DSC 5 kac

Created on 14 04 28 by students, last modified by KAC on 14 08 25

Page 1 of 11
Week 1: DSC on PEG and PPG

Computer Setup:
1) Open the TA Instrument explorer icon on the desktop and select the Q20-
2367 icon.
2) Turn the large metal gas valve (very slightly) to allow gas flow. Be sure the
pressure doesnt exceed 20 psi.
3) Check the Sample Purge Flow under Flow Rate settings in the Notes tab on
the instrument interface and be sure that it is 50.00 mL/min.
4) Make sure the refrigerator power switch is on, and the second switch is set to
manual. Do not remove the piece of tape.
5) Under the control tab, select event and click On. The fridge will need time
to cool. Once it is ready, the Cool light on the fridge will turn on.

PEG Sample Prep:
Note: Whenever handling the sample pan, wear gloves and use calipers.
1) Using the tweezers, place a T-Zero aluminum sample pan on a weight boat (or
weigh paper) and place the weigh boat on a scale and tare it. Add 3-5 mg of
PEG to the sample pan and record the weight.
2) Using the tweezers, place a lid on top of the sample pan, so that the edges of
the lid are facing upwards.
3) Obtain two black dies from the kit: the smaller, flat die and the largest die.
4) Place the smaller, flat die in the top of the sample press. It will attach
magnetically.
5) Using the tweezers, place the lid and pan in the largest black die.
6) Place the larger lower die in the bottom of the sample press.
7) Press the sample pan and lid together by pushing down the lever of the sample
press. It is not necessary to press hard. TA recommends 5 presses.
8) Remove both dies from the press.
9) Using tweezers, remove the sample pan from the larger die.
10) Remove the large lid from the calorimeter.
11) Using tweezers, remove the inner two metal disk tops in the calorimeter and
set them aside.
12) Using tweezers, remove the bottom right pan (if one is present) and replace
with the pressed sample pan. The back left pan is the reference pan and should
not be moved. If the reference spot is empty, make your own reference pan.
13) Replace the two metal disk tops back in the calorimeter and place the large lid
back on top. The sample is now ready to be run.



DSC 5 kac
Created on 14 04 28 by students, last modified by KAC on 14 08 25

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PEG Computer Procedure:
1) In summary tab:
a) Set mode to modulated
b) Set test to Conventional MDSC.
c) Input sample size
2) In procedure tab:
- Set test to Conventional MDSC
a) Set amplitude to 0.5 C
b) Set modulation to 10 s.
c) Set ramp rate to 5 C per minute.
d) Set start temp to 25 C.
e) Set final temp to 85 C.
After setting procedure hit apply at bottom of screen
3) Change the file name before starting the run as the program automatically
saves data. Create a new folder to save your lab groups data. Use common
sense when creating file/folder namesthey should mean something when
you look at them later on.
4) Under the control tab at the top of the screen, click start to begin the run.
5) The data will not show up until the start temperature is reached.
6) After the run, under the summary tab, click the data file name icon to
makes sure the data was saved properly.
Re-run the PEG sample scan setting mode to standard and setting test to
Ramp. Keep all parameters (temp range and rate) the same as before.

PPG Sample Prep (This sample prep should be done while collecting PEG data)
1) Place a sample pan on a weight boat/paper on a scale and tare.
2) Use a microcapillary (glass tube) to dab the viscous PPG polymer into the
aluminum sample pan. Aim for 5 mg of PPG in the pan. Avoid getting the PPG
on the rim of the pan.
3) Repeat steps 2-13 of previous sample preparation. When pressing the sample,
be sure that none of the PPG/PEG gets squeezed out onto the rim of the pan. If
so, wipe it (and the press die) clean with a KIM wipe. Replace the press die
when finished.






DSC 5 kac
Created on 14 04 28 by students, last modified by KAC on 14 08 25

Page 3 of 11

PPG Computer Procedure:
1) In summary tab:
a) Set mode to modulated
b) Set test to conventional MDSC.
c) Input sample size. Make sure to convert 10 micro-liters to milligrams
using the sample density.
2) In procedure tab:
a) set amplitude to 0.5 C
b) Set modulation to 10 s.
c) Set ramp rate to 5 C per minute.
d) Set start temp to -90 C.
e) Set final temp to -45C.
3) After setting procedure hit apply at bottom of screen.
4) Change the data file name and the sample name before starting the run as
the program automatically saves data.
a) Under Summary: Data File Name, push the button at the
end of the row to choose file location and name
b) DO NOT CHANGE the directory until the run is over. The
file must stay in the ta\data\dsc file (within the network
folder) or the run will not save. After the run, you may
move the file
5) Under the control tab at the top of the screen, click start to begin the run.
6) The data will not show up until the start temperature is reached.
7) After the run under the summary tab, click the data file name icon to make
sure the data was saved properly.
8) Re-run the PPG sample scan setting mode to standard and setting test to
Ramp. Keep all parameters the same as before.

