User:Matt Hartings/Notebook/AU Biomaterials Design Lab/2015/12/04

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Objective

Cassidy had previously incubated the Fe3O4 microgels with different metal salts.

Today I am going to run ICP to determine the concentration of metal left in solution.

Description

Standards I am using the ICP multi-element standard solution VII from Millipore (1.09492.0100, Lot HC43301592)

The rough concentration for all of the metal ions in this solution are 100 mg/L

  1. Solution 1
    1. Concentration: 10 mg/L
      1. Volume of standard used: 5 mL
      2. Final Volume: 50 mL
  2. Solution 2
    1. Concentration: 5 mg/L
      1. Volume of standard used: 2.5 mL
      2. Final Volume: 50 mL
  3. Solution 3
    1. Concentration: 1 mg/L
      1. Volume of standard used: 0.5 mL
      2. Final Volume: 50 mL
  4. Solution 4
    1. Concentration: 0.75 mg/L
      1. Volume of standard used: 0.375 mL
      2. Final Volume: 50 mL
  5. Solution 5
    1. Concentration: 0.5 mg/L
      1. Volume of standard used: 0.25 mL
      2. Final Volume: 50 mL
  6. Solution 6
    1. Concentration: 0.25 mg/L
      1. Volume of standard used: 0.125 mL
      2. Final Volume: 50 mL
  7. Solution 7
    1. Concentration: 0.1 mg/L
      1. Volume of standard used: 0.05 mL
      2. Final Volume: 50 mL

Note for solutions 6 and 7 I used a P200 pipet and added all of the solution in the tip. I did this based on a volume calibration that I had done before taking making solutions.

Metal Concentration In Standards (mg/L) and wavelengths used to evaluate concentration

  1. Cd (214.439 nm)
    1. Solution 1: 10.0
    2. Solution 2: 5.00
    3. Solution 3: 1.00
    4. Solution 4: 0.750
    5. Solution 5: 0.500
    6. Solution 6: 0.250
    7. Solution 7: 0.100
  2. Co (230.786 and 238.892 nm)
    1. Solution 1: 9.90
    2. Solution 2: 4.95
    3. Solution 3: 0.990
    4. Solution 4: 0.743
    5. Solution 5: 0.495
    6. Solution 6: 0.248
    7. Solution 7: 0.0990
  3. Cr (267.716 nm)
    1. Solution 1: 9.90
    2. Solution 2: 4.95
    3. Solution 3: 0.990
    4. Solution 4: 0.743
    5. Solution 5: 0.495
    6. Solution 6: 0.248
    7. Solution 7: 0.0990
  4. Cu (327.395 nm)
    1. Solution 1: 10.0
    2. Solution 2: 5.00
    3. Solution 3: 1.00
    4. Solution 4: 0.750
    5. Solution 5: 0.500
    6. Solution 6: 0.250
    7. Solution 7: 0.100
  5. Fe (238.204 and 259.940 nm)
    1. Solution 1: 10.1
    2. Solution 2: 5.05
    3. Solution 3: 1.01
    4. Solution 4: 0.758
    5. Solution 5: 0.505
    6. Solution 6: 0.253
    7. Solution 7: 0.101
  6. K (766.491 nm)
    1. Solution 1: 9.8
    2. Solution 2: 4.90
    3. Solution 3: 0.98
    4. Solution 4: 0.735
    5. Solution 5: 0.490
    6. Solution 6: 0.245
    7. Solution 7: 0.0980
  7. Mg (279.553 nm)
    1. Solution 1: 10.0
    2. Solution 2: 5.00
    3. Solution 3: 1.00
    4. Solution 4: 0.750
    5. Solution 5: 0.500
    6. Solution 6: 0.250
    7. Solution 7: 0.100
  8. Mn (257.610 nm)
    1. Solution 1: 10.0
    2. Solution 2: 5.00
    3. Solution 3: 1.00
    4. Solution 4: 0.750
    5. Solution 5: 0.500
    6. Solution 6: 0.250
    7. Solution 7: 0.100
  9. Na (588.995 nm)
    1. Solution 1: 10.1
    2. Solution 2: 5.05
    3. Solution 3: 1.01
    4. Solution 4: 0.758
    5. Solution 5: 0.505
    6. Solution 6: 0.253
    7. Solution 7: 0.101
  10. Ni (227.021 and 230.299 nm)
    1. Solution 1: 10.0
    2. Solution 2: 5.00
    3. Solution 3: 1.00
    4. Solution 4: 0.750
    5. Solution 5: 0.500
    6. Solution 6: 0.250
    7. Solution 7: 0.100
  11. Pb (220.353 nm)
    1. Solution 1: 10.0
    2. Solution 2: 5.00
    3. Solution 3: 1.00
    4. Solution 4: 0.750
    5. Solution 5: 0.500
    6. Solution 6: 0.250
    7. Solution 7: 0.100
  12. Zn (213.857 nm)
    1. Solution 1: 9.90
    2. Solution 2: 4.95
    3. Solution 3: 0.990
    4. Solution 4: 0.743
    5. Solution 5: 0.495
    6. Solution 6: 0.248
    7. Solution 7: 0.0990
  • Note: These wavelengths were chosen so that there was minimal overlap with the other wavelengths being used and that maximized the signal from the element of interest.

