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POLYTHECNIC INSTITUTE OF VISEU

SCHOOL OF TECHNOLOGY

Environmental department

Course:

Evaluation:
Period:
Academic
year:

Environmental
Engineering

Unit:

Exam

Teacher:

Normal

Year:

2010/2011

Date:

Methods in Chemical Analysis

Artur Figueirinha
3
5

Semester:

November

2012

1. A 101.3 mg sample of an organic compound known to contain Cl is burned in pure


O2 and the combustion gases collected in absorbent tubes. The tube used to trap CO2
increases in mass by 167.6 mg, and the tube for trapping H2O shows a 13.7 mg
increase. A second sample of 121.8 mg is treated with concentrated HNO3 producing
Cl2, which subsequently reacts with Ag+, forming 262.7 mg of AgCl. Determine the
percentage of Carbon, Hydrogen and Chorine in the sample.
(45,15% C; 1,51% H; 53,35% Cl)
2. The alkalinity of natural waters is usually controlled by OH, CO32, and HCO3,
which may be present singularly or in combination. Titrating a 100.0 mL sample to a
pH of 8.3 requires 21.36 mL of a 0.02812 M solution of HCl. A second 100.0-mL
aliquot requires 25.69 mL of the same titrant to reach a pH of 4.5. Identify the
sources of alkalinity and their concentrations in mg/L of Na2CO3, NaOH or
NaHCO3. (129,05 mg Na2CO3/L; 191,54 mg NaOH/L)
3. A sample of commercial vinegar was analyzed by acid-base volumetric method using
two different methods for assessing the equivalence point. For this purpose was used
a standard solution of sodium hydroxide 0.098 N. Three replicates were performed
for each method and the results are shown in the following table. The reaction
between the acetic acid of the vinegar and sodium hydroxide is as follows:

CH 3COOH + NaOH NaCH 3 COO + H 2 O

Chemical indicator method


(Methyl orange)

Potentiometric method
(Grans plot)

Sample (g)

End point (mL)

Sample (g)

Grans equation

28,1875

7,30

28,5781

Y = 3,875x106X +
4,324x107

28,2010

7,35

26,0120

Y = 4,175x106X +
4,324x107

27,9899

7,23

28,5090

Y = 3,975x106X +
4,195x107

a) Briefly explain how you would obtain the data for tracing the Grans plot.

b) Using the formula below, calculate the concentration in % acidity


acid obtained by
each method. (indicator method: 0,153%; potentiometric method: 0,227 %).
%)

%acidity =

acetic acid ( g )
x100
sample mass ( g )

c) Determine whether there are significant differences between the results


obtained for the two samples, at a confidence level of 95%. (0,077>0,01453;
there are differences).
differences)

4. The following
owing chart resulted in a condutimetric titration of chloride present in
50.00 ml of a water sample with a standard solution of silver nitrate 0.001986 M. Based
on the data obtained, calculate the concentration of chlorides in the water sample
expressing the result in mg NaCl / liter. (2,9 mg NaCl / liter).

5. The following figure shows two spectrophotometric titration curves at 746 nm of


30.00 mL EDTA 15 mM in acetate buffer with a solution of copper sulfate in the same
buffer.

a)

ain the shape of the two titration curves


Explain

b)
c)

Calculate the molar concentration of CuSO4. (0,015 M)


Plot the titration curve obtained using EDTA as titrant and copper
sulfate as sample.
sample
FORMULAS

X Xt

x1 x2 t S acum

tS
N

N1 + N 2
N1 N 2

MA(H) = 1.00794
MA(Ag) = 107.868
MA(Cl) = 35.4527
MA (O) = 15.9994
MA(N) = 14.00674
MA (C) = 12.0107
MA(Cd) = 112.41
MA (S) = 32.066
MA (Ca) = 40.078
MA(Na) = 22.990

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