Standard Method of Test for Quantitative Extraction of Bitumen from Bituminous Paving Mixtures 1. SCOPE LA These methods cover the quanti- tative determination of bitumen in hot mixed paving mixtures and pavement samples. Aggregate obtained by these methods may be used for sieve analysis using T 30. 1.2 The values stated in SI unit to be regarded as the standard 1.3 This standard may involve haz ardous materials, operations, and equip- ment. This standard does not. purport to address all of the safety problems associated with its use, It isthe responsi bility oF the user of this standard to establish appropriate safery and health practices and determine the applicability Of regulatory limitations prior to use Specific hazards are given in Section 7 NOTE 1—The results obianed by these methods may be affected by the age of the material teste, with older samples tending (0 yield slighty lower bitumen content. Best (quanitative results are obtained when the test Js made on mixtures and pavements shortly after their preparation is difficult to remove all the asphalt when some aggregates are used and some solvent may main within the minceal matter afecting the measured siphalt conten 2. REFERENCED DOCUMENTS 2A AASHTO Standards: T 30 Mechanical Analysis of Extracted Aggre- ate T44 Solubility of Bitumi- Rous Materials T 84 Specific Gravity and Absorption of Fine Aggregate This method simile to ASTD 2172.85 302 AASHTO DESIGNATION: T 164-94! (ASTM DESIGNATION: D 2172-88) T 110 Moisture oF Volatile Distillates in Bitua- nous Paving Mixtures ‘Sampling Bituminous Paving Mixtures Recovery of Asphalt from Solution by Ab- son Method Specific Gravity of Semi-Solid Bitumi- nous Materials Reducing Field Sam- ples of Aggregates to Testing Size ASTM Standarde: C670 Recommended Prac tive for Preparing Precision Statements for Test Methods for Construction Materi- als (Annual Book of ASTM Standards, Vol. 04.03) Specification for Dia temaceous Silica Pigment (Anaual Book of ASTM Stan- dards, Vol. 06.02) D 2111 Test for Specific Gravity of Haloge- nated Organic Sol vents and their Ad- mixtures (Annual Book of ASTM Stan. ards Part 30) Federal Specifications T 6s T 170 T 228 T 20g, 22 D 608 23 OT (atest revision) 1.1, 620 Trichloroethane, Technical (Inhibited Methyl Chloroform) OT (latest) Trichloroeth- 634 ylene, Technical (available from Naval Publications and Forms Center, $801 Tabor Ave., Philadel hia, PA 19120) 3. SUMMARY OF TEST METHODS. mixture is extracted with ichloroethylene, 1,1, L-trichloro- ethane, or methylene chloride, using the extraction equipment applicable to the ppanicular method, The bitumen content is calculated by differences from the -mass ofthe extracted agerezate, moisture content, and mineral marterin the extract The bitumen content is expressed as mass percent of moisture-free mixtures SIGNIFICANCE AND USE 4.1 All of the methods can be used for quantitative determinations of bitue men in hot-nixed paving mixtures and pavement samples for specification ac ceptance, service evaluation, control. and research. Each method prescribes the sol- vent or solvents and any other reagents that can be used in the method. Method T 170 requires that Method A or E (NOTE 2) and reagent grade trichloro- ethylene be used when asphalt is recov- cred from solution. NOTE 2—The vacuum extractor, Section 25.1.1, can be modified by 2 vacuum tap tached to the top of the “end point sight tube to collect the extract toa recoveries (Figure 65) APPARATUS, Sl_Oven, capable of maintaining the temperature at 110 * 5°C 230 * 9°F, 5.2 Pan, flat. of appropriate size to ‘warm test specimens. 5.3 Balances or scales and masses ‘meeting the requirements of M231 shallT 164 METHODS OF SAMPLING AND TESTING 303, TABLE OSHA Limits for Air Contaminants, ppm 29 CFR Ch, XVH See. 1910.1000 conform to the mass requitement shown (G-1-91 Edition) in Table 2 (NOTE 4) Solvent Twa TEL” CEILING PEAK me NOTE 4 When the mass of the test spec: \uLtTrehorostane os my i a men exceeds the capacity ofthe equipment ‘Tichloroedhylene 7 ae) 7 a used (Vora particular method, he tes specie Methylene Chloride soo = 1.000 2.000 be provided as appropriate for the sam: ple mass, 54 Hor plate, electric, with adjust able heating rate 33° Cylinders, graduated, 1000 or 2000-ml- capacity. Optional cylinder, 100-m. capacity 5.6 Ignition dish, at least 125-ml. ‘minimum capacity. 5.7 Desiccator. 6. REAGENT 6.1 Ammonium Carbonate Solu- tion Saturated solution of reagent grade ammonium carbonate ((NH).CO;). 