CCIL / LA BORATORY INSPECTION INSPECTION CHECKLIST Standard Standard Test Method Method fo r Quantit Quantit ative Extractio Extractio n of Bitu men from Bit umino us Paving Paving Mixtures - ASTM D2172/D2172M-11
APPA RATUS RATU S
1. Ovens / Clause 5.1: Maintains the temperature at 110 ± 5.0°C (230 ± 10.0°F) ………… ____ 2. Balance / Clause 5.3: Accurate to at least 0.01 % of the sample mass …………………… …………………… ____ 3. Hot Plate / Clause 5.4: Electric, 700-W continuous or low, medium, and high settings …. ____ 4. Small-Mouth Graduate Graduate / Clause 5.5: 1000 or 2000 mL capacity – See See Clause 5.5 for optional ………………………………………… ………………………………………………. ……. ____ 5. Ignition Dish / Clause 5.6 ………………………………………………………………………... ………………………………………………………………………... ____ 6. Desiccator / Clause 5.7 ……………………………………… ………………………………………………………………………….. ………………………………….. ____ ____ 7. Analytical Balance / Clause 5.8 …………………………………………… …………………………………………………………………. …………………….____ 8. Extraction Apparatus (Test Method A) / Section 10.0 + -
Extraction Bowl (See Fig. 1 / Pg 3) + apparatus capable of revolving bowl at variable controlled speeds up to 3600 r/min. …………………. …………………. ____ Container to catch solvent flowing from bowl …………………………….. ____ Filter Rings (felt or paper) ……………………………………… …………………………………………………... …………...____ or Low-ash paper filter rings as specified in clause 10.1.3 ………………… ____
Heat-resistant Glass jar (cylindrical, plain) ……………………………….. ____ Cylindrical Metal frames (1 or 2) as per clause 13.1.1.2 13.1.1.2 ……………….. ____ Condenser: fabricated with a truncated hemispherical condensing surface and a truncated conical top with a suitable water inlet and outlet (refer to clause 13.1.1.3 for further details) ………………………………. ____ Filter Paper (medium grade, fast-filtering) / clause 13.1.1.4 …………… ____ Baffle (heat resistant-coated wire mesh) approximately 3 mm thick to be used as insulation between glass jar and hot plate ………………….. ____ Electric Hot Plate (Thermostatically Controlled) …………………………. ____ Further options
10. Extraction Apparatus (Test Method C) – Refer to Section 17.0 + f or details ……………. ____ 11. Extraction Apparatus (Test Method D) – Refer to Section 21.0 + f or details ……………. ____ 12. Extraction Apparatus (Test Method E) – Refer to Section 25.0 + for details ……………. ____
Page 2 Standard Test Method for Quantitative Extraction of Bitumen from Bituminous Paving Mixtures - ASTM D2172/D2172M-11 APPA RATUS (co nt in ued )
12. High Speed Centrifuge: Continuous flow type (high-speed (3000 g or higher) ………….. ____ Note 1: Above used in 1 of 3 methods to determine the amount of mineral matter in the extract. REAGENTS / Clause 6.0
a. b. c. d.
Ammonium Carbonate Solution [(NH4)2CO3] ……………………………………… ____ Methylene Chloride, technical grade …………………………………………………____ Normal-Propyl Bromide (nPB) ………………………………………………………. ____ Trichloroethylene, technical grade, Type 1 ………………………………………….____ Note 2: Refer to Clause 6.1 for Purity of Reagents. Note 3: Refer to clause 7.0 (Hazards) for cautionary note.
SAMPLING / Clause 8.0
a.
Samples obtained in accordance with Practice D979? …………………………… ____
SAMPLE PREPARATION / Clause 8.2
a.
