Calcium around us

PROCEDURE
Part 1: Preparation of samples for measurement by the AA spectrophotometer
A. Sea Shell sample
1. Weigh out accurately (to 4 decimal places) about 0.25 g of sea shell in a clean and dry 100 mL conical flask. Record the mass in
the results sheet.
2. Add 5 drops EtOH and 10 mL of 2 M HCl.
3. Boil the solution on the hot plate for 2 minutes, to complete the reaction. The sea shell should completely dissolve.
4. Allow the flask to cool then remove any remaining undissolved material by filtering through a fluted paper (See Laboratory
Techniques in the front of the laboratory manual) into a clean 100 mL volumetric flask (often referred to as a standard flask),
washing the filter paper at least twice with 5 mL portions of distilled water. The transfer of the solution containing calcium ions must
be complete. It is best achieved by several rinses of your filter paper, over its entire surface. This step is crucial for good results.
Using distilled water, carefully make the volume up to 100 mL. Mix well by inverting the flask repeatedly.
5. Pipette 1 mL of this solution into a clean 50 mL volumetric flask and dilute to the 50 mL mark with distilled water. Mix well.
6. Pipette 5 mL of this diluted solution into a clean 10 mL volumetric flask and dilute to the 10 mL mark with 3000 ppm Sr 2+ solution.
Mix well.

Part 2: Determination of the Ca2+ concentration in the prepared samples by atomic absorption spectroscopy
The computer controls all stages of the Atomic Absorption analysis.
1. Clear any previously-stored results by clicking on the “Results” button, then “New” (top left) followed by “Create” (accept the
displayed filename) and “Overwrite”. Click “Start” to initiate the sample sequence on the computer.
2. Aspirate the blank solution (1500 ppm Sr2+), and set the absorbance to zero (click button on screen).
3. Calibrate the spectrophotometer by aspirating the 5 calcium standards supplied in the order:

standard 1: 2 ppm; standard 2: 5 ppm; standard 3: 10 ppm; standard 4: 15 ppm; standard 5: 20 ppm.
4. Rinse the delivery tube between measurements by aspirating with distilled water.
5. When the last sample is measured, the computer automatically displays the results. Plot a graph of absorbance versus Ca2+
concentration (in ppm) showing the line of best fit used as the calibration curve using Excel. Your tutor will print a copy of the
results for each student.
6. Determine the absorbance values for each of the final diluted samples (A, B, C) prepared in Part 1 of the procedure.

Standard Concentration (ppm) (X) Absorbance (Y)

1 2 0.015
2 5 0.035
3 10 0.070
4 15 0.100
5 20 0.150
0.053 7.53 100 753

0.25

0.075

30.12

30.12