User:Moira M. Esson/Notebook/CHEM-581/2012/09/07 - Revision history

Karlena L. Brown: /* PVOH(MW 130,000) Films */

Karlena L. Brown — Mon, 22 Oct 2012 22:59:16 GMT

PVOH(MW 130,000) Films

←Older revision		Revision as of 22:59, 22 October 2012
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	\|}		\|}
	'''Note''':Complete dissolution of the PVOH required a longer amount of stirring(~2hours) and the addition of more deionized H<sub>2<sub/>O. To prompt complete dissolution, solutions were transferred to larger beakers(~50mL) with larger amounts of H<sub>2<sub/>O.		'''Note''':Complete dissolution of the PVOH required a longer amount of stirring(~2hours) and the addition of more deionized H<sub>2<sub/>O. To prompt complete dissolution, solutions were transferred to larger beakers(~50mL) with larger amounts of H<sub>2<sub/>O.
		+
	==Crosslinking PVOH Films==		==Crosslinking PVOH Films==
	Standard Protocol for Crosslinking of films:		Standard Protocol for Crosslinking of films:

Moira M. Esson: /* DSC on PVOH Films */

Moira M. Esson — Tue, 25 Sep 2012 00:32:24 GMT

DSC on PVOH Films

←Older revision		Revision as of 00:32, 25 September 2012
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	# Cut and weigh out ~ 280 - 320mg of PVOH film sample to place in the Tzezo pan		# Cut and weigh out ~ 280 - 320mg of PVOH film sample to place in the Tzezo pan
	# Once each sample is placed in the pan, then place the lid onto the pan		# Once each sample is placed in the pan, then place the lid onto the pan
-	# Use a ~~Tzezo~~ press to secure and press the lid tightly over top the sample within the pan	+	# Use a Tzero press to secure and press the lid tightly over top the sample within the pan
	# Open TA instrument explorer on computer. Select instrument to be used(in this case DSC)		# Open TA instrument explorer on computer. Select instrument to be used(in this case DSC)
	# On control button, click event to create a new event		# On control button, click event to create a new event
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	# To modify a run, go to the experimental command and run a method edit		# To modify a run, go to the experimental command and run a method edit
	# Save all changes made to an experimental run in order to analyze samples		# Save all changes made to an experimental run in order to analyze samples
-	*Further notes on DSC program
-	~~# Set flange temperature at -80°C~~
-	~~# Equilibrate at 20.00°C~~
-	~~# Ramp 20.00°C/min to 240.00°C~~
-	~~# Ramp 20.00°C/min to 20.00°C~~
-	~~# Repeat steps 5 and 6 one time~~
	<br>		<br>
	To Collect the information from the DSC:		To Collect the information from the DSC:

Moira M. Esson: /* DSC on PVOH Films */

Moira M. Esson — Tue, 25 Sep 2012 00:31:13 GMT

DSC on PVOH Films

←Older revision		Revision as of 00:31, 25 September 2012
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	'''General Protocol for DSC:'''		'''General Protocol for DSC:'''
	# Weigh out the mass of a Tzero pan+Tzero lid(Record this measurement)		# Weigh out the mass of a Tzero pan+Tzero lid(Record this measurement)
		+	# Cut and weigh out ~ 280 - 320mg of PVOH film sample to place in the Tzezo pan
		+	# Once each sample is placed in the pan, then place the lid onto the pan
		+	# Use a Tzezo press to secure and press the lid tightly over top the sample within the pan
	# Open TA instrument explorer on computer. Select instrument to be used(in this case DSC)		# Open TA instrument explorer on computer. Select instrument to be used(in this case DSC)
	# On control button, click event to create a new event		# On control button, click event to create a new event
		+	# To create a new event or run, click either the apply or append commands
		+	# To modify a run, go to the experimental command and run a method edit
		+	# Save all changes made to an experimental run in order to analyze samples
		+	*Further notes on DSC program
	# Set flange temperature at -80°C		# Set flange temperature at -80°C
	# Equilibrate at 20.00°C		# Equilibrate at 20.00°C
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	# Ramp 20.00°C/min to 20.00°C		# Ramp 20.00°C/min to 20.00°C
	# Repeat steps 5 and 6 one time		# Repeat steps 5 and 6 one time
-		+	<br>
-		+	To Collect the information from the DSC:
		+	# Click on export data file command
		+	# Go to file and plot signals command
		+	# Export the information obtained and save it(if possible save on flash drive)
		+	# Go to signals command and select signal section, then time command underneath
		+	# Select the analyze data command, then afterwards the integrate peaks command underneath
		+	# Accept values established by integrating the peaks
		+	# Click the analyze data command again to assign the glass transition value
		+	# Select the area in which the glass transition point is seen and integrate that information
		+	# Accept the values established from the glass transition point