6.2 Methylene Chloride, technical sgrade. Caution, see Section 7 T.1.1-Trichtoroethane, conform- ing to Federal Specification 0-T-620 (lat est revision). Caution, see Section 7, 6 Trichloroethylene, reagent grade (NOTE 3) or technical grade Type 1 Federal Specification 0-T-634, latest re- vision. Caution, see Seetion 7. NOTE 3Reagent grade Trichloroethy- ‘ene may be requited when asphalt i recovered from the solution (See T 170, Note 1) 7. PRECAUTIONS. 7.1. The solvents listed in Section 6 should be used only under a hood oF with an effective surface exhaust system in well-ventilated agea, since they are all toxic to some degree as indicated in Table 1 7.2. Trichloroethylene and 1,1.1-Tri chloroethane in the presence of heat and ‘moisture may form acids that are ex: tremely corrosive to certain metals, par= ticularly when subject to contact over lengthy periods of time. Proper precau- tions should be taken to not allow these two solvents to remain in small quantities jn the effluent tanks of aluminum va 7.3. Trichloroethylene when stored in 8 steel container and in continuous con- tact with moisture may decompose by ddehydrohalogenation to form unsaturated hydrocarbon liquids and hydrogen chlo- ride. Steel drums containing tichloroeth ylene should be stored in a cool, dry location, kept tightly sealed and opened a8 infrequently as possible. Trichloroeth- yylene should be transferred from the ‘drums to clean, dry brown glass bottles for laboratory use. ‘The hydrogen chlo- Tide in decomposed trichloroethylene ‘may harden an asphalt during the extrac- tion and Abson recovery test (TF 170), 8. SAMPLING 8.1 Obtain samples in. accordance with Method T 168, 8.2 Proparation of Test Specimens: 821 If the mixture is not suffi ciently soft to separate with a spatula or trowel, place it in a large, flat pan and ‘warm in a 110 * S°C (230 = 9°F) oven only until it can be handled or separated, Split or quarter the material until the ‘mass of material required for testis ob- tained, 822 The size of the test sample shall be govemed by the nominal maxi- ‘mum aggregate size of the mixture and TABLE 2 Size of Sample Nominal Maximum Minimum Aggregate Sire aver ‘am inch Sample, ke ory a5 95 hin ' Bs hin bs 190 vin 2 250 Vin 3 men may be divided into stale increments, tested, and the ests appropsately combined for calculation of bitumen content (Section 2) 823. Unless the mixture sample is free of moisture (NOTE 6). atest speci- men is requited for the determination of moisture (Section 9) in the mixtures, ‘Take this test specimen from the re maining sample in the mixture immedi ately after obtaining the extraction test specimen. NOTE SIF the extraction test is only being performed to tecover bitumen from the ‘mixture and the percent bitumen s not being elermined. it 18 unnecessary to determine ‘the moisture content of the mixture 9. MOISTURE CONTENT. 9.1 When required, dotermine the moisture content of the mixture (see Sec- tion 8.2.3) in accordance with the proce: dure described in Method T 110, NOTE 61 recovery ofbiturnen from the solution obtained from the extraction test 15 ‘not required. the entire test specimen may be dried to constant mass in an oven at a temperature of 149-163°C (300-325°F) for 2 { 25 hours pros to extaction instead of determining the moistte content (Section 9). 9.2 Calculate the mass of water (W:, 12.1) in the extraction test portion by ‘multiplying mass percent water (9.1) by the mass of the extraction test portion 0, 12. ‘TEST METHOD A 10. APPARATUS. 10.1 In addition to the apparatus listed in Section 5, the following appara tus is required for Method A: 101A Extraction Apparatus, con sisting of @ bowl approximating that shown in Figure 1 and an apparatus in Which the bow! may be revolved at con504 METHODS OF SAMPLING AND TESTING T 164 TABLE Dimensional Equivalents trolled variable speeds up t0 3600 s/n Eee f ocean PP TET PGP eee speed may be controlled manually —= or with preset speed cone. The ap, ne Tatus should be provided with a container Is for atching Ue solvent town roe 2 the ov and dain for removing he 7 scent. The appre prferay Sa 2 be provided wth explosion pros fen 3 tures and installed int hood or an eff os lve surface exhaust system to provide > sentation. 33 127 NOTE 7—Similar apparatus of larger size 13 may be ed FA 1012 Fier Rings fel or paper a Ft he rim ofthe bow ea 1013" LowAsh Paper Fiter Rings a may be used in place of the fel flee os tng (Secon 10412). Such iter rn a3 shal consis of ow as iter paper sock ag 127 £003 mm (005 = Os a) 79 mm thick, ‘The nominal base weigh the 13m paper shall be 150 * 14 ke G30 + 30 Ib) for a ream (300 sheets, 635 by 965 ‘mm (25 by 38 in.) The ath content of ae i. { : \ PA FIGURE. 