Sample unworkable – place sample in a large, flat pan and heat to 110 ± 5.0°C (230 ± 10.0°F) until warm enough to be mixed? ………………………………….. ____ b. Split or quartered (ASTM C702) the material to the required mass as specified in Table 1? …………………………………………………………………………….. ____ c. Moisture sample obtained from remaining mixture? ……………………………… ____ d. Moisture content determined in accordance with clause 9.0? …………………… ____ Note 4: Specimen can be dried to a constant mass in oven at 110 ± 5.0°C (230 ± 10.0°F) if recovery of AC from solution (obtained from extraction) is not required – Procedure for moisture content can be omitted. Table 1
Nominal Maximum Size of Aggregate - mm 4.75 mm 9.5 mm 12.5 mm 19.0 mm 25.0 mm 37.5 mm
Sieve Size
Minimum of Test Sample - Kg
4.75mm 9.5 mm 12.5 mm 19.0 mm 25.0 mm 37.5 mm
0.5 Kg 1.0 1.5 2.0 3.0 4.0
Page 3 Standard Test Method fo r Quantit ative Extractio n of Bitu men from Bit umino us Paving Mixtures - ASTM D2172/D2172M-11
PROCEDURE (Phase 1) Test Method “ A” using Tric hlorethyl ene / Clause 11.0
a. Placed test sample into extraction bowl? …………………………………………… ____ b. Bowl containing test sample placed into extraction apparatus (centrifuge)? …… ____ c. Covered test sample with trichloroethylene? ………………………………………. ____ d. Allow sufficient soaking time for solvent to disintegrate material (not to exceed 1 hour)? ………………………………………………………………………………… ____ e. Place filter ring (dried and weighed) around rim of bowl? ………………………… ____ f. Tightly clamped cover on the bowl – set up beaker to collect the extract? …….. ____ g. Slowly start centrifuge – speed gradually increased to a maximum of 3600 r/min or until solvent ceases to flow from drain? ………………………………………… ____ h. Centrifuge stopped? …………………………………………………………………. ____ i. Add an additional 200 mL of solvent to sample and repeat procedure? ………. ____ j. Procedure repeated with an additional 200 mL of solvent? ……………………… ____ k. Extract from centrifuge a straw colour – if not, repeat procedure until extract becomes a straw colour (not less than 3 soakings)? …………………………….. ____ l. Extract collected in a suitable container? ………………………………………….. ____ m. Centrifuge stopped / Remove Filter Rings as per clause 11.5? …………………. ____ n. Contents carefully removed from bowl and placed into a pan? …………………. ____ o. Sample dried on a steam bath and then dried to a constant mass in an oven or hot plate at 110 ± 5.0°C (230 ± 10.0°F)? ……………………………………….. ____ Note 4: Preliminary drying on steam bath may be omitted if trichloroethylene or Propyl Bromide is used as a sol vent. p.
Determined the amount of mineral extract using 1 of 3 methods: As hen ; Centrifuge; or Volumetric Method ? ……………………………………………… ____
Test Method “ B” using Trich lorethyl ene / Clause 15.0
a. Determined moisture content of mixture in accordance with clause 8.2 & 9.0? ____ b. Determined mass of each filter paper for each frame used and fold in accordance with clause 15.2.1? …………………………………………………………………… ____ c. Determined mass of each numbered frame with its filter paper to the nearest 0.5 gm and record? …………………………………………………………………… ____ d. Test sample placed in frame or proportionately into 2 frames with the top of the sample below the upper edge of the paper liner? ………………………………… ____ e. Weigh and record the mass of each loaded frame separately to the nearest 0.5 gm? ………………………………………………………………………………… ____ f. Pour solvent into glass cylinder and set frame inside cylinder with solvent below apex of frame. Upper frame, if required is pl aced on lower frame as specified in clause 15.2.4? ……………………………………………………………____ g. Place cylinder on hot plate with an insulting pad inserted between them? ……. ____ h. Cover condenser and begin circulating a steady stream of cool water through condenser? ……………………………………………………………………………. ____
Page 4 Standard Test Method fo r Quantit ative Extractio n of Bitu men from Bit umino us Paving Mixtures - ASTM D2172/D2172M-11 Test Method “ B” (continued)
i.
Hot plate adjusted to allow the solvent to boil gently and to maintain the solvent stream at a rate necessary to keep m aterial in cone(s) completely covered with condensed solvent? ………………………………………………………………….. ____ j. Reflux continued until solvent becomes a light straw colour? …………………… ____ k. Hot plate turned off allowing apparatus to cool down with water still running in condenser? ……………………………………………………………………………. ____ l. Boiling stopped and cylindered has cooled - condenser turned off and removed from cylinder? ………………………………………………………………………… ____ m. Frame assembly removed from cylinder to be air dried and then oven dried at a constant mass 110 ± 5.0°C (230 ± 10.0°F)? ………………………………………. ____ n. Determined mass at a suitable temperature to prevent moisture absorption? … ____ o. Determined the amount of mineral extract using 1 of 3 methods: As hen ; Centrifuge; or Volumetric Method ? ……………………………………………… ____ Note 5: Methylene Chloride or Normal-Propyl Bromide (nPB) can be used as a substitute for Trichlorethylene (clause 15.2.4).
Note 6: Addi ti on al Tes t M eth od s c an b e fo un d i n ASTM D2172: Sect io n 17; 21; 25; and 28.
PROCEDURE (Phase 2) Determination of Amo unt o f Mineral Matter in Extr act (3 Methods )
a. Determined mass of clean centrifuge cup to 0.01 ± 0.005 g - place in centrifuge? …………….…………………………………………………………………………….. ____ b. Transfer effluent to feed container equipped with a feed control valve? ……….. ____ c. Start centrifuge until operational speed obtained – open control valve to allow effluent to flow at a rate of 100 t o 150 mL/min.? ………………………………….. ____ d. Wash feed mechanism with solvent after all the effluent has passed through the Centrifuge – effluent should be colourless? ……………………………………….. ____ e. Stop centrifuge and remove cup? …………………………………………………… ____ f. Dry cup in oven at 110 ± 5.0°C (230 ± 10.0°F)? ………………………………….. ____ g. Allow cup to cool - determine mass immediately to prevent moisture absorption ____ CALCULATIONS
a. In accordance with ASTM D2172-05? ……………………………………………… ____
