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Gravimetric Method of Analysis – deals with the measurement of the Ex. A 0.6407-g sample containing chloride and iodide ions gave a silver
mass of a substance that is chemically related to the analyte. halide precipitate weighing 0.4430 g. This precipitate was then strongly
heated in a stream of Cl2 gas to convert the AgI to AgCl; on completion
Basic Steps on Precipitation Method of this treatment, the precipitate weighed 0.3181 g. Calculate the
1. Sample is dissolved in an appropriate solvent. percentage of chloride and iodide in the sample. Ans. 4.72% Cl- and
2. A precipitant is used to convert the analyte into a sparingly 27.05%% I-.
soluble precipitate.
3. The precipitate is converted into a product of known Volumetric Methods of Analysis – measures the volume of solution
composition by a suitable heat treatment. necessary to react completely with the analyte
4. The percentage of the analyte in the sample is calculated using
the gravimetric factor (GF): Standard Solution – solution of known concentration
Standardization – process of determining the concentration of an
wt . of precipitate × GF unknown solution
%analyte ∈the sample= ×100 % Primary standard – a substance of high purity
wt . of sample
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a. 12.04% b. 7.69% c. 15.59% d. 10.93% Precipitation. In the case of precipitation, the titrant forms an insoluble
product with the analyte. An example is the titration of chloride ion
Ex. A 5.8734-gram sample beef was analyzed for its N content and the with silver nitrate solution to form silver chloride precipitate. Again,
liberated NH3 was collected in a 50.00 mL of 0.4691 M HCl and a 12.55 indicators can be used to detect the end point, or potential of the
mL back titration with 0.0256 M NaOH was required. Calculate the solution can be monitored electrically.
percentage protein in the beef sample.
a. 17.32% b. 5.54% c. 34.64% d. 11.08% One of the oldest analytical techniques that started in the mid-
1800’s. Silver nitrate (AgNO3) is commonly employed in such technique.
Ex. A 2060 mg sample of flour was taken through a Kjeldahl procedure Titration with AgNO3 is often termed as argentometric titration.
and the ammonium produced was distilled into 100 mL of 0.1006 M
H3BO3 solution. If this solution required 34.7 mL of 0.174 M HCl for Indicators in Precipitimetry
The equivalence point can be observed by the following:
titration to methyl red end point, what is the percentage of protein in
flour? Use 5.70 for flour. Ans. 23.89%
a. Formation of a colored secondary precipitate
2. Double Indicator Method (Mixture of Bases)
Mohr Method (K.F. Mohr, Germany, 1865)
Direct Method for halides and cyanides
Ex. A sample that may contain NaOH, Na2CO3, NaHCO3, and inert
Titrant: Silver Nitrate, AgNO3
matter alone or in compatible combination is titrated with 0.1000 N HCl Titration Reaction: Ag+ + Cl- → AgCl(s) white
with phenolphthalein as the indicator and the solution became Indicator: sodium chromate, Na2CrO4
colorless after the addition of 48.8 mL. Methyl orange is then added Indicator Reaction: 2Ag+ + CrO42- → Ag2CrO4(s) red
and 14.55 mL more of the acid are needed for the color change. If the Primary Standard for AgNO3: NaCl
sample weighs 2.345 grams, it contains
a. 5.842% NaHCO3 and 6.577% Na2CO3 Titration is carried out between pH of 7-10. Usually, a low
b. 6.577% Na2CO3 and 5.842% NaOH concentration of chromate is desired to detect the endpoint clearly
c. 65.77% Na2CO3 and 5.842% NaHCO3 since a chromate ion imparts an intense yellow color.
d. 65.77% Na2CO3 and 5.842% NaOH
Ex. What is the molar concentration of AgNO 3 solution standardized
Ex. A sample consisting of Na2CO3, NaHCO3 and inert matter weighs against 712 mg primary standard NaCl (58.45 g/mol) requiring 23.8 mL
1.179 grams. It is titrated with 0.100 N HCl with phenolphthalein as the of the solution for titration?
indicator, and the solution became colorless after the addition of 24.00 a.0.5027 M b. 0.5118 M c. 0.5263 M d. 0.5329 M
mL. Another duplicate sample was titrated with HCl using methyl
orange as indicator. It required 50.25 mL of the acid for the color Ex. A 1.500-gram sample of impure AlCl3 was dissolved in water and
change. What is the percentage of NaHCO3 in the sample? treated with 45.32 mL of 0.1000 M AgNO3 using Mohr method.
