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UNIVERSITY OF MINNESOTA DULUTH

DEPARTMENT OF CHEMICAL ENGINEERING


ChE 3211-4211

DIFFUSION OF A LIQUID

OBJECTIVE

The objective of this experiment is to determine the diffusion coefficient of 2M NaCl


solution in deionized water. You will use a data acquisition system from DATAQ and
WINDAQ/Lite software.

INTRODUCTION

Physical and chemical processes depend on the properties of the materials involved. 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 allows students to measure this property by a
well established technique.
The rate of diffusion is expressed by the equation:

∂C
J = -D (1)
∂x

J = the diffusion flux across unit area at right angles to the x-direction.
D = the diffusion constant.
∂C
= the concentration gradient in the x-direction.
∂x

The negative sign indicates the flow is going from high to low concentrations.

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If
J is in mole/cm2sec.
C is in mole/cm2sec.
x is in cm.
t is in sec.
D is in cm2/sec.

The Diffusion apparatus (See Figure 1) uses vertical capillaries 5 mm long with a diameter
of 1 mm, which restricts the diffusion to one dimension. The concentration at the lower ends is
assumed constant and the concentration at the top ends is effectively zero during the experiment.

V dk π d2 M
• = −D • N• (3)
C M dt 4 x

4Vx dk
D=- • (4)
π d NMC M dt
2

Where

V= the volume of water in the outer vessel in cm3.


x= the length of capillaries in cm.
d= the diameter of capillaries in cm.
N= the number of capillaries.
M= the molarity of the salt solution.
CM = the electrical conductivity change per unit molarity change (dilute solutions) Ω-1 M-1 or
Siemens M-1).
dk
= the rate of change of conductivity with time (Ω-1 sec-1 or Siemens sec-1).
dt

REFERENCES

Harned, H.S., Owen, B.B., "The Physical Chemistry of Electrolytic Solutions", 3rd Edition,
Reinhold Publishing Corporation, New York, 1958, pp. 254-255. (QD561.H3274 1958)

Armfield Engineering Teaching and Research Equipment, Diffusion of a Liquid Apparatus;


Instruction Manual, April 1993.

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Figure 1. Equipment used to determine the diffusion coefficient of a liquid

EQUIPMENT

1. Variable speed magnetic stirrer with stirring bar.


2. Specially designed diffusion cell.
3. Test vessel with cell holder (1 liter).
4. Conductivity cell (connects to the test vessel).
5. Conductivity meter.
6. 100 mL volumetric flask.
7. Stopwatch.
8. Ring stand
9. Small clamp
10. Eye dropper
11. 600 mL beaker

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CHEMICALS

1. 2 M NaCl solution.
2. Deionized water.

EXPERIMENTAL PROCEDURE

NOTE: Thoroughly clean all equipment and utensils with deionized (or distilled) water
before use!

Data Acquisition program

The data used in the calculations for this experiment will be collected using a Data
Acquisition system TI-700-PGL from DataQ and WINDAQ/Lite software which you will have
to learn how to operate before conducting the experiment.
There are a number of things that will have to done in this experiment. These include: learn
the operation of the TI-700 and software, setup the program parameters needed to collect data;
determine the conversion factor for converting the voltage values to the conductivity values;
determine the value of CM by calibrating the apparatus; and determine the diffusion coefficient.

**********

Determine the Conversion Factor to convert from voltage to conductivity units (Siemens) and
calibrate the apparatus to determine CM.

The output from the conductivity meter is a voltage value which the TI-700 system and
software program collects. A conversion factor will have to be determined so the voltage values
can be converted to conductivity values (Siemens). You will also have to determine the correct
range (right hand switch) to use on the WPA CM35 conductivity meter to measure the
conductivity. The setting of this range switch will affect the conversion factor. You will also
have to calibrate the apparatus in order to determine the value of CM. These two activities can be
done at the same time.

