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

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(Preparation of Magnetite nanoparticles with gold)
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==Objectives==
 
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#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
 
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#Attempt preparation of magnetite nanoparticles with gold to produce fibers using new synthetic protocol.
 
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#Analyze any remaining data (AA, UV/vis, FTIR, XRD, microscope, etc.)
 
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<br>
 
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==AA Standard Preparations==
 
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*Because AA is destructive 10mL of each iron standard will be prepared.
 
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* 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 H<sub>2</sub>O will also be used.)
 
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<br>
 
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General Protocol:
 
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# Add the necessary volume of AA/ICPMS Fe 1003±3 μg/mL, 4% HNO<sub>3</sub> solution to a clean 10mL volumetric flask.
 
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# Fill the volumetric flask to the line with deionized H<sub>2</sub>O. Cap and shake the volumetric flask for ~2min.
 
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# Pour the iron solution into a falcon tube for storage. Parafilm the cap of the falcon tube to ensure no H<sub>2</sub>O evaporates.
 
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<br>
 
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'''Table 1. AA standard solutions preparation'''
 
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<br>
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Concentration(μg/mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''Amount Stock solution added (mL)'''
 
-
|-
 
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| 5||0.049850449
 
-
|-
 
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| 10||0.099700897
 
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|-
 
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| 15||0.149551346
 
-
|-
 
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| 20||0.199401795
 
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|-
 
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| 25||0.249252243
 
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|}
 
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<br>
 
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'''Table 2. Calibration Curve Data'''
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Standard concentration (ug/mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''Absorbance'''
 
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| align="center" style="background:#f0f0f0;"|'''Background'''
 
-
|-
 
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| 0||0.0146||0.0183
 
-
|-
 
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| 5||0.1517||0.016
 
-
|-
 
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| 10||0.2295||0.0233
 
-
|-
 
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| 15||0.3289||0.0222
 
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|-
 
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| 20||0.4261||0.0231
 
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|}
 
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<br>
 
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'''Table 3. Atomic Absorption Data'''
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Sample number'''
 
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| align="center" style="background:#f0f0f0;"|'''Sample name'''
 
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| align="center" style="background:#f0f0f0;"|'''Abs'''
 
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| align="center" style="background:#f0f0f0;"|'''Water'''
 
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| align="center" style="background:#f0f0f0;"|'''actual abs.'''
 
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| align="center" style="background:#f0f0f0;"|'''background'''
 
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|-
 
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| 1||13000:1 BSA-Mag .5 KNO3||0.8166||0.8033||0.0133||0.0537
 
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|-
 
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| 2|| 10000:1 BSA-Mag oven||0.7463||0.7342||0.0121||0.058
 
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|-
 
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| 3||13000:1 BSA-Mag oven||0.7873||0.7747||0.0126||0.0576
 
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|-
 
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| 4||10000:1 Heme-Mag oven||0.8384||0.8244||0.014||0.0586
 
-
|-
 
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| 5||130:1 BSA-Mag N2 prep||0.8652||0.8552||0.01||0.0544
 
-
|-
 
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| 6||13000:1 Heme-Mag oven||0.8735||0.869||0.0045||0.0587
 
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|-
 
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| 7||10500:1 Heme-Mag oven||0.8876||0.8754||0.0122||0.0585
 
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|-
 
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| 8||13500:1 Heme-Mag oven||0.8889||0.8855||0.0034||0.0598
 
-
|-
 
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| 9||14000:1 Heme-Mag oven||0.8919||0.8857||0.0062||0.0622
 
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|-
 
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| 10||14500:1 Heme-Mag oven||0.8834||0.8894||-0.006||0.0646
 
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|-
 
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| 11||15000:1 Heme-Mag ||0.8842||0.8841||1E-04||0.0632
 
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|-
 
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| 12||11000:1 Heme-Mag||0.8753||0.8763||-0.001||0.0648
 
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|-
 
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| 13||11500:1 Heme Mag||0.8712||0.8712||0||0.0632
 
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|-
 
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| 14||12000:1 Heme-Mag||0.8581||0.8647||-0.0066||0.0669
 
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|-
 
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| 15||12500:1 Heme Mag||0.8523||0.8536||-0.0013||0.067
 
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|}
 
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==Preparation of Magnetite nanoparticles with gold==
 
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*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|03/05/2014]]
 
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<br>
 
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'''General Protocol:'''
 
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#Prepare 5mL of reaction mixture for preparation of magnetite nanoparticles using general protocol described on [[ in a 20mL test tube.
 
