Difference between revisions of "User:Moira M. Esson/Notebook/CHEM-571/2014/04/01"

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(Atomic Absorption)
 
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==Objectives==
 
#Schlenk line method sample prep
 
#Fe atomic absorption of samples prepared on [[User:Moira M. Esson/Notebook/CHEM-571/2014/03/18|03/18/2014]] and [[User:Moira M. Esson/Notebook/CHEM-571/2014/03/19|03/19/2014]]
 
#Samples were prepared for DSC analysis
 
<br>
 
==Schlenk line sample preparation==
 
*The general protocol for the Schlenk line method of preparation described on [[User:Moira M. Esson/Notebook/CHEM-571/2014/01/29|01/29/2014]] was followed.
 
*For the addition of gold using the Schlenk line method, an equivalent volume of gold:protein samples were prepared, de-gassed using N<sub>2</sub>, and added to the magnetite reaction mixture using a syringe.
 
<br>
 
Table 1. BSA stock preparation
 
{| {{table}}
 
| align="center" style="background:#f0f0f0;"|'''Preparation of BSA stock'''
 
| align="center" style="background:#f0f0f0;"|''''''
 
|-
 
| Molecular weight (g/mol)||66463
 
|-
 
| mass (g)||0.0167
 
|-
 
| volume stock (L)||0.01
 
|-
 
| Concentration (M)||2.51268E-05
 
|}
 
<br>
 
Table 2. Preparation of FeSO<sub>4</sub>*7H<sub>2</sub>O stock
 
{| {{table}}
 
| align="center" style="background:#f0f0f0;"|'''Preparation of FeSO4 stock'''
 
| align="center" style="background:#f0f0f0;"|''''''
 
|-
 
| Molecular Weight (g/mol)||278.01
 
|-
 
| mass(g)||0.83403
 
|-
 
| volume stock (L)||0.01
 
|-
 
| Concentration (M)||0.3
 
|}
 
<br>
 
Table 3. KOH stock
 
{| {{table}}
 
| align="center" style="background:#f0f0f0;"|'''Preparation of KOH stock'''
 
| align="center" style="background:#f0f0f0;"|''''''
 
|-
 
| Molecular Weight (g/mol)||56.11
 
|-
 
| mass(g)||1.5
 
|-
 
| volume stock (L)||0.025
 
|-
 
| Concentration (M)||1.069328106
 
|}
 
<br>
 
Table 4. Potassium Nitrate stock solution
 
{| {{table}}
 
| align="center" style="background:#f0f0f0;"|'''Preparation of KNO3'''
 
| align="center" style="background:#f0f0f0;"|''''''
 
|-
 
| Molecular Weight (g/mol)||101.1
 
|-
 
| mass(g)||0.8088
 
|-
 
| volume stock (L)||0.01
 
|-
 
| Concentration (M)||0.8
 
|}
 
<br>
 
Table 5. Gold stock solution preparation
 
<br>
 
{| {{table}}
 
| align="center" style="background:#f0f0f0;"|'''Preparation gold stock'''
 
| align="center" style="background:#f0f0f0;"|''''''
 
|-
 
| Molecular weight Au (g/mol)||393.83
 
|-
 
| mass Au(g)||0.01446
 
|-
 
| volume stock(L)||0.01
 
|-
 
| Concentration (M)||0.003671635
 
|}
 
<br>
 
Table 6. Magnetite:Protein solution preparation
 
{| {{table}}
 
| align="center" style="background:#f0f0f0;"|'''Ratio'''
 
| align="center" style="background:#f0f0f0;"|'''concentration BSA (M)'''
 
| align="center" style="background:#f0f0f0;"|'''volume of BSA added (mL)'''
 
| align="center" style="background:#f0f0f0;"|'''amount of FeSO4 added(mL)'''
 
| align="center" style="background:#f0f0f0;"|'''amount of KOH added (mL)'''
 
| align="center" style="background:#f0f0f0;"|'''amount of KNO3 added (mL)'''
 
| align="center" style="background:#f0f0f0;"|'''volume Water added (mL)'''
 
|-
 
| 13500||2.22222E-06||0.442202262||0.5||0.467583333||2.5||1.090214405
 
|}
 
<br>
 
Table 7. Magnetite:Protein and Gold:Protein solution preparation
 
{| {{table}}
 
| align="center" style="background:#f0f0f0;"|'''Ratio'''
 
| align="center" style="background:#f0f0f0;"|'''concentration BSA (M)'''
 