1 Extraction Unit Bow! (Method A)T 164 the paper should not exceed 0.2 percent (approximately 0.034 g per rin 1. PROCEDURE ILA Determine the moisture content of the material in accordance with Sec: tion 9. 12 Place the test portion into a bowl, See Annex Al for altemative pro- cedures to those prescribed herein and in Section 11.5. 13 Cover the test portion in the bowl with tichloroethylene, 1,1,1-ti- chloroethane or methylene chloride and allow sufficient time for the solvent disintegrate the test portion (not over | hous). Place the bowl containing the test Portion and the solvent in the extraction apparatus. Dry the filter ring toa constant mass in an oven at 110 = 5°C (230 FP) and fit it around the edge of the bowl. Clamp the cover on the bow! tightly and place an appropriate container under the drain to collect the extract M14 Start the centrifuge revolving slowly and gradually increase the speed toa maximum of 3600 r/min until solvent ceases t flow from the drain. Allow the machine 10 stop. add 200 mL (or more as appropriate for mass of sample) tc. chloroethylene, 1,1,L-trichloroethane oF ‘methylene chloride, and repeat the proce: dure. Use sufficient 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 ‘an appropriate container for mineral mat- ter determination, 115 Carefully transfer the filter ring and all of the aggreate in the certifuge owl into a tared metal pan, Dry in air under a hood until the fumes dissipate, and then to a constant mass in an oven ‘at 110 + 5°C (230 + 9°F) (Notes 7 and '8). The mass of the extracted aggregate (0) is equal to the mass of the contents in the pan minus the initial dry mass of the filter ring, NOTE 8—The fier and agaregate may be left inside the centrifuge bow! and dried fo constant mass in an oven at HO = $C (230 + 9°F) and the mase determined NOTE 9—The filter ring may be dried Separately to constant mass in an oven at 110 = S'C 230 * OF) provided that cue is taken not to lose any’ of the fine material clinging tothe filter If this procedure 1s used, METHODS OF SAMPLING AND TESTING the aggrepate may then he dred 10 constant macs eithe ian oven oF on 8 Rot plate at Ho = SC O30 = OF) ILS Use the following alternative procedure when low-ash filter rings are tused. 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 bbumer or mateh. Determine the mass of the extracted aggregate in the pan (W) NOTE 10—Since dey agerer moisture when exposed 10. ain contain moisture, determine the mass ofthe exact ageregate immediately after cooing (0 suit able temperature 16 Determine the amount of min- feral matter in the extract by any of the following test methods: TL61 Aching Method: 1.6.1.1 Determine the volume of the total extract (Section 11.4). Condition the ignition dish in furnace, e001 in a desicea tor, and determine the mass of the ignition dish (0 the nearest 0.001 2. Agitate the ‘extract thoroughly and immediately mea sure approximately 100 mi. into the i tion dish, Evaporate to dryness ona steam ‘bath or hot plate. Ash the residue at dall red heat (500-600°C) and cool. Determine the mass of the ash and add 5 mL of saturated ammonium carbonate solution per gram of ash, Digest at room tempera ture for I hour. Dry in an oven at 110 5°C to constant mass, coo) ina dessa. tot, and determine the mass to the nearest 0.001 g. 116.12 Calculate the mass of min- ‘ral matter in the total volume of extract (WW) as follows: We= GIMAY ~ Vo} Where: G = ashin aliquot, g, V, = total volume, mL, and VY: = volume after removing aliquot. mL. 11.62 Consrfuge Method: 1.6.2.1 For this method use any suitable highspeed (3000 r/min or higher) 305 centrifuge of the continuous-flow type.* 1.62.2 Determine the mass of @ clean empty cenuituge cup (or bowl) to 0.01 g and place in the centrifuge. Posi tion a container at the appropriate spout tocatch the effluent from the centiifuging ‘operation, ‘Transfer all of the extract (from Method A. B, C, D, or E as appro- priate) to an appropriate (feed) container suitably equipped with a feed control (valve or clamp, etc.). To ensure quantita tive 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 cootainer, Start the centrifuge and allow to reach a Constant operational speed (for example 9000 r/min for the SMM type and 20000 + r/min for the Sharples type). Open the feed line and feed the extract into the centifuge at a rate of 100 to 150 mL/ ‘min. After all the extract has passed through the centrifuge, wash the feed ‘mechanism (with centrifuge still running) ‘with several increments of clean solvent, allowing each increment to run through the centrifuge until the effluent is essen- tially colorless 11.6.2.3 Allow the centrifuge to stop and remove the cup (or bow), Clean the ‘outside with fresh solvent. Allow the re sidual solvent to evaporate ina funnel or steam hood and then dry the container in ‘an oven controlled at 110 = 5°C (230 = 9°F). Cool the container and redetermine the mass immediately. The increase in ‘mass is the mass of mineral matter W.. (12.1) in the extract. 