Mixing Lab

OBJECTIVE

The purpose of this experiment is to explore non-ideal mixing in a continuously

stirred tank reactor (CSTR). Plots of concentration vs. time will be compared to
theoretical calculations. Residence time and experimental volume will be calculated to
determine dead volume.

INTRODUCTION

In a CSTR a species enters a reactor at a constant flow rate, is mixed, reacts and
eventually leaves the reactor. In this experiment there is no reaction so the species
leaving is the same as when it enters. If perfect mixing were the case, every molecule of
the species would spend the same amount of time in the reactor which would mean that
the reactor was perfectly mixed. However, in real life this is not the case. The amount of
time a molecule of a species spends in the reactor depends on the path it takes through it.
In practice, mixing performance in a reactor can be evaluated by running trials without a
reaction occurring and changing the factors affecting mixing such as agitator speed,
impeller design and flow rate.

EQUIPMENT

1. Stop watch
2. 6 – 100 mL volumetric flasks
3. 5 – 100 mL beakers
4. 100 mL graduated cylinder
5. 10 mL graduated pipet
6. 2 mL graduated pipet
7. 2 L graduated cylinder
8. Mixer: Fisher Scientific - StedFast Stirrir SL 300
9. Mixer Blades: Large - 5” diameter (x 2 blades), Small – 2.25” diameter
10. Tanks (approximate volume): Large – 18,200 mL, Small – 38,100 mL
11. Holding tank: 55 gallon drum
12. Pump: Cole-Parmer – GB – P35.PVS.A.B1
 Figure 1. Mixing Lab Schematic

CHEMICALS/MATERIALS

1. Tap water
2. NaCl

PROCEDURE

CREATING A STANDARD CURVE

Sodium Chloride Standards should be made up in room temperature tap water because
the experiment is run with tap water.

1. Make up a 10,000 mg/L stock NaCl standard.

a. Weigh out 5 grams of NaCl. Transfer to a 500 mL volumetric flask. Fill
the volumetric flask half full of room temperature tap water. Let the NaCl
dissolve and then dilute to the mark with room temperature tap water and
mix by inverting the flask several times. The stock standard will not have
to be made up each time.

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 2. Make up a standard curve by pipetting the following volumes of 10,000 mg/L
stock standard to 100 mL volumetric flasks. Dilute to the mark with room
temperature tap water and mix by inverting the flask several times.

Concentration mL of stock standard

a. 0 mg/L 0.0
b. 50 mg/L 0.5
c. 100 mg/L 1.0
d. 500 mg/L 5.0
e. 1000 mg/L 10.0

MIXING TANK EXPERIMENTAL SETUP

1. Before starting the experiment the following has to be done.

a. Insert the mixer in the reactor. Note the position of the stirring blade.
b. The volume of the reactor has to be determined. A 2 L graduated cylinder
is used to fill the reactor with tap water. Record the volume of liquid that
is needed to fill the reactpr so the liquid just starts to run over the outlet.
c. Determine the amount of NaCl that has to be weighed to make a 1000
mg/L solution based on the volume of the reactor. Weigh this amount out
and dissolve in the water in the reactor.
d. The volumetric flow rate of the Cole-Parmer Gear Pump has to be
determined for the pump setting(s) that you will be using in your
experiment. Use the 2000 mL graduated cylinder and a stopwatch. At the
pump setting you have selected, collect 1000 mL of water and record the
amount of time it takes to pump this amount. Five (5) trials can be input
into the data acquisition Excel spreadsheet template.
e. The water used in this experiment (supply holding tank and the reactor)
should be within ±3°C of room temperature.

COMPUTER AND DATA ACQUISITION MODULE PREPARATION

1. Turn on the laptop. Select the student account on the computer. The password
for the student account is student.
2. Start the data acquisition program by double clicking on the Windaq Hardware
Manager icon on the desktop.
3. A window opens up labeled DATAQ Instruments Hardware Manager.
a. Allow some time for the software to search for the data acquisition devices.
b. When Model DI-710-UL appears – select it if it is not already selected.
c. Click on the Start Windaq button on the bottom right.
4. A chart labeled DI-710 Acquisition 4E304DDO 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

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 one (differential input) and one data point should be collected every 10 seconds
[(1/10) = 0.1].
a. Click on Edit and then on Sample Rate. Sample rate should be set at 0.1
(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.
5. Turn on the conductivity meter. Leave the Ref Temperature, Slope, Zero and Cell
Constant settings alone. The function switch should be set to A.T.C. ON. The
range switch should be set to D. Temperature can be read by changing the
function switch to Temp. Do not change any of the switches while collecting data
into the spreadsheet. If the standards are run at the D range, all data has to be
collected using the D range.
6. Turn on the Masterflex pump power switch. Check the flow setting, a pump rate
of 3.0 mL/min is sufficient for this experiment. Place the first standard (0 mg/L)
into a 100 mL beaker. Insert the flow thru conductivity cell into the liquid. And
place the discharge tubes from the pump into the plastic bottle. When the data
acquisition program and spreadsheet is set up and ready to run (see below for the
spreadsheet setup), press the start button on the pump. Pump the standard
solution thru the cell until the conductivity reading has stabilized. Then start the
data acquisition system. 20 data points (1 every 10 seconds) will be collected for
each standard. The data acquisition system is actually importing voltage data into
the spreadsheet that corresponds to the conductivity shown on the conductivity
meter at each standard concentration. Additional standard solution may have to
be added to the beaker to insure there is enough for stabilizing the reading and
collecting the 20 data points. You should also record the actual reading on the
conductivity meter. Insert the conductivity probe into the next standard and
continue until all the standards have been done.

