Q1.
The Fe concentration in a sample was determined 6 trials by a single method as the
following (19.4, 19.5, 19.6, 19.8, 20.1 and 20.3 ppm). Calculate mean, standard deviation,
variance, spread, relative standard deviation, coefficient of variation, absolute error and
relative error for the method, based upon these obtained data (true value is 20.00 ppm):
Q2. The mercury in samples of seven fish taken from Chesapeake bay was determined by a
method based on the absorption of radiation by gaseous elemental mercury. Calculate a
pooled estimate of the standard deviation for the method, based upon the first three columns
of data:
Specimen Number of Hg Content, ppm
samples
Measured
1 3 1.80, 1.58, 1.64
2 4 0.96, 0.98, 1.02, 1.10
3 2 3.13, 3.35
4 6 2.06, 1.93, 2.12, 2.16, 1.89, 1.95
5 4 0.57, 0.58, 0.64, 0.49
6 5 2.35, 2.44, 2.70, 2.48, 2.44
7 4 1.11, 1.15, 1.22, 1.04
Q2. The mercury in samples of seven fish taken from Chesapeake bay was determined by a
method based on the absorption of radiation by gaseous elemental mercury. Calculate a
pooled estimate of the standard deviation for the method, based upon the first three columns
of data:
Mean
( xi − x ) 2
Specimen Number of Hg Content, ppm
samples Ppm Hg
Measured
1 3 1.80, 1.58, 1.64 1.673 0.0258
2 4 0.96, 0.98, 1.02, 1.10 1.015 0.0115
3 2 3.13, 3.35 3.240 0.0242
2.06, 1.93, 2.12, 2.16, 1.89, 2.018 0.0611
4 6 1.95
5 4 0.57, 0.58, 0.64, 0.49 0.570 0.0114
6 5 2.35, 2.44, 2.70, 2.48, 2.44 2.482 0.0685
7 4 1.11, 1.15, 1.22, 1.04 1.130 0.0170
Q3. The mercury in a fish sample is determined to be 1.80, 1.58 and 1.64 ppm.
Calculate the 80% and 95 % confidence limits for (a) the first entry (1.80 ppmHg) and (b) the
mean value (1.67 ppmHg) assuming s →σ = 0.1.
CL for = x z
N
Q4. The analysis of a calcite sample yielded CaO percentage of 55.95, 56.00, 56.04,
56.08, and 56.23. The last value appears anomalous; should it be retained or rejected at
90% confidence level?
Qexp = xq − xn /w
where xq = questionable result
xn = nearest neighbour
w = spread of entire set Xq
55.95, 56.00, 56.04, 56.08, and 56.23
Xn
Qcrit (reject if Qexpt > Qcrit)
No. of observations 90% 95% 99% confidencelevel
3 0.941 0.970 0.994
4 0.765 0.829 0.926
5 0.642 0.710 0.821
6 0.560 0.625 0.740
7 0.507 0.568 0.680
8 0.468 0.526 0.634
9 0.437 0.493 0.598
10 0.412 0.466 0.568
Q4. The analysis of a calcite sample yielded CaO percentage of 55.95, 56.00, 56.04,
56.08, and 56.23. The last value appears anomalous; should it be retained or rejected at
90% confidence level?
Qexp = xq − xn /w
where xq = questionable result
xn = nearest neighbour
w = spread of entire set Xq
55.95, 56.00, 56.04, 56.08, and 56.23
Xn
Q1. A 0.3516 g sample of a commercial phosphate detergent was ignited at a red heat to
destroy the organic matter. The residue was then taken up in hot HCl, which converted the P to
H3PO4. The phosphate was precipitated as MgNH4PO4 • 6H2O by addition of Mg2+ followed by
aqueous NH3. After being filtered and washed, the precipitate was converted to Mg2P2O7
(222.57 g/mol) by ignition at 1000 °C. This residue weighed 0.2161 g. Calculate the percent P
(30.974 g/mol) in the sample.
Step 1:
No. of mol of Mg2P2O7 = Mass / Molecular weight of Mg2P2O7
= 0.2161 g / 222.57 g/mol
= 0.000971
Step 2:
The reaction reveals that 2 mol of P reacted with Mg2+ to give 1 mol of
Mg2P2O7
Therefore, no. of mol of P = 2 X no. of mol of Mg2P2O7
= 2 X 0.0009709 mol
= 0.00194
Step 3:
Mass of P = no of mol of P X Molecular weight of P
= 0.00194 mol X 30.974 g/mol
= 0.06015 g
Step 4:
% of P = 0.06015 / 0.3516 * 100% = 17.107 % = 17.1 %
Q2. What is the temperature programming as used in gas chromatography?
Temperature programming involves increasing the temperature of a gas-
chromatographic column as a function of time.
This technique is particularly useful for samples that contain constituents whose
boiling points differ significantly.
Low-boiling point constituents are separated initially at temperatures that
provide good resolution.
As the separation proceeds, the column temperature is increased so that the
higher boiling constituents come off the column with good resolution and at
reasonable lengths of time.
Q3. Define (a) stationary phase; (b) retention time; (c) selectivity
factor; (d) isocratic elution and (e) normal-phase packing.
(a) The stationary phase in a chromatography column is a solid or liquid that is fixed
in place. A mobile phase then passes over or through the stationary phase.
(b) The retention time for an analyte is the time interval between its injection onto
column and the appearance of its peak at the other end of the column.
(c) The selectivity factor of a column toward two species is given by the equation α =
tB/tA , where tB is the retention time of the more strongly held species B and tA is the
corresponding retention time for the less strongly held solute A.
(d) In an isocratic elution, the solvent composition is held constant through the
elution.
(e) In a normal-phase packing, the stationary phase is quite polar and the mobile
phase is relatively non-polar.
Q4. Please predict the order of elution of (i) n-hexane, (ii) n-hexanol,
and (iii) benzene in normal and reversed-phase separation.
For normal-phase separation,
n-hexane, benzene, n-hexanol
For reversed -phase separation,
n-hexanol, benzene, n-hexane