CHE 4002

Plug Flow Reactor Rotameter Calibration

and Acid-Base Titration

Katharine Stroukoff

Shelli Schoolcraft

Devon Waren
Executive Summary

A calibration was performed on the rotameter for the plug flow reactor. The objective was to

develop an equation representing the relationship between the increments on the rotameter and

the volumetric flow rate in mL/s. A detailed procedure for titrating a weak acid and strong base

was also developed and tested. The objective was to design a reliable method for performing a

titration to verify the composition of products in the plug flow reactor.

To perform the rotameter calibration, three independent “stopwatch and bucket” trials were

recorded. Corresponding to every fifteen rotameter increments, a specific volume of water was

collected in a graduated cylinder and timed with a stopwatch. This data was used to calculate the

volumetric flow rate. The titration was conducted using 0.01M solutions of acetic acid and

sodium hydroxide with phenolphthalein and an electronic pH meter as indicators. Water was

chosen as the fluid for the rotameter calibration because it is nontoxic. Weak solutions of acetic

acid and sodium hydroxide were used in the titration because it is easier to measure larger

volumes in a burette and also to reduce the hazard.

The calibration equation for the rotameter was Rm=38.78Q-7.409, where Rm is the rotameter

reading and Q is the flow rate in mL/s. The slope is steep because there is a linear relationship

between the rotameter increments and the volumetric flow rate, but the maximum rotameter

reading is 150 and the maximum volumetric flowrate is only 3.8mL/s. The intercept should have

been zero, and is lower than expected. The titration was successfully carried out to ±0.2 pH

points as claimed on the pH meter’s instructions.

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The calibration equation for the rotameter is most accurate between readings of 30 and 120. It is

advisable to wear gloves that cover the arm to the elbow when adjusting the flow rate of the plug

flow reactor because fluid can splash onto the operator. The equation is valid for incompressible

liquid flow. The titration is most accurate when accurate measuring devices are used. Pipettes

should be favored over graduated cylinders, and utmost care should be taken when preparing

stock solutions.

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Table of Contents

Objectives…………………………………………………………………………………………5

Background………………………………………………………………………………………5

Approach

Development of Method of Analysis…………………………………………………………6

Description of Experimental Equipment……………………………………………………6

Safety and Environmental Information……………………………………………………..7

Experimental Procedures…………………………………………………………………….8

Results

Error and Uncertainty Analysis……………………………………………………………10

Discussion and Interpretation………………………………………………………………14

Conclusions and Recommendations…………………………………………………………...14

Appendix A: Figures and Tables.……………………………………………………………...16

Appendix B: Sample Calculations.......………………………………………………………...18

Appendix C: Raw Data…………………………………………………………………………19

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Objectives

The goal of this experiment was to develop a calibration reference for the rotameter of the plug

flow reactor with water as the feed. The other deliverable was a detailed procedure for

conducting a weak acid/strong base titration using a 0.01M acetic acid solution and a 0.01M

sodium hydroxide solution. The calibration of the plug flow rotameter and the titration

procedure can serve as resources for our colleagues conducting experiments in the future.

Background

Calibration of a rotameter with water as the feed:

Flow rate Q has a linear relationship with rotameter reading Rm. The purpose of a calibration

chart is to document this relationship in order to select appropriate rotameter readings for desired

flow rates.

Titration of a weak acid and strong base:

The following reaction took place during the titration:

HC2H2O(aq) + OH- Æ C2H3O2- (aq) + H2O

Phenolphthalein was used as an indicator because it changes color when the solution has a pH of

9, which is the equivalence point of this reaction. The equivalence point was calculated using

the equilibrium constant below.

1 1
Kb = = −10
= 1 .8 x10 9
( K bC 2 H 3O 2 ) (5 .6 x10 )
−

We mixed a 0.01M solution of sodium hydroxide by adding 0.020 grams solid sodium hydroxide

salt to 500mL DI water.

moles of solute
M =
liters of solution

Where M is the molarity concentration of the solution.

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We mixed a 0.01 molar solution of acetic acid by adding 166.6 µL 18M glacial acetic acid to

300mL DI water. This amount was calculated using the following equation.

McVc = MdVd

Where

Mc is molarity of the concentrated solution

Vc is the volume of the concentrated solution

Md is the molarity of the dilute solution

Vd is the volume of the dilute solution 2

Approach

Development of Method of Analysis:

In order to analyze the variance and propagation of error in our measurements and calculations,

we used two main methods. We used standard deviation for our variance analysis as a simple

and effective method for calculating relative variances. For both the rotameter calibration and

the titration, we calculated the propagation of maximum and probable errors using the analytical

method. We chose this method because it provides a sound basis for the accuracy of our results.

