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CBE Laboratory Guidelines – Summary

Spring 2018 – 461L


Becky Pinkelman

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Information on F drive

• F:Dept/cheme-bioe/Unit Operations Laboratories


• Syllabus & organization
• Updated Experiments
• May be updated during the semester –
• Supplemental information, e.g., screencast, analytical solution, data, etc.
• Updated Lab Manual
• Technical writing reference (more detailed explanation of expectations)
• Error propagation explanation

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• Standardized rubrics
Points Percent
• Scaled points to %
0 0.00
• Designated roles (reflected in Rubrics) 25 38.62
• Team Leader & Experimental Engineer 50 67.75
• Analyst 1 – Experimental 60 76.85
• Analyst 2 – Model 70 84.48
75 87.75
80 90.66
90 95.38
100 100.00

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• Standardized rubrics
• Designated roles (reflected in Rubrics)
• Team Leader & Experimental Engineer
• Analyst 1
• Analyst 2
• Lab notebooks are required & must be signed before leaving lab
• Follow guidelines in Lab Manual
• All prelabs, reports, etc., should submitted via D2L as pdfs.
• Safety
• CBE Safety Regulations – Will be sent home to change & lose points if
unprepared
• Long pants, long sleeves, hair pulled back, close-toed shoes (no boat shoes, toms,
ballet flats; we should not be able to see the top of feet and/or socks), safety glasses,
hard hats (first floor), no food or drinks

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Prelab Requirements

DUE BY 12:00 P.M. DAY BEFORE SCHEDULED LAB

• Prelab & JSA Form – fill out (available on F: drive)


• Purpose
• Qualitative Theory
• Experimental Plan
• Safety
• Operating Conditions
• Label P&ID – should be available for every experiment
• Data Analysis & Expected Results

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Memo Report Requirements

Length: Maximum 10 pages, 1.5 line spacing, 1” margins, 12 pt. font

From Lab Manual


• Abstract
• Background
• Includes theory, equations, experimental methods, safety
• Specific objectives/goals
• Results & Discussion (including associated error)
• Conclusions & Recommendations
• Appendices
• Supplemental information, sample calcs (including error)

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Oral Report Requirements

Time – 12-15 minutes + Questions

From Lab Manual


• Introduction
• Theory & equations
• Specific goals & objectives
• Materials & Methods (including Safety)
• Results & Discussion (including Error Analysis)
• Conclusions & Recommendations
**All team members required to submit individual abstracts
**Same requirements for posters
**Submit appendices with sample calcs, raw data (as a team)

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Executive Summary & Meeting Requirements

Length: Maximum 4 pages, 1.5 line spacing, 1” margins, 12 pt. font

Extended Abstract
• 3-4 pages – summarizes key concepts, ideas, & results
• Theory, experimental methods, safety
• Specific objectives/goals
• Results & Discussion (including associated error)
• Conclusions & Recommendations
• Appendices
• 5 pages of additional supplemental information
• Sample calcs (including error)

Meeting
• 15-30 minutes with each team –
• Discuss results & recommendations with supervisor

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For all reports…

• “Thread” or story that runs through the entire report/presentation


• Be succinct & concise – but include all necessary information
• Use common fonts, templates, & markers – you may not control printing
of the report &/or someone in your audience may be color blind
• Avoid using the first person (I, we, etc.)
• BUT replacing we with the team is not an acceptable replacement
• Use active & passive voice appropriately
• References – APA style (in text and reference list)
• See Lab Manual for examples
• OWL at Purdue – great source on examples

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For all reports… Examples

• Completion of the tests were carried out for the purpose of ensuring that system
would work properly
• Tests were completed to ensure that the system will work properly
• There are several types of chromatography and the chosen method depends on
the phase considered for analysis as well as the material used for separation
• Chromatography systems are categorized according to the type of carrier fluid (gas or
liquid). In addition, the stationary phase may be a liquid or solid.
• Density of the air must also be calculated from known atmospheric and testing
conditions.
• The density of the air was calculated from the ideal gas law, using the atmospheric
pressure indicated by the mercury manometer in the lab.
• Overall, various characteristic behavioral trends were determined for the four
control logic types investigated.
• Rise time, overshoot, and offset values were measured for the four different control
systems.

