Liquid Diffusion Coefficients Apparatus

CHE420-ChE Laboratory
Student Manual (Ver 1.0)

CERB

(NOTE: This is an abbreviated manual. Full manual available upon request from instructor. In the
following, instructors additions/comments are in this font: red, italic, bold)

ISSUE 12

September 2016
Armfield Ltd Student Manual – Diffusion system CERB

Table of Contents

1 Disclaimer.........................................................................................................................3
2 Copyright and trademarks.................................................................................................3
3 General Overview.............................................................................................................4
4 Equipment Diagrams........................................................................................................5
5 Description........................................................................................................................6
5.1 Overview....................................................................................................................6
5.2 Diffusion Vessel.........................................................................................................6
5.3 Diffusion Cell..............................................................................................................6
5.4 Conductivity Meter and Electrode..............................................................................7
5.5 Magnetic Stirrer.........................................................................................................7
6 Laboratory Teaching Exercises........................................................................................8
6.1 Index to Exercises.....................................................................................................8
7 Exercise A - Diffusion of a liquid.......................................................................................9
8 Contact Details for Further Information...........................................................................14

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1 Copyright and trademarks

Copyright © 2016 Armfield Limited. All rights reserved.

Any technical documentation made available by Armfield Limited is the copyright work of
Armfield Limited and wholly owned by Armfield Limited.

Brands and product names mentioned in this manual may be trademarks or registered
trademarks of their respective companies and are hereby acknowledged.

2 General Overview

Physical and chemical processes depend on the properties of the materials involved.
Process engineering concerns itself with the transformation and distribution of materials in
bulk. The design and operation of engineering plant to achieve the desired changes in
materials has therefore to take into account the physical and chemical properties of these
materials. The most convenient medium is the fluid state and hence the majority of plant
operations involve gases or liquids.

One of the most important properties of fluids in such situations is diffusivity. Fluid flow and
mass transfer operations depend partially on this property and such data is always needed
in plant design. The Armfield ‘Diffusion of a liquid apparatus’ (Product code CERB) allows
students to measure to a reasonable degree of accuracy this property, by a well-established
technique. The practical exercise involved in this measurement allows students an
introduction to handling the basic equations of mass and momentum transfer and is a
complement to, rather than a substitute for, the more exacting measurements made by
physical chemists.

Measurements are effected using the supplied conductivity meter. A connecting lead and
software are supplied that allow data logging using a PC with serial data port.

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CERB Diffusion of a Liquid apparatus

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3 Equipment Diagrams

Figure 1: CERB Diagram

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4 Description

Where necessary, refer to the drawings in Equipment Diagrams section 3.

Refer to the Equipment Specifications section for technical details about each of the items
described below.

4.1 Overview

Armfield has developed a unique diffusion cell which overcomes the traditional problem of
slow diffusion rates in liquids requiring long observation times, but without sacrificing
accuracy or introducing convective effects. Essentially, the cell consists of a honeycomb of
accurately dimensioned capillaries, positioned between two liquids of differing concentration
of solute whose diffusion coefficient is to be determined.

In practice a small volume of concentrated solution is placed on one side of the honeycomb,
whilst the other side consists initially of a large volume of pure solvent (water). As diffusion of
the solute occurs, the solute concentration within the larger volume increases and is
monitored with a conductivity electrode and digital meter. The mixture is continuously stirred
with a magnetic stirrer to ensure uniform concentration within the bulk liquid. Whilst the
conductivity electrode may be readily calibrated for any required aqueous system, for
introductory studies, dilute solutions of sodium chloride are recommended, for which
conductivity data are provided.

The equipment consists of a glass diffusion cell mounted on top of an acrylic vessel that is
stirred by a battery operated magnetic stirrer. Conductivity of the vessel contents is
monitored using the supplied conductivity meter and electrode. The change in conductivity
with time is used to determine the Diffusion Constant for the salt solution tested.

4.2 Diffusion Vessel

The diffusion vessel is constructed from clear acrylic and is designed to stand on top of the
battery operated magnetic stirrer. A gland in the side of the vessel allows the conductivity
electrode associated with a conductivity meter to be inserted.

