Thursday, August 26, 2021

Assay of hydrogen peroxide

Learn about the assay of hydrogen peroxide solution (H2O2) through a laboratory experiment or practical.

Aim:

To perform the assay of hydrogen peroxides using standard 0.1 N KMnO4 solution by permanganometry (20 Vol).


Requirements:

Glasswares: Burette, burette stand, conical flask, volumetric pipette, beaker, volumetric flask, funnel, glass rod, and wash bottle, etc.
Chemicals: LR grade potassium permanganate (KMNO4), hydrogen peroxide (H2O2), and sulphuric acid (H2SO4), etc.
Apparatus: Digital/analytical balance, and Ultrasonicator.

Principle of hydrogen peroxide assay:

As an oxidizing agent, hydrogen peroxide is used. The assay of hydrogen peroxide solution is based upon the oxidation-reduction (permanganometry) titration. It gets oxidized to water and oxygen when titrated with a strong oxidizing agent in an acidified solution. The presence of hydrogen peroxide in an H2SO4-acidified solution is used to titrate the strength of KMnO4. Potassium permanganate works as a self-indicator and may be used to determine the endpoint by the appearance of permanent pink color.
The following is the reaction that is involved in this titration.
Assay of hydrogen peroxide

Preparation and standardization of 0.1 N KMn04:

Click here to get the procedure of preparation and standardization of potassium permanganate solution (0.1 N).

Preparation of 5N sulphuric acid solution:

Take 13.58 ml of sulfuric acid (H2SO4) using a pipette, dilute in 100 ml of distilled water in a volumetric flask, and properly mixing it.

Titration procedure:

  • All glassware should be cleaned and dried according to standard laboratory procedures.
  • Before filling the burette for the titration, rinse it with distilled water and then pre-rinse it with a portion of the titrant solution. Pre-rinsing is required to make sure that all solution in the burette is the desired solution, not a contaminated or diluted solution.
  • Take the unknown stock solution of titrant in a clean and dry beaker then fill the burette using the funnel.
  • Remove air bubbles from the burette and adjust the reading to zero.
  • Take 10.00 ml of hydrogen peroxide using a pipette, dilute in 250 ml of distilled water in a volumetric flask, and properly mixing it.
  • Take 25.00 ml of prepared dilution, pour into a conical flask and add 05.00 ml of sulphuric acid solution (5 N).
  • Titrate the sample solution with potassium permanganate solution until the endpoint is reached.
  • When the solution is swirled for up to 10 seconds, a pink color appears and fades, indicates that the endpoint is approaching. The actual endpoint of the titration is indicated by a pink color that lasts longer than 30 seconds.
  • To get accurate results, repeat the titration three times.
  • Properly record the readings of the burette.
  • Take their mean and calculate the normality of hydrogen peroxide.

Observation table:-

Sr. No.

Content in conical flask

Burette reading

Volume of titrant used (ml)

Initial

Final

1

 

 

 

 

2

 

 

 

3

 

 

 

 

Mean:


Calculations:


g/100 ml of H2O2 = V x E x N x 100 / 10

Where,
V is the volume of KMn04 used
E is an equivalent factor
N is the normality of KMnO4
For 1 ml of 0.1 N KMnO4, the equivalent factor of H2O2 is 0.0001701.

Result:

The given sample of hydrogen peroxide solution contains ___g/100 ml of H2O2.


Commonly asked quetions of the assay of of H2O2 are as follows.

Which indicator is used in the assay of hydrogen peroxide?
Potassium permanganate is a self-indicator, hence there is no indication is required in the hydrogen peroxide assay by permanganometry.

What is hydrogen peroxide used for in chemistry?
Hydrogen peroxide is mainly used in chemistry as an oxidizer, antiseptic, and bleaching agent.
 
How do you test hydrogen peroxide?
Titration, light detection, and chromatography are among the several methods for testing hydrogen peroxide.


Wednesday, August 25, 2021

Assay of calcium gluconate

Learn about the assay of calcium gluconate through a laboratory experiment or practical.

