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Density Determination using Pycnometry and

Displacement Method
Jc Malenab Ancheta between particles within the bulk sample. While the
Department of Mining, Metallurgical, and Materials second type is the bulk density where the volume
Engineering, College of Engineering includes total volume of the closed pore, open pore,
University of the Philippines Diliman and solid material. The third type, which was
Quezon City, Philippines determined in the experiment, is the apparent density
where the volume of the solid material and closed
Abstract- The main objective of the experiment is to pore are measured (Totten,G., Funatani, K., Xie,L,
determine the density of a 10% v/v acetic acid and an ore 2004).
sample using displacement method and pycnometry. The
density of the solid was determined first using the Density Determination is important in many
displacement volume of water in the graduated cylinder
industries. In agriculture, the density of grains, feeds,
and its preweighed mass. The other method was using the
fertilizer and soil samples are measured. In the
pycnometer where it uses water as working liquid and
displaced volume water when poured in apparatus will be pharmaceutical industry, density measurements are
used to calculate for its density. The calibrated volume is correlated with solubility rates of powders and
24.94 1.23 ml and the measured density acetic acid is tablets. In powder metallurgy, it permits distinction
1.0103 0.00001 with a 3.78 % error. While the density of between different materials as well as determination
the solid using the analytical balance and using the of inaccessible porosity of powder or a finished P/M
pycnometer was 4.98 6.10 g/ml and 3.22541.6940 g/ml part (Angelo; Subramanian,2008). Density can
respective. These data cant be compared and Its accuracy
influence mechanical strength, hardness,
cant be validated because of the unknown theoretical
density of the solid. The experiment is said to be a success electrical conductivity and magnetic and gas
since the densities were determined. permeability of PM compacts.

I. Introduction There are other ways of density determination


like Float-sink Method and microscopic
Density is a physical property of matter. It can be
examinations. In their experiment, Bateni et al.,
measured without changing the chemical identity of
they used In Situ X-ray radiography to porous
the substance. Density values which are unique in
pure substances can help identify that substance. The
samples and a relationship has been found
density of an object is the ratio of mass to volume: between the density of the radiographic film and
the surface density of the compacts (2011).

= (1) In the first part of the experiment, the

density of an ore sample was determined by
The units are usually expressed in g/cm3 for solids, measuring its mass using an analytical balance and
g/ml for liquids, and g/L for gases. (Boljanovic, volume displaced with the graduated cylinder which
2007). is called the displacement method.
Many materials have within their structures The next two parts are the density measurement of a
are pores made up of cracks, and crevices which liquid sample and of a particulate solid using a device
leads to three different kinds of density, each called pycnometer. The method uses distilled water
requiring different techniques for measurement. The for which temperature dependent values of density
first type is the true density where the volume H2O are shown in Table 1. The pycnometer is a glass
measured excludes the pores as well the void spaces flask with a close-fitting ground glass stopper with a

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capillary hole through it so that air bubbles may pycnometer with the sample. Water will be added and
escape from the apparatus. This enables given the its mass can be obtained.
volume of working liquid to be measured precisely.
(Kucerka, 2006). The density of the solid is given by:

= V (6)

where the volume of the solid, V , is the difference


between the volume of the added water in the
pycnometer with solid, 2 , and the calibrated
volume of the pycnometer, , which was
computed earlier in eq. 2.

The pycnometer will be calibrated first by filling it 2


V = = (7)
2
with distilled water. Basing from eq. 1, the volume of
the water filling the pycnometer can be written as:
Incorporating equation 7 to 8 we get:
2
V= (2)
2
= 2 (8)

2
The mass of the water can be determined by
subtracting the mass of the empty pycnometer to the The main objective of the experiment is to determine
mass of pycnometer filled with water. density of a liquid and non-soluble particulate
powder and to demonstrate the proper use of
To identify the unknown density of a liquid, which in
pycnometer.
this experiment is Acetic Acid, CH3COOH, the same
procedure will be repeated where the mass of the
liquid after filling the pycnometer will be the one that
is weighed. II. Methodology


Vl = (3) The first part of the experiment was the

determination of the density of a 5-gram Baguio ore
sample using the analytical balance. A 50ml
Equation 3 shows the volume of the liquid with
graduated cylinder was first filled with distilled water
unknown density and this volume obtained is just
up to the 30 ml mark before pouring the ore sample.
equal to the volume of water in eq. 2.
The sample was carefully transferred to avoid spilling
outside the cylinder. The final volume of the pulp
Combining Equations 2 and 3
was then recorded and the density of the material was
2 calculated using equation 1. Three trials were
(4)
2 =
performed.