Description of Experimental Equipment:

The equipment for the plug flow reactor consisted of a power strip, a reservoir tank, a centrifugal

pump, a rotameter, a heat exchanger, a plug flow reactor, a large beaker, two graduated

cylinders, and a stopwatch. The reservoir tank held several liters of water before circulation

through the apparatus. A ball valve attached to the outlet of the tank initiated flow, and the

centrifugal pump provided the pressure necessary to maintain flow in the entire reactor. We did

6
not utilize the heat exchanger in this experiment. The rotameter displayed increments that

corresponded to volumetric flow rates. The increment level was established using the fine

adjustment knob at the system outlet. See Appendix A1 for schematic.

The titration consisted of many standard items available in a chemistry lab. The equipment

included two empty reagent bottles, a 150mL beaker, a 50mL beaker, a scoopula, an electronic

balance, a 500mL graduated cylinder, a micropipette, a 50mL burette, a small reagent bottle, a

pH meter, certified pH 10 buffer, and a ring stand with rings. The stock solutions and

phenolphthalein filled the empty reagent bottles. The scoopula, balance, graduated cylinder, and

micropipette measured the components of the stock solutions. The pH 10 buffer calibrated the

electronic pH meter. The 150mL beaker contained the initial acid to be neutralized by titration.

See Appendix A2 for schematic.

Safety and Environmental Information:

The plug flow apparatus had minimal safety hazards associated with the flow components.

Water was kept clear of all nearby electrical equipment, and spilled drops were wiped dry

immediately. If a fluid other than water were used, it would be advisable to wear gloves that

cover the elbow when adjusting the flow rate because fluid splashes onto the skin.

When mixing stock solutions, it is imperative to handle materials such as glacial acetic acid with

care. Safety goggles and gloves must be worn at all times and hazardous reagents must be

handled in the fume hood. The risks associated with 0.1M acid and base solutions are minimal,

but spilled and splashed materials on the skin should be rinsed with excess water to prevent

irritation. Waste materials were poured into appropriately labeled containers denoting the

contents, date, and people responsible for the experiment.

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In case of an emergency involving the plug flow reactor, the procedure was to shut off the pump

and close the ball valve on the reservoir tank. If there were a spill of glacial acetic acid while

preparing the stock solution, the laboratory would have been evacuated of all occupants.

Experimental Procedures:

Rotameter Calibration:

Water at room temperature was poured into the large reservoir at the top of the system. The ball

valve at the base of the reservoir was turned to the open position and the water flowed into the

centrifugal pump. It was important to wait until water flowed into the pump to turn it on to

prevent cavitation. At the outlet of the system, we collected the water in a large beaker to

contain the outflow while the flow rate was adjusted. The level of the rotameter was controlled

by turning the fine adjustment knob nearest the outlet. Once a satisfactory rotameter reading was

achieved, the water was collected in a graduated cylinder and timed with a stopwatch until it

reached a pre-determined volume in the cylinder. The procedure was repeated for readings

ranging from zero to 150 in intervals of fifteen increments. To shut down the system, the

centrifugal pump was turned off first, and afterward the ball valve at the base of the reservoir

was switched to the off position.

Titration Procedure:

In order to ensure an accurate titration, stock solutions were carefully mixed using the most

accurate equipment available in the laboratory. A 0.01M solution of sodium hydroxide was

mixed using 0.200grams ground sodium hydroxide salt and 500mL DI water. A 0.01M solution

of acetic acid was mixed by adding 166μL 18M glacial acetic acid to 300mL DI water. A

1g/100mL solution of Phenolphthalein was created by adding 0.25grams Phenolphthalein

powder to 25mL DI water. Before beginning the titration, the electronic pH meter was calibrated

8
using approximately 25mL of a certified pH 10 buffer solution in a small beaker. Since the

volumes of the acid and base should be equal at the equivalence point, our group chose to begin

with 40mL 0.01M acetic acid and approximately five drops phenolphthalein in a 200mL beaker.

50mL 0.01M sodium hydroxide solution was poured into a 50mL burette and affixed to the ring

stand. The sodium hydroxide solution was initially added to the acetic acid solution in five mL

increments. At each increment, the pH of the acetic acid solution and the volume of the sodium

hydroxide solution consumed were recorded. Once 30mL of sodium hydroxide was consumed,

the pH of the acetic acid solution was recorded after every 1.0mL sodium hydroxide added.

