User:Benjamin Friedel/Notebook/CHEM 471/2016/02/16

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Objectives

  1. Set up 1ml AgNP and AuNP synthesis reactions for SPI, WPI, Casein, Pea Protein and Brown Rice Protein
  2. Set up 20ml WPI AuNP, SPI AuNP, Pea Protein AgNP and Casein AgNP reactions

Materials

  1. Used same nutritional proteins on 02/02/16
  2. Protein and gold stocks prepared fresh every day
  3. Ocean Optics UV Vis was used to record UVVIS Spectra of Casein AgNPs. The other machine broke and is unusable.
    1. Integration time= 10ms and Average =100.
    2. A water blank in the same quartz cuvette was subtracted from the spectra before running any samples.


Procedure

  1. Further reduce stock protein concentrations (and thus concentrations in reaction mix) to increase metal/protein ratio to spur NP formation as we saw protein aggregate and nanofiber formation in previous reactions
  2. using citrate instead of fructose as reducing agent and increase concentration from 02/10/16 trial
  3. comparing citrate to no citrate samples, and vary citrate concentration
  1. Prepare 20ml reaction to synthesize large quantities of reactions known to work
    1. SPI AuNP, WPI AuNP, and Casein AgNP as shown below.
      1. Note that spectra of reaction mixes before reacting need to be taken
      2. Also note that this is just one size of nanoparticle that can be made with these reactions, its possible to change variables and change size and functionality of nanoparticle, these were just the first reactions to work.


Detailed Reaction Setup shown Below (4 hours 80˚C, 1ml rxns)

20ml Reactions ' ' ' ' ' ' ' '
Vial # 2.5mM HAuCl4 (µL) 5mMAgNO3 (µL) Protein (µL) 10 mM Citrate (µL) Water (µL) Au/Ag:Protein Notes
Casein 0.5 1 0 800 11200 0 8000 dark yellow nanoparticles
SPI 0.25 2 800 0 4000 400 14800 gold nanoparticles made
WPI 0.25 3 800 0 4000 400 14800 gold nanoparticles made
Pea Protein 0.25 4 0 800 4000 0 15200 protein agregates at bottom
2.5mMAgNO3 2.5mM HAuCl4 Citrate-Silver Citrate-Gold
Casein x –––––––––– x
Soy x x
Whey x
Pea x
Rice x
1mL Reactions
Vial # 2.5mM HAuCl4 (µL) 5 mMAgNO3 (µL) Protein (µL) 10 mM Citrate (µL) Water (µL) Au/Ag:Protein Notes
0.25 mg/mL Casein 1 40 0 560 40 360 -added 4 drops of 1M NaOH to dissolve, no reaction
Dilute from .5mg/ml Casein 2 40 0 560 60 340 no reaction
grams weighed: 12.91mg 3 40 0 200 40 720 no reaction
Stock: 26mL 4 40 0 200 60 700 no reaction
5 40 0 200 20 740 gold NPs w/ precipitate
6 40 0 200 40 720 gold NPs w/ precipitate
0.25 mg/mL Soy 7 40 0 100 0 860 gold NPs, fibers/aggregates?on sides w/ precipitate
grams weighed: 3.8mg 8 40 0 100 20 840 gold NPs w/ less precipitate
Stock: 15mL 9 0 40 560 40 360 slight NP (possibly due to citrate?)
10 0 40 560 60 340 slight NP (possibly due to citrate?)
11 0 40 200 40 720 slight NP (possibly due to citrate?)
12 0 40 200 60 700 slight NP (possibly due to citrate?)
13 40 0 200 20 740 gold NPs with some gold precipitate
14 40 0 200 40 720 gold NPs with some gold precipitate
0.25 mg/mL Whey 15 40 0 100 0 860 gold NPs with some gold precipitate
grams weighed:4.1mg 16 40 0 100 20 840 gold NPs with some gold precipitate
Stock: 16.5mL 17 0 40 560 40 360 slight NP (possibly due to citrate?)
18 0 40 560 60 340 slight NP (possibly due to citrate?)
19 0 40 200 40 720 slight NP (possibly due to citrate?)
20 0 40 200 60 700 slight NP (possibly due to citrate?)
0.15 mg/mL Pea 21 40 0 560 40 360 Added 20 Drops of 4M HCl, no rxn
Diluted from .25mg/ml 22 40 0 560 60 340 no rxn
grams weighed:7.8mg 23 40 0 200 40 720 no rxn
Stock: 31 mL 24 40 0 200 60 700 no rxn
25 40 0 560 0 400 add 10 drops 1M NaOH, no rxn
0.15 mg/mL Rice 26 40 0 560 20 380 no rxn
grams weighed: 1.5mg 27 40 0 200 0 760 no rxn
Stock: 10 mL 28 40 0 200 20 740 no rxn
29 0 40 560 0 400 AgNPs formed
30 0 40 560 20 380 AgNPs formed
31 0 40 200 0 760 AgNPs formed
32 0 40 200 20 740 AgNPs formed



Results

20ml Samples

  1. SPI and WPI AuNP formed purple colored NPs
  2. Casein AgNP formed gold colored NPs
  3. Pea Protein solution remained clear with some white precipitation, possibly not total dilution

UV-Vis data at SRB Lab Notebook Data