Pharmaceutical Analysis - Unit 1: 1. Oxalic Acid (COOH) 2

Pharmaceutical Analysis .
Unit 1
PREPARATION AND STANDARDIZATION OF VARIOUS MOLAR SOLUTIONS.

1. Oxalic acid (COOH)2
Oxalic acid is available in pure state and its standard solutions can, therefore, be prepared by the
direct method.
Eq. wt. of hydrated oxalic acid (C2H2O4.2H2O), being 63 its 0.1N solution would contain 6.3
gm/litre, and 0.05 N solution would contain 3.15 gm/litre.
These standard solutions are employed to find the strength of solutions of alkalies (NaOH and
KOH) whose standard solutions cannot be prepared by the direct method.
PRINCIPLE – REDOX TITRATION

KMnO4, potassium permanganate is a strong oxidizing agent. Oxalic acid is oxidized by
potassium permanganate in acidic solution to produce CO2 and H2O
2KMnO4 + 3 H2SO4 + 5 (COOH)2 2MnSO4 + K2SO4 +10 CO2 + 8H2O
HCl cannot be used in place of sulphuric acid as it readily get oxidized to chlorine in presence of
KMnO4
Preparation Of 0.1N Oxalic Acid Solution

Weigh accurately 6.3 gm of oxalic acid & dissolve in distilled water & finally make up the
volume to one liter in a volumetric flask.
Standardization Of 0.1 N Oxalic Acid

- Clean and dry al the glasswares as per standard laboratory procedure.
- Take 20 ml of prepared oxalic acid in a conical flask
- Add 5 ml of sulphuric acid , and warm at 70 0C
- Rinse the burrete with distilled water and pre rinse with the portion of potassium
permanganate soln.
- Start the titration with 0.1N KMnO4 until the end point. 1
- End point is the appearance of pink colour that persists for more than 30 seconds.
- Record the reading repeat the titration 3 times to get th precise values.
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Pharmaceutical Analysis . Unit 1
Calculation
Normality of Oxalic Acid = Weight Taken x Expected Normality
Equivalent Weight Factor x Titre Value
Sl Content in conical Burette reading Indicator/color Volume used.

no flask Initial Final change
1. 20ml oxalic acid + KMnO4/persistence

5ml Sulphuric acid of pink colour.
2.
2. SODIUM HYDROXIDE
Sodium hydroxide is hygroscopic and absorbs water from the air when you place it on the
balance for massing. This water will prevent you from being able to find the exact mass of
sodium hydroxide.
In order to determine the exact concentration of a sodium hydroxide solution you must
standardize it by titrating with a solid acid that is not hygroscopic.
Potassium hydrogen phthalate, KHC8H4O4 (abbreviated KHP/PHP), is a non-
hygroscopic, crystalline, solid that behaves as a monoprotic acid.
It is water soluble and available in high purity. Because of its high purity, you can
determine the number of moles of KHP directly from its mass and it is referred to as a
primary standard. You will use this primary standard to determine the concentration of a
sodium hydroxide solution
-
PRINCIPLE – ACID BASE TITRATION
An acid-base titration is a procedure used to compare the amount (moles) of acid in one
sample with the amount (moles) of base in another. In this laboratory exercise you will
carry out such a titration to standardize (determine the exact concentration of) a NaOH
solution by measuring accurately how many milliliters of it are required to exactly
2
neutralize a known amount of acid. A burette filled with the titrant (NaOH solution) is
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used to measure the volume of NaOH solution added to the known amount of acid in a
flask. An indicator is added to signal the endpoint has been reached
Procedure
1. Preparation of 0.1 M NaOH
- Weigh about 402 g of sodium hydroxide in a 1000ml volumetric flask. Add water mix the
solution well and make up to 1000ml with distilled water
2. Standardization of 0.1M Sodium hydroxide
- Weigh accurately about 0.500g of Pottasium hydrogen phthalate, previously powdered
and dried at 120 0C for 2 hrs and dissolve in 75ml of CO2 free water in a conical flask.
- Add 0.1ml phenolphthalein solution
- Fill the burette with prepared 0.1M NaOH
- Titrate the PHP with 0.1M NaOH until thr colour change of a permanent pink colour.
- Repeat the titration for 3 times to get the precise reading
- Equivalent weight factor of PHP for 0.1 M NaOH = 0.020422 g
Calculation
Normality of Sdoium hydroxide = Weight Taken x Expected Normality
3. HYDROCHLORIC ACID
Principle- A known concentration or strength of sodium carbonate is titrated directly with HCl.
End point can be detected by using methyl orange or methyl red indicator. Reaction involves,
Na2CO3 + 2 HCl 2 NaCl + H2O + CO2 3

(Sodium carbonate)
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Preparation of 0.1 M HCl
Pipette out 8.5 ml of HCl and dilute upto 1000 ml with distilled water.
Standardization of 0.1 M HCl.
- Clean and dry al the glasswares as per standard laboratory procedure.