	* About 3 mg ± 20% PVOH film was placed in a DSC pan.		* About 3 mg ± 20% PVOH film was placed in a DSC pan.

Moira M. Esson: /* DSC on PVOH Films */

Moira M. Esson — Tue, 25 Sep 2012 00:20:29 GMT

DSC on PVOH Films

←Older revision		Revision as of 00:20, 25 September 2012
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	** Sample mass: 3.15 g		** Sample mass: 3.15 g
	* [[Media:PVOH(22K), 15%M, H3PO4.pdf\|Graph of heat flow of uncrosslinked PVOH (MW 22000) + 15% maleic acid + H<sub>3</sub>PO<sub>4</sub>]].		* [[Media:PVOH(22K), 15%M, H3PO4.pdf\|Graph of heat flow of uncrosslinked PVOH (MW 22000) + 15% maleic acid + H<sub>3</sub>PO<sub>4</sub>]].
		+	** Two possible glass transitions at 105.79°C and at 155.16°C were observed(able to observe on graph by looking at the change in slope). Running DSC on the sample a second time may clarify which is the true glass transition temperature.
		+	** Two sharp peaks at 144.66°C and at 155.64°C were observed. A reaction may have occurred at these temperatures or a phase change may have occurred
	* [[Media:PVOH(22K), H3PO4.pdf‎\|Graph of heat flow of uncrosslinked PVOH (MW 22000) + H<sub>3</sub>PO<sub>4</sub>]].		* [[Media:PVOH(22K), H3PO4.pdf‎\|Graph of heat flow of uncrosslinked PVOH (MW 22000) + H<sub>3</sub>PO<sub>4</sub>]].
		+	** A glass transition was observed at 82.61°C.
		+	** A sharp peak was observed at 179.47°C. This may be caused by a reaction or phase change.

	==Notes==		==Notes==

Moira M. Esson: /* DSC on PVOH Films */

Moira M. Esson — Tue, 25 Sep 2012 00:17:30 GMT

DSC on PVOH Films

←Older revision		Revision as of 00:17, 25 September 2012
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	DSC will be used to determine the different thermal transitions of the various films		DSC will be used to determine the different thermal transitions of the various films
	'''General Protocol for DSC:'''		'''General Protocol for DSC:'''
-	#Weigh out the mass of a Tzero pan+Tzero lid(Record this measurement)	+	# Weigh out the mass of a Tzero pan+Tzero lid(Record this measurement)
-	#	+	# Open TA instrument explorer on computer. Select instrument to be used(in this case DSC)
		+	# On control button, click event to create a new event
		+	# Set flange temperature at -80°C
		+	# Equilibrate at 20.00°C
		+	# Ramp 20.00°C/min to 240.00°C
		+	# Ramp 20.00°C/min to 20.00°C
		+	# Repeat steps 5 and 6 one time

