User:Tamanika Tinsley/Notebook/Chem 581 Biomaterials Design Lab/2014/09/03

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Sept 3 UV Vis-FTIR-DSC

  • Group Members Andrew Farag Sr (Undergrad) and Michael Bible Jr (Undergrad)
  • Group Name : AMT

Objective

  • ALL groups will continue their film synthesis from the last week. And ALL groups will start new film syntheses (PVA only and PVA with 10% sodium montmorillonite)
  • Groups A* and B* will be using the UV-Vis to make calibration curves for malachite green absorbance and to determine the equilibrium of their malachite green/dye samples
  • Groups C* and D* will take a powder X-ray diffraction of one (or two) of their films. They will take Fourier Transform Infrared Spectra (FTIR) of all of their films. They may (time permitting) perform differential scanning calorimetry (DSC) of all of their films.

My group was assigned to use the UV-Vis today, and to use the FTIR, DSC, PXRD on Friday.

Note: On Friday Groups A and B will perform the tasks Groups C and D perform on Wednesday and vice versa.

Description

Tasks

  1. Film preparation
    1. See previous protocols: 1 and 2
  2. Calibration Curves
    1. Take UV Vis spectra for Malachite green concentrations: 0ppm, 0.20ppm, 0.50ppm, 1.1ppm, 1.4ppm, 1.7ppm, and 2.0ppm Malachite Green
    2. Find the two absorbance maxima in the spectra. Plot the absorbance value vs concentration at each ppm for each maximum you find.
    3. For each absorbance max, determine the slope of your A vs concentration plots. This will give you the extinction coefficient for the wavelengths you are analyzing
  3. Malachite Green Equilibrium
    1. We will use UV-Vis spectroscopy to determine the amount of Malachite green absorbed into a film
    2. Upon determining the amount of Malachite green in the film, we can determine the equilibrium of free Malachite green vs bound malachite green by creating an I.C.E. table. (Remember those from Gen Chem II??)
    3. We can also determine the mass of malachite green absorbed per mass of film
    4. To properly determine MG concentration, we will need to dilute our samples so that their absorbance is similar to the absorbance of our calibration curve samples.
      1. You can see from the intense color of your MG/film solutions that they are much darker (and will absorb more light) than those you used for your calibration curves (except for the 2ppm).
      2. Before you get to lab, figure out how you are going to need to make your dilutions.
        1. Hint 1: Use a 10mL volumetric flask (only 1 per each group)
        2. Hint 2: Transfer your dilutions to a glass test tube and label (you'll only need 3mL for your absorbance measurement)
        3. Hint 3: The two groups who are running UV Vis should take turns running 1 sample at a time. (At the end of the day, each group will have run 6 calibration samples and 8 diluted samples)
        4. Hint 4: Delegate responsibility among your group members for:
          1. Running Spectra
          2. Cleaning Cuvettes
          3. Making Dilutions
          4. Analyzing Spectra and making calibration curves
        5. Hint 5: Acetone is fantastic for really cleaning MG out of volumetric flasks and cuvettes.
  4. Powder X-ray diffraction
    1. Sample prep
      1. To be discussed in class
    2. Instrument Settings
      1. 2o start angle
      2. 40o stop angle
      3. 1o/second scan speed (this seems too fast, will check on this)
      4. 0.5o sampling width
  5. FTIR
    1. We will be using attenuated total reflectance (ATR) mode for our samples
    2. Place the film in the sample holder. Execute measurement
    3. Save measurement data onto thumb drive
  6. DSC
    1. Will update this section soon

(Description from Dr. Hartings lab notebook Dr. Hartings)

Data

Figure 1. Shows the weights of the pans, lids and films used for DSC Image:DSCweights2.jpg Figure 2. Shows the calibration curve for wavelength 423nm. Beer's Law explains that A= Ɛbc, where Ɛ = molar absorptivity in the units of cm-1*M-1, b = path length, and c = concentration. The molar absorptivity of the malachite green at 617nm is 0.1193. This is identified by translating Beer's Law to the slope of the calibration curve y=mx+b; where y = absorbance (y axis), x = concentration (x axis), and m = molar absorptivity. The standard curve for wavelength 423 has an line fit that is below acceptable values for calibration plots. This is due to the calibration point 1.1. Image:Calibration423.png


Figure 3. Shows the calibration curve for wavelength 617nm. Beer's Law explains that A= Ɛbc, where Ɛ = molar absorptivity in the units of cm-1*M-1, b = path length, and c = concentration. The molar absorptivity of the malachite green at 617nm is 0.1193. This is identified by translating Beer's Law to the slope of the calibration curve y=mx+b; where y = absorbance (y axis), x = concentration (x axis), and m = molar absorptivity.



Figure 4.Shows the Initial Change Equilibrium table to determine the amount of malachite film in the films.
ICE Table Image:ICE table.png


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