User:Matt Hartings/Notebook/NIST/2017/01/27: Difference between revisions

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# Ramp to -20 at 10 C/min
# Ramp to -20 at 10 C/min
# Repeat Step 2, 2 times
# Repeat Step 2, 2 times
==Partial Results==
The results shown below highlight the observed melting points. Note: Melting points were only observed in the first heating scans for each sample. They were not reversible. Also, for the PNI PAm variants, glass transitions were observed at higher temperatures (130-160) but are not listed/shown here. In the graphs below, the number in parentheses is the measured melting point, determined from the derivative graph [d(mW)/dT], which aren't shown here.
[[Image:20170127 mrh DSC 52CWax1.png|400px]]
[[Image:20170127 mrh DSC 66CWax1.png|400px]]
[[Image:20170127 mrh DSC 79CWax1.png|400px]]
[[Image:20170127 mrh DSC 93CWax1.png|400px]]
[[Image:20170127 mrh DSC 107CWax1.png|400px]]
[[Image:20170127 mrh DSC 121CWax1.png|400px]]
[[Image:20170127 mrh DSC 135CWax1.png|400px]]
[[Image:20170127 mrh DSC CarboxyPNIPAm1.png|400px]]
[[Image:20170127 mrh DSC PNIPAm1.png|400px]]
[[Image:20170127 mrh DSC PNIPAmCOOH1.png|400px]]
[[Image:20170127 mrh DSC PNIPAmNH21.png|400px]]
The thymine sample didn't show very much change at all.


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Revision as of 12:07, 30 January 2017

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Comments

Zeeshan sent me some samples to run on the DSC. These include waxes and several polymers.

Samples

The following include sample names, pan masses, sample masses, and DSC sample numbers. Aluminum Tzero pans from TA instruments were used. No caps or seals were used.

Sample Name Pan Mass (mg) Sample Mass (mg) DSC Sample #
135 Wax 42.42 2.60 26
79 Wax 42.60 4.70 27
52 Wax 42.97 6.13 28
107 Wax 42.36 1.77 29
93 Wax 42.65 6.15 30
121 Wax 42.40 1.95 31
66 Wax 42.47 1.93 32
Carboxy PNI-PAm 43.01 1.67 33
Thymine 42.86 3.33 34
PNI-PAm NH2 42.80 1.60 35
PNI-PAm COOH 42.64 2.76 36
PNI-PAm 42.25 1.41 37

Note: The mass of the 135 wax might be a little low. the balance was doing something funny. Check this later.

DSC run parameters

  1. Equilibrate at -20 C
  2. Isothermal for 2 minutes
  3. Ramp to 200 C at 10 C/min
  4. Isothermal for 2 minutes
  5. Ramp to -20 at 10 C/min
  6. Repeat Step 2, 2 times

Partial Results

The results shown below highlight the observed melting points. Note: Melting points were only observed in the first heating scans for each sample. They were not reversible. Also, for the PNI PAm variants, glass transitions were observed at higher temperatures (130-160) but are not listed/shown here. In the graphs below, the number in parentheses is the measured melting point, determined from the derivative graph [d(mW)/dT], which aren't shown here.

The thymine sample didn't show very much change at all.


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