User:Moira M. Esson/Notebook/CHEM-571/2014/03/18

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(Preparation of Magnetite nanoparticles with gold)
(Preparation of Magnetite nanoparticles with gold)
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==Preparation of Magnetite nanoparticles with gold==
==Preparation of Magnetite nanoparticles with gold==
-
*As the synthesis on [[User:Moira M. Esson/Notebook/CHEM-571/2014/03/05|03/05/2014]] did not produce fibers (though appears to have produced gold nanoparticles and magnetite nanoparticles), a new method will be used.  
+
*As the synthesis on [[User:Moira M. Esson/Notebook/CHEM-571/2014/03/05|03/05/2014]] did not produce fibers (though appears to have produced gold nanoparticles and magnetite nanoparticles), a new method will be used for the potential preparation of fibers. Although the method utilized on [[User:Moira M. Esson/Notebook/CHEM_571/2014/03/05|
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'''General Protocol:'''
'''General Protocol:'''
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Table 7. Preparation of KOH Stock solution
 +
{| {{table}}
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| 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
 +
|}
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<br>
 +
Table 8. Preparation of BSA stock solution
 +
{| {{table}}
 +
| align="center" style="background:#f0f0f0;"|'''Preparation of BSA stock'''
 +
| align="center" style="background:#f0f0f0;"|''''''
 +
|-
 +
| Molecular weight (g/mol)||66463
 +
|-
 +
| mass (g)||0.0174
 +
|-
 +
| volume stock (L)||0.01
 +
|-
 +
| Concentration (M)||2.618E-05
 +
|}
 +
<br>
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Table 9. Preparation of Gold stock solution
 +
{| {{table}}
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| 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>
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Table 10. Preparation of Magnetite:BSA Reaction Mixtures
 +
{| {{table}}
 +
| align="center" style="background:#f0f0f0;"|'''Ratio'''
 +
| align="center" style="background:#f0f0f0;"|'''Concentration BSA (M)'''
 +
| align="center" style="background:#f0f0f0;"|'''Volume 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)'''
 +
|-
 +
| 13000||2.30769E-06||0.440736074||0.5||0.467583333||2.5||1.091680592
 +
|-
 +
| 13500||2.22222E-06||0.424412516||0.5||0.467583333||2.5||1.108004151
 +
|}
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<br>
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Table 11. Preparation of Magnetite:Hemoglobin Reaction Mixture
 +
{| {{table}}
 +
| align="center" style="background:#f0f0f0;"|'''Ratio'''
 +
| align="center" style="background:#f0f0f0;"|'''Concentration Hemoglobin (M)'''
 +
| align="center" style="background:#f0f0f0;"|'''Volume Hemoglobin 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)'''
 +
|-
 +
| 16500||1.81818E-06||0.589310187||0.5||0.467583333||2.5||0.943106479
 +
|-
 +
| 17000||1.76471E-06||0.571977535||0.5||0.467583333||2.5||0.960439132
 +
|}
 +
<br>
 +
Table 12. Preparation of Au:BSA reaction mixtures
 +
{| {{table}}
 +
| align="center" style="background:#f0f0f0;"|'''Ratio'''
 +
| align="center" style="background:#f0f0f0;"|'''Amount of gold added (mL)'''
 +
| align="center" style="background:#f0f0f0;"|'''Concentration BSA (M)'''
 +
| align="center" style="background:#f0f0f0;"|'''volume BSA added (mL)'''
 +
| align="center" style="background:#f0f0f0;"|'''volume water added (mL)'''
 +
|-
 +
| 130||0.340447787||1.92308E-06||0.367280062||4.292272151
 +
|-
 +
| 135||0.340447787||1.85185E-06||0.353677097||4.305875116
 +
|}
 +
<br>
 +
Table 13. Preparation of Au:Hemoglobin reaction mixtures
 +
{| {{table}}
 +
| align="center" style="background:#f0f0f0;"|'''Ratio'''
 +
| align="center" style="background:#f0f0f0;"|'''Amount of gold added (mL)'''
 +
| align="center" style="background:#f0f0f0;"|'''Concentration Hemoglobin (M)'''
 +
| align="center" style="background:#f0f0f0;"|'''volume Hemoglobin added (mL)'''
 +
| align="center" style="background:#f0f0f0;"|'''volume water added (mL)'''
 +
|-
 +
| 165||0.340447787||1.51515E-06||0.491091823||4.16846039
 +
|-
 +
| 170||0.340447787||1.47059E-06||0.476647946||4.182904267
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|}
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__NOTOC__
__NOTOC__

Revision as of 19:17, 18 March 2014

Project name Main project page
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Objectives

  1. Run AA of all solutions prepared up to this point. This is to determine the amount of Fe remaining in solution after synthesis of magnetic nanoparticles
  2. Attempt preparation of magnetite nanoparticles with gold to produce fibers using new synthetic protocol.
  3. Analyze any remaining data (AA, UV/vis, FTIR, XRD, microscope, etc.)


AA Standard Preparations

  • Because AA is destructive 10mL of each iron standard will be prepared.
  • 5 standard solutions (25μg/mL, 20μg/mL, 15μg/mL, 10μg/mL, 5μg/mL) will be prepared. In total 6 standard solutions will be run as a calibration for the AA (deionized H2O will also be used.)


