User:Moira M. Esson/Notebook/CHEM-581/2012/09/21

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(Glutaraldehyde film preparation)
Current revision (14:28, 15 October 2012) (view source)
(Fixant Solution preparation)
 
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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
 +
 +
 +
 +
 +
   

Current revision

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Objectives

  • Analyze DSC data taken on 9/14/2012
  • Dilute 20 ppm SO4-2 stock solutions made on 9/19/2012 to be used for atomic absorption calibration
    • Dilute to 1ppm, 2ppm, 5ppm, 10ppm, 15ppm
  • Prepare a 500mL solution of 1.25g CuSO4 using HPLC grade H2O
  • Prepare more glutaraldehyde films
  • Prepare a thin PVOH film for use in FTIR
  • Run X-Ray diffraction of 2:1 NaMT:Fe2O4 clay dried on 9/19/2012\
  • 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)


Fixant Solution preparation

  1. Weigh out 200g Na2SO4 (actually measured out 200.1459g)
  2. Place in a 2000mL Erlenmyer flask
  3. Using a graduated cylinder, add 1000mL deionized H2O. Add a large magnetic stir bar to the flask
  4. Place Erlenmyer flask on a stir plate. Stir until all dissolves
  5. Add 20mL concentrated H2SO4
  6. Gently mix solution and using a funnel pour the solution into four 250mL capped bottles
  • Note: H2SO4 is highly corrosive. Use extreme caution


Actual Preparation:

Mass Na2SO4 used(g) 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 H2SO4 so dissolved the Na2SO4 in 1000mL deionized H2O using a magnetic stir bar and a stir plate. Then transferred into a 2000mL solution bottle with cap.

Film preparation

  1. Glutaraldehyde film preparation

The films were prepared following the General Protocol described on2012/09/12

  • Prepared films
    • 1.000gPVOH MW 22,000+0.8wt% glutaraldehyde
    • 0.9499gPVOH MW 22,000+0.8wt% glutaraldehyde+0.052mL PDMS
    • 1.002gPVOH MW 22,000+0.8wt% glutaraldehyde
  • Calculations for film preparation
*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
  1. Thin Film preparation

The film was prepared following the General Protocol described on2012/08/29

  • Prepared film
    • 0.2g PVOH MW 22,000 in a large dish

SO42- Dilutions

General Protocol for Dilutions:

  1. All necessary calculations were performed prior to preparation
  2. An automatic pipette was used to administer completely accurate volumes of stock solution to plastic tube(If necessary a 1mL pipette was used)
  3. HPLC grade H2O was added to the tube using an automatic pipette to total volume
  • Dilution Calculations:
   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
  • Please refer to Karleena Brown's notebook for further dilution calculations

X-Ray

The General Protocol for X-Ray described on 2012/09/19 was used

  • 2:1 NaMT:Fe3O4 clay prepared on 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
Graph of heat flow of uncrosslinked PVOH (MW 22000) + 10% succinic acid + HCl.

  • A glass transition was observed at 105.17°C.


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.


Graph of heat flow of uncrosslinked PVOH (MW 22000) + 10% maleic acid + HCl.

  • A glass transition was observed at 109.61°C.


Graph of heat flow of crosslinked PVOH (MW 22000) + 10% maleic acid + HCl.
Graph of heat flow of uncrosslinked PVOH (MW 22000).

  • A glass transition was observed at 70.62°C.


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 H2O at 25°C
Trial [ ] Time [s]
1 207.68
2 207.95
3 208.47
  • Average time = 208.03 s


  • Viscosity of PVOH MW 22,000+[HCl]+10%maleic acid at 25°C
Trial [ ] Time [s]
1 207.61
2 207.96
3 207.29
  • Average time = 207.62 s







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