Beckman Model 930 Air Comparison Pycnometer

Accurate determination of volume for solids.

AUTHOR: JW Marnoch APPROVED BY: JW Marnoch

REV. No: 1

REV. Date: May 12th 2010 Approve Date: 18th May 2010

PART (A) – INTRODUCTION

PRINCIPLES.
The principle of the air comparison pycnometer is as follows: There are two chambers and two pistons as
sketched in Fig. 1. For purposes of illustration, the chambers are assumed to be equal in volume, and there is
no sample in either cylinder. Under these conditions, with the coupling valve closed, any change in the
position of one piston must be duplicated by an identical stroke in the other in order to maintain the same
pressure on each side of the differential pressure indicator.

If a sample, Vx, is inserted into chamber B, the coupling valve closed and both pistons advanced the same
amount from position 1 to position 2, the pressures will not remain the same.

However the pressures can be maintained equal if piston B instead is moved only to position 3. Then the
remaining displacement dx, from position 3 to position 2, is equal to the volume of the sample, Vx. If piston
A always is advanced exactly the same distance each time a measurement is made, the distance that piston B
differs from position 2, when the pressures in both cylinders are equal, will always be proportional

to the volume, Vx. The distance (dx) between positions 2 and 3 can be calibrated and made to read directly
in terms of cubic centimetres, employing a digital counter.

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PART (B) – REFERENCES

n/a

PART (C) – EQUIPMENT

1. Beckman Pycnometer
2. Two place balance

PART (D) – HEALTH SAFETY & ENVIRONMENT

1. Observe all precautions necessary for the materials to be tested.

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PART (E) – METHOD

The pycnometer is used to determine the volume of a substance sample, in particular porous materials and
powders which by their nature are difficult to measure by any other method.

OPERATION.

1 Weigh the sample to be measured into the sample cup to an accuracy of 10 mg; if the sample is a
powder, tap the cup gently on the bench to settle the material and exclude as much air as possible.
2 Turn the Reference (right) handwheel anticlockwise until it stops.
3 Turn the Measuring (left) handwheel anticlockwise until the counter reads the Starting Number.
4 Insert the sample cup into the sample compartment and lock in place by pressing firmly on the
handle. Do not use too much force.
5 Close the purge valve.
6 After 5 seconds, close the coupling valve.
7 Observing the needle on the differential pressure indicator, and keeping it always between the two
outer lines, turn both handwheels simultaneously clockwise until the reference piston (r.h.
handwheel) reaches the stop.
8 At this point, adjust the measuring (l.h.) handwheel until the needle is zeroed on the middle line.
Use the mirror to avoid parallax error.
9 When certain that the needle is stable, open the coupling valve. The needle should not move – if it
does, the needle was not zeroed.
10 Note the reading on the counter. This is the volume in millilitres.
11 Open the purge valve slowly to release all pressure from the system and return the pistons to the
starting point as described in stages 2 & 3 above.
12 Repeat this process (2 – 11) until stable readings are obtained for the volume.
NOTE: Do not remove the sample cup before opening the purge valve. This will entail tedious clean-up.
PART (F) – QUALITY CONTROL CHECKS

Calibration / Starting Number Check.

The calibration of the pycnometer shall be checked annually, unless any repairs or changes are made to the
instrument which could affect the volumes of the tubing etc within the equipment, when it must be
recalibrated before returning to service.

With an EMPTY sample cup in place, follow steps 2 – 11 described above. The end point should be reached
when the counter reads zero. If this is not the case, take careful note of the error and add/subtract that
from the Starting Number and repeat the process until the counter reads zero at the end. Make sure that
the new Starting Number is marked on the machine for future use

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