| align="center" style="background:#f0f0f0;"|'''volume of BSA added (mL)'''
 
| align="center" style="background:#f0f0f0;"|'''amount of FeSO4 added(mL)'''
 
| align="center" style="background:#f0f0f0;"|'''amount of KOH added (mL)'''
 
| align="center" style="background:#f0f0f0;"|'''amount of KNO3 added (mL)'''
 
| align="center" style="background:#f0f0f0;"|'''volume Water added (mL)'''
 
|-
 
| 13500||2.22222E-06||0.442202262||0.5||0.467583333||2.5||1.090214405
 
|-
 
| ||||||||||||
 
|-
 
| Ratio||Amount of gold added (mL)||Concentration BSA (M)||volume BSA added (mL)||volume water added (mL)||||
 
|-
 
| 135||0.340447787||1.86124E-07||0.037037037||4.622515176||||
 
|}
 
 
==Atomic Absorption==
 
*The general protocol for AA was followed. Samples were analyzed for the presence of iron.
 
[[Image:Chem572day4-1.png|500px]]
 
<br>
 
Table 1. Atomic Absorbance Data for Magnetite:Protein hydrogel samples
 
{| {{table}}
 
| align="center" style="background:#f0f0f0;"|'''Sample number'''
 
| align="center" style="background:#f0f0f0;"|'''Sample name'''
 
| align="center" style="background:#f0f0f0;"|'''Abs'''
 
| align="center" style="background:#f0f0f0;"|'''background'''
 
| align="center" style="background:#f0f0f0;"|'''actual abs.'''
 
|-
 
| 1||13000:1 mag- BSA+ 130:1 Au-BSA ||0.0117||-0.0005||0.0122
 
|-
 
| 2||13000:1 mag-BSA  sonicated||0.0029||0.007||-0.0041
 
|-
 
| 3||13500:1 Mag-BSA + 135:1 Au-BSA||0.0022||-0.0019||0.0041
 
|-
 
| 4||17000:1 Mag-Heme +170:1 Au-Heme||0.0029||-0.0013||0.0042
 
|-
 
| 5||16500:1 Mag-Heme +165:1 Au-Heme||0.002||-0.0021||0.0041
 
|-
 
| 6||16500:1 Mag-Heme sonicator||-0.0009||0.0162||-0.0171
 
|-
 
| 7||16000:1 Mag-Heme+ 160:1 Au-Heme||0.0023||0.00066||0.00164
 
|}
 
<br>
 
Table 2. Concentration of Iron present in each sample
 
<br>
 
{| {{table}}
 
| align="center" style="background:#f0f0f0;"|'''Sample name'''
 
| align="center" style="background:#f0f0f0;"|'''Concentration Iron in sample (ug/mL)'''
 
| align="center" style="background:#f0f0f0;"|'''Total concentration Iron originally in solution (ug/mL)'''
 
| align="center" style="background:#f0f0f0;"|'''Concentration Iron incorporated (ug/mL)'''
 
| align="center" style="background:#f0f0f0;"|'''Percent Iron incorporated (%)'''
 
|-
 
| 13000:1 mag- BSA+ 130:1 Au-BSA ||-0.01359993||1765.35||1765.3636||100.0007704
 
|-
 
| 13000:1 mag-BSA  sonicated||-0.01375041||1765.35||1765.36375||100.0007789
 
|-
 
| 13500:1 Mag-BSA + 135:1 Au-BSA||-0.01376238||1765.35||1765.363762||100.0007796
 
|-
 
| 17000:1 Mag-Heme +170:1 Au-Heme||-0.01375041||1765.35||1765.36375||100.0007789
 
|-
 
| 16500:1 Mag-Heme +165:1 Au-Heme||-0.0137658||1765.35||1765.363766||100.0007798
 
|-
 
| 16500:1 Mag-Heme sonicator||-0.01381539||1765.35||1765.363815||100.0007826
 
|-
 
| 16000:1 Mag-Heme+ 160:1 Au-Heme||-0.01376067||1765.35||1765.363761||100.0007795
 
|}
 
<br>
 
==DSC Sample preparation==
 
General protocol:
 
#Record the mass of a Tzero pan
 
#Using a pipette, add ~10μL of sample to the pan(vortex sample prior to removal of 10μL to ensure homogeneous distribution of hydrogels).
 
#Place pan in fume hood until sample is completely dry.
 
#Repeat process as necessary (until a large amount of sample is present in the pans)
 
 
 
  
 +
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