When the acetic acid solution began to turn pink, the sodium hydroxide solution was added in

increments of 0.5mL, and the pH was tested at each increment. When the solution in the flask

remained pale pink, the titration was past complete. The volume previous to that measurement

was the proper volume of sodium hydroxide. This visual indication confirmed what the pH

meter already showed. At the conclusion of the titration, all neutralized materials were

combined in a labeled waste canister. The stock solutions were saved for future use.

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Results

Error and Uncertainty Analysis:

We estimated that there would be a total of ±2 increments on the rotameter, ±1 second on the

stopwatch, and ±0.5mL on the graduated cylinder. The calibration equation we developed using

Excel is as follows:

The correlation coefficient is 0.981, and reflects a close relationship between the points and the

regression equation. In order to establish a 95% confidence interval for our data, we referenced

J. L. Devore’s Probability and Statistics for Engineering and the Sciences1 and used the

following equation:

⎛ 2 ×σ 2 2 ×σ 2 ⎞
⎜⎜ , ⎟⎟
⎝ 7.378 0.051 ⎠

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Where σ2 is the standard deviation squared. Our data were all well within the confidence

interval. Our slope was not significantly different from what we expected, but the y-intercept

was unusual. We expected the line to intercept at y=0, and the actual intercept is y=-7.4.

To calculate the propagation of error, we stacked the impacts of the three main uncertainties and

were able to ascertain that the maximum error on the measured volumetric flow rate should be

+0.34mL/s or -0.29mL/s. We calculated the probable error using the analytical method

presented in Dr. Rhinehart’s handout “Propagating and Reporting Uncertainty in Engineering

Calculations”3 and the equation:

σ y2 = σ x21 + σ x22

Where:

∂ 12 ∂ 22 ∂ × ∂2
σ x21 + σ x22 = + + 1
( N − 1) ( N − 1) ( N − 1)

And δ1=+0.34 and δ2=-0.29

Using the equation:

ε95%probable=±1.96σy

We calculated that the probable error was ±0.07mL/s. This result is consistent, because the

probable error is much less than the maximum error.

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The maximum propagation of error is depicted graphically on the following chart:

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For the measurement of the titration materials, we ran the first two trials using a graduated

cylinder to measure the acid and the second two trials using a 10mL pipette. As the results will

show, the pipette is more accurate by a minimum of ±0.1mL than the graduated cylinder. The

following chart illustrates the difference between the trials.

Trials 3 and 4 are much closer to an ideal titration curve than trials 1 and 2.

When considering the standard deviation of the four trials, it was very high, on the order of 1.5.

When the inaccurate trials 1 and 2 were eliminated, the standard deviation of the pH was quite

reasonable, and within the ±0.2 that the manufacturer of the pH meter claimed. We estimated

that in all the measurements, there was a variance of ±0.5mL in the graduated cylinder, ±0.1mL

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in the burette, ±0.1mL in the pipette (times 4 measurements is ±0.4), and ±0.2 in the pH. The

error that we found was higher than these, but that could be due to inaccuracies mixing the stock

solutions or deviations in concentration throughout the solution.

Discussion and Interpretation:

The speed of the flow through the plug flow reactor is quite slow, and the maximum measurable

flow rate is 3.7mL/s. The slope of the line is large, but this is due in part to the fact that the units

on the rotameter are significantly different than those of the flow rate. The maximum rotameter

reading is 150, which is much larger than the maximum flow rate of 3.7mL/s.

The titration was reasonably successful, even considering the first two trials. The most

inaccurate trial only deviated from the ideal by 7.5%, which is considered accurate in many

chemistry laboratories. The best trial deviated from the ideal by 1.8%. The accuracy of the

titration was aided by the use of dilute solutions of acetic acid and sodium hydroxide, which

made the visualization of the equivalence point easier by dispersing the concentration in a larger

volume.

Conclusions and Recommendations

The rotameter calibration equation is most accurate for flow rates corresponding to rotameter

readings of 30-120. In the lower ranges of the rotameter, the ball has a tendency to fluctuate

between 2 and 5 increments above and below the desired reading. In the higher ranges, changes

in the flow rate have no effect on the rotameter reading because the possible flow through the

system is much higher than what can be measured on the rotameter. It is advisable for the

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operator adjusting the flowrate to wear gloves that cover the arm to the elbow to protect against

splashes from harmful materials.