116.3. Volumeirie Method, L631 Place the extract in a pre- viously tared and calibrated Mask, Place the flask in a controlled-temperature bath controlled to = O.1°C (+ 02°F), and allow to come tothe temperature at which the flask was calibrated. When the desired temperature has been reached, fill the ‘ask with solvent which has been kept atthe same temperature. Bring the level of the liquid in the flask up to the neck, insert the stopper, making sure the liquid overflows the capillary, and remove from, tie bath. Wipe the flask dry, determine the mass 0 the neavest 0.1 g, and record {his mass as the massof flask plus extrac.306 See Annex Al for a volumetric test ‘method alternative procedure if a con twolled-temperature bath is not used as prescribed herein, 1.6.3.2 Calculate the volume of as phalt and fines in the extract as follows (n= My) @ V, = volume of asphalt and fines in the extract, Volume of the flask, mass of the contents ofthe flask; ‘mass of the asphalt and fines ia the extract (or mass of the total samples minus the mass of the ex- tracted aggregate), and G,_ = specific gravity of the solvent de- termined to the nearest 0.001 in ‘accordance with ASTM D 2111 1.6.33 Calculate the mass of fines in the extract as follows: M. = Kish, - Gv) Where: mass of fines in the extract, specific gravity of fines as deter mined in accordance with T 84, G, = specific gravity of asphalts as de termined in accordance with T 228, K G G-G Vi = as given in Section 11.63.2, and ‘M, = as given in Section 11.632 12. CALCULATION OF BITUMEN CONTENT 121 Calculate the percent bitumen im the test portion as follows Bitumen conten, se = Wh = Wy = OW + Wy W. x “ loo Where Wy = mass of test portion, W, = mass of water in test portion, W, = mass of extracted mineral agere- ‘gate, and W, = mass of mineral matter in the ex tract METHODS OF SAMPLING AND TESTING NOTE 11—When ashlese filter ri ot used. ad the increase i mase of the NOTE 12—When it i desired 19 express, the bitumen content as a mass percent of the ‘moisture-free aggregate, substitute the mass WW. forthe mass W ~ W: inthe divisor ofthe equation in Section 12. TEST METHOD B 13, APPARATUS. 13.1 In addition to the apparatus listed in Section 5, the following appara- tus is required for Test Method B: IB.LL Extraction Apparatus, similar to that shown in Figure 2, IBAA Glass Jar cylindrical, plain, ‘made of heat-resistant glass. The jar shall, FIGURE 2 Extraction Apparatus (Method B} T 164 be free of cracks, scratches, or other evi dence of flaws that might cause breakage during heating 1B11.2 Cylindrical Metal Frames, fone of two, The lower frame shall have legs of sufficient length to suppor the frame, including the apex of the metal cone and paper cone liner above the sol- vent level. When two frames are used, the ‘upper frame shall have legs of sufficient length to suppor the metal cone and pa Per 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 frames shall be essentially unreactive tothe solvents used in the test IBLL3 Condenser, fabricated with 2 truncated hemispherical condensing surface and a truncated conical top. Other suitable geometric shapes may also be used provided they accomplish the con ensing and flow functions intended. The ‘material used in fabricating the condenser shall be essentially unreactive to water and to the solvent used and shall be pro: Vided with suitable water inlet and outlet. 1BL14 Filer Paper mediun grade, fast-filtering, The diameter of the paper shall be such that when folded in accordance with the directions given be- low, it shall completely tine the metal ‘cones in the frames, 13 Thermal Distributing Pro tective Pad. approximately 3 mm thick for use as insulation between the glass Jar and hot plates, 13.1.1.6 Electric Hot Plate, Thermo- statically Controlled of sufficient dimen sions and heat capacity to permit reflux. ing of the solvent as described in Sec tion 15.25, 14, PREPARATION OF TEST PORTION 14.1 Prepare a test portion for mois ture determination and extraction in ace ceordance with the procedure described in Section &U METHODS OF SAMPLING AND TESTING NOTE—See Table 3 or dmesso egies, Al dmensons a in mils uns owise note FIGURE 3. Extraction Apparatus (Method C) 15, PROCEDURE ASA Moisture: determine the moi ture content of the mixture (see Section 8.2) in accordance with the method de- senibed in Section 9. 