2.

0 Methodology

2.1 Preparation of Standard Copper Solution for Calibration

From the standard copper solution, 1000 ppm, five standard copper solution (S1, S2,
S3, S4 and S5) with varying copper concentration (1 ppm, 2 ppm, 3 ppm, 4 ppm, and 5 ppm)
will be provided to us.

Dilution method for preparing the copper standard solution will be shown by the
technical staff.

2.2 Preparation of Sample Solution for the Analysis of Copper

By using the analytical balance, two samples were weighted with each having a
weight of 0.1xxx g into two separate 250 ml beaker and labeled as sample A and B
respectively. The two samples were decomposed by adding 20 ml of aqua regia solution that
has been prepared into both the beakers. The beakers were covered with a watch glass and
were placed on a hot plate. Heat and evaporate just to dryness until 1-2 ml residual volume
left inside the beaker.

Then the watch glass was rinsed with some deionized water and the rinse solution was
added back into the beaker. Into each beaker, 5 ml of concentrated HCl and about 50 ml
volume of deionized water were added. Each beaker was covered with a watch glass, and was
boiled gently to dissolve the salts. Both the samples A and B in the beakers were cooled.

Samples A and B were transferred quantitatively into two separate 100 ml volumetric
flask. The above solutions were diluted with deionized water by making up the volume to the
mark of the volumetric flasks. Both the volumetric flask were labeled as A and B accordingly.

20 ml of aliquot was pipetted from volumetric flask, then put into 100 ml volumetric
flask and made up to volume 100 ml. Both volumetric flasks were labeled as A1 and B1
accordingly.

2.3 Interference Effect of Other Ions in the Copper Analysis

*The chalcopyrite sample solution has presents in it many more ions than the standards which
have Cu2+ + SO42-. There has been an underlying assumption that none of these ions interfere.
To test this, prepare a dilution of the sample and another identical solution containing a
further 2.5 ppm Cu from the stock.
 From the sample solution A1 and B1, 20 ml of aliquot of solution A and B were
transferred into two separate 100 ml volumetric flask. Both the volumetric flask were labeled
as sample C and D respectively.

Then, 2.5 ppm of copper standard solution and 5 ml of HCl were added. Both the
samples in the volumetric flask were diluted using deionized water by making up to the mark.
The absorbance values were recorded and the concentrations from the AAS were compared
and then a conclusion regarding interference was drawn.

2.4 Copper Analysis Using AAS

The technical staff assisted in the operation of the AAS. From the standard copper
solution prepared for us, we are required to determine the concentration of copper in the
samples (A1, B1, C and D) given to us. This is done by plotting the calibration curve which is
the values of absorbance (Abs) plotted against the concentration of copper in ppm.

First, the readings of absorbance from the copper standard solution are taken to obtain
the calibration plot for the standard copper solution. Then aspirate the copper sample
solutions into the AAS.

The absorbance values for the unknown were recorded. If the absorbance values were
not in the linear range of the standards, make a suitable dilution to bring the absorbance
within the linear range of the standards. The absorbance (Abs) for all samples prepared were
measured and recorded. From the calibration plot, the concentration of copper in the samples
were obtained.