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For all reports… Examples

• The need in the company for great increases in the are of the new system
design has necessitated the addition of analyst/programmers to the division of
system development.
• Because the company is greatly increasing its system design work, it must hire
additional analyst/programmers in the system development division.
• A report appeared in a British medical journal. Migraine headaches might be
caused by food allergies. The journal published a report of research. The
research was conducted at two London hospitals. The research took two years.
Thirty-three patients had food allergy-related migraine attacks.
• According to a research report published in a British medical journal, migraine
headaches might be caused by food allergies. The two-year study, conducted at two
London hospitals, showed that thirty-three patients completing the tests had migraine
attacks related to food allergies.

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Abstracts

Maximum 1 page, 1.5 spacing, 1” margins, 12 pt. font


• A concise summary that represents the essence of the work that was
done. In a few sentences, the Abstract tells what was done, why it
was done, how it was done, key results, and the essential
conclusions.
• Abstracts should demonstrate thorough understanding of the
experiment, results, conclusions, and recommendations.

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Abstracts – Example

This experiment will determine what will make enzymes affective and what
will make them ineffective. We tested different sample of enzymes in a
spectrophotometer but two contained no enzyme; these acted as blanks
for the other samples. The four remaining samples contained Catecholase
ranging from 0.5 ml to 1.75 m. The second half of the experiment
contained four test tubs with a constant amount of Catecholase, but the
pH levels ranged from four to eight. It was found that if the enzyme was
present in large amounts, then the absorption rate was high, and if the pH
level ranged from 6 to eight then the absorption rate was high. Therefore it
can be said that enzymes work well in neutral pH levels and in the large
amounts.

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Abstracts – Example

This experiment was performed to determine the factors that positively


influence enzyme reaction rates in cellular activities since some enzymes
seem to be more effective than others. Catecholase enzyme activity was
measured through its absorption rate in a spectrophotometer, using light with
a wavelength of 540 nm. We compared the absorbance rates in samples with
varying enzyme concentrations and a constant pH of 7, and with samples with
constant enzyme concentration and varying pH levels. The samples with the
highest enzyme concentration had the highest absorption rate of 24 percent.
This suggest that a higher concentration of enzymes leads to a greater
production rate. The samples with pH between six and eight had the greatest
absorption rate of 70 percent compared to an absorption rate of 15 percent
with a pH of four; this suggest that Catecholase is most effective in a neutral
pH range from six to eight.
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Safety

• Go beyond wear proper PPE,


water/steam/electricity
• Hazards associated with equipment
• Look at & reference P&ID
• Close NO valve
• Industrial perspective

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Results & Discussion

• Directly address all of your specific goals/objectives


• Discuss choice of parameters
• Interpret results in light of presented theory
• Discussion of error sources & implications should be included
• Be specific – use quantitative values as much as possible & avoid
emotional judgements
• Original: The results were good… The data points weren’t too far apart…
• Rewrite: The average yield was 99 % of the theoretical… The data points
were 51.1 and 52.5 cm/s with a mean velocity of 51.8 cm/s and a standard
deviation of 0.00 cm/s. The precision was within the instrument’s published
range.

