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ABSTRACT:
different burner height than the highest signal:background; the spectroscopy runs
show strongest signals for atomic Ca absorption and ionic Mg absorption; the
chemical interference trials demonstrate the hindering effect of phosphoric acid and
the beneficial, preventative effect of strontium and EDTA in the Ca solutions destined
for spectral analysis; by the external standards method, the concentration of Ca (aq) in
the unknown was determined to be 1.457 ± 0.097 ppm (± 6.657 %). There is,
however, limited data in certain sections and so conclusions are not as binding.
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INTRODUCTION:
atomic absorption spectrophotometer) to excite the analyte atoms and measure their
absorption/emission spectra.
The first section was the optimising the instrumentation setup; the second
section saw the main experiment where the analyte (Ca and Mg) was volatilised,
ionised and its spectra measured as per the sub-species (atomic or ionic Ca or Mg)
under study, this was done by adjusting the wavelengths corresponding to the sub-
in the third section where the effect of additives such as K (aq), EDTA, phosphoric
acid and strontium were studied. The fourth section involved application of the
250mL of a 10 ppm Ca (aq) solution from the stock solution of 1,000 ppm. This was
done by diluting 2.5 mL of the stock solution with de-ionised water to the mark in a
volumetric flask. 94.51 g of the Ca solution and 55.03 g of water were added to two
separate plastic bottles. The sample tube was inserted in the Ca solution bottle and the
drain tube in the water bottle. The flame was then lit. Aspiration and nebulisation
were conducted for five minutes (blue flame), at the end of which the flame was shut
off and the bottles were re-weighed at 70.34 g and 76.70 g for the Ca (aq) and water
respectively. The sample uptake rate was calculated at 0.5 mL/min and the experiment
The next section involved the process for selecting the optimum burner height.
The burner heights of 2, 2.5, 2.75, 3, 3.25, 3.5 and 4 were tried and for each height
value, the mean detector response was noted for the 10 ppm Ca solution and the
blank. The optimal burner height was deemed to be 3.25. During this aspiration, the
FAS section 2: The 1,000 ppm Ca and Mg stock solutions were used to
extracts of the solutions with de-ionised water to the mark in separate volumetric
flasks.
The solutions were analysed and the emission intensities recorded; the
scanning wavelengths were set from 1 nm less to 1 nm beyond the literature emission
! $!
wavelength for the particular species to be analysed: 421.5 nm ! CaI ! 423.5 nm,
554.0 nm ! CaOH ! 556.0 nm and 284.2 nm ! MgI ! 286.2 nm; the scan rate was set
at 1 nm/min. The next step was measuring the signal intensities of the CaI, CaII, MgI
and the MgII species at their respective wavelengths of 422.5 nm, 393.3 nm, 285.2
nm and 279.5 nm respectively. The (H)ollow (C)athode (L)amp was turned on, set to
the suitable current and the signals were recorded for CaI and MgI at their respective
concentration each were prepared (as before). To one pair of Ca and Mg solutions,
0.1 mL of 10,000 ppm K (aq) were added to bring its K (aq) concentration to 10 ppm;
10 mL of the stock K (aq) solution were added to another pair to bring the K (aq)
concentration to 1,000 ppm and no K (aq) was added to the third pair. The emission
intensities of the Ca (CaI) solutions were measured and the absorption intensities of
the Mg (MgI) solutions were measured. Four more 100 mL Ca (aq) of 10 ppm were
prepared in the following manner. 10 mL of 0.01 mol/L H3PO4 was added to one 100
of 0.01 mol/L H3PO4 + 10 mL of 10,000 ppm Sr2+ to have 0.01 mol/L concentration
of the acid and 1000 ppm of the Sr2+ (aq) was added to another, the same volume of
the acid (and thus concentration) + 50 mL of 0.05 mol/L EDTA were added to the
third flask, and nothing was added to the fourth flask; 1 mL of the stock Ca solution
was added to each flask and were all diluted to the mark with de-ionised water. Their
intensities were measured at the CaI line (422.5 nm). The presence of Sr (aq) caused
FAS section 4: The vessels used as the containers for the following are
volumetric flasks. Ca (aq) solutions of 10, 5, 1, 0.1 and 0.01 ppm were prepared. The
10 ppm solution was prepared as before; the 5 ppm one was prepared by diluting 0.5
mL of the 1,000 ppm Ca solution to the 100 mL mark; the 1 ppm solution was
prepared by diluting 10 mL of the 10 ppm solution to the mark; 0.1 ppm solution by
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diluting 1 mL of the 1 ppm to the mark and so on and so forth for further lower
phosphoric acid + 2.5 mL of the 1,000 ppm Ca sol to the 250 mL mark with de-
ionised water. The HCL lamp was turned off and the emission intensities of CaI were
measured using the Ca solutions prepared. Multiple readings were taken for each
concentration and the averages recorded. The unknown was measured five times as
well.
25 mL aliquots of the unknown was made, to which 0, 0.2, 0.4, 0.6 and 0.8 mL
of the 1,000 ppm Ca stock solution was added then diluted to the 50 mL mark. Their
! FAS section 1: -
mg g
24.17 mL of 10 ppm Ca (aq) " 24.17 mL #10 ÷ 40.08 # NA
L mol
= 1.21#1016 atoms /s
!
! '!
" Q1: -
! " Q3: -
! error : "
2
s 1 1 ( yc " y)
sc = y + +
m M N m 2 Sxx
2
1 (0.226 " 2 (0.693 " 0.145))
1
0.005
= • 1+ +
0.059 4 0.059 2 # 40.67
4 ("0.048) 2
= 0.084 • +
3 0.145
!
concentration of unknown: 1.457 ± 0.097 ppm
! *%!
" Q4, Q5: -
" FAS 1:
in the calculation of the nebulisation efficiency, plastic bottles were used and
not glass. Plastic is lighter, easier to handle and wield and that it would still allow for
The best S/N ratio is found at a lower burner height than the for the best S/B
ratio. As the burner height is raised, the inter-zonal region is reached, which is the
most efficient region for atomisation and contains the highest concentration.
Mg: from the negative emission intensities, it can be seen that absorption is
more suited to Mg. The best signal is from the ionic emission since it has a higher net
Ca: from the limited data, the absorption mode for atomic Ca provides the
best signal ! lowest error margin and a reasonable net signal strength.
Ionisation equilibria: -
consumes more energy of the system, so Ca or Mg has less and that by its own
Chatilier’s principle. As the concentration rises even further, other factors such as
energy loss due to inter-atomic collisions come into play, since there exist more
A hotter flame would raise the rate of decomposition and volatilisation of the
The greater the concentration of H3PO4, the higher the concentration of the
analyte). This particular substance does not break apart as easily in the flame, nor
does it volatilise; hence the signal intensity is, in a way, doubly reduced.
! *(!
2-
Sr would react and bind with the HPO4 ion, thereby allowing for the Ca
analyte to remain free. In other words, it would block the interfering acid and prevent
EDTA forms volatile complexes with Ca thereby saving it from forming the
Due to likely experimental errors and the more cumbersome calculations in the
evaluation of error margins with the standard addition method, the external standard
It is proven that due to the inherent characteristics of a flame, the best S/N is
obtained at a different burner height than the best S/B. The subsequent data shows the
absorption mode for atomic Ca and ionic Mg as the most reliable signals, though the
data is limited and this cannot be satisfactorily proven. The interference section shows
the hindering effect of phosphoric acid and the beneficial, preventative effect of
strontium and EDTA in the Ca solutions destined for spectral analysis. Lastly, by the
external standards method, the concentration of Ca (aq) in the unknown was 1.457 ±