Moira M. Esson: /* Solubility of PVOH Films */

Moira M. Esson — Fri, 21 Sep 2012 18:10:42 GMT

Solubility of PVOH Films

←Older revision		Revision as of 18:10, 21 September 2012
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	#Place ~0.1g of film to be tested in a 100mL beaker.		#Place ~0.1g of film to be tested in a 100mL beaker.
	#Add a stir bar to the beaker		#Add a stir bar to the beaker
-	#Place plastic ~~mesh~~ above the film and stir bar	+	#Place plastic stemless buchner funnel top above the film and stir bar
	#Using a plastic pipette(s) to hold down the plastic mesh, add ~75mL of deionized H<sub>2<sub/>O to the beaker.		#Using a plastic pipette(s) to hold down the plastic mesh, add ~75mL of deionized H<sub>2<sub/>O to the beaker.
	#Allow the film to completely dissolve		#Allow the film to completely dissolve

Moira M. Esson: /* DSC on PVOH Films */

Moira M. Esson — Fri, 14 Sep 2012 19:18:39 GMT

DSC on PVOH Films

←Older revision		Revision as of 19:18, 14 September 2012
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	** Pan mass: 51.02 g		** Pan mass: 51.02 g
	** Sample mass: 3.15 g		** Sample mass: 3.15 g
		+	* [[Media:PVOH(22K), 15%M, H3PO4.pdf\|Graph of heat flow of uncrosslinked PVOH (MW 22000) + 15% maleic acid + H<sub>3</sub>PO<sub>4</sub>]].
		+	* [[Media:PVOH(22K), H3PO4.pdf‎\|Graph of heat flow of uncrosslinked PVOH (MW 22000) + H<sub>3</sub>PO<sub>4</sub>]].

	==Notes==		==Notes==

Moira M. Esson: /* DSC on PVOH Films */

Moira M. Esson — Fri, 14 Sep 2012 17:04:28 GMT

DSC on PVOH Films

←Older revision		Revision as of 17:04, 14 September 2012
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	==DSC on PVOH Films==		==DSC on PVOH Films==
	DSC will be used to determine the different thermal transitions of the various films		DSC will be used to determine the different thermal transitions of the various films
		+	'''General Protocol for DSC:'''
		+	#Weigh out the mass of a Tzero pan+Tzero lid(Record this measurement)
		+	#
		+
		+
		+
	* About 3 mg ± 20% PVOH film was placed in a DSC pan.		* About 3 mg ± 20% PVOH film was placed in a DSC pan.
	* Uncrosslinked PVOH (MW 22000) + 15% maleic acid + H<sub>3</sub>PO<sub>4</sub>		* Uncrosslinked PVOH (MW 22000) + 15% maleic acid + H<sub>3</sub>PO<sub>4</sub>

Moira M. Esson: /* PVOH(MW 22,000) Films */

Moira M. Esson — Fri, 14 Sep 2012 13:55:41 GMT

PVOH(MW 22,000) Films

←Older revision		Revision as of 13:55, 14 September 2012
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	* The viscometer used for previous tests was discovered to be cracked. A new viscometer was subsequently used.		* The viscometer used for previous tests was discovered to be cracked. A new viscometer was subsequently used.

-	~~==PVOH(MW 22,000) Films==~~	+
-	~~'''Prepared PVOH(MW 22,000) Films'''~~	+
-	~~{\| {{table}}~~	+
-	~~\| align="center" style="background:#f0f0f0;"\|''''''~~	+
-	~~\| align="center" style="background:#f0f0f0;"\|'''No acid'''~~	+
-	~~\| align="center" style="background:#f0f0f0;"\|'''HCl'''~~	+
-	~~\| align="center" style="background:#f0f0f0;"\|'''H<sub>3</sub>PO<sub>4</sub>'''~~	+
-	\|-	+
-	~~\| No acid\|\|1.0115\|\|0.5181\|\|1.0054~~	+
-	\|-	+
-	~~\| 10 wt% maleic acid\|\|\|\|0.5181\|\|~~	+
-	\|-	+
-	~~\| 15 wt% maleic acid\|\|\|\|\|\|1.0054~~	+
-	\|-	+
-	~~\| 10 wt% succinic acid\|\|\|\|0.5163\|\|~~	+
-	\|-	+
-	~~\| 15 wt% succinic acid\|\|\|\|\|\|1.0125~~	+
-	\|}	+