18.2 Extraction, 15.2.1. Dry one sheet of filter paper for each frame used to a constant mass Jn an oven at 110 * $°C (230 = 9°F), Fold each paper on its diameter, fold the fends over, and spread it open to form 2 Proper size to fit inside the metal cones, 15.2.2 Determine the mass of each 307 frame with its filter paper liner to the nearest 0.5 g. Record the mass. identi fying each frame by number 15.2.3 Place the test portion in the frame or frames. If two frames are used, distribute the test portion approximately equally between the two. The top of the {est portion must be below the upper edge of the paper liner. Determine the ‘mass of each loaded frame separately to the nearest 0.5 g. Again, record the mass 15.24 Use one of the solvents (NOTE 13) specified in Sections 6.2. 6.3, or 64. Pour the solvent into the glass eylinder and place the bottom frame into it. The solvent level should be below the apex of the one inthe (lower) frame If two frames are used, place the upper frame in the lower frame, fting its legs into the holes in the upper rim of the Tower frame NOTE 13—Sufficient denatured ethyl al- «obo may’ be poured over the test portion(s) to wet the Ole pape. A mittee of 20 percent denatured alcohol and 80 percent LI. Lave chloroethane. oF ichloroethylene. has proven tw be a beter solvent for some S Place the thermal insulating pad if required on the hot plate and then the eylinder on the pad. Cover the condenser. Circulate a gentle steady stream of cool water through the con denser. Adjust the temperature of the hot plate so that the solvent will boil gently and a steady stream of condensed solvent flows into the cone, If necessary, adjust, the temperature of the hot plate to main- tain the solvent stream at arate necessary to Keep the test portions in the cone(s) completely covered with condensed sol- vent. 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 color (when viewed against a white background). At this point, tum off the hhot plate and allow the apparatus to cool ‘enough to handle, turn off the condenser and remove from the cylinder, 18.2.6 Remove the frame assembly from the cylinder. Allow to dry in air (hood) and dry to constant mass in an oven at 110 = 5°C (230 * °F) (see NOTE 9), 15.2.7 Determine the mineral matter308, METHODS OF SAMPLING AND TESTING ges spout 1ST above suPhOnt Posse SENG CLOFn DENSE 210 SUGGER FINS aL TeRWATE PRY A356 To Nave 19 f0WS OF Fins 12 0.4 How INE 7038 17 mn 59 WIE 5 an SCO aan Tam Soros Selsseciaay arene ‘UoUwo. FoR Dea cock use ‘OuSrAuC iON NOTE See Tle 3 for dimes equvaems All dscns ae mili ks tee nt in the extraction solution by one of the Procedures in Section 11.6, 16. CALCULATION OF BITUMEN CONTENT 16.1. Calculate the percentage of bit ‘men in the test portion in accordance with the procedure deseribed in Section 12, FIGURE 4 Extractor Unit (Method C) TEST METHOD C 17. APPARATUS 17.1 In addition to the apparatus listed an Section 5, the following is 1e- quired for Test Method C. VIAL Extraction Apparatus. con. sisting of a container, condenser ld, and stand, Suitable types are shown in ures 3 and 4; however, other extractors of different shapes may also be used successfully. A’ standard 25-L. (26-91) aluminum cooking utensil has been found to be suitable. The important fea tures regardless of the shape are that the ‘extractors have smug-fiting lids, be of sufficienly large size to accommodateT 16s the required test portion. and include cooling fins arranged so 2s to provide tor efficient refluxin 1712 Basker, for wst portion as shown in Figure 3 or one designed for use with an extractor of different shape. TTA. Filter cloth’, of approxi mately 185 mesh, placed over the 4.75- ‘mm (No. 4) sereen and shaped to cover the inside of the basket completely to ensure retention of all aggregate sizes eater than the cloth mesh during extrac 18, PREPARATION OF TEST PORTIONS 18.1 Prepare test portions for mois- tore determination and extraction in ac- ‘cordance with the procedure described in Section 8. 