User:Moira M. Esson/Notebook/CHEM-581/2012/09/21: Difference between revisions
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*Run X-Ray diffraction of 2:1 NaMT:Fe<sub>2</sub>O<sub>4</sub> clay dried on 9/19/2012\ | *Run X-Ray diffraction of 2:1 NaMT:Fe<sub>2</sub>O<sub>4</sub> clay dried on 9/19/2012\ | ||
*Prepare glutaraldehyde fixant solution | *Prepare glutaraldehyde fixant solution | ||
*Dry prepared clay in oven for 90 minutes(over 90°C but not over 200°C. Today the over was heated at 105°C) | |||
<br> | <br> | ||
==Fixant Solution preparation== | ==Fixant Solution preparation== | ||
#Weigh out 200g Na<sub>2</sub>SO<sub>4</sub> (actually measured out 200.1459g) | #Weigh out 200g Na<sub>2</sub>SO<sub>4</sub> (actually measured out 200.1459g) | ||
Line 25: | Line 27: | ||
*'''Note''': H<sub>2</sub>SO<sub>4</sub> is highly corrosive. Use extreme caution | *'''Note''': H<sub>2</sub>SO<sub>4</sub> is highly corrosive. Use extreme caution | ||
<br> | <br> | ||
'''Actual Preparation''': | |||
{| {{table}} | |||
| align="center" style="background:#f0f0f0;"|'''Mass Na2SO4 used(g)''' | |||
| align="center" style="background:#f0f0f0;"|'''200.1495''' | |||
|- | |||
| Volume H2SO4 used(mL)||20 | |||
|- | |||
| Amount H2O used(mL)||1000 | |||
|} | |||
*Note: At first put the solution in an Erlenmyer flask, but needed to add 20mL H<sub>2</sub>SO<sub>4</sub> so dissolved the Na<sub>2</sub>SO<sub>4</sub> in 1000mL deionized H<sub>2</sub>O using a magnetic stir bar and a stir plate. Then transferred into a 2000mL solution bottle with cap. | |||
==Film preparation== | ==Film preparation== | ||
Line 41: | Line 53: | ||
*Prepared film | *Prepared film | ||
**0.2g PVOH MW 22,000 in a large dish | **0.2g PVOH MW 22,000 in a large dish | ||
==SO<sub>4</sub><sup>2-</sup> Dilutions== | |||
General Protocol for Dilutions: | |||
#All necessary calculations were performed prior to preparation | |||
#An automatic pipette was used to administer completely accurate volumes of stock solution to plastic tube(If necessary a 1mL pipette was used) | |||
#HPLC grade H<sub>2</sub>O was added to the tube using an automatic pipette to total volume | |||
*Dilution Calculations: | |||
1ppm: | |||
M<sub>1</sub>V<sub>1</sub>=M<sub>2</sub>V<sub>2</sub> | |||
(20ppm CuSO<sub>4</sub>stock)(V<sub>1</sub>)=(1ppm)(50mL) | |||
V<sub>1</sub>=2.5mL= volume of stock needed to prepare | |||
<br> | |||
2ppm: | |||
V<sub>1</sub>=(2ppm)(50mL)/20ppm | |||
V<sub>1</sub>=5mL | |||
<br> | |||
5ppm: | |||
V<sub>1</sub>=(5ppm)(50mL)/(20ppm) | |||
V<sub>1</sub>=12.5mL | |||
<br> | |||
10ppm: | |||
V<sub>1</sub>=(10ppm)(50mL)/(20ppm | |||
V<sub>1</sub>=25mL | |||
<br> | |||
20ppm: | |||
V<sub>1</sub>=(15ppm)(50mL)/(20ppm) | |||
V<sub>1</sub>=37.5mL | |||
*Please refer to Karleena Brown's notebook for further dilution calculations | |||
==X-Ray== | |||
The General Protocol for X-Ray described on [[User:Moira_M._Esson/Notebook/CHEM-581/2012/09/19|2012/09/19]] was used | |||
*2:1 NaMT:Fe<sub>3</sub>O<sub>4</sub> clay prepared on [[User:Moira_M._Esson/Notebook/CHEM-581/2012/09/12|2012/09/12]] was used for x-ray | |||
**The sample was prepared by grinding the clay to a fine powder using a mortar and pestle | |||
'''Note''': This clay was particularly difficult to grind. It is also reddish brown in color | |||
==DSC== | |||
DSC ran on 9/14/2012 was analyzed. Glass transition states were calculated using the program | |||