The lid of the vessel incorporates a gland that allows the glass diffusion cell to be inserted
and clamped at the correct depth inside the vessel.

A 1 litre measuring jug is supplied to assist when filling the vessel with the correct volume of
pure water.

4.3 Diffusion Cell

The diffusion cell is manufactured from glass in the shape of a hook. The lower end of the
glass hook is enlarged and incorporates a PVC disk that is perforated with a honeycomb of
parallel capillaries.

The top end of the glass hook is parallel to allow mounting through a gland in the lid of the
diffusion vessel.

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A plastic hypodermic syringe is supplied to assist when filling the glass diffusion cell with salt
solution of the required concentration.

4.4 Conductivity Meter and Electrode

The battery operated conductivity meter supplied with CERB is a digital instrument that
incorporates automatic compensation for changes in temperature of the solution. The
electrode supplied utilises carbon rods to measure the conductivity giving a robust sensor
that has a long life when compared with similar glass electrodes. An RS232 serial interface
on the conductivity meter allows the temperature and conductivity readings to be exported to
a suitable PC for logging against time using the RS323 to USB adaptor and simple data
logging software supplied with the CERB. Alternatively, the readings can be read from the
display on the meter and logged by hand using a stopwatch to determine the changes with
time. You should use the PC data acquisition system.

Note: The meter will automatically switch off after 10 minutes to preserve the battery.
To disable this automatic power-off function, press the RECORD button. With ‘REC’
indicated on the display the instrument will continue to operate until the POWER
button is pressed. If you don’t press the REC button, the system will stop recording
data after 10 min! Details of the meter operation are in the manual in the lab.

4.5 Magnetic Stirrer

The battery operated magnetic stirrer supplied with CERB utilises a PTFE coated bar that is
inserted into the bottom of the diffusion vessel to stir the contents. The speed of the stirrer
can be adjusted by rotating the speed control on the front of the housing. The rotary control
must be turned fully anticlockwise until it clicks to switch off the stirrer. When switched off the
indicator alongside the control knob will not be illuminated.

In use the speed of the stirrer should be adjusted until the contents of the diffusion vessel is
gently agitated without undue motion at the surface (The speed must not be sufficient to
allow a vortex to form at the surface).

Also, you don’t want the stir bar to be jumping around the vessel.

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5 Laboratory Teaching Exercises

5.1 Index to Exercises

Please find below a sample of our Teaching Exercises for the CERB.

Exercise A - Diffusion of a liquid

A full list of Teaching Exercises for this equipment is shown below. For further details please
contact our Sales Department using the contact information shown at the rear of this
manual.

Teaching Exercises available for the CERB Liquid Diffusion Coefficients Apparatus:

Exercise Description

Exercise A Diffusion of a liquid

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6 Exercise A - Diffusion of a liquid

Objective
To determine the Diffusion Coefficient of 1M NaCl solution.

Method
A small volume of concentrated solution is placed on one side of the honeycomb of
capillaries, inside the glass diffusion cell, whilst the other side consists initially of a large
volume of pure solvent (water). As diffusion of the solute occurs, the concentration within the
larger volume increases and is monitored with a conductivity meter. The mixture is
continuously agitated with a magnetic stirrer to ensure uniform concentration within the bulk
liquid. Whilst the apparatus may be used with any required aqueous system, for introductory
studies, we solutions of Sodium Chloride up to 4.0M are recommended. It is suggested that
the diffusivity of NaCl in water be measured for different NaCl concentrations.

Equipment Required
Armfield CERB comprising:

Magnetic stirrer

Acrylic diffusion vessel incorporating conductivity electrode

Lid for vessel incorporating glass diffusion cell

Conductivity meter

1 Litre measuring beaker

Plastic syringe

Filter paper (not supplied)

Deionised / demineralised water (Not supplied)

solution of NaCl (Not supplied)

Volumetric glassware and balance for making up solutions of known concentration (not
supplied).