Shutting Down the Calorimeter and Waste Disposal (**To be done as soon as
measurements end**)

1) Switch off cooler (the big green switch).
2) Control Go to Standby Temp
2) Locate flange temperature in the software interface and wait for it to reach
about 25
o
C. This should take about 15 to 20 minutes.
3) After reaching room temperature, turn off the gas.
Do not turn off the calorimeter itself (do not press the big red button with the
inverted triangle).
4) Waste disposal: place the aluminum pans/lid in the labeled waste beaker.
Make sure the hood sample prep area is cleaned properly.
DSC 5 kac
Created on 14 04 28 by students, last modified by KAC on 14 08 25

Page 4 of 11

Analysis
1) Open desired data file in TA Universal Analysis Program.
2) Click and drag cursor to create a box around the desired peak, then click inside
this box to zoom in on desired peak.
3) Right click inside the peak and select Integrate Peak Linear. Two red
crosshairs will appear on either side of the screen.
4) Drag the crosshairs to either edge of the peak (the point where the slope starts
to increase or decrease, depending on if the peak is positive or negative). Use
your judgment to decide where the curve begins and ends.
5) Right click again and choose Accept Limits. The change in enthalpy should
appear with units of J/g. Save (analysis and data), and upload the scan files
and pdfs to UTBox and/or personal flashdrive.


Week 2: DSC on Liquid Crystals
Computer Setup:
1) Open the TA Instrument explorer icon on the desktop and select the Q20-
2367 icon.
2) Turn the large metal gas valve (very slightly) to allow gas flow. Make sure the
pressure doesnt exceed 20 psi.
3) Check the Sample Purge Flow on the Instrument interface and make sure
that it is ~50.00 mL/min.
4) Make sure the refrigerator power switch is on, and the second switch is set to
event.
5) Under the control tab, select event and click On. The fridge will need time
to cool. Once it is ready, the Cool light on the fridge will be on.

LC Sample Prep:
Note: Whenever handling the sample pan, wear gloves and use calipers.
1) Using the tweezers, place a T-Zero aluminum sample pan on a weight boat and
place the weight boat on a scale and tare it. Add 3-5 mg of LC to the sample
pan and record the weight.
Liquid crystals to be analyzed:
Pentyloxybenzoic acid
Hexyloxybenzoic acid
Heptyloxybenzoic acid
Nonyloxybenzoic acid
Decyloxybenzoic acid
2) Using the tweezers, place a lid on top of the sample pan, so that the edges of
the lid are facing upwards.
DSC 5 kac
Created on 14 04 28 by students, last modified by KAC on 14 08 25

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3) Obtain two black dies from the kit: the smaller, flat die and the largest lower die
located second from the bottom of the column in the kit.
4) Place the smaller, flat die in the top of the sample press. It will attach
magnetically.
5) Using the tweezers, place the lid and pan in the largest black die.
6) Place the larger lower die in the bottom of the sample press.
7) Press the sample pan and lid together by pushing down the lever of the sample
press. It is not necessary to press hard.
8) Remove both dies from the press.
9) Using tweezers, remove the sample pan from the larger die.
10) Remove the large lid from the calorimeter.
11) Using tweezers, remove the inner two lids in the calorimeter and set them
aside.
12) Using tweezers, remove the bottom right pan (if one is present) and replace
with the pressed sample pan. The back left pan is the reference pan. Hopefully
you have saved your empty reference pan from week 1.
13) Replace all three lids back in the calorimeter. The sample is ready to be run.
14) Repeat the procedure for the remaining liquid crystals. Replace the press die
when finished.

LC Computer Procedure:
1) In summary tab:
a) Set Mode to Standard
b) Set test to Ramp.
c) Input sample size
2) In procedure tab:
- Set test to Ramp.
a) Set ramp rate to 7 C per minute.
b) Set start temp to 80 C.
c) Set final temp to 165 C.
3) After setting procedure hit apply at bottom of screen.
4) Under the control tab at the top of the screen, click start to begin the run.
5) The data will not show up until the start temperature is reached.
6) After the run, under the summary tab, click the data file name icon.
7) In the pop up window, find the data you just obtained (by date and time) and
rename it so you can find it later.