19, PROCEDURE 19.1 Moisture: determine the mois ture content of the mixture (see Section 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 10000 g) in the tared basket assembly to the nearest Ig and Place in the extractor. Pour 1150 t0 1250 ml of trichloroethylene, 1, 1, T-trichlo- roethane, or methylene chloride (Section ©) over the test portion. Fit the extractor lid tightly in place and allow water (0 circulate freely in the top. Apply heat from either @ gas bumer or an electric hot plate 19.2.2 Reflux the sample 15 t0 3 hours unti all bitumen is extracted from the aggregate. Shut down the extractor after 1.5 hours and inspect the test por tion, Mix the test portion with a trowel and continue extraction to completion. NOTE 14—the tet postion is completely ‘extracted when, upen inspection, no discolor ation is found on the aggregate or on the surface ofa towel that has thorou the test portion, ‘Chicago ers mS the porons METHODS OF SAMPLING AND TESTING 19.2.3 Remove the basket with the test portion, dry in air and then to con: Scant mass on a hot plate oF in an oven at 110 5°F (230 = 9F). 19.24 Drain the extract from the ex teactor and wash clean with fresh solvent. Combine the extract and the washings in a graduated cylinder, 19.25 Determine the mass of min. ‘ral matter in the extract solution by one Of the procedures in Section 11.6, 20. CALCULATION OF BITUMEN CONTENT 20.1 Calculate the percentage of bi tumen in the test portion in accordance with the procedure described in Sec- tion 12. TEST METHOD D 21. APPARATUS: 21.1 In addition to. the apparatus listed in Section 5. the following appara tus is required for Test Method D: 2A Extraction Apparatus, Figure 5. consisting of an extraction kettle of ‘metal or borosilicate glass, fited with @ perforated basket and a condenser top. ‘The underside of the condenser shall be covered with numerous rounded knobs to distribute the condenser solvent uni- formly over the surface of the sample ‘The suspension of the basket shall be arranged to support the basket 13 mm (Ch in.) above the bottom of the kettle, for immersion of test portion in the sol- vent, and at least 75 mm G in.) above he bottom of the kettle for refluxing (see NOTE 1). 21.1.2 Cloth Filter Sacks, with an clastic hem for lining the basket 22. PREPARATION OF TEST PORTIONS, 22.1. Prepare test portions for mois- tuxe determination and extraction in ac- cordance with the procedure described 309 23. PROCEDURE 23.1 Mouture: determine the mois- ture content of the mixtures (see Section 8.2) in accordance with the method de- scribed in Section 9, 22 Eviraction 23.2.1 Insert a filter sack in the ex- traction basket and determine the mass with the tare pan to determine the total tare mass. Place the test portion in the filter sack and determine the total mass Calculate the mass of the test 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 (Section 6.2, 6.3, of 6.4) over the test portion. Set the condenser cover in place on the kettle. Provide flow of cold water through the condenser lid. Raise the basket to immersion level, for example 13 mm. Cs im.) above the bottom of kettle, by the support pin tuo per hole of the suspens! ‘extractor on the bot plate and adjust the heating rate so that solvent is maintained ata genile boil, avoiding vigorous boil- ing which might wash fines aver sides of basket 23.2.3 Continue heating with the test portion in immersion pesition for 15 to 30 minutes and then raise the basket to refluxing level. Increase the heat and ‘maintain active boiling until solvent drip- Ping from the basket appears light straw color when viewed against a white back- ‘ground. Ifa stainless steel ketle is used, Tift out the basket and the condenser cover assembly for examination of the solvent 23.24 Remove the extractor from the hot plate and allow to cool for several ‘minutes. Lift out the basket and con- enser assembly. Cover the kettle, 1e- ‘move the filter sack, distribute its con- temts into the tazed’ 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 110 = SC 230 = 9F) to constant mass. Transfer the extract solution to a 1000- mL. graduate. Wash the extractor clean with solvent and add the washings to the extract solution, 23.2.5 Determine the mineral matter in the extract in accordance with any of the procedures in Section 11.6310 __] eal meron sawn StaNcest eTEEL Om ear sonosticare class METHODS OF SAMPLING AND TESTING s2DA ee Fan Sispenston Frersoq | Nz oa [NOTE Sse Table 3 for simenional equvalens All dimension ae in mils less oberwne sud 24. CALCULATION OF BITUMEN CONTENT 24.1 Calculate the percentage of bi- fumen in the test portion in accordance with the procedure described in. Sec tion 12 ‘TEST METHOD E 25. APPARATUS 25.41 In addition to the apparatus listed in Section 5, the following appara lus is required for Test Method E. 28.1 Vacuum Extractor, complete with the