Application Note

Determination of the Density of Bitumen and Highly Viscous

Materials with Anton Paar's DMA HP
1 Introduction
Bituminous materials include bitumen (asphalt),
pitch, tar and related substances, which are
residues of the distillation processes of coal or
petroleum products. These substances (as well as
certain crude oils) are highly viscous or even solid
at room temperature, but melt at temperatures of
100 to 150 °C to give liquids with lower viscosity.
The density of these products is measured for
quality control on a routine basis.

2 Density measurement
The measurement of density at temperatures up to Fig. 1 Measuring setup
200 °C can comfortably be performed with the • Heat up the sample until it reaches a flowing
external measuring cell DMA HP connected to an consistency and transfer the sample to the
evaluation unit DMA 4100/4500/5000. supplied glass beaker.
Temperature control:
• Heat up the external heating block to the desired
The measuring temperature of DMA HP is temperature.
controlled by a built-in Peltier thermostat.
• Before filling the pre-heated sample into the
Measuring range: external measuring cell, make sure that the
DMA HP has reached the measuring
Temperature: The temperature range of DMA HP is
temperature.
–10 °C (14 °F) to +200 °C (392 °F).
Pressure: The U-tube of the DMA HP external • Put then the glass beaker with the sample into
measuring cell is made of Hastelloy C-276 and can the external heating block.
operate at sample pressures up to 700 bar (10,000 • Use the lab jack to move the external heating
psi). block up to the DMA HP till both tubes are in the
opening of the external heating block.
3 Measurements
• Put the cover on the external heating block.
Note: As this application involves working with
hazardous materials at high temperatures, only • Cut a piece of at least 30 cm of silicone hose
trained and experienced personnel should perform and connect it with the luer adapter.
these measurements. Obey all safety regulations
and wear protective clothing: safety goggles and
protective gloves against heat!
Measuring procedure:
The measuring set-up is shown in Fig. 1.
• Place the DMA HP on a podium.
• Next to the DMA HP put a lab jack and on top
put a heating plate.
• Mount the filling tube and the sample tube into
the threads in the DMA HP.

Fig. 2: Density measurement of bituminous

materials

Tel.: +43 (0)316 257-0 Created on 8/14/2007 8:45 XDLIA05H_bitumen.doc

www.anton-paar.com Created by Ruth Weissenbacher Page 1 of 2
Application Note
• Move the luer adapter into the sample tube and
connect a syringe with the silicone hose.
• Slowly pull back the plunger of the syringe to
suck the sample into the measuring cell.
• Perform the measurement.
The sample may solidify in the silicone hose. At the
end of the measurement, the hose and the syringe
are removed and discarded.
The total time required to complete one
measurement, including cleanup, is approx. 15 - 20
min. Most of that time is spent waiting for the
sample to attemperate.
4 Cleaning
Note: Organic solvents represent a fire hazard!
Make sure all safety regulations are obeyed! Only
use solvents with a flash point considerably higher
than the operating temperature of the external
heating block. Always operate in a well-functioning
fume hood!
• Remove the rest of the sample from the
measuring cell.
• Fill solvent into a new syringe.
• Push the solvent through the measuring cell.
Normally, 25 to 50 ml of solvent are required.
• Remove the external heating block.
• Dry the measuring cell e.g. with the integrated
air pump of DMA 4100/4500/5000.
5 Adjustment
Adjustment of the external cell can be performed
with air (ρ at 150 °C = 0.000801 g/cm3) and n-
undecane (ρ at 150 °C = 0.6399 g/cm3 according to
API tables) or other pure liquids with a high boiling
point.
6 Additional information
Some customers with a broad range of products
are very satisfied with a combination of one DMA
4100/4500/5000 and two DMA HP external cells,
which are connected to DMA 4100/4500/5000
alternately using a switchbox.
Example: The DMA 4100/4500/5000 is set to 15 °C
and used for the measurement of gasoline and
lubricants. One external cell is set to 90 °C for the
measurement of waxes and intermediate products.
The second external cell is set to 150 °C for the
measurement of heavy products like bitumen and
asphalts. The adjustment parameters for all three
density cells are stored in the DMA
4100/4500/5000.
Tel.: +43 (0)316 257-0 Created on 8/14/2007 8:45
www.anton-paar.com Created by Ruth Weissenbacher
7 Other methods for determination
ASTM D70-03 describes the determination of
density and specific gravity of bituminous materials
using the pycnometer method. This method is
unpopular because it is hazardous, very time-
consuming and difficult to perform in terms of
sample preparation and cleanup.
EN 15326 describes the measurement of density
and specific gravity of bituminous materials using
pycnometer method. The measuring procedure is
similar to the ASTM D70-03, the only difference is
the determination in duplicate with a maximum
deviation of 1 kg/m3. Otherwise the measurement
has to be repeated.
Measurements with a pycnometer take 2 to 4
hours. Preparation of the sample includes heating
and pouring molten asphalt or tar into the
pycnometer. The operator is at risk of severe burns
in the event of spillage. Cleanup is extremely
difficult since the sample, which has been allowed
to solidify, has to be reheated and cleaned out with
large quantities of solvent.
8 Benefits of the Anton Paar method
• Fast and reliable results
• Small sample volumes, easy cleaning
• Reduced health risk for the operator
• Densities of other liquids can be measured with
the DMA HP a repeatability of ± 0.00001 g/cm3
(under optimum conditions)
• Long working life construction of the instrument,
virtually maintenance-free
• Tables and/or equations can be programmed
into the evaluation unit for the calculation of
density-related results (API, concentrations,
etc.)
• Connection to PC or printer through standard
serial interface possible
9 Literature
ASTM D70-03 Standard Test Method for Specific
Gravity and Density of Semi-Solid Bituminous
Materials.
EN 15326:2007 Bitumen and bituminous binders.
Measurement of density and specific gravity.
Capillary-stoppered pycnometer method.
XDLIA05H_bitumen.doc
Page 2 of 2