Moira M. Esson: /* Objectives */

Moira M. Esson — Fri, 14 Sep 2012 13:55:03 GMT

Objectives

←Older revision		Revision as of 13:55, 14 September 2012
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	*Run solubility tests of crosslinked and uncrosslinked PVOH films		*Run solubility tests of crosslinked and uncrosslinked PVOH films
	*Run Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning calorimetry(DSC) on PVOH films		*Run Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning calorimetry(DSC) on PVOH films
		+	==PVOH(MW 130,000) Films==
		+	*The standard protocol for PVOH Film preparation was used.
		+	**Note: If indicated that acid was added
		+	'''Prepared PVOH(MW 130,000) Films'''
		+	{\| {{table}}
		+	\| align="center" style="background:#f0f0f0;"\|''''''
		+	\| align="center" style="background:#f0f0f0;"\|'''Film #1'''
		+	\| align="center" style="background:#f0f0f0;"\|'''Film #2'''
		+	\| align="center" style="background:#f0f0f0;"\|'''Film #3'''
		+	\| align="center" style="background:#f0f0f0;"\|'''Film #4'''
		+	\| align="center" style="background:#f0f0f0;"\|'''Film #5'''
		+	\| align="center" style="background:#f0f0f0;"\|'''Film #6'''
		+	\|-
		+	\| Mass PVOH used(g)\|\|1.0855\|\|0.9964\|\|1.0373\|\|1.0106\|\|1.0178\|\|1.0215
		+	\|-
		+	\| Amount of [HCl] added(drop)\|\|0\|\|2\|\|0\|\|2\|\|0\|\|2
		+	\|-
		+	\| Amount of [H<sub>3<sub/>PO<sub>4 added(drop)\|\|2\|\|0\|\|2\|\|0\|\|2\|\|0
		+	\|-
		+	\| Amount of succinic acid added(g)\|\|0\|\|0\|\|0\|\|0\|\|0.1528\|\|0.1021
		+	\|-
		+	\| Amount of maleic acid added(g)\|\|0\|\|0\|\|0.1556\|\|0.1071\|\|0\|\|0
		+	\|}
		+	'''Note''':Complete dissolution of the PVOH required a longer amount of stirring(~2hours) and the addition of more deionized H<sub>2<sub/>O. To prompt complete dissolution, solutions were transferred to larger beakers(~50mL) with larger amounts of H<sub>2<sub/>O.
		+	==Crosslinking PVOH Films==
		+	Standard Protocol for Crosslinking of films:
		+	#Weigh out ~0.2 grams of film
		+	#Place measured film in round metal tray
		+	#Place tray in oven at ~120 degrees C for 90 minutes
		+
		+	'''Crosslinked PVOH Films''':
		+	#PVOH(MW 22,000) with 15 wt% maleic acid
		+	#PVOH (MW 22,000) with 15 wt% succinic acid
		+
		+	==Solubility of PVOH Films==
		+	General Protocol:
		+	#Place ~0.1g of film to be tested in a 100mL beaker.
		+	#Add a stir bar to the beaker
		+	#Place plastic mesh above the film and stir bar
		+	#Using a plastic pipette(s) to hold down the plastic mesh, add ~75mL of deionized H<sub>2<sub/>O to the beaker.
		+	#Allow the film to completely dissolve
		+	**Gently stir the solution only with the stir plate. DO NOT add heat
		+	#Once the film is completely dissolved, test the viscosity of the solution three times
		+	<br>
		+
		+	Viscosity of uncrosslinked PVOH(MW 22,000) 15wt% maleic acid
		+	{\| {{table}}
		+	\| align="center" style="background:#f0f0f0;"\|'''Trial'''
		+	\| align="center" style="background:#f0f0f0;"\|'''Time [s]'''