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Error Analysis

• Discuss sources of error, including an estimation of the error associated


with each measurement
• Do not publish garbage data and say “there must have been an error”… It
is the troubleshooting skills and understanding that make us good
engineers!
• Include error propagation
• % difference from theoretical (if available)
• Significant figures – think logically about what you are reporting!
• 10,478.049 kW with an error of 5% ???
• 10,500 + 500 kW

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Conclusions

• Directly address all of the goals/objectives


• No discussion should be included
• Does the data make sense?
• What is the important information to present?
• Be careful that your conclusions & recommendations do not imply that
you were unable to adequately conduct the experiment
• Basically asking for a poor performance rating

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Recommendations

• Must improve the results of the project (model and/or experiment) –


this is great place to use error analysis
• Two parts for this lab
• Based on your results – what would be your recommendation(s) to your
supervisor?
• Substantive recommendation(s) on how the apparatus or available
equipment, procedure, etc., could be improved
• If including the purchase & installation of additional equipment or
replacements, recommend specific model numbers & vendors

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Appendices –

• Sample calculations
• Data analysis
• Error analysis
• Raw data
• Properly formatted excel sheet (or appropriate file type)
• Submitted as separate document to D2L
• Notebook pages

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Type your own equations to avoid poor copy-
paste quality

vs.
∆𝑃𝑉
𝑂𝑃 = 𝐾𝐶 ∙ 𝜀 + ෍(𝑇𝐼 𝜀∆𝑡) − 𝑇𝐷
∆𝑡

Where OP is the controller output,


Kc is the controller gain,
ε is the difference between the measured variable and the setpoint
TI is the reset time
TD is the derivative constant
t is time
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Making nice figures: SCALE AND COLOR

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Making nice figures: DATA VS. MODEL

1.5

0.5

0 Series1
-20 0 20 40 60 80 100 120 140 160 180

-0.5

-1

-1.5

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Writing good figure captions

“Figure 2”
Figure 2: Tank level Vs. Time
“Figure 2: Tank level as a function of time”
“Figure 2. Response of the measured variable (level) to a step change in
setpoint from 10 inches to 12 inches.

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Other table/figure notes

• Graphs should have axis labels with units. Easy to read


numbers on axes ( 1.2e-9 not 0.0000000012)
• Label tables and figures with a number (Word has a tool to
automatically update your figure/table numbers – see
captions under references tab.

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In-Class Exercise – What is correct and/or
incorrect in this figure?

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Cite your sources!
Plagiarism is illegal!

If you do need to copy someone else’s work then it must be


presented in quotes and referenced.
If you incorporate someone else’s work/ideas into your words
and thoughts then you must reference them, i.e. you must give
them credit for their work/ideas.
Every figure or picture that you use that YOU did not create requires a
citation.
Every equation that you use that YOU did not derive from basic principles
requires a citation.
Every statement of fact that is NOT common knowledge requires a citation.
 Example: Evaporators are commonly used in industry to evaporate milk.

 Required to use APA style


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ERROR PROPAGATION

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WHY PERFORM ERROR ANALYSIS?
Prior to Experiments
• Determine what procedures should be used for
measurement
• Identify appropriate instruments and
procedures to improve precision and accuracy

After Data is Collected


• Determine if measured phenomena are real
• Determine if hypotheses can be generated
based on results of experiments
• Determine if data agrees with theory

2
9
DEFINITIONS
• Error is defined as the difference between an
observation (directly measured or calculated
from measurements) and the true value
Error = Observation – True
• Uncertainty (Imprecision) is defined as the
estimate of the systematic and/or random errors
inherent in the measurement or calculation
• Bias (Inaccuracy) is defined as the systematic
deviation from the truth

3
0
TYPES OF ERRORS
• Blunders
• Illegitimate error resulting from misreading a gauge or
a calculation mistake
• Systematic
• Reproducible inaccuracy introduced by imperfect
equipment, calibration, or technique
• Can be quantified by understanding the equipment
and technique
• Random
• Measure in fluctuation in results during repeated
experimentation
• Can be quantified by repetition of measurements

WHICH TYPE OF ERROR IS THE EASIEST


(MOST DIFFICULT) TO REDUCE?