Isolating the density of liquid gives The second part is the density measurement of a
liquid in the pycnometer. The pycnometer was first

= x 2 (5) preheated to 105 C in the oven for one hour and was
2
cooled in a dessicator before weighing in the
The pycnometer will also be used in determining the analytical balance. To calibrate, distilled water was
density of an ore sample by measuring the weight of used to fill the pycnometer up to the neck. The
capillary tube was then inserted and was made sure

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that no air bubble is trapped inside. Subsequently, the Table 3.Calibration Volume of Pycnometer
exterior of the was washed with ethanol and wiped Trial Mass of Density of Calibration
with lint-free tissue. The pycnometer was weighed water (g) water at 29 volume (ml)
when it was completely dry. The calibration volume C (g/ml)
1 24.8678 0.995943 24.9690.710
was computed using eq. 2.
2 24.8186 0.995943 24.9200.710
The steps were repeated but 10% v/v acetic acid was
3 24.8293 0.995943 24.9300.710
used to fill the pycnometer. The density of liquid was
calculated using eq. 5.
The average calibration volume is 24.94 1.23 ml
The last part was the density determination of the ore and has 0.24% error from the theoretical volume of
sample. The dry pycnometer was weighed before the 25 ml. The calibration step is important because this
non-soluble particulate sample was poured to fill value can be used to determine the density of the
about 1/3 of its volume. It was weighed again before liquid and solid. The occupied volume of the tested
filling it up with distilled water up to the neck. The liquid in the pycnometer is just the same as the
capillary tube was inserted and bubbles trapped calibration volume, therefore we can manipulate the
inside was avoided. The exterior was washed with formula to calculate for its density. And the distilled
ethanol and the final weight was recorded. Equation 8 water was used as the working liquid because it is
will be used to calculated for the density of the solid. accessible and its density at different temperature
values is well-known.
III. Results and Discussion
Table 4. Density of Acetic Acid
The calculated density of solid using the
Trial Temp Mass of Mass of Density of
displacement method on three trials are shown on (C) water CH3COOH CH3COOH
Table 2. (g) (g) (g/ml)
0.000006
Table 2. Density of Solid using Displacement Method 1 29 24.8678 25.2308 1.0081
Trial Mass of Initial Final
Solid (g) volume Volume Density 2 29 24.8186 25.2641 1.0115
0.1 mg 0.5 ml 0.5ml g/ml
1 4.933 30 31 4.93.49 3 29 24.8293 25.2662 1.0111
2 4.9982 30 31 5.03.53
3 4.9996 30 31 5.03.54 Table 4 shows the experimental density of the acetic
acid. It has a mean density of 1.0103 0.00001 g/ml
and a standard deviation of 0.001831. The mean
The density values have an average of 4.98 6.10
experimental density has a 3.78 % error from the
g/ml and standard deviation of 0.03805.
theoretical density of 1.05 g/ml.
The mean value has a high uncertainty. The error can On the determination of the density of solid
be attributed to the mass of sample poured in the using pynometer, the following data was tabulated in
graduated cylinder, since the amount was small, the Table 5.
change in volume or the displacement was also small
Table 5. Density Measurement of Solid using
which cant be measured by the scaling of the Pycnometer
graduated cylinder accurately. Another error maybe Temp Mass of Mass of Density of
in the reading of the measurement. Trial (C) solid water (g) solid (g/ml)
0.1 mg 0.1 mg
The next part was the calibration and the volume of 1 29 8.2049 22.30508 3.22541.6940
pycnometer as shown on Table 3.
We cannot compare which of the two methods is
more accurate since the theoretical density of the
solid is unkown.

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The data from the other groups was compared as IV. Conclusions and Recommendations
shown in Tables 6-8.

