You are on page 1of 9

QUANTITATIVE EXTRACTION OF BITUMEN FROM BITUMINOUS PAVING

MIXTURE

Expt. No: Date:

AIM

To carryout quantitative extraction of bitumen from hot mix asphalt pavement samples using
centrifuge method as per ASTM D2172 and recovery of asphalt from solvent solution using the
rotary evaporator.

SIGNIFICANCE

This test procedure helps in estimating quantitatively the amount of bitumen in the hot mix
asphalt mix which can be used for specification acceptance, service evaluation and quality
control.

APPARATUS

Oven capable of maintaining temperature at 1105C.


Pan at least 300 mm long, 200 mm wide and 25 mm deep.
Balance accuracy of 0.01% of the sample mass.
Hot plate electric, 700W, continuous or low, medium or high.
Centrifuge Extraction apparatus consisting of bowl, with revolution speed of up to 3600
rpm.
Filler rings to fit the rim of the bowl.
Filter papers.
Vacuum system.
Reagents - Benzene

PROCEDURE

Use any suitable high speed (up to 3600 rpm) centrifuge of the continuous flow type.
Measure the weight of the empty bowl and filter papers before the test procedure is
started.
Place the compacted HMA sample in oven for loosening it and break and spread it in tray.
Fill the loosened sample into the bowl.
Note down the total weight of bowl and sample after placing a filter paper on top.
Place the bowl filled with the HMA mix inside the centrifugal apparatus.
Fill the bowl with benzene until the reagent rises up to a level of at least 2mm above the
HMA mix in the bowl.
Make sure the HMA mix is entirely soaked in benzene. The bowl is closed with a lid
having a filter paper placed below it and wait for 20 minutes.
Now, start the centrifuge apparatus and gradually increase the speed until the benzene
start to drain off and collected in a bottle. The benzene will be collected in the bottle with
bitumen and some filler particles. Hence the contents of the bottle should be kept safe for
further extraction.
Continue the rotation until no significant amount of solutions drains into the bottle.
The procedure is repeated for a couple more times, by again adding more benzene and
keeping it 15 minutes each.
Once the extraction is completed, keep the bowl containing the extracted aggregates and
filter papers in an oven for an hours at 110oC, to ensure the evaporation of all the benzene
content from the aggregates and filter paper.
Finally take the weight of the bowl containing dry aggregates and the dried filter paper.
The decrease in the final weight measurement indicate bitumen extracted.
The aggregate thus obtained is stored and sieve analysis is carried out on the same.

Recovery Of Asphalt from Solvent

Heat the oil bath to a temperature of 140 3C.


Apply a vacuum pressure of 5.3 0.7 kPa below atmospheric pressure.
Draw approximately 600mL of asphalt solution from the sample container into the
distillation flask.
Tart a nitrogen flow of approximately 500mL/min to the system.
Begin the rotation of the distillation flask and maintain a rotation rate of 40 rpm and
lower the distillation flask slowly into the oil bath
As the amount of asphalt solution in the distillation flask drops down to considerably low
levels, discontinue the nitrogen flow.
Now, add more asphalt solution from the sample container into the distillation flask and
readjust the nitrogen flow.
Repeat the above procedure until all of the sample solution is transferred into the
distillation flask.
Once the bulk of the solvent is distilled form asphalt, immerse the flask into the oil bath
to a depth of 40mm.
Now, apply a vacuum of 80 0.7 kPa and increase the nitrogen flow to 600 mL/min.
Also, increase the rotation rate to 45 rpm.
The system is maintained in the above mentioned condition for about 10 to 15 minutes.
At the end of 10 to 15 minutes, remove the distillation flask from the apparatus and wipe
the flask clean of any oil traces.
Now, extract the asphalt in the distillation flask into a container by placing the distillation
flask inverted in an oven maintained at 165 5C for about 10 to 15 minutes.

OBSERVATIONS AND CALCULATIONS

Aggregate Extraction (Centrifugal Extractor)


Empty weight of bowl + filter paper 1.3182 kg
Weight of bowl + mix + filter paper (before extraction) 2.6092 kg
Net weight of HMA mix 1.2910 kg
Weight of bowl + mix + filter paper (after extraction) 2.5355 kg
Net weight of aggregate in bowl 1.2173 kg
Net weight of bitumen 73.7 g

Net weight of HMA mixNet weight of aggregates


Bitumen Content =
Net weight of HMA mix

1.29101.2173
Bitumen Content = 100 =5.7087
1.2910

Bitumen Extraction (Rotary Evaporator)


Empty weight of distillation flask 296.30 g
Weight of distillation flask + extracted bitumen 369.92 g
Net weight of bitumen 73.62 g

RESULT

The bitumen content obtained from by centrifugal procedure is 5.71 %.

INFERENCE
The bitumen content actually added is 5.5 % and extracted bitumen content is 5.71 %..
This mismatch in the added and extracted bitumen can be attributed to the fact that the
centrifugal extraction method is an approximate method. The method doesnt ensure the
extraction of bitumen absorbed by aggregates and also doesnt account for the fillers
being present in the solution along with the solvent and bitumen.
The rotary evaporator was able to extract most of the bitumen present in the solution, the
difference being 0.08g.