Running Conditions Agilent Technologies 5100 ICP-OES

  1. Replicates 3
  2. Pump Speed: 12 rpm
  3. Sample Introduction: Manual
  4. Uptake delay: 5s
  5. Read Time: 5s
  6. RF power: 1.20 kW
  7. Stabilization time: 5s
  8. Viewing mode: Axial
  9. Viewing Height: 8mm
  10. Nebulizer Flow: 0.7 L/min
  11. Plasma Flow: 12 L/min
  12. Aux flow: 1 L/min
  13. Make up flow: 0 L/min

Sample Names

  1. hyd FeNP Pb acetate 3.79mg/L
  2. dry FeNP Pb acetate 3.79mg/L
  3. Pb acetate 3.79mg/L
  4. dry FeNP Cd acetate 1.12mg/L
  5. hyd FeNP Cd acetate 1.12mg/L
  6. Cd acetate 1.12mg/L
  7. hyd FeNP Mg SO4 1.2mg/L
  8. dry FeNP Mg SO4 1.2mg/L
  9. Mg SO4 1.2mg/L
  10. hyd FeNP Cr Cl3 2.66mg/L
  11. dry FeNP Cr Cl3 2.66mg/L
  12. Cr Cl3 2.66mg/L pulled too soon … re-running
  13. Cr Cl3 2.66mg/L
  14. hyd FeNP Zn SO4 2.88mg/L
  15. dry FeNP Zn SO4 2.88mg/L
  16. Zn SO4 2.88mg/L
  17. hyd FeNP Ni SO4 2.63mg/L
  18. dry FeNP Ni SO4 2.63mg/L
  19. Ni SO4 2.63mg/L
  20. hyd FeNP Co Cl2 2.38mg/L
  21. dry FeNP Co Cl2 2.38mg/L
  22. Co Cl2 2.38mg/L
  23. hyd FeNP Mn Cl2 1.98mg/L
  24. dry FeNP Mn Cl2 1.98mg/L
  25. Mn Cl2 1.98mg/L
  26. hyd FeNP Cu Cl2 1.705mg/L
  27. dry FeNP Cu Cl2 1.705mg/L
  28. Cu Cl2 1.705mg/L

Calibration Curves Not all standards gave good data for the calibration curves. Some concentrations were too high. The following points were used:

  1. Cd (214.439 nm)
    1. Solution 2: 5.00
    2. Solution 3: 1.00
    3. Solution 4: 0.750
    4. Solution 5: 0.500
    5. Solution 6: 0.250
    6. Solution 7: 0.100
  2. Co (230.786 and 238.892 nm)
    1. Solution 2: 4.95
    2. Solution 3: 0.990
    3. Solution 4: 0.743
    4. Solution 5: 0.495
    5. Solution 6: 0.248
    6. Solution 7: 0.0990
  3. Cr (267.716 nm)
    1. Solution 2: 4.95
    2. Solution 3: 0.990
    3. Solution 4: 0.743
    4. Solution 5: 0.495
    5. Solution 6: 0.248
    6. Solution 7: 0.0990
  4. Cu (327.395 nm)
    1. Solution 1: 10.0
    2. Solution 2: 5.00
    3. Solution 3: 1.00
    4. Solution 4: 0.750
    5. Solution 5: 0.500
    6. Solution 6: 0.250
    7. Solution 7: 0.100
  5. Fe (238.204 and 259.940 nm)
    1. Solution 2: 5.05
    2. Solution 3: 1.01
    3. Solution 4: 0.758
    4. Solution 5: 0.505
    5. Solution 6: 0.253
    6. Solution 7: 0.101
  6. K (766.491 nm) *Special Circumstances more info below
    1. Solution 1: 9.8
    2. Solution 2: 4.90
    3. Solution 3: 0.98
    4. Solution 4: 0.735
    5. Solution 5: 0.490
    6. Solution 6: 0.245
    7. Solution 7: 0.0980
  7. Mg (279.553 nm)
    1. Solution 3: 1.00
    2. Solution 4: 0.750
    3. Solution 5: 0.500
    4. Solution 6: 0.250
    5. Solution 7: 0.100
  8. Mn (257.610 nm)
    1. Solution 3: 1.00
    2. Solution 4: 0.750
    3. Solution 5: 0.500
    4. Solution 6: 0.250
    5. Solution 7: 0.100
  9. Na (588.995 nm) *Special Circumstances more info below
    1. Solution 1: 10.1
    2. Solution 2: 5.05
    3. Solution 3: 1.01
    4. Solution 4: 0.758
    5. Solution 5: 0.505
    6. Solution 6: 0.253
    7. Solution 7: 0.101
  10. Ni (227.021 and 230.299 nm)
    1. Solution 2: 5.00
    2. Solution 3: 1.00
    3. Solution 4: 0.750
    4. Solution 5: 0.500
    5. Solution 6: 0.250
    6. Solution 7: 0.100
  11. Pb (220.353 nm)
    1. Solution 1: 10.0
    2. Solution 2: 5.00
    3. Solution 3: 1.00
    4. Solution 4: 0.750
    5. Solution 5: 0.500
    6. Solution 6: 0.250
    7. Solution 7: 0.100
  12. Zn (213.857 nm)
    1. Solution 3: 0.990
    2. Solution 4: 0.743
    3. Solution 5: 0.495
    4. Solution 6: 0.248
    5. Solution 7: 0.0990
  1. For low values of K, the following standards were used
    1. Solution 4: 0.735
    2. Solution 5: 0.490
    3. Solution 6: 0.245

For these points the calibration curve is:

Intensity = 81938.54*Concentration + 3311.66

  1. For high values of K, the following standards were used
    1. Solution 2: 4.90

For these points the calibration curve is:

Intensity = 107499.38*Concentration + 3336.50

All of the data for Na was at/near/or below the baseline value. All Na values are assumed to be zero. Which they should be ... there was no Na used anywhere in this study.

Data

  • Add data and results here...

Notes

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