The calibration volume has only 0.24% error


Table 6. density solid using displacement method from the theoretical value of 25 ml, therefore we can
Density (g/ml) Stddev say that the calibration was properly handled. The
group 1 4.98 1.131541 density of acetic acid is density 1.0103 0.00001 g/ml
and has 2.78% error. While the density of the solid
group2 3.43
using pycnometry and displacement method are
group 3 2.78 3.22541.6940 and 4.98 6.10, respectively. The
accuracy of the density measurements of the ore
sample and the validity of methods cant be
Table 7. density solid using pycnometer
determined because of the unknown theoretical density
Density (g/ml) Stddev of the solid.
group 1 3.23 0.52148
Basing on the uncertainty budgets (see
group2 2.49
appendix), the volume gives the highest contribution
group 3 2.79
of uncertainty which leads to inaccurate results. For
future experiments, it is recommended to use more
accurate apparatus to measure the volume and to
Table 8. density liquid using pycnometer
know the theoretical density of the ore sample.
Density (g/ml) Stddev
group 1 1.0103 0.004935 The experiment is a success since the
group2 1.0033 density of the liquid and solid was determined using
group 3 1.0173 pycnometry and displacement method.

The data of the groups are most varied on the density


measurements using the displacement method.

The possible sources of error can be the


handling and weighing of the pycnometer. Constant
weighing of pycnometer was not done therefore the
mass of the pycnometer weighed may not be the real
mass. Another error is that the pycnometer was not
completely dried out before filing it up with water or
with the liquid, this extra moist can add to the
recorded mass of the sample.
One major source error is the failure to completely
eliminate the entrapped air in the pycnometer making
the recorded mass to be inaccurate.

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V. References

Boljanovic, Vukota. (2007). Applied Mathematical and Physical Formulas - Pocket Reference. Industrial Press.
http://app.knovel.com/hotlink/toc/id:kpAMPFPR01/applied-mathematical/applied-mathematical accessed
(accesed October 10,2015).

Kucerka,N. (2006) DENSITY DETERMINATION BY PYCNOMETER


http://novyweb.fpharm.uniba.sk/fileadmin/user_upload/english/Fyzika/Density_determination_by_pycno
meter.pdf (accessed October 7, 2015)

Totten, George, Kiyoshi Funatani, Lin Xie. (2004) Handbook of Metallurgical Process Design. (CRC Press). pp.373-
734
https://books.google.com.ph/books?id=3zjfgq8pUvcC&printsec=frontcover&source=gbs_atb#v=onepag
e&q&f=false (accessed October 4, 2015).

Angelo P., and R.Subramanian. (2008) POWDER METALLURGY: SCIENCE, TECHNOLOGY AND APPLICATIONS.
PHI Learning Pvt. Ltd., pp. 79-81

D854-92e1 Standard Test Method for Specific Gravity of Soils, AMERICAN SOCIETY FOR TESTING AND
MATERIALS (1997)

Material Safety Data Sheet .http://avogadro.chem.iastate.edu/MSDS/acglac.htm (accessed October 4, 2015).

Density Analysis . 2001. Micromeritics. http://www.micromeritics.com/Repository/Files/Density_Brochure.pdf


(accessed October 9, 2015).

Bateni,A; N. Parvin and M. Ahmadi. (2011)Density evaluation of powder metallurgy compacts using in situ X-ray
radiography.http://www.researchgate.net/publication/233545357_Density_evaluation_of_powder_metall
urgy_compacts_using_in_situ_X-ray_radiography. (accessed October 10, 2015).

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VI. Appendix

A. Density of Solid using Displacement Method

Uncertainty budget for Trial 1


Source Value sensitivity, ci ui ciui fraction (ciui)2
mass 4.933 1 0.0001 0.0001 0.002027123 0.00000001
final volume 31 -4.933 0.5 2.4665 49.99898644 6.08362225
initial volume 30 4.933 0.5 2.4665 49.99898644 6.08362225
calibration factor 1 4.933 0 0 0 0
Summation 4.9331 12.1672445
Uncertainty of density = ( 2 ) = 3.488158

Uncertainty budget trial 2


Source value sensitivity, ci ui ciui fraction (ciui)2
mass 4.9982 1 0.0001 0.0001 0.00200068 0.00000001
final volume 31 -4.9982 0.5 2.4991 49.99899966 6.24550081
initial volume 30 4.9982 0.5 2.4991 49.99899966 6.24550081
calibration factor 1 4.9982 0 0 0 0
summation 4.9983 12.4910016
Uncertainty of density = ( 2 ) = 3.534261