1. Fill the test vessel with one (1) liter of deionized water.
2. Connect the conductivity cell leads to the conductivity meter.
3. Turn on the meter.
4. Start the magnetic stirrer. Use the 1" magnetic stir bar and set the magnetic stirrer at
200 RPM.
5. Determine the amount of NaCl that should be weighed out to make up a liter of 0.001 M
NaCl solution. Weigh the NaCl on an analytical balance and transfer it to the test
vessel containing 1 liter of deionized water. Allow the sample to dissolve.

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6. Set the conductivity meter range switch (right hand switch) so the meter reading is on
scale.
7. Set up the data acquisition program to collect data for 10 minutes at 30 second intervals
(see instructions for data acquisition program).
8. Every time the voltage data is entered into a cell in the spreadsheet by the data
acquisition software, manually record the conductivity reading from the conductivity
meter into the computer. Do this for three of the six standards indicated in step 10
below. This will give you sufficient data to determine the relationship between the
voltage readings and the conductivity of the solution in Siemens so you can convert
from voltage to Siemens for your calculations.
9. Determine the amount of NaCl that should be weighed out to increase the concentration
by 0.0002 M. Weigh the NaCl on an analytical balance and transfer it to the test vessel
containing the NaCl solution in step 5 above. Let the salt dissolve. Using the data
acquisition program, collect 10 minutes of data at 30 second intervals.
10. Continue adding salt and collecting conductivity data until you have data for standards
in the following range 0.001, 0.0012, 0.0014, 0.0016, 0.0018 and 0.002 M.
11. After you have finished collecting the voltage data for all six standards, you can use the
voltage data and the data you manually collected from the conductivity meter for the
three standards to calculate a conversion factor to convert the voltage data to a
conductivity value in Siemens.
12. Convert your voltage readings for your standards into conductivity values using the
conversion factor calculated in step 11 above.
13. In the spread sheet calculate the average of each column of conductivity data.
14. Plot the concentration of NaCl versus conductivity (Siemens). The slope of this line is
the (CM).
15. After you are done, disconnect the meter from the conductivity cell and empty the test
vessel of liquid and rinse with deionized water to remove all traces of salt.

**********

Collect data to determine the Diffusion Coefficient.

1. Determine the volume of water needed to fill the test vessel to the black line. This
volume should be determined with everything in the test vessel that will be there during
the test. Includes the diffusion cell; the magnetic stir bar; and any baffles/other items
placed into the cell to modify the experiment..

2. Determine the number of capillaries in the diffusion cell.

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3. Make up a 2.0 M NaCl solution. Using an analytical balance, weigh into a small beaker
the calculated amount (gm) of NaCl to make up 100 mL of a 2 M NaCl solution.
Quantitatively transfer the crystals to a 100 mL volumetric flask. Fill the flask half full
of deionized water and swirl to dissolve the NaCl. After the NaCl has dissolved, dilute
to the mark with deionized water and mix.

4. Fill the test vessel containing a 1.0 inch magnetic stir bar with deionized water to
approximately one centimeter below the black fill line (this leaves room for the addition
of the diffusion cell).

5. Connect the wires from the test vessel conductivity cell to the conductivity meter. Turn
on the meter and set the range scale to the setting determined earlier.

6. Outside the test vessel carefully fill the diffusion cell with the 2 M NaCl solution so the
liquid just reaches the tops of the capillaries. Use an eyedropper to remove air from the
capillaries. Rinse the outside of the diffusion cell with deionized water and wipe off the
excess liquid with a soft tissue. Clamp the diffusion cell into its holder in the test
vessel.

7. Start the magnetic stirrer and set to run at 100 RPM.

8. Fill the test vessel with deionized water from a squeeze bottle to avoid splashing so the
capillary tops are submerged approximately 5 mm below the surface of the water.

9. At the same time as the capillary tops are submerged, start the data acquisition program
and collect data for a time period of at least 30 minutes.

10. The data acquisition program will write the data to an Excel spreadsheet.

11. Turn off the conductivity meter and disconnect the wires from the conductivity cell.

12. Remove the diffusion cell from the test vessel. The liquid in the cell can be disposed of
in the sink. Rinse the cell several times with deionized water.

13. The liquid in the test vessel can also be disposed of in the sink. Rinse the test vessel
several time with deionized water to remove all traces of the salt.