Imaging the LCs
1) Locate the Olympus light microscope and the prepared LC samples (on a
DSC 5 kac
Created on 14 04 28 by students, last modified by KAC on 14 08 25

Page 6 of 11
microscope slide).
2) Place one of the LC slides into the heated sample chamber, and close the
hinged lid.
3) Turn on the microscope (switch at bottom front), and look through the
eyepiece to focus.
4) Turn on the temperature controller, and set the temperature (green lower
temperature is the set temperature, and the red upper temperature is the
sample temperature) to a value that is 5-10 degrees higher than a transition
temperature (which youve previously measured and recorded using the DSC).
The initial set temperature (green) should be 40
o
C.
5) As the sample temperature reaches the transition temperature(s), observe and
note how the LCs change. Watch as the LC cools back down. Rotate the
polarizer below the sample stage and observe the optical changes.
6) Remove the LC sample (be careful about the sample temperature use
tweezers).
7) Repeat for the other prepared LC sample(s).
8) When finished, set the green temperature back to 40
o
C. Turn off the
temperature controller and the microscope.

Shutting Down the Calorimeter (**To be done as soon as measurements end**)
1) Switch off cooler (the big green switch).
2) Control Go to Standby Temp
3) Locate flange temperature in the software interface and wait for it to reach
about 25
o
C. This should take about 15 to 20 minutes.
3) After reaching room temperature, turn off the gas.
4) Do not turn off the calorimeter itself (do not press the big red button with the
inverted triangle).
5) Waste disposal: place the aluminum pans/lid in the labeled waste beaker. Make
sure the hood sample prep area is cleaned properly.

LC Analysis:
1) Open desired data file in TA Universal Analysis Program.
2) Click and drag cursor to create a box around the desired peak, then click inside
this box to zoom in on desired peak.
3) Right click inside the peak and select Integrate Peak Linear. Two red
crosshairs will appear on either side of the screen.
4) Drag the crosshairs to either edge of the peak (the point where the slope starts
to increase or decrease, depending on if the peak is positive or negative). Use
your judgment to decide where the curve begins and ends.
5) Right click again and choose Accept Limits. The change in enthalpy should
DSC 5 kac
Created on 14 04 28 by students, last modified by KAC on 14 08 25

Page 7 of 11
appear with units of J/g. Save (analysis and data), and upload the scan files
and pdfs to UTBox and/or personal flashdrive.
6) Compare the data.




Week 3: Effect of Chain Length on Bilayer Membrane Phase Transitions

Computer Setup:
1) Open the TA Instrument explorer icon on the desktop and select the Q20-
2367 icon.
2) Turn the large metal gas valve (very slightly) to allow gas flow. Make sure the
pressure doesnt exceed 20 psi.
3) Check the Sample Purge Flow on the Instrument interface and make sure
that it is ~50.00 mL/min.
4) Make sure the refrigerator power switch is on, and the second switch is set to
event.
5) Under the control tab, select event and click On. The fridge will need time
to cool. Once it is ready, the Cool light on the fridge will be on.

Lipid Sample Preparation:
Note: Whenever handling the sample pan, wear gloves and use calipers.
1) Add 1.0 mL degassed, distilled water (high purity) to the small round bottom
flask containing the lipid. Swirl the flask under hot running water until a cloudy
white dispersion appears and the walls of the flask appear clear.
Samples to prepare:
High purity water (reference)
L--phosphatidylcholine, dimyristoyl (DMPC)
L--phosphatidylcholine, dipalmitoyl (DPPC)
L--phosphatidylcholine, distearoyl (DSPC)
2) Using the tweezers, place a T-Zero aluminum sample pan on a weight boat and
place the weight boat on a scale and tare it. Add 3-5 mg (5 to 10 microliters) of
redispersed lipid with a glass syringe to the sample pan and record the weight.
3) Using the tweezers, place a lid on top of the sample pan so that the edges of
the lid are facing upwards.
3) Obtain two black dies from the kit: the smaller, flat die and the largest lower die
located second from the bottom of the column in the kit.
4) Place the smaller, flat die in the top of the sample press. It will attach
magnetically.
5) Using the tweezers, place the lid and pan in the largest black die.
DSC 5 kac
Created on 14 04 28 by students, last modified by KAC on 14 08 25

Page 8 of 11
6) Place the larger lower die in the bottom of the sample press.
8) Press the sample pan and lid together by pushing down the lever of the sample
press. It is not necessary to press hard.
9) Remove both dies from the press.
10) Using tweezers, remove the sample pan from the larger die.
11) Remove the large lid from the calorimeter.
12) Using tweezers, remove the inner two lids in the calorimeter and set them
aside.
13) Using tweezers, place the reference pan filled with high purity water on the
top-left holder. Remove the pan on the bottom-right holder (if one is present)
and replace with the pressed sample pan.
14) Replace all three lids back in the calorimeter. The sample is ready to be run.
15) Repeat the procedure with the remaining bilayer membranes.
16) Replace the press die when finished.