vacuum pump, gasket, rubber tubing, filter paper, support plate, and funnel ring, similar to that shown in Figure 6a, 6b, and 66, 28.1.2 Filler Paper, medium-grade, fascfitering, 330 mm in diameter 25.1.3 A sample container, 3.8 L (4 99) capacity or greater 1d Erlenmeyer Flasks, glass, ‘ovo, having a capacity of 4000 ml. each 254.5 Graduate, Glass, having aca pacity of 500 mL. 25.1.6 Wash Bottle, Plastic, having 2 capacity of 500 mL. 28.1.7 Dial Thermometer, having a ange from 10 to 82°C (50 to 180°F), 25.1.8 Mixing Spoor, approximately 300 mm (12 in.) tong 25.1.9 Spatula, approximately mam (9 in.) long, 0 FIGURES Extractor Unit (Method D) 25.110 SiffBristled Brush, approx- imately 25 mun (1 in.) wide, 2SAM Erlenmeyer Flask, hhaving a capacity of 1000 mL. 251.12 Warch Glass, having ap- Proximately a 100 mm (4 in.) diameter 2.1.13 "Metal Tongs, 130 to 200 mm (6 10 8 in) long, 25114 305mm (12-in,) Diameter 1.18-mm (No. 16) and 75-4m (No. 200) Sieves. (Optional) lass, NOTE 15—Use apparatus and matrils listed under Sections 25111, "25.112, 25.113, 26.1, and 262 only with paving mix tures hard to fier, asim Method E-11 26. REAGENTS AND MATERIALS: 26.1 Diatomaceous Silica Filtering Aig conforming to Type B of Specifica- tion ASTM D 608." 26.2 Ethyl Alcohol, denatured. (Op- tional). 26.3. Methylene Chloride 16). (ore, NOTE 16—Any of the solvents listed in [GE TO marae by Johnie, hs moe foes Section 6 may be substituted for methylene chloride 27. PREPARATION OF TEST PORTIONS 27.1 Prepare test portions for moi ‘re determination and extraction in ace cordance with the procedure described in Section 8, 28. PROCEDURE 28.1 Determine the moisture content of the mixture (see Section 8.2) in accor: dance with the method described in Section 9, 28.2 Extraction 28.2.1. Place the extraction test por- tion into the tared stainless steel beaker and determine the mass (NOTE 18). 28.2.2 If the test portion is above 54°C (130°F), allow it to cool to a term: Perature fess than 54°C (130°F), When sufficiently cool. pour 200 mL of dena. tured alcohol over the specimen (NOTE 17). Add approximately 700 mL. of methMETHODS OF SAMPLING AND TESTING (09 sect meal 5207 a Finer Sepoon Crone or S018 x84 Neogene “O° Ring ws NOTE I—wnen 2 more postive sei ‘eguved atthe tunnet ng, use a lates supe Bort which its inside the neoprene “Orne ‘wi tis alternate contiguraton 3 prove {© prowse separation of the liter supson rom the top surlace of tne tane is sicy ‘eevee to msure acequate sucton cunng NOTE 2—Fiter suoport plates tninner tnan 1324 may be usea wnen postive oro. sions are provioea to assure Separation ot the ster support slate anc ne lop te tank FIGURE 6a Vacuum Extractor312. METHODS OF SAMPLING AND TESTING c 09 nee metal 3207 dia Fitter Support 950. Sie: Tube Mote: A 9607 Exneeen ts Outnte NOTE dimensions we mili es here note FIGURE 6b Vacuum ExtractorT 164 rove (or 3088 6 Neoprene “O° Rig Puan i Finer 1 064 ELEVATION ~ Fitter Stand FIGURE 6b Vacuum Extractor—Continued ylene chloride and stir until the asphalt is visually in sotution (NOTE 18). NOTE 17—Use of the sleoho is optional. NOTE 18—1f equipment is avilable, an lurasonie cleaning tank may be used instead ‘ofthe beaker (Section 28.2.1) and the bitumen trough int solution (Section 282.2) in the cleaning apparatus, METHOD E-1 282.3. Dry the filter paper (more than one filter paper may be used) to Constant mass in an oven at 110 = SC (230 = 9°F), place the filter paper on the extractor taking care to center the filter paper and tighten the wing nuts finger tight (NOTE 19) erence has shown that if of the filter may be reduced by METHODS OF SAMPLING AND TESTING | 95 Bot Stona «solution through nested and 75-ym (No, 200) . When sieves are used, the solution will be decanted onto the 118 mm (No. 16) sieve instead ofthe filter 28.2.4 Start the vacuum and slowly ddecant extract solution from sample con- tainer onto the filter, When all solution hhas been removed from the filter paper, the vacuum may be stopped of left run 28.2.5 Cover the sample remaining in the container with methylene chlo ride, up to 700 mL. Stir gently until bitumen and aggregate fines appear to be im suspension (or start ultrasonic cleaner if used). Repeat Section 28.2.4 282.6 Repeat Section 28.2.5 until the solution is a light straw color and the aggregate is visually clean, Care fully transfer the clean aggregate from the container to the remaining a; zate on the filter. Wash any aj repate ELEVATION = Finer seaport 313 PLAN Furnet reg, showing. section of perlorotee (Some os shown on Fig 6a) forme ong (Some 0s snoun on Fig 60) 3 an toraye of clinging to the container onto the filter with methylene chloride. Operate the vacuum pump for a few minutes after the last wash to aid in drying the test portion. The solvent may be slowed for color observation by partially opening, the vacuum valve and reducing the vac tuum. 