14. Prepare the test vessel and diffusion cell for the next test.

15. The test should be run in triplicate at a minimum. You may also want to investigate the
effect of different stirring speeds on the diffusion coefficient.

16. You may want to investigate the diffusion coefficient of another salt such as KCl.

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The velocity of the water across the capillary tips affects the rate of diffusion, and
consequently affects the diffusion coefficient. Different stir speeds will give different results.
The purpose of the stirring is to mix the solution in the test vessel so the conductivity cell can
measure the change in concentration of the salt solution. It is not there to affect the rate of
diffusion. Slow is better.

SAFETY NOTES

1. At a minimum safety glasses with side shields shall be worn. Safety goggles are the
preferred eye protection, if you have them, since there is a possibility of chemical
splashes.

WASTE DISPOSAL PROCEDURES

1. The salt solutions can be disposed of in the drain.

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ATTACHMENT 1
COMPUTER AND DATA ACQUISITION MODULE PREPARATION

1. Check out the required equipment (see equipment list on last page).
2. Assemble the data acquisition instrument DI 700 if it is not already assembled..
a. Connect the two leads to the proper terminals on the data acquisition module. The
data will be acquired thru a differential input on channel 1 so the positive lead should
be attached to number 37 and the negative lead to number 18.
b. Connect the two banana plugs to the conductivity meter (recorder output - Cond.).
Red is positive and black is negative.
3. Turn on the laptop. Select the student account on the computer. The password for the
student account is student.
4. Start the data acquisition program by double clicking on the WinDaq 700 USB0 icon on
the desktop.
5. A chart should appear and after 10 to 20 seconds you should see the cursor line start to
move. The proper settings should have been saved but may have been changed. Data
should be collected on channel one (differential input) and one data point should be
collected every 30 seconds [ 0.03333].
a. Click on Edit and then on Sample Rate. Sample rate should be set at 0.03333 (It
may be slightly different because of the clock rates.)
b. Click on Edit and then on Channels. In the line that says DI-700, channel 1 should
have a + and channel 9 should have a – in the box. If not, double click on channel 1.
If other channels are checked, delete them (instructions are at the bottom of the
form). Click OK to return to the chart.
6. Turn on the conductivity meter. Set the range switches as indicated on the Conductivity
meter.

DATA ACQUISITION PROGRAM

In order to collect data into the Excel spreadsheet from the data acquisition program, WinDaq
700 must be running. Start Excel by double clicking on the Excel icon on the desktop
1. On the spreadsheet is a small dialogue box that stays on the spreadsheet all the time
named WinDaq-XL. This box is used to set up the parameters needed to import the data
into the spreadsheet. Click on the round circle in this box and another dialogue box
opens.
a. Under “Select the WinDaq Device” click on 700 USB(0) to highlight it.
b. In the “Starting Cell” entry field, enter the cell designator for the upper left corner
where you want to begin putting the data.
c. In the “Rows to Fill” entry field enter the number of rows to fill (no of data points).
d. Click on start to start collecting data.

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2. Do not enter data into the spreadsheet while it is collecting data from Windaq. If you
press Enter or click on another cell to enter data into a cell at the same time that data is
being entered into a cell by the data acquisition system, the data acquisition system will
lock up and you may lose your data. You will have to restart the run. (There are times
when the computer will have to be rebooted.)
3. The spreadsheet should be saved after each run.
4. Data from additional experimental runs can be put to the right of the previous run. Data
can not be collected in columns beyond column HZ. Data from each experimental run
can also be put into a new sheet.

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Department of Chemical Engineering
Stockroom Checkout slip

Diffusion of a Liquid - DATAQ System ChE 3211

Name: Date:
(print name)

Lab No.: Lab 1 Tuesday 12:00 - 4:50 PM Lab 2 : Thursday 12:00 - 4:50 PM
(circle one)

Equipment Out In Equipment Out In


100 mL vol flask 600 mL beaker
1 - 1.0 inch magnetic stir bar 1 L graduated cylinder
Stopwatch 100 mL beaker
Spatula Clamp - 3 prong, small
Eyedropper Clamp holder

Name:
(Signature)

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