- Rinse the burette with distilled water and again rinse the same with a portion of 0.1M
Hcl. This is necessary to ensure that all of the solution in the burette is of desired solution
not of diluted or contaminated solution.
- Weigh accurately 0.150 g of sodium carbonate heated previously for 1 hr, t 270 0C and
transfer it into a conical flask.
- Add 20 ml of distilled water and shake well or sonicate for 5 min.
- Add 2 drops of methyl orange indicator
- Titrate with 0.1 m HCl by adding small quantities of HCl soln from burrette.
- End point is the appearance of pink colour that persists for 30 seconds.
- Repeat the titration for 3 times to get the precise reading
- Equivalent weight factor of sodium carbonate for 0.1 M HCl= 0.00529 g
Calculation
Normality of 0.1 N HCl = Weight Taken x Expected Normality
4, SODIUM THIOSULPHATE
Sodium thiosulfate is an inorganic sodium salt composed of sodium and thiosulfate ions in a 2:1
ratio. It has a role as an antidote to cyanide poisoning, a nephroprotective agent and an
antifungal drug.
- Synonyms: SODIUM THIOSULFATE
- Molecular Formula: Na2O3S2 or Na2S2O3
It is typically found in its pentahydrate form which is either white in colour, or colourless
altogether. This pentahydrate of sodium thiosulfate is described by the following chemical
formula: Na2S2O3.5H2O.
In its solid form, it is a crystalline solid which has a tendency to readily lose water.
4
Sodium thiosulfate is readily soluble in water and is also referred to as sodium hyposulfite.
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PRINCIPLE
-Redox Titration (IODOMETRY)
The principle of standardization of sodium thiosulphate is based on redox iodometric titration
with potassium iodate (primary standard).
Potassium iodate is a strong oxidizing agent, it is treated with excess potassium iodide in
acidic media which liberates iodine which is back titrated with sodium thioslphate.
Uniformity of reactions between iodine and sodium thiosulphate forms basis for utilizing the
standard solution of iodine in the analysis of sodium thiosulphate.
. KIO3+ 5KI + 3H2SO4→ 3K2SO4+3I2+3H2O
I2 3I2+2Na2S2O3→ 2NaI + Na2S4O6
PROCEDURE:
Preparation of 0.1N Sodium thiosulphate
- Dissolve 24.8g of sodium thiosulphate pentahydrate(Na2S2O3.5H2O) in 800 ml of
freshly boiled and cooled water and mix thoroughly by shaking for approximately 15
minutes.
- Make up the volume to 1000 ml.
Preparation of 0.1N Potassium Iodate
- Weigh accurately about 356 mg of KIO3 and dissolve in 100 ml distilled water.
Preparation of Starch indicator
- Take 1 gm of soluble starch and triturate with 5 ml of water and add it to 100 ml of
Boiling water containing 10 mg of Mercuric iodide with continous stirring.
Standardization of 0.1N sodium thiosulphate
- Take 10 ml of Potassium Iodate solution .
- Add 2 gm of Potassium Iodide and 5 ml of dilute H2SO4,keep it in dark for 10
minutes.
- add 2 to 3 drops of starch indicator and titrate with sodium thiosulphte using starch
solution as indicator until the blue colour is disappeared. 5
- Record the reading , Repeat the titration for 3 times to get the precise reading
- Equivalent weight factor of sodium carbonate for 0.1 M HCl= 0.00529 g
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Calculation
Normality of 0.1 N sodium thio sulphate = Weight Taken x Expected Normality
-
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Pharmaceutical Analysis .

PREPARATION AND STANDARDIZATION OF VARIOUS MOLAR SOLUTIONS.

PRINCIPLE – REDOX TITRATION

Preparation Of 0.1N Oxalic Acid Solution

Standardization Of 0.1 N Oxalic Acid

Sl Content in conical Burette reading Indicator/color Volume used.

1. 20ml oxalic acid + KMnO4/persistence

Na2CO3 + 2 HCl 2 NaCl + H2O + CO2 3

Preparation of 0.1 M HCl

Standardization of 0.1 M HCl.

- Clean and dry al the glasswares as per standard laboratory procedure.

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