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#Cap test tube using aluminum foil and place in oven at 80°C for two hours.
 
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#While magentite nanoparticles are heating, prepare 5mL of the equivalent ratio of gold:protein reaction mixture using the general protocol described on [[User:Moira M. Esson/Notebook/CHEM-571/2014/01/28|01/28/2014]].
 
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#Add 5mL of gold reaction mixture to the heated magnetite reaction mixture.
 
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#Quickly cap the 20mL test tube and place back into the 80°C oven and heat for another 2 hours.
 
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<br>
 
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Table 4. Preparation of FeSO<sub>4</sub>*7H<sub>2</sub>O stock solution
 
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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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|-
 
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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 5. Preparation of KNO<sub>3</sub> 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)||4.044
 
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|-
 
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| volume stock (L)||0.05
 
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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 6. Preparation of Hemoglobin stock solution
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Preparation of hemoglobin Stock solution'''
 
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| align="center" style="background:#f0f0f0;"|''''''
 
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|-
 
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| Molecular weight (g/mol)||64500
 
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|-
 
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| mass hemglobin (g)||0.0995
 
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|-
 
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| volume solution (L)||0.1
 
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|-
 
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| Concentration (M)||1.54264E-05
 
-
|}
 
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<br>
 
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Table 7. Preparation of KOH Stock solution
 
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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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<br>
 
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Table 8. Preparation of BSA stock solution
 
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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)||0.0174
 
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|-
 
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| volume stock (L)||0.01
 
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|-
 
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| Concentration (M)||2.618E-05
 
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|}
 
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<br>
 
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Table 9. Preparation of Gold stock solution
 
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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 10. Preparation of Magnetite:BSA Reaction Mixtures
 
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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 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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| 13000||2.30769E-06||0.440736074||0.5||0.467583333||2.5||1.091680592
 
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|-
 
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| 13500||2.22222E-06||0.424412516||0.5||0.467583333||2.5||1.108004151
 
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|}
 
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<br>
 
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Table 11. Preparation of Magnetite:Hemoglobin Reaction Mixture
 
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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 Hemoglobin (M)'''
 
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| align="center" style="background:#f0f0f0;"|'''Volume Hemoglobin 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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| 16500||1.81818E-06||0.589310187||0.5||0.467583333||2.5||0.943106479
 
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|-
 
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| 17000||1.76471E-06||0.571977535||0.5||0.467583333||2.5||0.960439132
 
-
|}
 
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<br>
 
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Table 12. Preparation of Au:BSA reaction mixtures
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Ratio'''
 
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| align="center" style="background:#f0f0f0;"|'''Amount of gold added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''Concentration BSA (M)'''
 
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| 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
 
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|-
 
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| 135||0.340447787||1.85185E-06||0.353677097||4.305875116
 
-
|}
 
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<br>
 
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Table 13. Preparation of Au:Hemoglobin reaction mixtures
 
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{| {{table}}
 
-
| align="center" style="background:#f0f0f0;"|'''Ratio'''
 
-
| align="center" style="background:#f0f0f0;"|'''Amount of gold added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''Concentration Hemoglobin (M)'''
 
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| align="center" style="background:#f0f0f0;"|'''volume Hemoglobin added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''volume water added (mL)'''
 
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|-
 
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| 165||0.340447787||1.51515E-06||0.491091823||4.16846039
 
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|-
 
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| 170||0.340447787||1.47059E-06||0.476647946||4.182904267
 
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|}
 
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<br>
 
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==Notes==
 
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*A method for the control of magnetite nanoparticle/nanogel formation must be developed. Another reaction will be performed using the Schlenk line method in order to determine whether this preparation method produces nanoparticles/nanogels of uniform size (these will be analyzed under the microscope)
 
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*The sonication method will be utilized again for further analysis
 
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*DSC analysis will be performed on the dried nanoparticles/nanogels in order to determine the distinct melting points of the prepared magnetic nanoparticles/nanogels
 

Revision as of 07:39, 18 April 2014

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