REFERENCES

3http://heliumpycnometer.com/supporting_information
2http://www.istcgroup.com/pdf/Auto_Pycnometer.pdf
1http://pubs.acs.org/doi/abs/10.1021/ef301193x
4http://www.quantachrome.com/articles_pdf/2010_ceramicindustry.pdf
5http://paginas.fe.up.pt/~sereno/publ/2007/IJFP_Determ_Particle_Density_&_Porosity
_Foods.pdf
6http://books.google.com.ph/books?
id=qBrJrXV2arIC&pg=PA294&dq=progress+of+gas+pycnometer&hl=en&sa=X&ei=
1pT6UaHANIeekAWZuoCYDQ&ved=0CEAQ6AEwAw#v=onepage&q=progress%20of
%20gas%20pycnometer&f=false
http://gold-app.diytrade.com/sdp/2005967/4/pd-6708454/11316949.html
http://www.pmiappeurope.com/publications/docs/gas_pycnometer.pdf
http://www-odp.tamu.edu/publications/tnotes/tn26/CHAP2.PDF (pentapyc)
11http://www.pharmacopeia.cn/v29240/usp29nf24s0_c699.html (mano)
12http://www.quantachrome.de/4149bD1lbg-/de/messmethoden/Gaspyknometrie/gaspyknometrie_dichte.html

[2] 2013. Automatic Gas Pycnometers for True Density: Pentapyc 5200e & Ultrapyc
1200e. Quantachrome Instruments. Florida, USA.
[3]1969. Air and Helium Pycnometer. Powder Technology, 3(3), pp.179-180.
[4]Thomas, Martin A. Density Solutions: Ceramics & Structural Materials.
Quantachrome Instruments.
Sereno, Alberto M., Silva, Maria A. and Mayor, Luis (2007). Determination of Particle
Density and Porosity in Foods and Porous Materials with High Moisture Content.
International Journal of Food Properties, 10(3), pp. 455 469.

[5] Ehrmann U., Strubinger A., & Len, V. (September 2012). Using the Gas
Pycnometer to Determine API Gravity in Crude Oils and Blends. Energy Fuels,
26 (11), pp.68636868.
[7] 2013. Gas Pycnometer Helium True/Absolute Density Analyzer. Gold APP
Instruments.
[6] Tsotsas, E. & Mujumdar, A. (2009). Modern Drying Technology, Experimental
Techniques. Wiley-VCH.
[2] Farhan, J. A., Gauray, J., & Roop, K. (2012). Theory and Practice of Physical
Pharmacy. Elsevier.
[8] Speight, J. G. (2005). Handbook of Coal Analysis. New Jersey: John Wiley & Sons,
Inc.
[9] Germaine, J & Germaine, A. 2009. Geotechnical Laboratory Measurements for
Engineers. New Jersey: John Wiley & Sons, Inc.
[11] Gas Pycnometry for the Measurement of Density. Pharmacopeia Forum, 31(3),
p.912.
[10] 2009. Gas Pycnometer. Porous Materials Inc. Ithaca, New York.

http://books.google.com.ph/books?
id=Cw2DDYPN3McC&pg=PT125&dq=progress+of+gas+pycnometer&hl=en&sa=X
&ei=1pT6UaHANIeekAWZuoCYDQ&ved=0CDkQ6AEwAg#v=onepage&q=progress
%20of%20gas%20pycnometer&f=false

First, the air in the sample holder is removed by vacuum and helium passes into
the chamber through the valve. The pressure is adjusted with the help of a movable
piston and the reading on the scale at this stage denotes P1. This represents the volume
of the empty chamber.
In the next step, the pycnometer is calibrated by placing a standard sample,
usually stainless steel spheres, of known true volume (V c) in the sample holder
chamber. The sample holder chamber is sealed, air is removed and the same amount of
helium gas is introduced. The pressure is again adjusted to the preset value by moving
the piston. The reading on the scale at this stage denotes P2. The difference between P1
and P2 gives the volume occupied by the spheres.
The last step involves determining the volume of the sample. Instead of stainless
spheres, the chamber is to be filled with sample powder. After weighing, the sample is
to be placed into sample chamber. A helium atmosphere is created inside the instrument
to rinse the sample intensively. [1] The sample holder chamber is sealed, air is removed
and the same amount of helium gas is introduced. The pressure is again adjusted to
pre-set value by moving the piston. The reading on the scale at this stage denotes Ps.
the difference between P1 and Ps gives the volume occupied by the powder sample. The
working equation for the gas pycnometer is
V s=V c

P 1Ps
P1P 2

Although pycnometers are recognized as density-measuring devices, they are in fact

devices for measuring volume only. Density is merely calculated as ratio of mass to
volume, mass being invariably measured on a discrete device, usually by weighing.
The density () is given by the equation:
=

ms
Vs

where

ms

and

Vs

is the mass and volume of the sample, respectively.