		+	\|-
		+	\| 1\|\|246.67
		+	\|-
		+	\| 2\|\|253.48
		+	\|-
		+	\| 3\|\|250.68
		+	\|}
		+	*Average time:250.28 s
		+
		+	==DSC on PVOH Films==
		+	DSC will be used to determine the different thermal transitions of the various films
		+	* About 3 mg ± 20% PVOH film was placed in a DSC pan.
		+	* Uncrosslinked PVOH (MW 22000) + 15% maleic acid + H<sub>3</sub>PO<sub>4</sub>
		+	** Pan mass: 49.42 mg
		+	** Sample mass: 3.13 mg
		+
		+	* Uncrosslinked PVOH (MW 22000) + 15% succinic acid + H<sub>3</sub>PO<sub>4</sub>
		+	** Pan mass: 51.02 g
		+	** Sample mass: 3.15 g
		+
		+	==Notes==
		+	#For Solubility still need to test:
		+	*PVOH (MW 22,000) uncrosslinked with 15wt% succinnic acid
		+	*PVOH (MW 22,000) uncrosslinked with 10wt% maleic acid
		+	*PVOH (MW 22,000) crosslinked with 15wt% maleic acid
		+	*PVOH (MW 22,000) crosslinked with 15wt% succinnic acid
		+	*PVOH (MW 22,000) uncrosslinked with 10wt% succinnic acid
		+	*PVOH (MW 22,000) uncrosslinked
		+	*PVOH (MW 22,000) crosslinked
		+	#For films need to prepare:
		+	*PVOH (MW 130,000) uncrosslinked with 15wt% maleic acid
		+	*PVOH (MW 130,000) uncrosslinked with 10wt% maleic acid
		+	*PVOH (MW 130,000) crosslinked with 15wt% maleic acid
		+	*PVOH (MW 130,000) crosslinked with 10wt% maleic acid
		+	*PVOH (MW 130,000) uncrosslinked with 15wt% succinic acid
		+	*PVOH (MW 130,000) uncrosslinked with 10wt% succinic acid
		+	*PVOH (MW 130,000) crosslinked with 15wt% succinic acid
		+	*PVOH (MW 130,000) crosslinked with 10wt% succinic acid
		+	*PVOH (MW 130,000) uncrosslinked(and crosslinked) with 15wt% succinic acid and HCl
		+	*PVOH (MW 130,000) uncrosslinked(and crosslinked) with 10wt% succinic acid and H<sub>3</sub>PO<sub>4
		+	*PVOH (MW 130,000) uncrosslinked(and crosslinked) with 15wt% maleic acid and HCl
		+	*PVOH (MW 130,000) uncrosslinked and crosslinked with 10wt% maleic acid and H<sub>3</sub>PO<sub>4
		+	*PVOH (MW 22,000) uncrosslinked and crosslinked with 10wt% maleic acid
		+	*PVOH (MW 22,000) uncrosslinked and crosslinked with 15wt% maleic acid
		+	*PVOH (MW 22,000) uncrosslinked and crosslinked with 10wt% succinic acid
		+	*PVOH (MW 22,000) uncrosslinked and crosslinked with 15wt% succinic acid
		+	*PVOH (MW 22,000) uncrosslinked and crosslinked with 10wt% maleic acid and H<sub>3</sub>PO<sub>4
		+	*PVOH (MW 22,000) uncrosslinked and crosslinked with 15wt% maleic acid and HCl
		+	*PVOH (MW 22,000) uncrosslinked and crosslinked with 10wt% succinic acid and H<sub>3</sub>PO<sub>4
		+	*PVOH (MW 22,000) uncrosslinked and crosslinked with 15wt% succinic acid and HCl
		+
		+	==Observations==
		+	* Crosslinked PVOH films became more rigid and changed color from transparent to faintly yellow-brown.
		+	* The viscometer used for previous tests was discovered to be cracked. A new viscometer was subsequently used.
		+
	==PVOH(MW 22,000) Films==		==PVOH(MW 22,000) Films==
	'''Prepared PVOH(MW 22,000) Films'''		'''Prepared PVOH(MW 22,000) Films'''