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, Also wash sides of funnel ring to remove any fines Stop vacuum and remove the ring and brush the clinging aggregate into the tared drying pan. Then pick up the filter paper and aggregate by holding the pa- er on opposite sides and raising it straight up. Transfer aggregate on filter paper to the tared drying pan and brus the clinging agaregate from the filter into the pan 28.2.7 Dry the extracted aggregate34 and filter t0 a constant mass in an oven at 110 + 5°C 230°F = 9°F) (NOTE 17), NOTE 20—See atemate procedure in Se ‘ion 11.5 when low ath filer paper is used Determine the mass ofthe fil regate in the pan and record, Subtract the mass of the filter and pan to determine the mass of the extracted 3 _sregate. 282.9 Determine the mineral matter in the extract solution by one of the Procedures in Section 11,6 (NOTE 20) NOTE 21—Sections 28.2.9 and 282.15 ray be omitted when this method is used ‘only for contol of paving mixture bitumen content during construction (plan conto} TEST METHOD F-II 282.10 To extract a slow-filtering Paving mixture efficiently, prepare the lest portion as in Sections 28.2.1 and 28.2 282.11 Dry the filter paper to con- Stant mass in an oven at 110 = 5° (230 = 9°F), place the filter paper on the extractor taking care to center the filter Paper and tighten the wing nuts finger ht (NOTE 18). 28.212 Weigh between 50 and 100 8 of oven-dried diatomaceous silica fi tering aid into a 1000 mL Erlenmeyer flask, record mass, then add 500. ml. of methylene chloride. Swirl until the iatomaceous silica is completely in sus. pension, 282.13 Immediately pour the diato- maceous silica and methylene chloride over the filter, Start the vacuum pump fand let it run until the pad formed by the diatomaceous silica is surface dry ‘and begins to erack slightly (NOTE 22) METHODS OF SAMPLING AND TESTING NOTE 22—Some diatomaceous silica may bbe washed thru the filer and included the mineral mater doteination of Section 282.15. Bank tests are recommended to de Ne the amount of diatomaceous sila, 'f any, Jost th the filter Am appropriate correction will be required ia the mineral 282.14 Place the watehglass in the extractor and slowly decant the solvent from the container over the watch glass (NOTE 23), Stop vacuum when all solu. tion has been removed from the filter Repeat asin Section 28.2.5 except decant solution onto watchglass. Complete pro- cedure as in Section 28.2.6 except te- _move watchglass with tongs prior to add ing remaining clean aggregate from the container. (Also wash watchglass with solvent to remove fines onto filer.) NOTE 23—When nested sieves are used ‘he watchglas may be omitted. 28.2.15 Determine the amovat of ‘mineral matter in the extract solution by fone of the porcedures in Section 11.6 (NOTE 20) 29, CALCULATION OF BITUMEN CONTENT (APPLICABLE TO BOTH METHOD E-1 AND. METHOD E-1), 29.1 Calculate the percentage of bi- tumen in the test portion in accordance With the procedure described in Sec- tion 12. T 164 30. PRECISION AND BIAS 30.1 The single-laboratory standard eviation has been found to be 0.18 per- cent (NOTE 24). Therefore, results of ‘wo properly conducted tests by the same operator on the same batch should not dliffer_by more than 0.52 percent (NOTE 25), 30.2 The multlaboratory standard deviation has been found to be 0.29 per- cent (NOTE 24). Therefore, the results of two properly conducted tests from two sifferent laboratories on samples from the same batch should not differ by more than 0.81 percent (NOTE 25) NOTE 24—These numbers represent r= spectively the (1S) and (D2S) limits a¢ de serited in Recommended Practice ASTM C 670, NOTE 25—These precision statements are based on one pair of reference samples with 59 laboratories participating and 3 Isborstory results deleted a5 outlying observations. The reference samples contained agsrepate with 98 percent passing the 9.5 mm (i in.) screen Alltest methods were used inthe inteslabora- ‘ory test program. ANNEX Al, TEST METHOD A (VOLUMETRIC METHOD) ALTERNATIVE PROCEDURE, AJL Instead of using a controlled temperature bath as prescribed in Section 11.63.1, measure the temperature of the extract and make necessary corrections {0 the volume of the flask and density of asphalt and the solvent