Analytical (Pratical) Lec.1

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Volumetric Analysis (Titration)

Volumetric analysis: It is based on accurate measurements offinal volume of a


standard reagent solution of known concentration needed to react with the analyte
in a known volume of sample.

Titration: is a process in which a standard reagent (known conc.) is added to a


solution of an analyte until the reaction between the analyte and standard reagent
is attained equivalence point.

Equivalence point: Is the point in a titration when the amount of added standard
reagent is exactly equivalent to the amount of analyte.

equivalent point: The point in a titration where stoichiometrically equivalent


amounts of analyte andtitrant react (theoritical end of titration).
(no. of eq.wt titrant) = (no. of eq.wt. titrand)
(N = no.of eq.wt / V)
(N × V) Standard = (N × V)Analyte
End point: Is the point in a titration when a physical change occurs that is
associated with the condition of chemical equivalence.

Titrant: The standard solution of known concentration added from the burette.
Analyte: An unknown solution which is to be determined
Indicators: A colored compound reagent added to the analyte solution to produce

an observable physical change (usually change in color) at or near the equivalence

point when the titration reaction is complete, and so mark the endpoint e.g:

Phenolphthalein, Methyl Orange, Methyl red, etc

Color in acidic Color in basic


Indicator
medium medium pH range
Thymol blue Red Yellow 1.2 – 3.0
Methyl orange Red Yellow 3.1 – 4.4
Methyl red Red Yellow 4.2 – 6.2

Phenolphthalein Colorless Pink 8.3 – 10


Primary standard: Is a pure compound from which a standard solution of
accurately known concentration can be prepared directly, without any need for
standardization.
Requirements For The Primary Standard Material
1. High purity.
2. High stability.
3. It has a large molecular weight to minimize the relativeerror during
weighing the substance.
4. It must be not hygroscopic.
5. Low cost.
6. The substance must not be poison.
7. Soluble in a solvent (especially water).
Secondary standard: Is a solution that its concentration is not accurately known so
it is to be standardized by “Primary Standard” before use in titration.
Standard solution:Is a reagent of exactly known concentration that is used in a
titrimetric analysis, and it's prepared either from primary standard material or its
concentration determined by standardization with primary standard material
Standardization:The process of finding the actual concentration of the secondary
standard solution by titrating it with a suitable primary standard solution.

For use in titrimetric analysis, a reaction must fulfill the following conditions:
1. There must be a simple reaction that a chemical equation can express. The
substance to be determined should react completely with the reagent.
2. The reaction should be relatively fast. (Most ionic reactions satisfy this
condition).
3. There must be an alteration in the solution's physical or chemical property at
an equivalence point.
4. An indicator should be available which, by a change in physical properties
(color or formation of a precipitate), should sharply define the end point of the
reaction.
Types of titration according to the chemical reaction
1. Neutralization titration (Acid-base titration).
NaOH + HCl NaCl + H2O
2. Precipitation titration.
AgNO3 + NaCl AgCl + NaNO3
3. Reduction-oxidation titration (Redox titration).
5Fe2+ + Mn7+ + 8H+ 5Fe3+ + Mn2+ + 4H2O
4. Complexation titration.
Hg2+ + 4I- HgI42-
Neutralization titration (Acid-base titration)
These include the titration of free bases with a standardacid, and the titration of free
acids with a standard base. These reactions involve the combination of hydrogen
and hydroxide ions to form water.
Example:

NaOH+HCl NaCl+H2O

Na2CO3+2HCl 2NaCl+ CO2+H2O


VOLUMETRIC (Titration) CALCULATIONS

𝐰𝐞𝐢𝐠𝐡𝐭 (𝐠)
𝐍𝐨. 𝐨𝐟 𝐦𝐨𝐥𝐞𝐬 𝐀 = 𝐠
𝐟𝐨𝐫𝐦𝐮𝐥𝐚 𝐰𝐞𝐢𝐠𝐡𝐭 ( )
𝐦𝐨𝐥𝐞
No. of moles A = volume(L) x Molarity of A (mol / L )

No. of mmoles A = volume(mL) x Molarity of A (mmol /mL )

Example 1:

Calculate the concentration of 100.0 mL of NaOH solution titrated to


the end point with 75.8 mL of a 0.100 M standard solution of HCl.

HCl(aq) + NaOH(aq) → NaCl(aq) + H2O(l)

na = 1 nb = 1 ( stiochiometric mole ratios of acid and base)

No of moles = Molarity (M) x volume(L)

No of mmoles = Molarity (M) x volume(mL)

Ma Va Mb Vb
** =
na nb

75.8 𝗑 0.10 𝐶𝑏 𝗑 100


=
1 1

75.8 𝗑 0.10
Mb = = 0.0758 M
100

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