This experiment is performed in two parts i.e.
A: Preparation and standardization of 0.05 M EDTA solution.
B: Assay of calcium gluconate

Aim:

To perform the assay of calcium gluconate using standard 0.1 N EDTA (Replacement titration).

Requirements:

Glasswares: Burette, burette stand, conical flask, volumetric pipette, beaker, volumetric flask, funnel, glass rod, and wash bottle, etc.
Chemicals: LR grade calcium gluconate (C12H22CaO14), disodium edetate (EDTA), ammonia (NH3), calcium chloride (CaCl2), ammonium chloride (NH4Cl), magnesium sulphate ( MgSO4), hydrochloric acid (HCL), and solochrome black-T indicator or mordant black II, etc.
Apparatus: Digital/analytical balance, and Ultrasonicator.

Principle of assay of calcium gluconate:

The assay of calcium gluconate is based upon a replacement complexometric titration. Magnesium forms a complex with the mixture of indicator mordant black II which indicates the first color.

The magnesium-indicator complex is more stable compared to the calcium-indicator complex; hence calcium does not affect the magnesium-indicator complex. When titrated against disodium edetate, calcium and EDTA formed.

When all of the calcium has been consumed, the drop of EDTA breaks the magnesium-indicator complex, allowing the free indicator to form a complex with the magnesium. The endpoint is determined by detecting the second color at that time.

The following is the reaction that is involved in this titration.

Assay of calcium gluconate

Preparation of 0.05 M magnesium sulphate:

Take 600 mg of anhydrous MgSO4 and dissolve in 50 ml of distilled water in a volumetric flask, and properly mixing it. Once it has completely dissolved, make up the volume to 100 ml.

Preparation of strong ammonia-ammonium chloride solution:

Take 10 ml of water and 20 ml of strong ammonia solution in a beaker and saturate it with ammonium chloride.

Click here to get the procedure of preparation and standardization of 0.05 M EDTA solution.

Titration procedure:

  • All glassware should be cleaned and dried according to standard laboratory procedures.
  • Before filling the burette for the titration, rinse it with distilled water and then pre-rinse it with a portion of the titrant solution. Pre-rinsing is required to make sure that all solution in the burette is the desired solution, not a contaminated or diluted solution.
  • Take the unknown stock solution of titrant in a clean and dry beaker then fill the burette using the funnel.
  • Remove air bubbles from the burette and adjust the reading to zero.
  • Take 0.5 gm of calcium gluconate and pour it into a conical flask, and dissolve in 50 ml of warm water.
  • Allow the solution to cool to ambient temperature, add 05 ml of 0.05 M magnesium sulphate solution
  • Using a pipette, add 10.00 ml of strong ammonia-ammonium chloride solution.
  • Then, as an indicator, add 2 drops of mordant black II mixture and properly mix it.
  • Titrate the sample solution with standardized disodium edetate until the endpoint is reached. The actual endpoint is indicated by a change in the color of the solution.
  • Properly record the readings of the burette.
  • To get accurate results, repeat the titration three times.
  • Take their mean and calculate the percentage purity of calcium gluconate.
  • For a blank reading (B), repeat the titration using the same procedure but without the calcium gluconate.

Observation table:

Sr. No.

Content in conical flask

Burette reading

Volume of titrant used (ml)

Initial

Final

1

 

 

 

 

2

 

 

 

3

 

 

 

 

Mean:



Calculations:

Percentage Purity = V x E x AM x 100/ W x RM

Where,
V is a volume of EDTA used
V = A – B
A is the volume of EDTA used in the titration with calcium gluconate
B is the volume of EDTA used in the titration without calcium gluconate
E is an equivalent factor
AM is an actual molarity
RM is a required molarity
W is the weight of the sample
For 01 ml of calcium gluconate, the equivalent factor of 0.05 M disodium edetate is 0.02242

Result:

The percentage purity of calcium gluconate was found to be_____.



Commonly asked question on titration of calcium gluconate are as follows.

Assay of calcium gluconate is based on which titration?
Assay of calcium gluconate is based on complexometric titration.

Which reagent is used in the assay of calcium gluconate?
0.05 M magnesium sulphate solution, 0.05 M EDTA solution, and strong ammonia-ammonium chloride solution are used in the assay of calcium gluconate.

