User:Puja Mody/Notebook/AU Biomaterials 572/2014/01/29

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==Observations & Notes==
==Observations & Notes==
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*The samples prepared [[User:Puja Mody/Notebook/AU Biomaterials 572/2014/01/28|01/28/2014]] which were placed in the oven for 3 hours had changed to a dark blue color upon removal from the oven. This physical characteristic combined with the observed reactivity of the solutions when a magnet was placed up against the test tube leads to the conclusion that magnetic magnetite particle were successfully prepared. Furthermore, a mix of various precipitate/ fiber-esque particulate was observed to have formed in all of the AuNP:Magnetite: BSA solutions. Compared to other previously prepared fibers,  these substances were not as long and wide and therefore appeared to be smaller. We hope to filter these solutions in order to collect the fiber samples for further analysis.
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*The solution prepared in the round bottom flask remained a shade of dark green throughout the entire process with little to no variance during the de-gassing and heating processes. Also, a stir bar was placed into the reaction mixture causing an imbalance in the reaction. This addition will be omitted in the future.
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*The temperature of the hot water bath remained a 75-85°C. The temperature never reached 90°C.

Revision as of 22:53, 3 February 2014

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Day 2

  • Goals
  1. Prepare a new BSA-Magnetite solution without any gold in order to synthesize magnetite nanoparticles which have been incorporated into the BSA fibers.
  2. Analyze the AuNP-BSA and Magnetite-AuNP-BSA solutions which were prepared on 01/28/2014 using UV-Vis spectroscopy

Procedure

- We adopted a different method of preparation on this day in order to compare the effectiveness between the technique of today and yesterday. This protocol was adopted from the following reference [[1]].

  • Preparation of Magnetite-BSA solution.
  1. The Following stock solutions were prepared using deionized water.
    1. A 1M stock solution of KOH in a 10mL volumetric flask
    2. A 0.8M stock solution of KNO3 in a 50mL volumetric flask.
    3. A 0.3M stock solution of FeSO4*7H2O in a 10mL volumetric flask.
  2. Add the appropriate volume of BSA and gold in a 10mL test tube to obtain the desired ratio of BSA:Au. Adjust levels so that the total volume of the solution does not exceed 5mL at this time.
  3. Add the appropriate volume of FeSO4*7H2O to each test tube so that the solution has a concentration of 0.03M FeSO4*7H2O.
  4. Add the appropriate volume of KOH to each test tube so that the solution has a concentration of 0.1M KOH.
  5. Add the appropriate volume of KNO3 to each test tube so that the solution has a concentration of 0.4M KNO3.
  6. Add the necessary amount of water into the flask in order to bring the solution up to 5mL in volume. Seal the round bottom flask with a septum and make sure that it is secure.
  7. Use a Schlenk Line apparatus to funnel nitrogen gas into the solution thereby de-gassing it. Conduct this process at room temperatue for 5 minutes prior to heating the magnetite-BSA solution in a hot water bath at 90°C for 4 hours. Maintain a continuous flow of nitrogen gas throughout the mixture during this time.


  • Note: A previously prepared stock solution of 15mM BSA was used for the preparation.

Calculations

Table 1. Preparation of BSA:MagnetiteNP solution

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)
1300.0001153850.7354058980.50.5004459512.50.764148151

Table 2. 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 3. Preparation of KOH stock solution

Preparation of KOH stock '
Molecular Weight (g/mol)56.11
mass(g)0.5606
volume stock (L)0.01
Concentration (M)0.999108893

Table 4. 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

Data

  • Please see Moira's Notebook for the procedure used for UV-Vis and the collected absorbed spectra.

Observations & Notes

  • The samples prepared 01/28/2014 which were placed in the oven for 3 hours had changed to a dark blue color upon removal from the oven. This physical characteristic combined with the observed reactivity of the solutions when a magnet was placed up against the test tube leads to the conclusion that magnetic magnetite particle were successfully prepared. Furthermore, a mix of various precipitate/ fiber-esque particulate was observed to have formed in all of the AuNP:Magnetite: BSA solutions. Compared to other previously prepared fibers, these substances were not as long and wide and therefore appeared to be smaller. We hope to filter these solutions in order to collect the fiber samples for further analysis.
  • The solution prepared in the round bottom flask remained a shade of dark green throughout the entire process with little to no variance during the de-gassing and heating processes. Also, a stir bar was placed into the reaction mixture causing an imbalance in the reaction. This addition will be omitted in the future.
  • The temperature of the hot water bath remained a 75-85°C. The temperature never reached 90°C.





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