Computer Procedure:
2) 1) In summary tab:
a) Set Mode to Standard
b) Set test to Ramp.
c) Input sample size
2) In procedure tab:
- Set test to Ramp.
a) Set heating rate to 1C per minute (60
o
C per hour).
b) Lower ramp rate increases sensitivity of the phase change measurement.
c) Set start temp to 8C for DMPC, 25C for DPPC, and 35C for DSPC.
d) Set final temp to 27C for DMPC, 55C for DPPC, and 65C for DSPC.
3) After setting procedure hit apply at bottom of screen.
4) Change the file name before starting the run as the program automatically
saves data.
5) Under the control tab at the top of the screen, click start to begin the run.
6) The data will not show up until the start temperature is reached.
7) After the run, under the summary tab, click the data file name icon to make
sure the data was saved properly.

Shutting Down the Calorimeter (*To be done as soon as measurements end*)
) 1) Switch off cooler (the big green switch).
) Locate flange temperature in the software interface and wait for it to reach
about 25
o
C. This should take about 15 to 20 minutes.
2) After reaching room temperature, turn off the gas.
3) Do not turn off the calorimeter itself (do not press the big red button with the
inverted triangle).
DSC 5 kac
Created on 14 04 28 by students, last modified by KAC on 14 08 25

Page 9 of 11
4) Waste disposal: place the aluminum pans/lid in the labeled waste beaker. Make
sure the hood sample prep area is cleaned properly.


Analysis
1) Open desired data file in TA Universal Analysis Program.
2) Click and drag cursor to create a box around the desired peak, and then click
inside this box to zoom in on desired peak.
3) Right click inside the peak and select Integrate Peak Linear. Two red
crosshairs will appear on either side of the screen.
4) Drag the crosshairs to either edge of the peak (the point where the slope starts
to increase or decrease, depending on if the peak is positive or negative). Use
your judgment to decide where the curve begins and ends.
5) Right click again and choose Accept Limits. The change in enthalpy should
appear with units of J/g. Save (analysis and data), and upload the scan files
and pdfs to UTBox and/or personal flashdrive.
Lab Report Summary Sheet (TA Copy)
Student: Fill out ALL white blocks.
Lead Author
(Printed):
Author of Exp. 1
(Printed):
SafeAssign
Submitted?
YES / NO
Lab #:
_____
Signature: Signature:

Author of Exp. 2
(Printed):
Author of Exp. 3
(Printed):
Report Grade:
Signature: Signature: Late penalty:
By our signatures, we agree that the work on this assignment
was split acceptably to ALL team members.
Grade inc. penalty:
Start Date: Report Due Date/Time Date/Time Received:
TA Comments: Grading TA:

DSC: Differential Scanning Calorimetry
Your report should follow the Lab Report format given in the Writing module on Canvas. Show any
plots called for, samples of all calculations, and including all things recommended for inclusion in the
report.
Global Feedback
A) Three strengths of the paper: B) Three areas for improvement:
1) 1)
2) 2)
3) 3)
Main Report Your Score
/
Out of a
possible
Overall Assessment

/
10
Abstract

/
10
Introduction

/
20
Experimental

/
15
Results and Discussion

/
10
Conclusion

/
10
Citations/Use of References

/
10
WritingGlobal Issues

/
5
WritingLocal Issues

/
10
TOTAL / 100
Lab Report Summary Sheet (Student Copy)
Student: Fill out ALL white blocks.
Lead Author
(Printed):
Author of Exp. 1
(Printed):
SafeAssign
Submitted?
YES / NO
Lab #:
_____
Signature: Signature:

Author of Exp. 2
(Printed):
Author of Exp. 3
(Printed):
Report Grade:
Signature: Signature: Late penalty:
By our signatures, we agree that the work on this assignment
was split acceptably to ALL team members.
Grade inc. penalty:
Start Date: Report Due Date/Time Date/Time Received:
TA Comments: Grading TA:

DSC: Differential Scanning Calorimetry
Your report should follow the Lab Report format given in the Writing module on Canvas. Show any
plots called for, samples of all calculations, and include all things recommended in the report.
Global Feedback
A) Three strengths of the paper: B) Three areas for improvement:
1) 1)
2) 2)
3) 3)
Main Report Your Score
/
Out of a
possible
Overall Assessment

/ 10
Abstract

/ 10
Introduction

/ 20
Experimental

/ 15
Results and Discussion

/ 10
Conclusion

/ 10
Citations/Use of References

/
10
WritingGlobal Issues

/
5
WritingLocal Issues

/ 10
TOTAL / 100