Which indicator is used in the assay of calcium gluconate?
Mordant black II indicator is used in the assay of calcium gluconate.


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Tuesday, August 24, 2021

Preparation and standardization of 0.05 M EDTA solution

Learn about the preparation and standardization of 0.05 M EDTA solution through a laboratory experiment or practical.

Aim:

To prepare and standardize 0.05 M EDTA solution using calcium chloride.

Requirements:

Glasswares: Burette, burette stand, conical flask, volumetric pipette, beaker, volumetric flask, funnel, glass rod, and wash bottle, etc.
Chemicals: LR grade disodium edetate (EDTA), ammonia (NH3), calcium chloride (CaCl2), ammonium chloride (NH4Cl), hydrochloric acid (HCL), and solochrome black-T indicator, etc.
Apparatus: Digital/analytical balance, and Ultrasonicator.

Principle:

The standardization of EDTA solutions is based on complexometric titration. When the indicator is introduced to a calcium chloride solution, the Ca-indicator complex forms. When titrating against disodium edetate, the complex converts calcium to EDTA, releasing a blue-colored indicator, indicating the reaction's endpoint.
The following is the reaction that is involved in this titration.

Preparation and standardization of EDTA solution

The molecular weight of disodium edetate (EDTA)is 336.21 g/mol.

Preparation of 0.05 M EDTA solution:

Take 18.16 gm of EDTA and dissolve in 300 ml of distilled water in a volumetric flask, and properly mixing it. Once it has completely dissolved, make up the volume to 1000 ml.

Preparation of 0.05 M calcium chloride:

Take 07.35 gm of CaCl2 and dissolve in 500 ml of distilled water in a volumetric flask, and properly mixing it. Once it has completely dissolved, make up the volume to 1000 ml.

Preparation of 1 M ammonia solution:

Take 75.00 ml of ammonia (Strong) using a pipette, dilute in 100 ml of distilled water in a volumetric flask, and properly mixing it.

Preparation of ammonia buffer of 10 pH:

Take 05.40 gm of NH4Cl, and 35.00 ml of 10 M ammonia solution and dissolve in 100 ml of distilled water in a volumetric flask and properly mixing it.

Titration procedure:

  • All glassware should be cleaned and dried according to standard laboratory procedures.
  • Before filling the burette for the titration, rinse it with distilled water and then pre-rinse it with a portion of the titrant solution. Pre-rinsing is required to make sure that all solution in the burette is the desired solution, not a contaminated or diluted solution.
  • Take the unknown stock solution of titrant in a clean and dry beaker then fill the burette using the funnel.
  • Remove air bubbles from the burette and adjust the reading to zero.
  • Take 10.00 ml of calcium chloride solution and pour it into a conical flask.
  • To make it alkaline, add 05 mL of buffer solution previously adjusted to pH 10.
  • Add 2 drops of solochrome black-T indicator.
  • Titrate the sample solution with EDTA until the endpoint is reached. The actual endpoint is indicated by a change in the color of the solution.
  • Properly record the readings of the burette.
  • To get accurate results, repeat the titration three times.
  • Take their mean and calculate the molarity of EDTA.

Observation table:

Sr. No.

Content in conical flask

Burette reading

Volume of titrant used (ml)

Initial

Final

1

 

 

 

 

2

 

 

 

3

 

 

 

 

Mean:


Calculations:

M1V1= M2V2
M2 = V1 M1 / V2

Where,
M1 is molarity of calcium chloride
V1 is volume of calcium chloride
M2 is molarity of disodium edetatesolution.
V2 is volume of disodium edetate solution used

Result:

The strength of the prepared EDTA solution was found to be_____M.


Commonly asked questions on titration of EDTA are as follows.

Why buffer solution is used in EDTA titration?
In EDTA titration, a buffer of ammonium chloride (pH 10) is used as it resists pH change. This is since all reactions involving metal ions and EDTA are pH-dependent.

Why do we standardize the EDTA solution?
Standardization of a prepared EDTA solution is performed to determine its exact molarity.