General Protocol:

  1. Add the necessary volume of AA/ICPMS Fe 1003±3 μg/mL, 4% HNO3 solution to a clean 10mL volumetric flask.
  2. Fill the volumetric flask to the line with deionized H2O. Cap and shake the volumetric flask for ~2min.
  3. Pour the iron solution into a falcon tube for storage. Parafilm the cap of the falcon tube to ensure no H2O evaporates.


Table 1. AA standard solutions preparation

Concentration(μg/mL) Amount Stock solution added (mL)
50.049850449
100.099700897
150.149551346
200.199401795
250.249252243


Table 2. Calibration Curve Data

Standard concentration (ug/mL) Absorbance Background
00.01460.0183
50.15170.016
100.22950.0233
150.32890.0222
200.42610.0231


Table 3. Atomic Absorption Data

Sample number Sample name Abs Water actual abs. background
113000:1 BSA-Mag .5 KNO30.81660.80330.01330.0537
2 10000:1 BSA-Mag oven0.74630.73420.01210.058
313000:1 BSA-Mag oven0.78730.77470.01260.0576
410000:1 Heme-Mag oven0.83840.82440.0140.0586
5130:1 BSA-Mag N2 prep0.86520.85520.010.0544
613000:1 Heme-Mag oven0.87350.8690.00450.0587
710500:1 Heme-Mag oven0.88760.87540.01220.0585
813500:1 Heme-Mag oven0.88890.88550.00340.0598
914000:1 Heme-Mag oven0.89190.88570.00620.0622
1014500:1 Heme-Mag oven0.88340.8894-0.0060.0646
1115000:1 Heme-Mag 0.88420.88411E-040.0632
1211000:1 Heme-Mag0.87530.8763-0.0010.0648
1311500:1 Heme Mag0.87120.871200.0632
1412000:1 Heme-Mag0.85810.8647-0.00660.0669
1512500:1 Heme Mag0.85230.8536-0.00130.067

Preparation of Magnetite nanoparticles with gold

  • As the synthesis on 03/05/2014 did not produce fibers (though appears to have produced gold nanoparticles and magnetite nanoparticles), a new method will be used for the potential preparation of fibers. Although the method utilized on [[User:Moira M. Esson/Notebook/CHEM_571/2014/03/05|


General Protocol:

  1. Prepare 5mL of reaction mixture for preparation of magnetite nanoparticles using general protocol described on [[ in a 20mL test tube.
  2. Cap test tube using aluminum foil and place in oven at 80°C for two hours.
  3. While magentite nanoparticles are heating, prepare 5mL of the equivalent ratio of gold:protein reaction mixture using the general protocol described on 01/28/2014.
  4. Add 5mL of gold reaction mixture to the heated magnetite reaction mixture.
  5. Quickly cap the 20mL test tube and place back into the 80°C oven and heat for another 2 hours.


Table 4. Preparation of FeSO4*7H2O stock solution

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


Table 5. Preparation of KNO3 stock solution

Preparation of KNO3 '
Molecular Weight (g/mol)101.1
mass(g)4.044
volume stock (L)0.05
Concentration (M)0.8


Table 6. Preparation of Hemoglobin stock solution

Preparation of hemoglobin Stock solution '
Molecular weight (g/mol)64500
mass hemglobin (g)0.0995
volume solution (L)0.1
Concentration (M)1.54264E-05


Table 7. Preparation of KOH Stock solution

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


Table 8. Preparation of BSA stock solution

Preparation of BSA stock '
Molecular weight (g/mol)66463
mass (g)0.0174
volume stock (L)0.01
Concentration (M)2.618E-05


Table 9. Preparation of Gold stock solution

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 10. Preparation of Magnetite:BSA Reaction Mixtures

Ratio Concentration BSA (M) Volume BSA Added (mL) amount of FeSO4 added(mL) amount of KOH added (mL) amount of KNO3 added (mL) volume Water added (mL)
130002.30769E-060.4407360740.50.4675833332.51.091680592
135002.22222E-060.4244125160.50.4675833332.51.108004151


Table 11. Preparation of Magnetite:Hemoglobin Reaction Mixture

Ratio Concentration Hemoglobin (M) Volume Hemoglobin Added (mL) amount of FeSO4 added(mL) amount of KOH added (mL) amount of KNO3 added (mL) volume Water added (mL)
165001.81818E-060.5893101870.50.4675833332.50.943106479
170001.76471E-060.5719775350.50.4675833332.50.960439132


Table 12. Preparation of Au:BSA reaction mixtures

Ratio Amount of gold added (mL) Concentration BSA (M) volume BSA added (mL) volume water added (mL)
1300.3404477871.92308E-060.3672800624.292272151
1350.3404477871.85185E-060.3536770974.305875116


Table 13. Preparation of Au:Hemoglobin reaction mixtures

Ratio Amount of gold added (mL) Concentration Hemoglobin (M) volume Hemoglobin added (mL) volume water added (mL)
1650.3404477871.51515E-060.4910918234.16846039
1700.3404477871.47059E-060.4766479464.182904267




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