the determination of density, relative density, and API gravity of all kinds of petroleum products with the oscillating U-tube method. The question arose: why couldn’t this easier way of density measurement also be applicable to bitumen samples?


Table 1. Density results obtained with a pycnometer and the DMA 4200 M density meter Pycnometer


Mean value [kg/m³] Standard deviation [kg/m³]


Sample 1 Sample 2 Sample 3


1042.34 1035.38 1029.08


0.499 0.439 0.422


the DMA 4200 M density meter. Ms. Schultze injected the heated sample with a syringe, as can be seen in Figure 2, into the density meter’s measuring cell which was held at 120 °C. Once the density measurement was fi nished, the instrument automatically converted the density value obtained at 120 °C to the density value that corresponds to 15.6 °C, thus making the cooling of the sample or conversion with a table obsolete. This way, a lot of time is saved and no more additional working steps are required.


Figure 2. Ms. Schultze handles the DMA 4200 M density meter effortlessly As easy as it looks


A few months ago, I.M.U. acquired a DMA 4200 M density meter from Anton Paar GmbH in Graz, Austria. DMA 4200 M complies with the “Standard Test Methods ASTM D4052 Standard Test Method for Density, Relative Density, and API Gravity of Liquids” and “D5002 Standard Test Method for Density and Relative Density of Crude Oils” and therefore appeared to be a promising solution for determining the density of bitumen, especially for research purposes, but also as an eagerly awaited standardized determination method for bitumen as a fast, reliable, and user- friendly alternative to the pycnometer method.


With this density meter a measurement only takes around 12 minutes. Considering the number of bitumen samples per day and the potential of savings for future determinations it is not surprising that this technology appealed to Ms. Schultze. “When I get a chance I love to try out new technologies,” states Ms. Schultze. “The DMA 4200 M density meter is very user-friendly. We not only save time and cumbersome cleaning steps, but we also get the information we need right away without needing to re-calculate the result – which is required with the pycnometer - as DMA 4200 M automatically converts the result obtained at the measuring temperature to the density at 60 °F / 15.6 °C or 77 °F / 25 °C as required by the standard.”


Handling a bitumen sample with a DMA 4200 M is straightforward: once the sample is heated, bitumen is fi lled into a syringe as is shown in Figure 1, and injected into the measuring cell of the density meter. The measuring cell is also held at an elevated temperature which can be up to 200 °C. Even the fact that different samples require different temperatures to soften does not pose a problem: DMA 4200 M’s software provides custom-tailored measuring conditions and allows users to create user functions which can be attributed to certain samples and recalled upon request.


Density measurement easily withstands the comparison


To evaluate how precisely the results obtained with a pycnometer and a DMA 4200 M agree, Ms. Schultze dedicated a few weeks of parallel determinations to compare the traditional pycnometer results, carried out according to ASTM D70, with the results of


Figure 3: Density results of pycnometer and DMA 4200 M measurements on 3 different bitumen samples (reporting temperature 60 °F)


In order to obtain comparison data, Ms. Schultze selected three different bitumen samples and measured the density of the samples at 15.6 °C (60 °F) with a pycnometer according to the ASTM standard, and with the DMA 4200 M density meter at 120 °C. DMA 4200 M automatically referred the obtained density value to the reference temperature of 15.6 °C. Repetitive determinations of each sample were carried out and the mean values and standard deviations calculated. All results are summarized in Table 1.


According to ASTM D70, results of two properly conducted tests by the same operator on the same material should not differ by more than 3.7 kg/m³ at 15.6 °C: the difference between the mean values of the results obtained with DMA 4200 M and the mean values obtained with the pycnometer is well below the standard’s requirements. This suggests that the DMA 4200 M density meter is a suitable analysis method for bitumen samples and even more precise and effi cient than a pycnometer.


The obtained comparison data are graphically displayed in Figure 3.


It can be seen from the graph that the results obtained with DMA 4200 M satisfactorily matched the pycnometer results. The repeatability shown with DMA 4200 M is much higher and easily meets the specifi cation of the ASTM D70.


“I aim for a result accurate to the fourth decimal place,” says Ms. Schultze. This requirement is met easily and effortlessly with DMA 4200 M.


The DMA 4200 M density meter in its assigned working environment


Infobox DMA 4200 M


DMA 4200 M is equipped with a measuring cell made of Hastelloy C276 and is based on the oscillating U-tube principle. The instrument is designed for measuring heavy samples, samples at pressures up to 500 bar, samples at temperatures up to 200 °C, and samples with viscosities up to 35,000 mPa.s. The required sample amount is 2 mL; the measuring temperature is achieved and maintained with the aid of a Peltier element.


DMA 4200 M is suitable for the quality control of heavy process samples and intermediate products, and for fi nal product quality control of bituminous materials, LPG, heavy fuel oil (HFO), crude oil, and live crude oil. The fact that the instrument also copes with the quality control of bitumen, tar, and pitch in “heavy labs” as well as with R&D requests makes DMA 4200 M an asset for any petrochemical institution. Only small solvent volumes are needed for cleaning, which results in savings on cleaning time, a considerable reduction of cleaning agent, and less solvent waste to be disposed of.


1043.10 1036.38 1029.38


DMA 4200 M


Mean value [kg/m³] Standard deviation [kg/m³]


0.0524 0.0670 0.1031


DMA 4200 M makes itself useful


Over time, DMA 4200 M also proved useful for the quality analysis of many other samples commonly submitted to the I.M.U. laboratories such as crude oil, and for measurements on heavy intermediates from the production process.


Sometimes, especially in the winter months, the reduced number of samples for road paving leaves Ms. Schultze a little more time for other topics, such as testing new bitumen mixtures. “Sometimes we do not know a lot about these samples,” says Natascha Schultze. “In this case I am very happy about the Hastelloy cell of DMA 4200 M as this material will not suffer any damage from unknown products.”


With its expertise and modern equipment, I.M.U. is well prepared to cover the steadily growing number of samples and measuring parameters, and the expected increase of its customers’ requirements on accuracy.


Difference [kg/m³]


0.758 0.997 0.297


Author Contact Details Dr. Karin Biebernik. Anton Paar • Anton-Paar-Str. 20, 8054 Graz, Austria • Tel +43 316 257-0 • Email: density@anton-paar.com • Web: www. anton-paar.com


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