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Chemical Analysis
Exam 1
3 __4____ (of 4)
5 __6____ (of 6)
KEY
Name:___________________________________________
(please print)
1. Quinine may be determined by measuring the fluorescence intensity in 1 M
H2SO4 solution. Standard solutions of quinine gave the following
fluorescence values.
concentration of quinine x (g mL-1) 0.00 0.10 0.20 0.30 0.40
Fluorescence intensity y (arb. units) 0.00 5.20 9.90 15.30 19.10
a. Calculate by the least squares method the equation of the best straight line for
the calibration curve. Report you result in the form y = [m(sm)]x + [b(sb)].
(15 points)
xi yi xi2 yi2 xiyi
0.00 0.00 0.00 0.00 0.00
0.10 5.20 0.01 27.04 0.52
0.20 9.90 0.04 98.01 1.98
0.30 15.30 0.09 234.09 4.59
0.40 19.10 0.16 364.81 7.64
2 2
xi = 1.00 yi = 49.5 xi = 0.30 yi = 723.95 xiyi = 14.73
xi = 0.20, i = 9.9
Sxx = xi2 (xi)2/N = 0.30 1/5 = 0.1
Syy = yi2 (yi)2/N = 723.95 2450.25/5 = 233.9
Sxy = xiyi (xi)(yi)/N = 14.73 (1)(49.5)/5 = 4.83
m = Sxy/Sxx = 48.3
b = y mx = 9.9 (48.3)(0.20) = 0.24
Syy - m2Sxx 2
233.9 - (48.3) (0.1)
sr = = = 0.4512944
N-2 5-2
sr2 (0.4512944)
2
sm = = = 1.4271183
Sxx 0.1
xi2 0.30
sb = sr = 0.4512994 = 0.3495677309
Nxi2 - (xi) 2 (5)(0.30) - 1
The initial amount of HCl in the receiver was (10.00 mL) x (0.02140 mmol/mL) =
0.214 mmol. The NaOH required for titration of unreacted HCl in the above
reaction was (3.26 mL)(0.0198 mmol/mL) = 0.0645 mmol. The difference ,
0.214 0.0645 = 0.1495 mmol, must be equal to the quantity of NH3 produced in
produced and distilled into the HCl.
Because 1 mol of nitrogen in the protein produces 1 mol of NH3, there must have
been 0.1495 mmol of nitrogen in the protein, corresponding to:
Mean x = 7.13%
H
OH O O
N N N
Ni2+ + 2 Ni + 2H+
N N N
OH O O
H
FM 58.69 DMG Bis(dimethylglyoximate)nickel(II)
FM 116.12 FM 288.91
If the nickel content is known to be near 3 wt % and you wish to analyze 1.0 g
of the steel, what volume of 1.0 wt% alcoholic DMG solution should be used
to give a 50% excess of DMG for the analysis? Assume that the density of
the alcohol solution is 0.79 g/mL. (10 points)
Because the Ni content is around 3%, 1.0 g of steel will contain about 0.03 g of
Ni, which corresponds to:
because 1 mol of Ni2+ requires 2 mol of DMG. A 50% excess of DMG would be
(1.5)(0.119 g) = 0.178 g. This much DMG is contained in
a. Is the standard deviation for procedure B significantly different from that of the
conventional procedure? (Ftable = 5.05) (3 points)
Fcalculated = 4.62/3.62 = 1.63 < Ftable = 5.05. Standard deviations are not
significantly different at the 95% confidence level.
s12(n1 - 1) + s22(n2 - 1)
spooled =
n1 + n2 - 2
4.62(6 - 1) + 3.62(6 - 1)
= = 4.13
6+6-2
x1 - x2 n1n2
tcalculated = spooled n1 + n2