User:Moira M. Esson/Notebook/CHEM-571/2014/04/01

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#Schlenk line method sample prep
#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]]
#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]]
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#Samples were prepared for DSC analysis
<br>
<br>
-
 
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==Schlenk line sample preparation==
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*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.
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*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.
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<br>
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Table 1. BSA stock preparation
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{| {{table}}
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| align="center" style="background:#f0f0f0;"|'''Preparation of BSA stock'''
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| align="center" style="background:#f0f0f0;"|''''''
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|-
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| Molecular weight (g/mol)||66463
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|-
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| mass (g)||0.0167
 +
|-
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| volume stock (L)||0.01
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|-
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| Concentration (M)||2.51268E-05
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|}
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<br>
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Table 2. Preparation of FeSO<sub>4</sub>*7H<sub>2</sub>O stock
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{| {{table}}
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| align="center" style="background:#f0f0f0;"|'''Preparation of FeSO4 stock'''
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| align="center" style="background:#f0f0f0;"|''''''
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|-
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| Molecular Weight (g/mol)||278.01
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|-
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| mass(g)||0.83403
 +
|-
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| volume stock (L)||0.01
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|-
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| Concentration (M)||0.3
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|}
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<br>
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Table 3. KOH stock
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{| {{table}}
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| align="center" style="background:#f0f0f0;"|'''Preparation of KOH stock'''
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| align="center" style="background:#f0f0f0;"|''''''
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|-
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| Molecular Weight (g/mol)||56.11
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|-
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| mass(g)||1.5
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|-
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| volume stock (L)||0.025
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|-
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| Concentration (M)||1.069328106
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|}
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<br>
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Table 4. Potassium Nitrate stock solution
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{| {{table}}
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| align="center" style="background:#f0f0f0;"|'''Preparation of KNO3'''
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| align="center" style="background:#f0f0f0;"|''''''
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|-
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| Molecular Weight (g/mol)||101.1
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|-
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| mass(g)||0.8088
 +
|-
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| volume stock (L)||0.01
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|-
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| Concentration (M)||0.8
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|}
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<br>
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Table 5. Gold stock solution preparation
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<br>
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{| {{table}}
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| align="center" style="background:#f0f0f0;"|'''Preparation gold stock'''
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| align="center" style="background:#f0f0f0;"|''''''
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|-
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| Molecular weight Au (g/mol)||393.83
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|-
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| mass Au(g)||0.01446
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|-
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| volume stock(L)||0.01
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|-
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| Concentration (M)||0.003671635
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|}
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<br>
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Table 6. Magnetite:Protein solution preparation
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{| {{table}}
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| align="center" style="background:#f0f0f0;"|'''Ratio'''
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| align="center" style="background:#f0f0f0;"|'''concentration BSA (M)'''
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| align="center" style="background:#f0f0f0;"|'''volume of BSA added (mL)'''
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| align="center" style="background:#f0f0f0;"|'''amount of FeSO4 added(mL)'''
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| align="center" style="background:#f0f0f0;"|'''amount of KOH added (mL)'''
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| align="center" style="background:#f0f0f0;"|'''amount of KNO3 added (mL)'''
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| align="center" style="background:#f0f0f0;"|'''volume Water added (mL)'''
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|-
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| 13500||2.22222E-06||0.442202262||0.5||0.467583333||2.5||1.090214405
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|}
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<br>
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Table 7. Magnetite:Protein and Gold:Protein solution preparation
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{| {{table}}
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| align="center" style="background:#f0f0f0;"|'''Ratio'''
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| 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)'''
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|-
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| 13500||2.22222E-06||0.442202262||0.5||0.467583333||2.5||1.090214405
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|-
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| ||||||||||||
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|-
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| Ratio||Amount of gold added (mL)||Concentration BSA (M)||volume BSA added (mL)||volume water added (mL)||||
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|-
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| 135||0.340447787||1.86124E-07||0.037037037||4.622515176||||
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|}
==Atomic Absorption==
==Atomic Absorption==

Revision as of 09:07, 29 April 2014

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Objectives

  1. Schlenk line method sample prep
  2. Fe atomic absorption of samples prepared on 03/18/2014 and 03/19/2014
  3. Samples were prepared for DSC analysis


Schlenk line sample preparation

  • The general protocol for the Schlenk line method of preparation described on 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 N2, and added to the magnetite reaction mixture using a syringe.