Optional Equipment
Compatible PC (Not supplied) for logging conductivity readings; requires USB Port

Armfield software for CERB (Supplied with CERB)

Theory
The rate of diffusion is expressed by the equation:

then D will be the diffusivity (diffusion coefficient) in cm2/sec. Always report values in cm2/s.

The apparatus uses 121 vertical capillaries, 4.5 mm long and 1 mm bore (diameter) to
restrict diffusion to one dimension. The concentration at the lower ends is equal to the
concentration in the J-tube and assumed to be constant. The concentration at the top
ends is assumed to be equal to the concentration in the stirred tank (assuming
convective rate in the tank is high enough so that there is no mass transfer
resistance).
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Equipment Set Up

Before using the equipment, examine the diffusion cell and vessel for any dirt or
deposits, and if necessary, rinse with clean water. Then, rinse both with DI water.

Fill the acrylic vessel with 1 litre of distilled or deionised water using the measuring jug
supplied. Locate the lid (with the glass diffusion cell fitted) on top of the vessel but locate it
eccentrically so that it does not locate in the recess and the lid is 5mm above its normal
operating position.

Steady the lid on top of the vessel and check that the top of the honeycomb of capillaries is
flush with the surface of the water. If necessary, adjust the height of the glass diffusion cell
by unscrewing the gland nut that secures it. After making any adjustments ensure that the
gland nut is tightened to clamp the glass diffusion cell at the correct height.

Remove the lid / diffusion cell and dry the cell to remove any excess water. Check that the
collar on the vertical shaft is located 5 mm above the tops of the capillaries to assist when
filling the cell.

Place the stirrer bar into the bottom of the acrylic vessel and locate the vessel on top of the
battery operated stirrer.

Connect the conductivity electrode to the socket at the top of the conductivity meter. If using
the CERB data logging software connect the lead supplied from the jack socket on the meter
(under a sealing grommet) to the USB port connector on the PC using the in-line RS232 to
USB adaptor supplied.

Set the range switch to 199.9 μS on the conductivity meter and switch the meter on by
pressing the POWER button.

Press the REC button to leave the meter permanently powered (if REC is not indicated on
the display the meter will automatically switch off after 10 minutes to save the battery).

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Fill the glass diffusion cell with desired concentration of NaCl solution, using the syringe
supplied. Ensure that the glass hook and plastic honeycomb are filled with the solution with
no air bubbles trapped. This can be achieved by immersing the hook into the NaCl solution
while forcing liquid through the capillaries using the syringe filled with the same solution; the
syringe is fitted with a flexible collar to fit the top of the cell. Wipe off any excess solution
from the outside of the cell and the tops of the capillaries using filter paper or similar
absorbent material but take care not to suck the salt solution through the capillaries. Check
again for bubbles in the capillaries (which can block diffusion), and remove
bubbles/liquid from the top of the capillaries with Pasteur pipet, if necessary. It is
important to adjust the level inside the cell so that the free surface is adjacent to the collar on
the vertical limb of the cell i.e. 5mm above the tops of the capillaries. This ensures that the
salt solution is not disturbed when the cell is immersed 5 mm below the surface of the water
in the vessel. Do not place the cell into the vessel until instructed.

Procedure
Ensure that the timer or CERB data logging software is ready for use as appropriate.

Switch on the magnetic stirrer and adjust the speed control until the contents of the diffusion
vessel is gently agitated without excessive motion at the surface (The speed must be
sufficient to give good mixing within the vessel but not to allow disturbance such as a vortex
to form).

Carefully install the lid / diffusion cell on top of the vessel ensuring that it is located squarely
into the recess. Take care not to tilt the cell as it is immersed in the water to prevent loss of
the salt solution.

Then add a little concentrated solution to the J-tube to “puff” the capillaries.
Start the stopwatch and record the conductivity reading or start the data logger as
appropriate.

If you do not get a steady increase in conductivity of bath water after a few minutes, you
can add some solution to the J-tube to puff it again.
If using a stopwatch record the conductivity reading at typically 200 second intervals. The
experiment should continue for at least 30 min, and there should be a steady rise in conductivity for
at least 4 hours, but you should only need about 30 min .

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