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MEASURES OF ERRORS
• Accuracy
• Measure of how
close a
measurement comes
to the true value
• Precision
• Measure of how
closely repeated
measured values
agree with each
other

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UNIT OPS ERROR ANALYSIS
• Pre-Experiment Error Evaluation
• List the variables that will be evaluated during the
experiment and measurements required in the execution of
the experiment
• Provide a qualitative description of the potential
uncertainties
• Describe whether bias errors or random errors are
expected to be of greater concern and techniques that
could be used to minimize the impact of errors
• Describe your approach to minimize or eliminate blunder
errors

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UNIT OPS ERROR ANALYSIS
• Include a table with the associated uncertainty for each
variable, including instruments
• Include the variable, units, value, error, and how
determined (e.g. assumed, data variance, propagated)
Instrument Smallest Uncertainty Source
Increment
Pressure gauge 1 psi ±0.25 psi Vendor literature
Pipet 1 ml ±0.5 ml Rule of thumb
Balance 0.1 g 0.03 g Vendor literature

• Include calculations in an Appendix showing the error


propagation for key variables
2 2 2
𝜕𝑓 𝜕𝑓 𝜕𝑓
𝛿𝑍 = 𝑑𝑋1 2 + 𝑑𝑋2 2 + ⋯+ 𝑑𝑋𝑛 2
𝜕𝑋1 𝜕𝑋2 𝜕𝑋𝑛

34
UNIT OPS ERROR ANALYSIS
• Include a table with the calculated values and
the associated error
• Include a conclusion from your error analysis,
including recommendations to reduce error
• Be cognizant of significant figures when
reporting results

Trial Flow Rate (gpm) Error % Error

1 1.0 ±0.10 gpm 1.0%

2 2.0 ±0.10 gpm 0.50%

3 3.0 ±0.10 gpm 0.33%

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SIGNIFICANT FIGURES
• Proper use of significant figures is a critical
piece of reporting results and associated
uncertainty
• Significant figures for exact measurements (e.g. number of
students currently in the lecture hall)?
• Significant figures for defined numbers (e.g. speed of light,
length of meter)?
• A rough indication of precision is given by the
use of significant figures
• Write a number with all digits known to be correct, plus one
doubtful figure

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ERROR PROPAGATION
• Calculations involving quantities which are
uncertain will lead to uncertainty in the result
• If z is a function of x (z = f(x)), z will contain some
uncertainty related to the uncertainty in x (z ± dz = f (x ± dx))
• There are mathematical relations that allow an
estimate of the uncertainty in a calculated
variable

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ERROR PROPAGATION
• If we measure variable X with an error of dx and
variable Y with an error of dy, what is the error in
the calculated variable, Z, if:
• Z = AX, where A is a numerical constant such as p
•Z=X+Y
•Z=X–Y
• Z = XY
• Z = X/Y
• Z is a general function of many quantities

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ERROR PROPAGATION
• General rule for combination of errors
• If Z = f(X1, X2, X3, …, Xn)

2 2 2
𝜕𝑓 2 𝜕𝑓 2 𝜕𝑓
𝛿𝑍 = 𝑑𝑋1 + 𝑑𝑋2 + ⋯+ 𝑑𝑋𝑛 2
𝜕𝑋1 𝜕𝑋2 𝜕𝑋𝑛

In the text, you could say Z was found to be 3.3 ± 4% OR 3.3 ± 0.13.

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ERROR PROPAGATION EXAMPLE 2
• In the distillation experiment, the refractive index is measured
to determine the mass fraction of ethanol in the sample
• The mass fraction is related to the refractive index by the
following polynomial:
Mass Fraction = 𝐴 ∗ 𝑅𝐼 3 + 𝐵 ∗ 𝑅𝐼 2 + 𝐶 ∗ 𝑅𝐼 + 𝐷