<br> | |||
[[Media:PVOH(22K),_10%S,_HCl.pdf|Graph of heat flow of uncrosslinked PVOH (MW 22000) + 10% succinic acid + HCl]]. | |||
* A glass transition was observed at 105.17°C. | |||
<br> | |||
[[Media:CL PVOH(22K),_10%S,_HCl.pdf|Graph of heat flow of crosslinked PVOH (MW 22000) + 10% succinic acid + HCl]]. | |||
* A glass transition was observed at 138.04°C. Note that this temperature is above the glass transition observed for the uncrosslinked film of same formulation. This indicates that some crosslinking successfully occurred. | |||
<br> | |||
[[Media:PVOH(22K),_10%M,_HCl.pdf|Graph of heat flow of uncrosslinked PVOH (MW 22000) + 10% maleic acid + HCl]]. | |||
* A glass transition was observed at 109.61°C. | |||
<br> | |||
[[Media:CL_PVOH_22K_10%M_HCl.pdf|Graph of heat flow of crosslinked PVOH (MW 22000) + 10% maleic acid + HCl]]. | |||
<br> | |||
[[Media:PVOH_(22K).pdf|Graph of heat flow of uncrosslinked PVOH (MW 22000)]]. | |||
* A glass transition was observed at 70.62°C. | |||
<br> | |||
[[Media:CL_PVOH_(22K).pdf|Graph of heat flow of crosslinked PVOH (MW 22000)]]. | |||
==Solubility== | |||
*The General protocol for testing viscosity was followed using viscometer 2190 | |||
*'''Observations''': | |||
**Mass of film used: 0.0987g | |||
**The PVOH MW 22000+[HCl]+10%succinic acid crosslinked film was allowed to stir for 1 hour. Although the film did not completely dissolve after 1 hour, the size of the film did not change | |||
**Stored the film that remained after 1hr. stirring for further testing | |||
'''Viscosity Calculations''' | |||
* Viscosity of pure H<sub>2</sub>O at 25°C | |||
{| {{table}} | |||
| align="center" style="background:#f0f0f0;"|'''Trial [ ]''' | |||
| align="center" style="background:#f0f0f0;"|'''Time [s]''' | |||
|- | |||
| 1|| 207.68 | |||
|- | |||
| 2|| 207.95 | |||
|- | |||
| 3|| 208.47 | |||
|- | |||
|} | |||
* Average time = 208.03 s | |||
<br> | |||
* Viscosity of PVOH MW 22,000+[HCl]+10%maleic acid at 25°C | |||
{| {{table}} | |||
| align="center" style="background:#f0f0f0;"|'''Trial [ ]''' | |||
| align="center" style="background:#f0f0f0;"|'''Time [s]''' | |||
|- | |||
| 1|| 207.61 | |||
|- | |||
| 2|| 207.96 | |||
|- | |||
| 3|| 207.29 | |||
|- | |||
|} | |||
* Average time = 207.62 s | |||
Revision as of 11:28, 15 October 2012
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Objectives
Fixant Solution preparation
Film preparation
The films were prepared following the General Protocol described on2012/09/12
*PDMS density=0.97g/mL 5%(1.00gPVOH)=0.95g+0.05gPDMS 0.05g(1mL/0.97g)=0.0515mL PDMS must be added to create 5% replaced PDMS film
The film was prepared following the General Protocol described on2012/08/29
SO42- DilutionsGeneral Protocol for Dilutions:
1ppm: M1V1=M2V2 (20ppm CuSO4stock)(V1)=(1ppm)(50mL) V1=2.5mL= volume of stock needed to prepare
2ppm: V1=(2ppm)(50mL)/20ppm V1=5mL
5ppm: V1=(5ppm)(50mL)/(20ppm) V1=12.5mL
10ppm: V1=(10ppm)(50mL)/(20ppm V1=25mL
20ppm: V1=(15ppm)(50mL)/(20ppm) V1=37.5mL
X-RayThe General Protocol for X-Ray described on 2012/09/19 was used
Note: This clay was particularly difficult to grind. It is also reddish brown in color DSCDSC ran on 9/14/2012 was analyzed. Glass transition states were calculated using the program
Solubility
Viscosity Calculations
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