Quantitative Extraction of Bitumen from Bituminous Paving Mixture

Expt No. Date:

Aim
To perform a quantitative extraction of bitumen from hot mix asphalt pavement samples using
centrifuge method, in accordance with ASTM D2172. The aggregate quantity obtained thus, is
taken for sieving analysis.

Significance and use

This test procedure is used for specification acceptance, service evaluation and control.

Apparatus Required
1. Oven capable of maintaining temperature at 1105C.
2. Pan at least 300 mm long, 200 mm wide and 25 mm deep.
3. Balance accuracy of 0.01% of the sample mass.
4. Hot plate electric, 700W, continuous or low, medium or high.
5. Centrifuge Extraction apparatus consisting of bowl, with revolution speed up to 3600 rpm.
6. Filler rings to fit the rim of the bowl.
7. Filter papers.
8. Vacuum system.

Reagents - Benzene

Procedure

1. For this test method any suitable high speed 3600 rpm, centrifuge of the continuous flow type
is used.
2. Measured the weight of the empty bowl and filter papers before the start of the test.
3. Keep a compacted sample in oven for loosening it and spread it in tray.
4. Take the loosen sample into the bowl with filter paper placed inside the bowl and take total
weight of bowl and sample.
5. Place the bowl filled with mix inside the centrifugal apparatus.
6. Fill the bowl with Benzene until the reagent rises up to 2mm above the HMA mix in the
bowl. Make sure the HMA mix is entirely soaked in benzene. Close the bowl with a lid, with
a filter paper placed below the lid and keep it for next 20 minutes.
7. Now start the centrifuge apparatus and gradually increase the speed until the benzene start to
drain off and is simultaneously collected in a bottle. Note, the benzene will drain off to the
bottle with the bitumen and some filler particles. Hence the contents of the bottle should be
kept safe for further extraction.
8. Continue the rotation until all the benzene and bitumen comes out.
9. Repeat the same procedure for two more times, by again adding the benzene, keeping it for
next 15 minutes and rotating it each time.
10. Once the extraction is completed, keep the bowl with the extracted aggregates and filter
papers in the oven for 2 hours at 110oC, to evaporate all the benzene content from the
aggregate and filter paper.
11. Finally take the weight of the bowl with dry aggregate and dried filter paper. The decrease in
the final weight measurement indicate bitumen extracted. The aggregate thus obtained is
taken for sieving analysis.
12. Note that, the decrease in final weight alone cannot be taken as bitumen content, as there is
some amount of mineral matter present in the benzene mixture.

Mineral matter extraction

1. The mineral matter that is contained in the benzene mixture is further extracted by the slight
application of vacuum.
2. Take a conical flask and a funnel. Take some filter papers and make in shape of a cone, to be
placed inside the funnel. Take the empty weight of the filter paper.
3. Place the funnel with filter paper over the conical flask. Connect one end of the flask with the
vacuum system.
4. Pour the benzene mixture to flask through the filter paper placed over the funnel and
simultaneously apply vacuum, to speed up the process. The mineral matter which is
contained in the mixture is trapped over the filter paper and remaining mixture is collected in
the flask.
5. The process is repeated by using replacing with new filter papers.
6. Finally, take the oven dried weight of all the filter papers.
Observations and Calculations

Aggregate Extraction
Empty weight of bowl + filter paper 1315.38 g
Weight of bowl + mix + filter paper 2590.32 g
Net weight of HMA mix 1274.94 g
Weight of bowl and aggregate after oven
2512.1 g
drying
Net weight of aggregate in bowl 1196.72 g
Mineral Matter extraction
Weight of filter papers (5 nos) before test 27.72 g
Weight of filter paper (5 nos) after test 30.01 g
Net weight of mineral matter in filter paper 2.29 g
Final weight of aggregate 1199.01 g

Bitumen content =

1274.941199.01
= 100
1274.94

= 5.95 %

Result

The bitumen content obtained from by centrifugal procedure is 5.95 %.

Inference

The bitumen content actually added is 6.5 % and extracted bitumen content is 5.95 %. Thus,
there is slight error of 0.55 %. This can be due to mistakes during the experiment or the given
mix does not contain the 6.5 % bitumen content. Of course, Centrifugal procedure is an
approximate one.

References

ASTM D2172, Standard Test Methods for Quantitative Extraction of Bitumen from Bituminous
Paving Mixtures, ASTM International, DOI: 10.1520/D2172-11, West Conshohocken. United States.
 Determination of Asphalt content of HMA sample by Ignition Method

Expt No. Date:

Aim
To determine the asphalt content of hot-mix asphalt (HMA) pavement samples by removing the
asphalt cement in an ignition furnace, in accordance with ASTM D6307. Aggregates thus
obtained by this test method is taken for sieve analysis.