Table 1. BSA stock preparation

Preparation of BSA stock '
Molecular weight (g/mol)66463
mass (g)0.0167
volume stock (L)0.01
Concentration (M)2.51268E-05


Table 2. Preparation of FeSO4*7H2O stock

Preparation of FeSO4 stock '
Molecular Weight (g/mol)278.01
mass(g)0.83403
volume stock (L)0.01
Concentration (M)0.3


Table 3. KOH stock

Preparation of KOH stock '
Molecular Weight (g/mol)56.11
mass(g)1.5
volume stock (L)0.025
Concentration (M)1.069328106


Table 4. Potassium Nitrate stock solution

Preparation of KNO3 '
Molecular Weight (g/mol)101.1
mass(g)0.8088
volume stock (L)0.01
Concentration (M)0.8


Table 5. Gold stock solution preparation

Preparation gold stock '
Molecular weight Au (g/mol)393.83
mass Au(g)0.01446
volume stock(L)0.01
Concentration (M)0.003671635


Table 6. Magnetite:Protein solution preparation

Ratio concentration BSA (M) volume of BSA added (mL) amount of FeSO4 added(mL) amount of KOH added (mL) amount of KNO3 added (mL) volume Water added (mL)
135002.22222E-060.4422022620.50.4675833332.51.090214405


Table 7. Magnetite:Protein and Gold:Protein solution preparation

Ratio concentration BSA (M) volume of BSA added (mL) amount of FeSO4 added(mL) amount of KOH added (mL) amount of KNO3 added (mL) volume Water added (mL)
135002.22222E-060.4422022620.50.4675833332.51.090214405
RatioAmount of gold added (mL)Concentration BSA (M)volume BSA added (mL)volume water added (mL)
1350.3404477871.86124E-070.0370370374.622515176

Atomic Absorption

  • The general protocol for AA was followed. Samples were analyzed for the presence of iron.


Table 1. Atomic Absorbance Data for Magnetite:Protein hydrogel samples

Sample number Sample name Abs background actual abs.
113000:1 mag- BSA+ 130:1 Au-BSA 0.0117-0.00050.0122
213000:1 mag-BSA sonicated0.00290.007-0.0041
313500:1 Mag-BSA + 135:1 Au-BSA0.0022-0.00190.0041
417000:1 Mag-Heme +170:1 Au-Heme0.0029-0.00130.0042
516500:1 Mag-Heme +165:1 Au-Heme0.002-0.00210.0041
616500:1 Mag-Heme sonicator-0.00090.0162-0.0171
716000:1 Mag-Heme+ 160:1 Au-Heme0.00230.000660.00164


Table 2. Concentration of Iron present in each sample

Sample name Concentration Iron in sample (ug/mL) Total concentration Iron originally in solution (ug/mL) Concentration Iron incorporated (ug/mL) Percent Iron incorporated (%)
13000:1 mag- BSA+ 130:1 Au-BSA -0.013599931765.351765.3636100.0007704
13000:1 mag-BSA sonicated-0.013750411765.351765.36375100.0007789
13500:1 Mag-BSA + 135:1 Au-BSA-0.013762381765.351765.363762100.0007796
17000:1 Mag-Heme +170:1 Au-Heme-0.013750411765.351765.36375100.0007789
16500:1 Mag-Heme +165:1 Au-Heme-0.01376581765.351765.363766100.0007798
16500:1 Mag-Heme sonicator-0.013815391765.351765.363815100.0007826
16000:1 Mag-Heme+ 160:1 Au-Heme-0.013760671765.351765.363761100.0007795


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