SOAL-SOAL LATIHAN

Notes : learn about the external standard method, standard addition method
and internal standard method for detemination of a concentration of an analyte
in samples. After you learn about that please do this excercise and collected the
answer on April 14th. For number 1-3 you can choose just one question whatever
you like to answer. For number 4-5, please answer all question. I will explain
about this when we have class.

1. A compound X is to be determined by UV/visible spectrophotometry. A

calibration curve is constructed from standards solution of X with the
following results : 0.50ppm, A=0.24; 1.5ppm, A=0.36; 2.5ppm, A=0.44;
3.5ppm A=0.59; 4.5ppm, A=0.70. find the slope and intercept of the
calibration curve, the standard error in y, the concentration of the solution of
unknown X concentration and the standard deviation in the concentration of
X. Construct a plot of the calibration curve and determine the unknown
concentration by hand from the plot.
2. Nitrite is commonly determined by a colorimetric procedure using a reaction
called the Griess reaction. In this reaction, the sample containing nitrite is
reacted with sulfanilimide and N-(1-Naphtyl) ethylendiamine to form a colored
species that absorbs at 550 nm. By using an automated flow analysis
instrument, the following results were obtained for standars solution of nitrite
and for a sample containing an unknown amount :
solution

Absorbance
550 nm

2 M

0.065

6 M

0.205

10 M

0.338

14 M

0.474

18 M

0.598

unknown

0.402

at

Determine the concentration of unknown, find the slope and intercept of the
calibration curve
3. EDTA forms colored complexes that may serve as the basis for the
quantitative spectrophotometric method of analysis. The molar absorptivites
of the EDTA complexes of Cu 2+, Co 2+, Ni 2+ at threee different wavelength are
summarized in the following table (all values of are in M-1 cm-1)
Metal

462,9

732.0

378.7

Co2+

15.8

2.11

3.11

Cu2+

2.32

95.2

7.73

Ni2+

1.79

3.03

13.5

Using this information, determine (a) the concentration of Cu2+ in a solution

that has an absorbance of 0.338 at a wavelength 732.0 nm
b) the concentration of Cu2+ and Co2+ in a solution that has an absorbance
of 0.445 at a wavelength 732.0 and 0.107 at a wavelength of 462.9 nm. The
pathlength b for all measurement is 1.00 nm
4. Quigley and vernon report results for the determination of trace metals in sea
water using a graphite furnace atomic absorption spectrophotometer.
Calibration was achieved by the method of standard additions. The trace
metals were first separated from their complex, high salt matrix by
coprecipitating with Fe 3+. In a typical analysis a 5 mL portion of 2000 ppm Fe
3+
was added to 1L of sea water. The pH was adjusted to 9 using NH 4OH and
the precipitated of Fe(OH)3 allowed to stand overnight. After isolating and
rinsing the precipated, the Fe(OH) 3 and coprecipated metals were dissolved in
2 mL concentrated HNO3 and diluted to volume in a 50 mL volumetric flask. To
analyze for Mn 2+, a 1mL samples of this solution was diluted to 100mL in a
volumetric flask. The folowing samples were injected into the graphite
furnace and analyzed
Absorban
ce
2.5 L sample + 2.5L of 0 ppb Mn2+ standard

0.223

2.5 L sample + 2.5L of 2.5 ppb Mn2+

standard

0.294

2.5 L sample + 2.5L of 5 ppb Mn2+ standard

0.361

Report the part per billion of Mn2+ in the sample of sea water
5. Glodenins describes the use of ICP to analyze samples containing Pb and NI in
brass. The analysis for Pb uses external standard prepare from brass samples
containing known amounts of lead. The analysis for Ni uses an internal
standard. Results for a typical calibration are shown in the following table
% w/w Ni

Ratio of emmision intensity

0.000

0.00267

0.0140

0.00154

0.0330

0.00312

0.130

0.120

0.280

0.246

0.280

0.247

0.560

0.533

1.30

1.20

4.82

4.44

What is the % w/w Ni in a sample for which the ratio of emmision intensity is
1.10 x 10-3