1. Modern Drying Technology, Experimental Techniques

edited by Evangelos Tsotsas, Arun Mujumdar

The helium displacement pycnometer with five cells (penta-pycnometer),employs

Archimedes principle of fluid displacement todetermine the volume of solid objects. The
five measurement cells contain custom fabricated inserts that reduce the chamber to a
cylindrical space that holds exactly one 10-mL Pyrex beaker. The measurement
chamber must contain as little air space as possible to maximize measurement
precision. (The user should also ensure that the Pyrex beakers are filled as completely
as possible with core material.) Each sample cell of volume V C has an input valve (from
the gas tank) and an output valve (to the pressure transducer). An additional reference
cell of volume VAis located downvent of the sample cells, with an input valve (which
separates VA from the pressure transducer) and a vent valve (Figure on page 7). All cell
volumes must be calibrated periodically (see calibration section). The following is the
operation sequence of the pycnometer during the measurement of a specimen.

The specimen to be measured is placed in a cell of known volume, V C. It is pressurized,

using helium, to an exactly measured pressure of about 18 psi (~120 kPa). The solenoid
valve between sample cell and the reference cell of known volume V A is opened and the
helium from the pressurized chamber is ported to the reference cell. The subsequent
pressure in the system is measured. Using the ideal gas law, the sample volume can be
calculated from the pressure ratio. The following is the sequence of operation (Figure 2
2).
1. Gas input valves to all five cells are closed (corresponding light-emitting displays
[LEDs] on pycnometer are unlit). The five sample cell output valves, the reference cell
input valve, and the vent valve are open, ensuring that all cells are at the ambient
pressure, Pa.
2. For all cells in use all valves are opened and cells are purged in parallel (for a 1-min
minimum). Cells not being used (not identified by the user) are isolated by closing the
input and output valves.
3. At the end of the purge period, processing begins on the first cell to be used.
(Cells are run in ascending numerical order regardless of the order in which they were
specified). When a stable ambient pressure is reached, the vent valve of the reference
cell closes and the pycnometer acquires and stores a zero pressure value.
4. The reference cell input valve is closed to isolate V A from the cell.
Approximately 6 s later, the current sample cell input valve opens and the cell is
pressurized to approximately 17 psi or until 3 min elapse.

5. When the cell pressurization is complete, the current cell input valve closes. The
pycnometer waits until a stable pressure is detected and then acquires and stores the
pressure P1 (LED display: pressure A).
6. The VA input valve opens. This will cause a pressure drop in the sample cell that is
proportional to the change in volume because of the introduction of V A. When the
pressure stabilizes, the system acquires and stores the cell pressure P2 (LED display:
pressure B).
7. The vent valve is opened to return the cell to ambient pressure. After a short vent
period, the instrument begins processing the next specified cell (if any) by venting the
cell to ambient pressure.
8. After all cells defined for use have been processed, samples may be removed. The
pycnometer indicates this by displaying <RUN COMPLETED>.

http://www.pmiapp.com/products/docs/brochures/Gas_Pycnometer.pdf

Both pressure P1 and pressure P2 have to be monitored in an equilibrated state.

Assuming a constant temperature, the calculation of the sample volume is performed
by:

P1 ( V s Ch Vsample ) =P2 ( V sCh +V ref Vsample )

(s-ch=sample chamber, ref=reference chamber) which leads to the calculation of the
volume of the sample as:
V sample =V s Ch

V ref
P1
1
P2

The accuracy of the gas pycnometry in the determination of solid volume is at least
0.2% of the respective sample chamber volume. Moisture and volatile substances in
the sample can contribute to pressure change and, thus, cause errors and instabilities.
[6]