Significance
This test method can be used for quantitative determination of asphalt content in HMA paving
mixtures and pavement samples for quality control, specifications, acceptance and mixture
evaluation studies. This test method does not require the use of solvents.

Apparatus Required
1. Balance readable, 0.1g accuracy.
2. Sample tray should allow the sample to spread thinly.
3. Catch pan to hold the sample tray.
4. Catch pan/sample tray handling apparatus for inserting and removing the sample tray from
furnace.
5. Protective gloves- capable of withstanding 500C.
6. Ignition furnace, capable of maintaining up to 600oC
7. Oven.

Calibration
The Ignition apparatus should be calibrated before testing. There are two calibration done. One is
to ensure that the internal weighing scale in the furnace gives correct weight measurements and
other is to determine whether the loss of mass is showing correct results. Weight calibration can
be done in the apparatus itself. For the second, various mix of known bitumen content is tested
and results are used for calibration

Procedure

1. Heat the sample in the oven for certain time so that we can break it and spread it uniformly in
the tray.
2. Calibrate the Ignition furnace. Calibration should be done for the internal weighing scale and
for actual bitumen determination.
3. Take the empty weight of Ignition furnace basket and collect pan. Place the sample mix
evenly over the basket and collect pan and take weight again.
4. Place the basket with sample mix inside the furnace and initialize the furnace by setting the
temperature (540oC or auto control and burn profile, burn timing, etc)
5. After the burning, the furnace will give a beep sound. Take the sample basket out of the
furnace and spread the mix again. Repeat the burning cycle until the mass loss reaches below
0.01 %.
6. The mass loss on each cycle will be shown on the furnace. Record it. Obtain the bitumen lost.

Observations and Calculations

Empty weight of Basket + Collect pan + top cover 2.4978 kg

Weight of basket + collect pan + sample mix + top cover 3.7701 kg
Test cycle 1
Mass loss 84.2 g (2.24 %)
Test cycle 2
Mass loss 0.4 g (0.01%)
Total mass loss 84.6 g
Sample mix weight 1272.3 g

Bitumen Content =

84.6
= = 6.65 %
1272.3

Result
The bitumen content obtained by this test procedure is 6.65 %.

Inference

The actual bitumen content used for the sample s 6.5 %. But the bitumen content obtained by
above test procedure is 6.65 %. This is because some portion of the aggregate (probably fines) is
being burned during the Ignition process.
References

1. ASTM D6307 - 10, Standard Test Method for Asphalt Content of Hot-Mix Asphalt by
Ignition Method, ASTM International, DOI: 10.1520/D6307-10, West Conshohocken,
United States.

Sieving Analysis Results for the Extracted Aggregate from Centrifugal Procedure and Ignition
Method (Expt No. ):

IS Sieve Original aggregate Aggregate obtained Aggregate obtained

retained (mm) weight (g) from Centrifuge (g) by Iginition (g)

19 0.0 0.0 0.0

13.2 27.0 25.0 68.8
9.5 170.3 147.6 82.9
4.75 272.6 204.9 190.0
2.36 165.0 206.4 213.3
1.18 92.8 112.2 102.7
0.6 62.6 82.3 76.4
0.3 98.4 130.4 118.0
0.15 101.5 119.1 182.2
0.075 145.2 99.1 93.4
PAN 64.6 64.4 46.5
Sum 1200.0 1191.4 1174.2

Result and Inference:

The aggregate gradation obtained from two results seems to be similar to that of used originally
in sample preparation. And the gradation still is in the range of specification given by MoRTH.
However, ignition method, most of the large size particles are converted to fines as can be seen
from the table above shown.
 Orignal Centrufge extract Ignition Extract Specification
Cum %
IS Sieve Cum % of wt Cum % of wt Min Max
of wt
(mm) Passing Passing MoRTH MoRTH
Passing
19 100.00 100.00 100.00 100.00 100.00
13.2 97.75 100.00 94.14 90.00 100.00
9.5 83.55 87.27 87.08 70.00 88.00
4.75 60.84 69.60 70.90 53.00 71.00
2.36 47.09 51.79 52.73 42.00 58.00
1.18 39.36 42.12 43.99 34.00 48.00
0.6 34.14 35.02 37.48 26.00 38.00
0.3 25.95 23.77 27.43 18.00 28.00
0.15 17.49 13.50 11.91 12.00 20.00
0.075 5.39 5.55 3.96 4.00 10.00

Original Gradation Centrifuge Extract Ignition Extract Min MoRTH Max MoRTH

100.00

80.00
% cumulative passing

60.00

40.00

20.00

0.00
0.01 0.1 1 10 100
Sieve size (mm)