Which indicator is used in standardizing EDTA?
Eriochrome Black T indicator is used in the complexometric EDTA titration which produces color change from blue to pink.

To perform the assay of copper sulphate by iodometry

Learn about the assay of copper sulphate through a laboratory experiment or practical.

Aim:

Too perform the assay of copper sulphate using standard 0.1 N sodium thiosulphate (Iodometry).

Requirements:

Glasswares: Burette, burette stand, conical flask, volumetric pipette, beaker, volumetric flask, funnel, glass rod, and wash bottle, etc.
Chemicals: LR grade sodium thiosulphate (Na2O3S2), potassium iodide (KI), potassium thiocyanate (KSCN), copper sulphate (CuSO4), acetic acid, dilute sulphuric acid (H2SO4) and starch indicator, etc.
Apparatus: Digital/analytical balance, and Ultrasonicator.

Principle of assay of copper sulphate:

Copper sulphate assay is a type of iodometric titration. It is dependent on the instability of cupric iodide, which is formed when copper sulphate and potassium iodate react with the liberation of free iodine. Cupric iodide was formed when copper sulphate was allowed to react with potassium iodide in the presence of acetic acid.

The cupric iodide formed in the reaction is unstable, so it decomposes to give cuprous iodide with the liberation of iodine. The liberated iodine is titrated with 0.1 N sodium thiosulphate using a starch indicator.
The following is the reaction that is involved in this titration.
assay of copper sulphate

Preparation and standardization of sodium thiosulphate:

Click here to get the procedure of preparation and standardization of sodium thiosulphate (0.1 N).

Titration procedure:

  • All glassware should be cleaned and dried according to standard laboratory procedures.
  • Before filling the burette for the titration, rinse it with distilled water and then pre-rinse it with a portion of the titrant solution. Pre-rinsing is required to make sure that all solution in the burette is the desired solution, not a contaminated or diluted solution.
  • Take the unknown stock solution of titrant in a clean and dry beaker then fill the burette using the funnel.
  • Remove air bubbles from the burette and adjust the reading to zero.
  • Take 01 gm of copper sulphate, pour it into a conical flask and add 50 ml of distilled water.
  • After that, add 03 gm potassium iodide and 05 ml acetic acid to the mixture.
  • Add few drops of starch indicator.
  • Titrate the sample solution with sodium thiosulphate solution. When the solution is swirled for up to 10 seconds, a faint blue color appears and fades, indicates that the endpoint is approaching. The actual endpoint of the titration is indicated by a blue color that lasts longer than 30 seconds.
  • To get accurate results, repeat the titration three times.
  • Properly record the readings of the burette.
  • Take their mean and calculate the molarity of copper sulphate solution.

Observation table:

Sr. No.

Content in conical flask 

Burette reading

Volume of titrant used (ml)

Initial

Final

1

 

 

 

 

2

 

 

 

3

 

 

 

 

Mean:



Calculations:

Percent purity= V x E x AN x 100 / W x RN

Where,
V is a volume of sodium thiosulphate used.
E is an equivalent factor
AN is the actual normality of sodium thiosulphate.
RN is required normality of sodium thiosulphate
W is the weight of the sample
For 1 ml of 0.1 N sodium thiosulphate, the equivalent factor of copper sulphate is 0.02497.

Result:

The percentage purity of the copper sulphate (CuSO4), the sample was found to be_____.


Commonly asked questions on the assay of copper sulphate are as follows.

Why potassium iodide is used in the assay of copper sulphate?
When CuSO4 in aqueous reacts with KI in solid form, cuprous iodide forms as a precipitate liberates iodine gas and forming potassium sulphate in an aqueous state.

Which indicator is used in the estimation of copper sulphate?
The starch indicator is used in the assay of copper sulphate which produces a blue color at the endpoint of the reaction.

Assay of copper sulphate is based on which titration?
The assay of copper sulphate is based on the oxidation-reduction reaction of iodine/thiosulphate.


Monday, August 23, 2021

Assay of ferrous sulphate

Learn about the assay of ferrous sulphate through a laboratory experiment or practical.

Aim:

To perform the assay of ferrous sulphate using standard 0.1 N ceric ammonium sulpahte (Cerimetry).

