User:Matt Hartings/Notebook/AU Biomaterials Design Lab/2014/02/03

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(Description)
(Description)
Line 40: Line 40:
## FW 121.16g/mol
## FW 121.16g/mol
## measure out: 0.6058g
## measure out: 0.6058g
 +
## measured: 0.6068g
 +
## actual conc: 0.0200M
# 50mL of 100mM ZnSO<sub>4</sub>
# 50mL of 100mM ZnSO<sub>4</sub>
## FW 287.56g/mol
## FW 287.56g/mol
## measure out: 1.4378g
## measure out: 1.4378g
 +
## measured: 1.4365 g
 +
## actual conc: 0.100M
# 50mL of 10mM MnCl<sub>2</sub>
# 50mL of 10mM MnCl<sub>2</sub>
## FW 197.9g/mol
## FW 197.9g/mol
## measure out: 0.09895g
## measure out: 0.09895g
 +
## measured: 0.1022g
 +
## actual conc: 0.0103M
# 10mL 1M NaOH
# 10mL 1M NaOH
## FW 40.00g/mol
## FW 40.00g/mol
## 0.400g
## 0.400g
 +
## Final concentration a bit under 1M check pH carefully when adjusting!
# 50mL 100mM Na<sub>2</sub>S
# 50mL 100mM Na<sub>2</sub>S
## FW 240.18g/mol
## FW 240.18g/mol
## measure out: 1.2009g
## measure out: 1.2009g
 +
## measured: 1.2085g
 +
## actual conc: 0.101M
 +
 +
Protocol should be changed to:
 +
# To a 3-necked flask is added
 +
## 50mL of 20mM L-cysteine
 +
## 5mL of 100mM ZnSO<sub>4</sub> (0.5 mmol)
 +
## 5.437mL of 10.3mM MnCl<sub>2</sub> (0.056 mmol)
 +
## The pH of this mixture is adjusted to 11 with ~1M NaOH (should be on the order of 60uL)
 +
# This mixture is stirred under Ar (I'll use N<sub>2</sub>) for 30 minutes
 +
# 5.505mL of 101mM Na<usb>2</sub>S is quickly added.
 +
# The solution is stirred for 20 minutes
 +
# The solution is then aged at 50C under air for 2 hours.
 +
# The nano particles are purified through precipitation by ethanol and centrifuging at 5000rpm for 5 minutes
 +
## That's all they really say about this. I'm assuming it means:
 +
### The reaction mixture is cooled in an ice bath.
 +
### At least 200mL of chilled ethanol is added to the reaction mixture to precipitate the solid
 +
### The solid is collected by centrifugation (5 minutes at 5000 rpm)
 +
### The solid is re-dissolved in a minimum amount of cold water
 +
### The nanoparticles are precipitated through the addition of cold ethanol
 +
### Steps 4 and 5 are repeated once
 +
### The product is dried under vacuum and the product is stored in an inert environment.
==Data==
==Data==

Revision as of 16:10, 3 February 2014

Biomaterials Design Lab Main project page
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Objective

Notes on the synthesis of Mn-doped ZnS quantum dots. The aqueous-based synthesis that I'll be doing for Nancy Zeller and the Gen Bio 210 students.

Description

This synthesis is based on the protocols found in the following papers Nanoscale, 2013, 5, 9156 and Analytical Chemistry, 2008, 80, 3832

  1. To a 3-necked flask is added
    1. 50mL of 20mM L-cysteine
    2. 5mL of 100mM ZnSO4 (0.5 mmol)
    3. 5.6mL of 10mM MnCl2 (0.056 mmol) (Note: The Nanoscale paper states that the 5% Mn substitution has the best luminescence yield)
    4. The pH of this mixture is adjusted to 11 with 1M NaOH (should be on the order of 60uL)
  2. This mixture is stirred under Ar (I'll use N2) for 30 minutes
  3. 5.56mL of 100mM Na<usb>2</sub>S is quickly added. (Note: The authors of the other papers use 5 mL to match the amount of Zn. But logic states the S should be equimolar to the combination of Zn and Mn)
  4. The solution is stirred for 20 minutes
  5. The solution is then aged at 50C under air for 2 hours.
  6. The nano particles are purified through precipitation by ethanol and centrifuging at 5000rpm for 5 minutes
    1. That's all they really say about this. I'm assuming it means:
      1. The reaction mixture is cooled in an ice bath.
      2. At least 200mL of chilled ethanol is added to the reaction mixture to precipitate the solid
      3. The solid is collected by centrifugation (5 minutes at 5000 rpm)
      4. The solid is re-dissolved in a minimum amount of cold water
      5. The nanoparticles are precipitated through the addition of cold ethanol
      6. Steps 4 and 5 are repeated once
      7. The product is dried under vacuum and the product is stored in an inert environment.

The solutions I need to make are:

  1. 250mL of 20mM L-cysteine
    1. FW 121.16g/mol
    2. measure out: 0.6058g
    3. measured: 0.6068g
    4. actual conc: 0.0200M
  2. 50mL of 100mM ZnSO4
    1. FW 287.56g/mol
    2. measure out: 1.4378g
    3. measured: 1.4365 g
    4. actual conc: 0.100M
  3. 50mL of 10mM MnCl2
    1. FW 197.9g/mol
    2. measure out: 0.09895g
    3. measured: 0.1022g
    4. actual conc: 0.0103M
  4. 10mL 1M NaOH
    1. FW 40.00g/mol
    2. 0.400g
    3. Final concentration a bit under 1M check pH carefully when adjusting!
  5. 50mL 100mM Na2S
    1. FW 240.18g/mol
    2. measure out: 1.2009g
    3. measured: 1.2085g
    4. actual conc: 0.101M

Protocol should be changed to:

  1. To a 3-necked flask is added
    1. 50mL of 20mM L-cysteine
    2. 5mL of 100mM ZnSO4 (0.5 mmol)
    3. 5.437mL of 10.3mM MnCl2 (0.056 mmol)
    4. The pH of this mixture is adjusted to 11 with ~1M NaOH (should be on the order of 60uL)
  2. This mixture is stirred under Ar (I'll use N2) for 30 minutes
  3. 5.505mL of 101mM Na<usb>2</sub>S is quickly added.
  4. The solution is stirred for 20 minutes
  5. The solution is then aged at 50C under air for 2 hours.
  6. The nano particles are purified through precipitation by ethanol and centrifuging at 5000rpm for 5 minutes
    1. That's all they really say about this. I'm assuming it means:
      1. The reaction mixture is cooled in an ice bath.
      2. At least 200mL of chilled ethanol is added to the reaction mixture to precipitate the solid
      3. The solid is collected by centrifugation (5 minutes at 5000 rpm)
      4. The solid is re-dissolved in a minimum amount of cold water
      5. The nanoparticles are precipitated through the addition of cold ethanol
      6. Steps 4 and 5 are repeated once
      7. The product is dried under vacuum and the product is stored in an inert environment.

Data

  • Add data and results here...

Notes

This area is for any observations or conclusions that you would like to note.


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