, following the same procedure. ‘Tha Amaccan Society for Testing ad Materials takes no postion espactng tha val of any patent rights asserted in conection wih any art maciioned in the standard, Users ofthis standard we expressly advised thet Getaminaton ofthe vali of any such patent rghs, and th nak of iningersont of Such rights, are anil ter own responsibilty. ‘This stander is subject to rvison at any tne by the respansiba technical commits and must be reviewed avery fva yous and trootrevsed, otha reapproved or witcrawn Your comments ere ito otha or revise of ths stancard for econ standards tnd should be addressed f0 ASTM Headquators. Yaur comments wil fective caret consideration {echnical commen, which you may atond,H you lel Yat your comments have not received afar heerng you should make your ‘tows kon tothe ASTM Common on Standards, 1916 Race St. Phiaetpie, PA 19108. 43.2 Continue in accordance with 11.5 and 1.6.1 excep, evaporate the aliquot portion of the solvent (11.6.1) On the steam bath until trichloroethylene is removed. Then evap. rate the remaining solvent to dryness on 2 hot plate and ag, as directed in 11.6.1 'A3.3 Calculate the percent tar in the sample in acco, dance with Section 12. “tmocting of tho rasponsiie