REFERENCES

1. ASTM D2172 - 11, Standard Test Methods for Quantitative Extraction of Bitumen
from Bituminous Paving Mixtures, ASTM International, DOI: 10.1520/D2172-11,
West Conshohocken. United States.
2. ASTM D5404 - 12, Standard Practice for Recovery of Asphalt from Solution Using
the Rotary Evaporator, 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.

SIGNIFICANCE

This test method is more accurate than the solvent based centrifugal method as it accounts for
even the bitumen absorbed by aggregates. Also, it takes into account the problem of fillers
getting mixed with the asphalt solution. Thus, this test method can be better used for quantitative
determination of asphalt content in HMA paving mixtures and pavement samples for quality
control, specifications, acceptance and mixture evaluation studies.

APPARATUS

Balance readable, 0.1g accuracy.


Sample tray should allow the sample to spread thinly.
Catch pan to hold the sample tray.
Catch pan/sample tray handling apparatus for inserting and removing the sample tray from
furnace.
Protective gloves- capable of withstanding 500C.
Ignition furnace- capable of maintaining up to 600oC
Oven.

CALIBRATION

The Ignition apparatus should be calibrated before testing. There are two calibrations to be done.
One is to ensure that the internal weighing scale in the furnace is free of measurement errors and
other is to ensure that the loss of mass displayed by the apparatus is accurate. Weight calibration
can be done in the apparatus itself. For the later correction, various mixes of known bitumen
content are tested and results are used for calibration.

PROCEDURE

Heat the compacted HMA sample in an oven for a short time ( say 15 to 20 minutes).
Take out the sample from the oven and break it and spread it in a tray.
Calibrate the Ignition furnace. Calibration should be carried out for the internal weighing
scale and for actual bitumen determination.
Note down the empty weight of Ignition furnace basket, cover and the collection pan.
Place the sample mix evenly over the basket and collect pan and take weight again after
placing the cover on top.
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)
After the burning process is completed, 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 is atmost 0.01 %.
The mass loss on each cycle will be displayed in the on board display of the furnace. Record
it and calculate the bitumen lost.

OBSERVATIONS AND CALCULATIONS

Empty weight of Basket + Collect pan + top cover 2.4805 kg


Weight of basket + collect pan + sample mix + top cover 3.7730 kg
Trial 1 69.8g
Mass Loss Trial 2 2.41g
Trial 3 0.09g
Total mass loss 72.3g
Sample mix weight 1292.5 g

Totalmass loss
Bitumen Content=
Sample mix weight

72.3
Bitumen Content= 100 =5. 59
1292.5

RESULT

The bitumen content obtained by this test procedure is 5.59 %.

INFERENCE

The actual bitumen content used for the sample s 5.5 %. The bitumen content obtained by above
test procedure is 5.59 %. This small deviation of 0.09% may be because of some portion of the
aggregate (most probably fines) being burned during the Ignition process. The marginal
deviation may also be due to variation in addition of bitumen during mixing.

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

IS Sieve
Original aggregate Aggregate obtained Aggregate obtained by
retained
weight (g) from Centrifuge (g) Iginition (g)
(mm)

26.5 0 0 0
19 166.86 110.3 160.5
13.5 147.27 122.4 130.5
9.5 129.57 128.4 125.2
4.75 202.66 310.9 204.8
2.36 149.51 145.2 153.1
1.18 108.29 96.7 100.6
0.6 77.63 71.3 80.2
0.3 58.47 54.4 67.6
0.15 42.80 50.6 52.6
0.075 31.33 42.2 50.5
PAN 85.60 60.6 65.5
Total 1200 1193 1191.1
Cumulative Cumulative
Cumulative Cumulative Passing (%)
Passing (%) Passing (%)
Sieve Passing (%) Original
Centrifuge Ignition
(Original)
Method Method
Min. Max.
26.5 100.00 100.00 100.00 100 100
19 86.10 90.75 86.53 79 100
13.5 73.82 80.49 75.57 59 79
9.5 63.03 69.73 65.06 52 72
4.75 46.14 43.67 47.86 35 55
2.36 33.68 31.50 35.01 28 44
1.18 24.65 23.39 26.56 20 34
0.6 18.18 17.42 19.83 15 27
0.3 13.31 12.86 14.15 10 20
0.15 9.74 8.62 9.74 5 13
0.075 7.13 5.08 5.50 2 8

100.00
90.00
80.00
70.00
60.00
Cumulative Passing (%) 50.00
40.00
30.00
20.00
10.00
0.00
0 5 10 15 20 25 30
IS Sieve Size (mm)

Original Mix Centrifuge Method Ignition Method

INFERENCE
The aggregate gradation obtained from two results seems to be similar to that of the one used
originally in preparing the mix. The gradations were still found to be in the specification range
given by MoRTH.

You might also like