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ERROR PROPAGATION EXAMPLE 2
• Per instrument specifications, the uncertainty in refractive
index is equal to 0.00005 (d(RI))
• To calculate the resulting error in mass fraction for this
measurement and the resulting uncertainty in mass fraction,
evaluate the formula:
2
𝜕𝑓 2 𝜕𝑓 𝜕𝑓
𝛿𝑍 = 𝑑𝑋1 = 𝑑𝑋1 = 𝛿𝑅𝐼
𝜕𝑋1 𝜕𝑋1 𝜕𝑅𝐼

𝜕𝑓
𝛿 𝑀𝑎𝑠𝑠𝐹𝑟𝑎𝑐 = 𝛿𝑅𝐼
𝜕𝑅𝐼
= 3 ∗ 𝐴 ∗ 𝑅𝐼 2 ∗ 𝛿𝑅𝐼 + 2 ∗ 𝐵 ∗ 𝑅𝐼 ∗ 𝛿𝑅𝐼 + C ∗ 𝛿𝑅𝐼

41
ERROR PROPAGATION EXAMPLE 2
• Per instrument specifications, the uncertainty in refractive
index is equal to 0.00005 (d(RI))
• For a refractive index measurement of 1.3524, the predicted
mass fraction of ethanol is 0.28
• The propagated uncertainty in mass fraction is 0.035
• Therefore, the mass fraction can actually range from 0.245
up to 0.315

𝜕𝑓
𝛿 𝑀𝑎𝑠𝑠𝐹𝑟𝑎𝑐 = 𝛿𝑅𝐼
𝜕𝑅𝐼
= 𝐴 ∗ 𝑅𝐼 2 ∗ 𝛿𝑅𝐼 + 𝐵 ∗ 𝑅𝐼 ∗ 𝛿𝑅𝐼 + C ∗ 𝛿𝑅𝐼

42
CBE 461L Lab Schedule
Period Section Activity
Tuesday M052 Thursday M051 Distillation Triple Effect Reactor Absorber Solid-Liquid
1 9-Jan 11-Jan INTRODUCTION
2 16-Jan 18-Jan Team 1 Team 2 Team 3 Team 4 Team 5
3 23-Jan 25-Jan
4 30-Jan 1-Feb Team 5 Team 1 Team 2 Team 3 Team 4
5 6-Feb 8-Feb
6 13-Feb 15-Feb Team 4 Team 5 Team 1 Team 2 Team 3
7 20-Feb 22-Feb
8 27-Feb 1-Mar No Lab
9 6-Mar 8-Mar SPRING BREAK
10 13-Mar 15-Mar No Lab
11 20-Mar 22-Mar ORALS
12 27-Mar 29-Mar Team 3 Team 4 Team 5 Team 1 Team 2
13 3-Apr 5-Apr
14 10-Apr 12-Apr Team 2 Team 3 Team 4 Team 5 Team 1
15 17-Apr 19-Apr
16 24-Apr 26-Apr No Lab
17 1-May 3-May FINALS

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CBE 461L Report Schedule
Period Section
Tuesday M052 Thursday M051 Assignment Due
1 9-Jan 11-Jan
2 16-Jan 18-Jan Memo #1
3 23-Jan 25-Jan
4 30-Jan 1-Feb exective summary + meeting Memo #1
5 6-Feb 8-Feb
6 13-Feb 15-Feb Orals + indiv. Abstract exective summary
7 20-Feb 22-Feb meeting
8 27-Feb 1-Mar
9 6-Mar 8-Mar
10 13-Mar 15-Mar
11 20-Mar 22-Mar Orals + indiv. Abstract
12 27-Mar 29-Mar Memo #2
13 3-Apr 5-Apr
14 10-Apr 12-Apr Poster + indiv. Abstact Memo #2
15 17-Apr 19-Apr
16 24-Apr 26-Apr
17 1-May 3-May Poster + indiv. Abstact

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M051 Tuesday 14:00-16:50
Team 1 Team 2
1
2
3
4

Team 3 Team 4
1
2
3
4

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M052 Thursday 14:00-16:50
Team 1 Team 2
1
2
3
4

Team 3 Team 4
1
2
3
4

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