DATA ACQUISITION PROGRAM – EXCEL SPREADSHEET

In order to collect data into the Excel spreadsheet from the data acquisition program,
WinDaq 710 must be running. Start Excel by double clicking on the Excel icon on the
desktop. Load the template program located on the desktop. The name of the file is
Mixingcond Template.xlsx.
1. The first sheet labeled standarddataacq is used to collect the data for the standards.
On the spreadsheet menu bar click on Add-Ins. A second menu bar line appears
with a box that says Custom Toolbars. This box contains several icons, one of
which is used to set up the parameters needed to import the data into the
spreadsheet and start the data import into the spreadsheet. Click on the first icon
in this box and a dialogue window opens.
a. Under the Device Settings Tab check to see if DI-710-UL is highlighted
(by default it should be). If not click on it to highlight it.
b. Click on the Import Options Tab. In this Window under Mode select
Standard by clicking on the box (a check mark appears in the box). Under

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 Time Stamp do not select anything. In the “Starting Cell” entry field,
enter the cell designator for the upper left corner where you want to begin
putting the data. In column H of the spreadsheet this cell number is listed.
c. In the “Number of Rows” entry field enter the number of rows to fill
(number of data points). In column H of the spreadsheet the number of
rows is listed.
d. To begin data acquisition click on the Start Import button.
2. After all the standards have been run go to line 3. below.
3. The second sheet is labeled calibration-instrument. Switch to this sheet after the
standards have been run. The average of the voltage readings for the standards is
transferred to this sheet. A linear regression analysis has to be run on this data
which is shown in the upper left corner of the spreadsheet. If the linear regression
is run correctly, the concentration of NaCl will be calculated in the Concentration
template sheet while collecting the voltage data for the experimental runs.
4. The third sheet is labeled Concentration template. This sheet will be used to
collect the data during the experimental run. The sheet is set up so a number of
pieces of data can be entered into it. They include:
a. Pump flow rates – In fields N10-N15 up to five pump flow rates can be
entered if 1000 mL of water is collected during the pump calibration
procedure and time is input as seconds. The 5 data points will be averaged
and used in several calculations.
b. The tank volume can be entered into Field N19
c. The pump setting can be entered into Field N23
d. The number of grams of salt can be entered into Field N24
e. The reactor water temperature can be entered into Field N25
f. The supply water temperature can be entered into Field N26
g. The mixer speed can be entered into Field N27
h. When everything is set up in the reactor and ready for data collection,
click on the first icon in the custom tool bars to set the parameters for
collection of the conductivity data. Click on the Import Options tab if it is
not already open. Enter the starting cell as B8. Enter the number of rows
to fill. This number will be determined by 3 times the space time as a
minimum. If three space times is the total time that you are going to
collect data, the calculated number of rows can be entered. If you are
going to collect data until 99% of the salt is removed, it will take more
rows and you will have to stop the program manually. You can stop the
acquisition of data by clicking on the square in the box under Custom Tool
Bars at any time. The millivolt readings will be input into column B.
i. If you also want to record manual conductivity readings every 30 seconds,
this data can be entered manually into every third field in column G. In
order to calculate the concentration from the manually recorded
conductivity readings the conductivity readings for the standards would
have had to have been entered into columns L thru P on the
standarddataacq sheet during the running of the standards. Linear
Regression has to be run on this data so the constants can be used to
calculate the concentration. See number 5 below.

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5. The fourth sheet is labeled calibration-manual. This sheet is used if you also want
to do the calculations using the manual recorded conductivity readings from the
conductivity meter. The average of the manually recorded conductivity readings
from the meter for the standards have been transferred from the standarddataacq
sheet to the upper left hand corner of the spreadsheet in the column labeled
conductivity. A linear regression has to be run on this data in order to get the
constants used to calculate the concentration from the standard curve. These
constants are referenced by the Concentration template sheet to calculate the salt
concentrations from the conductivity data you recorded on that sheet.

02/2013

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 Department of Chemical Engineering
Stockroom Checkout Slip

Mixing ChE 4211

Name: Date:
(print name)

Lab No.: Lab 1 Tuesday 12:00 - 4:50 PM Lab 2 Thursday 12:00 - 4:50 PM

Lab No.: Lab 3 Tuesday and Thursday morning (9:30 – 11:50 AM)
(circle one)

Equipment Out In Equipment Out In

2-250 mL beakers Stopwatch

6-100 mL vol flasks 1-100 mL graduated cylinder

5-100 ml beakers 1-2000 mL graduated cylinder

pipet bulb 1-10 mL graduated pipet

1-500 mL volumetric flask 1-Spatula

Digital Thermometer

Name: ___________________________
(Signature)