Difference between revisions of "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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#Quickly cap the 20mL test tube and place back into the 80°C oven and heat for another 2 hours.
 
#Quickly cap the 20mL test tube and place back into the 80°C oven and heat for another 2 hours.
 
<br>
 
<br>
'''Table 4. Preparation of KNO'''
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Table 4. Preparation of FeSO<sub>4</sub>*7H<sub>2</sub>O stock solution
 
+
{| {{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
 +
|-
 +
| mass(g)||0.83403
 +
|-
 +
| volume stock (L)||0.01
 +
|-
 +
| Concentration (M)||0.3
 +
|}
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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
 +
|-
 +
| mass(g)||4.044
 +
|-
 +
| volume stock (L)||0.05
 +
|-
 +
| Concentration (M)||0.8
 +
|}
 +
<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
 +
|-
 +
| mass hemglobin (g)||0.0995
 +
|-
 +
| volume solution (L)||0.1
 +
|-
 +
| Concentration (M)||1.54264E-05
 +
|}
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Revision as of 14:56, 18 March 2014

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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)
5 0.049850449
10 0.099700897
15 0.149551346
20 0.199401795
25 0.249252243


Table 2. Calibration Curve Data

Standard concentration (ug/mL) Absorbance Background
0 0.0146 0.0183
5 0.1517 0.016
10 0.2295 0.0233
15 0.3289 0.0222
20 0.4261 0.0231


Table 3. Atomic Absorption Data

Sample number Sample name Abs Water actual abs. background
1 13000:1 BSA-Mag .5 KNO3 0.8166 0.8033 0.0133 0.0537
2 10000:1 BSA-Mag oven 0.7463 0.7342 0.0121 0.058
3 13000:1 BSA-Mag oven 0.7873 0.7747 0.0126 0.0576
4 10000:1 Heme-Mag oven 0.8384 0.8244 0.014 0.0586
5 130:1 BSA-Mag N2 prep 0.8652 0.8552 0.01 0.0544
6 13000:1 Heme-Mag oven 0.8735 0.869 0.0045 0.0587
7 10500:1 Heme-Mag oven 0.8876 0.8754 0.0122 0.0585
8 13500:1 Heme-Mag oven 0.8889 0.8855 0.0034 0.0598
9 14000:1 Heme-Mag oven 0.8919 0.8857 0.0062 0.0622
10 14500:1 Heme-Mag oven 0.8834 0.8894 -0.006 0.0646
11 15000:1 Heme-Mag 0.8842 0.8841 1E-04 0.0632
12 11000:1 Heme-Mag 0.8753 0.8763 -0.001 0.0648
13 11500:1 Heme Mag 0.8712 0.8712 0 0.0632
14 12000:1 Heme-Mag 0.8581 0.8647 -0.0066 0.0669
15 12500:1 Heme Mag 0.8523 0.8536 -0.0013 0.067

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.


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