A comparison of different analytical

methods to determine the concentration

of zinc ions in the sample.











Number and name of the unknown zinc sample: Blue 11
By A I Choudhury
Student number:702881

03/04/2012
Abstract
The concentration of zinc (Zn
2+
) in the Blue 11 sample was determined using gravimetric analysis, EDTA
titration and atomic absorption. Due to the fact the group had not carried out the gravimetric method it was
difficult to assess how accurate the results were. Therefore the gravimetric result was not taken into account
in calculating the final concentration of zinc which was 1975ppm.
Introduction
Various analytical methods were used to determine the concentration of zinc in the Blue 11 sample. Each
method had its own individual advantages and disadvantages. Several methods were collectively used to
analyse the concentration of zinc to eliminate the drawbacks associated with using just a single method. The
aim was to find the concentration of zinc in Blue 11 solution by gravimetric analysis, EDTA titration and atomic
absorption and the data was used to decide the best value for the concentration of zinc in the sample.
Method
The analyses were carried out as described in the laboratory script. However the lost samples from gravimetric
analysis were replaced by another groups results; the figures for the Blue 11 solution were given by Dr. Peter
Douglas.
Results
(i) Calibration of pipette
TABLE 1 Mass of water from 20ml pipette.
Stage Mass/g
Before water was added 17.9846
After water was added 37.8638
Difference 19.8792

TABLE 2 Volume of water from calibrated 20ml pipette.
Temperature/C Mass of water/g Density of water/gml
-1
Volume/ml
24.0 19.8792 0.99633 19.952

In future calculations the volume of the calibrated water was shown to 5 significant figures as 19.9524ml in
order to reduce rounding errors.
(ii) Volumetric analysis

TABLE 3 Volume of EDTA required to reach end point
Titre/ml
Stage Trial 1 2 3
Start 0.36 8.20 3.60 9.72
Finish 27.40 35.58 31.80 37.12
Difference 27.04 27.38 28.00 27.40

Titre 1 and 3 were within 0.05 ml of each other however 2 wasnt. Therefore the mean would only take into account titre 1 and 3.
TABLE 4 Calculations of zinc concentration in volumetric titrimetry
C(EDTA)/moldm
-3
Mean
titre/dm
3
10
-3
n(Zn
2+
)/mol10
-4
V(Zn
2+
)/dm
3
1
0
-3
C((Zn
2+
)/moldm
-3
M(Zn
2+
)/gmol
-1
C(Zn
2+
)/gdm
-3
C(Zn
2+
)/ppm
0.022005 27.39 6.0272 19.9524 0.030208 65.38 1.9750 1975

TABLE 5 Final results of zinc concentrations in volumetric titrimetry
Ion C/moldm
-3
C/gdm
-3
C/ppm
Zn
2+
0.03021 1.975 1975







(iii) Gravimetric analysis
TABLE 6 Calculations of zinc concentration in gravimetric analysis
Crucible
1/g
Crucible
2/g
Mean/
g
M(Zn(C
10
H
6
O
2
N)
2
.H
2
O/g
mol
-1
n(Zn
2+
)/mol10
-4
V(Zn
2+
)/dm
3
10
-3
C(Zn
2+
)/moldm
-3
M(Zn
2+
)/gmol
-1
C/gdm
-3
C/ppm
0.2537 0.2557 0.2547 427.721 5.9548 19.9524 0.029845 65.38 1.9513 1951

The calculations were carried out to 5 significant figures and the final results were shown to 4 significant figures in TABLE 7.

TABLE 7 Final results of zinc concentrations in gravimetric analysis
Ion C/moldm
-3
C/gdm
-3
C/ppm
Zn
2+
0.02984 1.951 1951

(iv) Atomic absorption
TABLE 10 The mean absorbance of each solution
Absorbance
C(Zn
2+
)/ppm 1 2 3 4 5 6 Mean
0.50 0.226 0.232 0.225 0.236 0.227 0.228 0.229
0.75 0.340 0.344 0.343 0.340 0.338 0.341 0.341
1.00 0.452 0.451 0.446 0.453 0.444 0.447 0.449
1.25 0.561 0.565 0.566 0.561 0.568 0.565 0.564
1.50 0.657 0.659 0.653 0.656 0.662 0.665 0.659
2.00 0.861 0.869 0.857 0.867 0.873 0.865 0.865
Unknown 0.434 0.432 0.441 0.431 0.432 0.433 0.434




Concentration of Zn
2+
in a 100ml solution obtained from atomic absorption graph (FIGURE 1) is 0.9875 ppm.
EXAMPLE 1 Calculate the concentration of Zn
2+
in a 0.471ml solution
0.9875ppm

=1975ppm
TABLE 11 Final results of zinc concentrations in atomic absorption
Ion C/moldm
-3
C/gdm
-3
C/ppm
Zn
2+
0.03021 1.975 1975

Conclusions
The best value for the concentration of zinc in sample Blue 11 was 1975ppm. The volumetric method was
accurate and precise and had low relative errors. The results for gravimetric methods were not ideal as they
were 0.01g away from the mean instead the two results from each crucible was supposed to be within 0.001g
within each other. There was moderate amount of uncertainty with the concentration of zinc obtained from
FIGURE 1 as it could only be determined to within 0.5% of the range in concentration therefore the method for
atomic absorption was not as accurate although the results were precise. However, the concentration of zinc
ions for atomic absorption was the same as volumetric analysis.
Critical assessment
The gravimetric method was slower than other analytical procedures. This was true if it based upon difference
between start and finish of analysis .But most of the time was used up in drying, digesting and evaporating
which required little attention by the operator. In terms of operator time it was the most efficient because
there was no need for standardisation. Other analytical methods required preparation of standard solutions to
either derive a calibration curve or titrate a solution of the analyte. In contrast, gravimetric method required a
table of atomic weights and the stoichiometric ratio between reactants and products. The analytical balance
used measured the mass in grams to 4 decimals places and it was feasible to obtain weight to within a few
parts per thousands of its true value, the weighing uncertainty was decreased to a few parts per millions.
However, the sensitivity and accuracy of a gravimetric method was limited by solubility losses, coprecipitation
errors and mechanical losses of precipitate. The equipment required for gravimetric analysis was simple,
relatively inexpensive, reliable and easy to maintain.
The equivalence point could not be determined experimentally but it was estimated by observing the physical
change called the end point. Therefore there an uncertainty in the difference between the equivalence and
end point called the titration error. The accuracy of the volumetric titrimetry method depended upon the
accuracy of the concentration of the standard solution. The accuracy also depended on how fast standard
solution reacted with the analyte so that the time required between additions of titrant is minimised and it
how far it reacted with the analyte. The method was fast and simple to follow. The equipment required for
volumetric titrimetry was relatively inexpensive reliable and easy to maintain.
The line of best fit for the calibration curve in FIGURE 1 was drawn and plotted by operator therefore various
operators interpreted the line of best fit differently and therefore there were personal errors. This affected the
accuracy of the results. The limitation was that the graphs could not been drawn using computer software
such as excel due to procedure stating that the graphs was to be drawn by hand. The errors for the line of best
fit would have been reduced if it was drawn on excel. Although the method was easy and fast to follow the
equipment for spectrometer was sophisticated and expensive and can cost around six thousand pounds.
Although the spectrometer is expensive the results for absorbance were highly precise and would have been
more accurate if there was a data logger recording the results in a spreadsheet and plotting results on a virtual
diagram.