Requirements:

Glasswares: Burette, burette stand, conical flask, volumetric pipette, beaker, volumetric flask, funnel, glass rod, and wash bottle, etc.

Chemicals: LR grade ferrous sulphate (FeSO4), sulphuric acid (H2SO4), and potassium permanganate (KMnO4), ceric ammonium sulphate, arsenic trioxide, potassium iodide, sodium hydroxide, osmic acid, ferroin sulphate, and 1, 10-phenanthroline hydrochloride, etc.
Apparatus: Digital/analytical balance, and Ultrasonicator.

Principle of assay of ferrous sulphate:

The assay of ferrous sulphate is based on redox titration (cerimetry). Ferrous sulphate is used as a reducing agent and is a powerful oxidant. Using ferroin solution as an indication, the known concentration solution of ceric ammonium sulphate is titrated with ferrous sulphate.

Ferrous sulphate is oxidized to ferric sulphate in the presence of dilute H2SO4. When the oxidation of ferrous sulphate is completed, a drop of KMnO4 is added. The endpoint of the titration is determined by the appearance of the permanent pink color and potassium permanganate (KMnO4) acts as a self-indicator.

Preparation and standardization of ceric ammonium sulphate (0.1 M):

Click here to get the procedure for the preparation and standardization of 0.1 M ceric ammonium sulphate.

Preparation of ferroin sulphate solution:

Take 0.7 gm of ferrous sulphate and 01.50 gm of 1, 10- phenanthroline hydrochloride and dissolve in 70 ml of distilled water in a volumetric flask, and properly mixing it. Once it has completely dissolved, make up the volume to 100 ml.

Preparation of sulphuric acid solution (1 M):

Click here to get the procedure for the preparation of 1 M sulphuric acid solution.

Titration procedure:

  • All glassware should be cleaned and dried according to standard laboratory procedures.
  • Before filling the burette for the titration, rinse it with distilled water, and then pre-rinse it with a portion of the titrant solution. Pre-rinsing is required to make sure that all solution in the burette is the desired solution, not a contaminated or diluted solution.
  • Take the unknown stock solution of titrant in a clean and dry beaker then fill the burette using the funnel.
  • Remove air bubbles from the burette and adjust the reading to zero.
  • Take 0.5 gm of ferrous sulphate and pour into a conical flask and to dissolve add a mixture of 20 ml sulphuric acid (1 M) and 30 ml of distilled water.
  • Add 0.1 ml of ferroin sulphate solution.
  • Titrate the sample solution with ceric ammonium sulphate solution until the endpoint is reached. The actual endpoint of the titration is indicated by the disappearance of the red color.
  • Properly record the readings of the burette.
  • To get accurate results, repeat the titration three times.
  • Take their mean and calculate the % purity of ferrous sulphate.

Observation table:-

Sr. No.

Content in conical flask

Burette reading

Volume of titrant used (ml)

Initial

Final

1

 

 

 

 

2

 

 

 

3

 

 

 

 

Mean:


Calculations:

Percentage purity of NH4Cl = V x E x AN X 100 / W x RN

Where,
V is a volume of KMnO4used
E is an equivalent factor
AN is an actual normality of KMnO4
RM is a required normality of KMnO4
W is the weight of the sample
For 0.1 M NaOH, the equivalent factor of ceric ammonium sulphate is 0.01519

Result:

The percentage purity of the ferrous sulphate (FeSO4) sample was found to be_____.


Commonly asked questions on the assay of ferrous sulphate are as follows.

Which indicator is used in the assay of ferrous sulphate?
No indicator is required in the assay of ferrous sulphate as potassium permanganate is a self-indicator. Generally, ferroin sulphate solution is used as an indicator which is prepared by ferrous sulphate and 1, 10- phenanthroline hydrochloride.

Which method is used for the estimation of ferrous sulphate?
The redox method is used for the estimation of ferrous sulphate from the sample solution.

How do you identify ferrous sulfate?
Ferrous sulfate can be identified by the identification tests are prescribed by pharmacopeias, that is to check the quality of the drugs, pharmaceutical aids, or any reagents necessary for the test.