a. 1.60% b. 5.17% c. 12.56% d. 21.58% Determine its purity as %AlCl3 (133.33)
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Ex. A 1.509-g sample of a Pb/Cd alloy was dissolved in acid and diluted Reduction-Oxidation. These “redox” titrations involve the titration of
to exactly 250.0 mL in a volumetric flask. A 50.00-mL aliquot of the an oxidizing agent with a reducing agent, or vice versa. An oxidizing
diluted solution was brought to a pH of 10.0 with an NH 4+/NH3 buffer; agent gains electrons and a reducing agent loses electrons in a reaction
the subsequent titration involved both cations and required 28.89 mL between them. There must be a sufficiently large difference between
of 0.06950 M EDTA. A second 50.00 mL aliquot was brought to a pH of the oxidizing and reducing capabilities of these agents for the reaction
10.0 with an HCN/NaCN buffer, which also served to mask the Cd 2+; to go to completion and give a sharp end point; that is, one should be a
11.56 mL of the EDTA solution were needed to titrate the Pb 2. Calculate fairly strong oxidizing agent (strong tendency to gain electrons) and the
the percent Pb and Cd in the sample. Ans. 55.16% Pb and 44.86% Cd other a fairly strong reducing agent (strong tendency to lose electrons).
You can use appropriate indicators for these titrations, or you may
a. Determination of Cyanide by the Liebig Method employ various electrometric means to detect the end point.
The titration is carried by the drop wise addition of AgNO 3 in a
solution of a cyanide forming a soluble cyanide complex of silver: 2CN - Combining Ratio, also (f)
+ Ag+ → Ag(CN)2-1. The endpoint of the titration is the formation of a OXIDANT
permanent faint turbidity: Ag(CN)2-1 + Ag+→Ag[Ag(CN2)](s) KMnO4 (a) 5
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KMnO4 (b,n) 3 Ex. A 0.200-g sample of pyrolusite is analyzed for manganese content
K2Cr2O7 6 as follows. Add 50.0 mL of a 0.100 M solution of ferrous ammonium
I2 2 sulfate to reduce the MnO2 to Mn+2. After reduction is complete, the
MnO2 2 excess ferrous ion is titrated in acid solution with 0.0200 M KMnO 4,
requiring 15.0 mL. Calculate the percent manganese in the sample as
REDUCTANT Mn3O4 (only part or none of the manganese may exist in this form, but
Na2C2O4 (C2O4-2) 2 we can make the calculations on the assumption that it does). Ans.
FeSO4 (Fe+2) 1 66.74%
Na2S2O3 1
KI 1 Ex. A hydrogen peroxide solution is analyzed by adding a slight excess
Fe metal 2 of standard KMnO4 solution and back-titrating the unreacted KMnO 4
with standard Fe+2 solution. A 0.587-g sample of the H2O2 solution is
As2O3 4
taken, 25.0 mL of 0.0215 M KMnO 4 is added, and the back-titration
H2O2 2
requires 5.10 mL of 0.112 M Fe2+ solution. What is the percent H2O2 in
Cu+ 1
the sample? Ans. 6.13%
Ex. What is the molarity of a KMnO 4 solution standardized against
Ex. A sample of a pyrolusite weighs 0.5000 g. To this is added 0.6674 g
1.356 gram Na2C2O4 (134 g/mol) requiring 25.1 mL of the solution in
of As2O3 and dilute acid. After solvent action has ceased, the excess
acidic medium MnO2. Ans. 78.19%?
three-valent arsenic is titrated with 45.00 mL of 0.1000 N KMnO 4.
a)0.161 M b. 0.403 M c. 1.008 M d. 0.856 M
Calculate the oxidizing power of the pyrolusite in terms of percentage
Ex. The percentage of MnO2 in a 500 mg sample which after the
addition of 80.00 mL of 0.1056 M FeSO4 solution required 8.50 mL of
0.0867 M K2Cr2O7 is
a)33.52% b. 35.00% c. 17.50% d. 67.04%
Ex. A 240-mg sample of pyrolusite was treated with excess KI. The
iodine liberated required 46.24 mL of 0.1105 M Na 2S2O3 solution.
Calculate the % MnO2 in the sample.
a)46.27% b. 30.85% c. 92.54% d. 76.12%
Ex. A sample of iron ore weighing 385.6 mg was dissolved in acid and
passed through a Jones redactor. If the resulting solution required
52.36 mL of 0.01436 M K2Cr2O7 for titration, calculate % Fe3O4 (231.55
g/mol) in the ore sample.
a)15.05% b. 45.15% c. 90.30% d. 67.98%
By: JACY/200510286