The titration is most accurate if performed using dilute solutions of the acid and base. Measuring

devices also play a role in the final outcome. Pipettes are more accurate than graduated

cylinders, and beakers are the least accurate. Masses of solids can be accurately measured up to

0.001 grams using the electronic balance. Micropipettes are useful for measuring small volumes

such as the volume of concentrated acetic acid required. Gloves and safety goggles should be

worn when conducting a procedure such as a titration, and the experiment should take place in

the fume hood.

Sources

1. Devore, Jay L., Probability and Statistics for Engineering and the Sciences, 6th edition,
Brooks/Cole, United States (2004).

2. Hurley, C.N., Masterson, W.L., Chemistry Principles and Reactions, Chapters 10 and14,
Brooks/Cole, United States (2004).

3. Rhinehart, R. Russell, “Propagating and Reporting Uncertainty in Engineering Calculations,”

Oklahoma State University, United States (2003).

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 Appendix A: Figures and Tables
A.1 Plug Flow Reactor Apparatus

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A.2 Titration Setup

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 Appendix B: Sample Calculations
Molarity

moles of NaOH needed

0.01M =
0.5 L of DI Water

Solving for moles of NaOH needed for the solution is 0.005moles of NaOH.

Then to find the mass of NaOH

39.97 gNaOH
0.005moles NaOH = 0.199 gNaOH
1moleNaOH

Diluted Volume

18 M (Vc ) = 0.01M (0.3 L )

Solving for Vc you get Vc equal to 166.6μL of the diluted liquid.

To find flow rate

20mL
Q=
10 sec

Q is equal to a flow rate of 2mL/s.

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 Appendix C: Raw Data

Rotameter Calibration Data:

Trial 1
reading time(s) flow rate(mL/s)
0 0.00 0.00
15 115.00 0.43
30 50.00 1.00
45 33.78 1.48
60 26.60 1.88
75 23.50 2.13
90 19.12 2.62
105 16.35 3.06
120 14.94 3.35
135 14.56 3.43
150 13.41 3.73
Trial 2
reading time(s) flow rate (mL/s)
0 0.00 0.00
15 111.90 0.45
30 53.30 0.94
45 33.84 1.48
60 26.69 1.87
75 22.91 2.18
90 19.35 2.58
105 17.18 2.91
120 16.38 3.05
135 14.85 3.37
150 14.00 3.57
Trial 3
reading time(s) flow rate(mL/s)
0 0.00 0.00
15 114.05 0.44
30 56.40 0.89
45 33.56 1.49
60 27.00 1.85
75 21.69 2.31
90 19.47 2.57
105 17.09 2.93
120 15.06 3.32
135 14.09 3.55
150 14.07 3.55

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20
21
The standard deviation between the three trials is
Standard
reading Deveation
0 0.000
15 0.006
30 0.057
45 0.006
60 0.015
75 0.091
90 0.024
105 0.081
120 0.163
135 0.092
150 0.096

Titration Data:

Trial 1
acid Base
(PH) (mL)

4.0 0.0
4.5 5.0
4.7 10.0
4.8 15.0
5.4 20.0
5.4 25.0
5.8 30.0
5.8 31.0
6.2 32.0
6.4 33.0
6.4 34.0
6.8 35.0
7.5 36.0
8.8 37.0
9.4 37.5
Trial 2
acid Base
(PH) (mL)

4.0 0.0
4.3 5.0
4.7 10.0
4.9 15.0
5.4 20.0
5.5 25.0
6.0 30.0
6.2 31.0
6.2 32.0

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 6.2 33.0
6.4 34.0
6.6 35.0
7.4 36.0
7.7 36.5
8.4 37.0
9.4 37.5
Trial 3
acid Base
(PH) (mL)

4.1 0.0
4.4 5.0
4.7 10.0
4.9 15.0
5.4 20.0
5.2 25.0
5.6 30.0
6.0 35.0
6.0 36.0
6.2 36.5
6.3 37.0
6.4 37.5
6.6 38.0
7.0 38.5
6.9 39.0
7.1 39.5
7.6 40.0
8.4 40.6
8.4 40.75
8.9 41.0
9.3 41.5
Trial 4
acid Base
(PH) (mL)

4.1 0.0
4.3 5.0
4.7 10.0
4.9 15.0
5.1 20.0
5.4 25.0
5.7 30.0
6.0 31.5
5.8 32.0
5.8 33.0
6.0 34.0
6.0 35.0
6.0 36.0
6.1 37.0
6.4 37.5

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6.6 38.0
6.6 38.5
6.9 39.0
7.1 39.5
7.5 40.0
8.2 40.5
9.2 41.0
9.7 41.5

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