User:Nicole Bonan/Notebook/Chem 571 Lab Notebook/2016/02/16

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Objective

Today's objective is to synthesize acetylsalicylic acid-doped AuNP fibers.

Protocol

First, we made two more stock solutions of acetylsalicylic acid from the stock solution synthesized on February 10. This stock solution was 20049µM.

  • We made a 10024µM stock solution of acetylsalicylic acid:
    • 25mL of the 20049µM acetylsalicylic acid stock was pipetted into a 50mL volumetric flask using a volumetric pipette
    • The acetylsalicylic acid was then diluted to 50mL in DI water
  • We made a 5012.2µM stock solution of acetylsalicylic acid:
    • 25mL of the 10024µM acetylsalicylic acid stock was pipetted into a 50mL volumetric flask using a volumetric pipette
    • The acetylsalicylic acid was then diluted to 50mL in DI water

We put all of the stock solutions in 50mL conical tubes.


We also made a new stock solution of lysozyme that was 43.63µM:

  • 0.03121g of lysozyme
  • Brought up to 50mL in DI water in a volumetric flask


Next, we synthesized samples according to the following layout:

The yellow box indicates that 9.976µL of DI water was added (this is included in the volume in the box) to the sample before putting the sample in the oven. The green box indicates that 9.976µL of DI water would need to be added (this volume is not included in the box) to the sample after taking it out of the oven. We needed to add these volumes of water to make up for the fact that adding acetylsalicylic acid to the other samples made the total volume 1000µL+9.976µL.

Data, Analysis, and Observations

See the entry for February 17 for the data collected on today's samples

Next Steps

Tomorrow, we'll use HPLC in order to measure the amount of acetylsalicylic acid in the supernatant.

  • A 0.5mL sample is ideal for use in HPLC. The loop that is currently in the machine is set to 250µL, so we will most likely use 250µL volumes of our samples and blanks.
  • For our standards, we'll inject twice the volume that the loop holds (i.e. 0.5mL) in order to flush the loop for each standard.
  • We will need the following standards:
    • Lysozyme
    • Lysozyme with nanoparticles (spun down in the centrifuge)
    • Acetylsalicylic acid
    • Chloroauric acid
    • Nanocolloid (i.e. the samples that fail to form fibers and form nanoparticles instead)
  • We'll use a C-18 column
  • We'll use water, methanol, and acetic acid for the mobile phase
  • We'll use reverse phase


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