User:Karlena L. Brown/Notebook/PVOH Research/2012/10/05

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OBJECTIVES

  1. Prepare CuSO4 exchanged clay dilutions from Cu2+ clay exchanged stock solution for atomic absorption
  2. Run absorption on all CuSO4 dilution samples prepared

Preparations For CuSO4 Clay Exchanged Solutions & Vacuum Filtration Procedures

Setup of a vacuum filtration system:

  * Clean 250mL Erlenmeyer Filter Flask
  * Large Buchner Funnel
  * Whatman #42 Filter Paper
  * Long Secure Rubber Hose
  1. Pour 20 mL of CuSO4 stock solution into a 100mL beaker with a stir bar
  2. As the solution stirs, measure out and add ~ 0.1 grams of NaMT clay and start the timer
  3. Time for ~ 1 min and then filter the solution using the vacuum filtration system setup
  4. Attach all parts of the apparatus to the vacuum filtrator system
  5. Place a piece of Whatman #42 filter paper in the Buchner Funnel
  6. Turn on the vacuum filtrator system
  7. Check the suction rate to ensure that enough pressure is applied
  8. Pour in the 1 min. exchanged NaMT CuSO4 aqueous solution
  9. Allow the vacuum filtration to continue until the clay is completely dry
  10. Collect the aqueous filtrate solution and place it in a labeled small closed cap vial
  11. Collect the soil filtrate on the filter paper and scrape it into a small labeled metal pan
  12. Place metal pan with the soil filtrate in the oven to dry for ~ 1 day
  13. Wash all glassware and equipment first with H2O and then with acetone for later use


REPEAT THE PROCEDURE ABOVE FOR TIME PERIODS OF 5 MIN & 10 MIN FOR EACH SAMPLE

REPEAT THE PROCEDURE ABOVE FOR THE 100% CEC NaMT, 50% CEC NaMT, & 2:1 Fe3O4 CLAYS AS WELL

Atomic Absorption CuSO4 Clay Exchanged Dilutions & Calculations

CuSO4 Dilution Standards

12mL 7.4 ppm CuSO4 requires:
 (636ppm CuSO4)V1 = (7.4ppm CuSO4)(12mL)
   V1 = 0.140mL
12mL 10 ppm CuSO4 requires:
 (636ppm CuSO4)V1 = (10ppm CuSO4)(12mL)
   V1 = 0.189mL


  • Total of 18 dilutions were made for every time interval (1 min, 5 min, and 10 min) during the NaMT, 50% CEC NaMT, and 100% CEC NaMT clay exchanges.

Atomic Absorption Results

Atomic Absorption Data and Calibration Curve Data from AA wizard:

Cu ' ' ' '
Action Sample ID True Value (ppm) Conc. (ppm) Abs.
AUTOZERO
STD STD 1 1 0.0054
STD STD 2 5 0.0118
STD STD 3 10 0.6531
STD STD 4 20 1.0516
STD STD 5 25 1.1173
STD STD 6 30 1.1773
STD STD 7 40 1.2726
STD STD 8 50 1.3179
UNK1 7.4ppm NaMT 1min 7.5551 0.3993
UNK2 10ppm NaMT 1 min 10.9678 0.4959
UNK3 7.4ppm NaMT 5 min 7.0393 0.3847
UNK4 10ppm NaMT 5 min 10.6639 0.4873
UNK5 7.4ppm NaMt 10 min 4.2696 0.3063
UNK6 10ppm NaMT 10min 7.2478 0.3906
UNK7 7.4ppm Fe3O4 1min 46.4402 1.5
UNK8 10ppm Fe3O4 1 min 44.9883 1.4589
UNK9 7.4ppm Fe3O4 5min 39.7598 1.3109
UNK10 10ppm Fe3O4 5min 43.9567 1.4297
UNK11 7.4ppm Fe3O4 10min 39.841 1.3132
UNK12 10ppm Fe3O4 10min 39.9647 1.3167
UNK13 7.4ppm CEC100% 1min 11.1939 0.5023
UNK14 10ppmCEC100% 1min 16.5283 0.6533
UNK15 7.4ppm CEC100% 5min 9.5123 0.4547
UNK16 10ppm CEC100% 5min 15.4473 0.6227
UNK17 7.4ppm CEC100% 10min 8.4171 0.4237
UNK18 10ppm CEC100% 10min 15.7794 0.6321
UNK19 7.4ppm CEC 50% 1min 10.5191 0.4832
UNK20 10ppm CEC 50% 1min 14.7443 0.6028
UNK21 7.4ppm CEC 50% 5min 9.802 0.4629
UNK22 10ppm CEC 50% 5min 15.3449 0.6198
UNK23 7.4ppm CEC 50% 10min 10.4449 0.4811
UNK24 10ppm CEC 50% 10min 15.0057 0.6102


Notes

  • Dilution standards listed above for CuSO4 are incorrect and inaccurate due to miscalculations of stock solution concentrations
    CuSO4 stock solution = 1283 ppm  
  • New original standards prepared were increasingly high in concentration; therefore, CuSO4 standards, 5-20ppm, must remade
  • All 2:1 α-Fe3O4 samples remade and tested because the solutions were diluted with CuSO4 instead of distilled H2O
  • Due to various errors regarding concentrations the calibration curve created was inaccurate
  • AA needs to be run again
  • IMPORTANT NOTE: Between each sample, distilled H2O must be run to clear out all left over residue from the previous sample. Allow the absorption value, while running distilled H2O, to reach the value of 0 on the computer before running another concentrated CuSO4 sample