Uncertainty Budget for Trial 3


Source value sensitivity, ci ui ciui fraction uici^2
mass 4.9996 1 0.0001 0.0001 0.00200012 0.00000001
final volume 31 -4.9996 0.5 2.4998 49.99899994 6.24900004
initial volume 30 4.9996 0.5 2.4998 49.99899994 6.24900004
calibration factor 1 4.9996 0 0 0 0
summation 4.9997 12.4980001
Uncertainty of density = ( 2 ) = 3.535251

B. Calibration of Volume

Uncertainty Budget Trial 1


Source value ci ui ciui fraction ciui^2
mass of pyc 21.1965 -1.004073526 0.5 0.502036763 50 0.252040912
Mass of pyc + water (W) 46.0643 1.004073526 0.5 0.502036763 50 0.252040912
density of water at T 0.995943 -25.07081192 0 0 0
Summation 1.00407352 0.0504081823

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Uncertainty of volume = ( 2 ) = 0.709987

Uncertainty Budget Trial 2


Source value ci ui ciui fraction ciui^2
mass of pyc 21.1965 -1.004073526 0.5 0.502036763 50 0.252040912
Mass of pyc + water (W) 46.0151 1.004073526 0.5 0.502036763 50 0.252040912
density of water at T 0.995943 -25.02121027 0 0 0
Summation 1.004073526 0.504081823
Uncertainty of volume = ( 2 ) = 0.709987

Uncertainty Budget Trial 3


Source value ci ui ciui fraction ciui^2
mass of pyc 21.1965 -1.004073526 0.5 0.502036763 50 0.252040912
Mass of pyc + water (W) 46.0258 1.004073526 0.5 0.502036763 50 0.252040912
density of water at T 0.995943 -25.03199762 0 0 0
Summation 1.004073526 0.504081823
Uncertainty of volume = ( 2 ) = 0.709987

C. Density measurement of Acetic Acid

Uncertainty Budget
Trial 1
Source value ci ui ciui fraction ciui^2
mass of pyc 21.1965 0.000583 0.0001 5.83266E-08 0.719358879 3.40199E-15
Mass of pyc + water 46.0643 -0.04054 0.0001 4.05407E-06 50 1.64354E-11
(W)
Mass of pyc + 46.4273 0.039957 0.0001 3.99574E-06 49.28064112 1.59659E-11
CH3COOH(S)
density of water at T 0.995943 1.012264 0 0 0
calibration factor 0.9977 1.010481 0 0 0 0
Summation 8.10813E-06 3.24048E-11
Uncertainty of density = ( 2 ) = 0.709987

Uncertainty Budget Trial 2


Source value ci ui ciui fraction ciui^2
mass of pyc 21.1965 0.000719 0.0001 7.18667E-08 0.88168587 5.16482E-15
Mass of pyc + water 46.0151 -0.04076 0.0001 4.07553E-06 50 1.66099E-11
(W)
Mass of pyc + 46.4606 0.040037 0.0001 4.00366E-06 49.11831413 1.60293E-11
CH3COOH(S)
density of water at T 0.995943 1.015609 0 0 0 0
calibration factor 0.9977 1.01382 0 0 0 0

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Summation 8.15105E-06 3.26444E-11
Uncertainty of density = ( 2 ) = 0.709987

Uncertainty Budget Trial 3


Source value ci ui ciui fraction ciui^2
mass of pyc 21.1965 0.000704 0.0001 7.04186E-08 0.864593805 4.95878E-15
Mass of pyc + water 46.0258 -0.04072 0.0001 4.07235E-06 50 1.65841E-11
(W)
Mass of pyc + 46.4627 0.040019 0.0001 4.00193E-06 49.13540619 1.60155E-11
CH3COOH(S)
density of water at T 0.995943 1.015256 0 0 0 0
calibration factor 0.9977 1.013468 0 0 0 0
Summation 8.14471E-06 3.26045E-11
Uncertainty of density = ( 2 ) = 0.709987

D. Density measurement of Solid using pycnometer

Source value ci ui ciui (ciui)^2 fraction


Mass of solid 8.2049 0.393111601 0.5 0.196555801 0.038634183 8.232525004
mass of water 22.30508 1.262814316 0.5 0.631407158 0.398674999 26.44579912
calibrated 24.93975 -1.267958424 1.23 1.559588861 2.432317416 65.32167588
volume
density of water 0.9959 -28.05290013 0 0 0 0
Summation 2.38755182 2.869626598
Uncertainty of density = ( 2 ) = 1.693997

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