Saturday, August 20, 2022

Preparation and standardization of 1N HCl

Learn about the preparation and standardization of 1N hydrochloric acid solution through a laboratory experiment or practical.

To prepare and standardize 1 N HCl using sodium carbonate as a primary standard.

Requirements:

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

Chemicals: LR grade concentrated hydrochloric acid (HCl), sodium carbonate, (Na2CO3), methyl red indicator, etc.

Apparatus: Digital/analytical balance

Principle of standardization of HCl:

In the titration of hydrochloric acid against the solution of sodium carbonate, methyl red (a weak base) which is yellow in the unionized form is used as an indicator.

When a weak base is used to titrate a solution that is just slightly acidic the endpoint is also slightly acidic. The solution is slightly alkaline when a weak acid is titrated with a strong base because the salt formed is partially hydrolyzed.

The reaction of sodium carbonate with hydrochloric acid is given below:

Na2CO3 + 2HCl → 2NaCl + H2O + CO2

In the process of acid-base titration, the portion of acid becomes chemically equivalent to the quantity of base present. When a strong acid and a strong base are tested at the same time, the solution turns out to be neutral.

Preparation of 1 N HCl solution:

Pipette out accurately 08.50 ml of concentrated hydrochloric acid (HCl) and dilute to 100 ml of distilled water in a volumetric flask, and properly mix 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 primary standard anhydrous sodium carbonate (Na2CO3) and dry it at 150°C for 1 hour in a Petri dish or crucible.
  • Once it is cool, weigh accurately 01.50 g sodium carbonate and pour it into a conical flask.
  • Pour in 100 ml of water and stir the mixture to dissolve.
  • Add 2-3 drops of methyl red indicator.
  • Titrate the sample solution with the prepared HCl solution until the light pink color appears.
  • Heat the solution to boiling until the color returns to yellow, then cool and titrate again until the light pink color is no longer affected by boiling.
  • To get accurate results, repeat the titration three times.
  • Properly record the readings of the burette.

Observation table:

Sr. No.

Content in conical flask

Burette reading

Volume of titrant used (ml)

Initial

Final

1

 

 

 

 

2

 

 

 

3

 

 

 

 

Mean:


Calculations:

Each ml of 1M HCl is equivalent to 0.05299g of Na2CO3.
Calculate the solution's molarity using the following formula.
Molarity = Wt. X 1 / volu. X 0.05299
Where,
Wt. is weight of Na2CO3 used,
Volu. is volume of HCl solution used in titration

Result:

The strength of the prepared hydrochloric acid (HCl) solution was found to be_____N.


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Thursday, August 18, 2022

Standardization of HCl solution

Learn about the preparation and standardization of hydrochloric acid solution through a laboratory experiment or practical.

To prepare and standardize 0.1 N HCl using sodium carbonate as a primary standard.


Requirements:

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

Chemicals: LR grade concentrated hydrochloric acid (HCl), sodium carbonate, (Na2CO3), methyl orange indicator, etc.

Apparatus: Digital/analytical balance

Principle of standardization of HCl:

In the titration of hydrochloric acid against the solution of sodium carbonate, methyl orange (a weak base) which is yellow in the unionized form is used as an indicator.

Standardization of HClWhen a weak base is used to titrate a solution that is just slightly acidic the endpoint is also slightly acidic. The solution is slightly alkaline when a weak acid is titrated with a strong base because the salt formed is partially hydrolyzed.

The reaction of sodium carbonate with hydrochloric acid is given below:

Na2CO3(aq) + 2HCl(aq) → 2NaCl(aq) + CO2(g) + H2O(l)
CO32-(aq) + 2H+(aq) → CO2(g) + H2O(l)

In the process of acid-base titration, the portion of acid becomes chemically equivalent to the quantity of base present. When a strong acid and a strong base are tested at the same time, the solution turns out to be neutral.

Preparation of 0.1 N HCl solution:

Pipette out accurately 08.50 ml of concentrated hydrochloric acid (HCl) and dilute in 500 ml of distilled water in a volumetric flask, and properly mix it. Once it has completely dissolved, make up the volume to 1000 ml with distilled water.

Preparation of sodium carbonate standard solution:

The molecular weight of sodium carbonate is 106. Therefore, weigh accurately 0.53 gm of Na2CO3 and dissolve in 50 ml of distilled water in a volumetric flask, once it has completely dissolved, make up the volume to 100 ml.

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 primary standard anhydrous sodium carbonate (Na2CO3) and dry it at 250°C for 4 hours in a Petri dish or crucible.
  • Once it is cool, weigh accurately 0.22 g sodium carbonate and pour it into a conical flask.
  • Pour in 50 ml of water and stir the mixture to dissolve.
  • Add 2-3 drops of methyl orange indicator.
  • Titrate the sample solution with the prepared HCl solution until the light pink color appears.
  • To get accurate results, repeat the titration three times.
  • Properly record the readings of the burette.

Observation table:

Sr. No.

Content in conical flask

Burette reading

Volume of titrant used (ml)

Initial

Final

1

 

 

 

 

2

 

 

 

3

 

 

 

 

Mean:


Calculations:

Calculate the normality of the HCl solution (N),

As follows:

N = A /0.053*B

Where
A - gram of Na2CO3 used,
B - used ml of HCl solution in titration.

Result:

The strength of the prepared hydrochloric acid (HCl) solution was found to be_____N.


Frequently Asked Question (FAQ):

Why methyl orange is used in the standardization of HCl with Na2CO3?

Methyl orange is a better indicator for the titration of hydrochloric acid with sodium carbonate since the endpoint of the reaction falls in the pH range of 3.0 to 4.4 which is the pH range of Methyl orange.

What is the purpose of standardizing HCl acid solution?

To determine the concentration of a prepared solution of HCl we perform the standardization. Standardization is the process of determining a solution's exact concentration (Molarity/Normality). We can also use standard NaOH to measure the molarity of a hydrochloric acid solution.

What primary standard is taken in HCl standardization?

Usually, sodium carbonate (Na2CO3) is used as the primary standard in the standardization of HCl, as it complies with all the requirements (properties) of the primary standard. It has a high molecular weight, high purity, is non-toxic, is easy to weigh, and is non-hygroscopic.



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Wednesday, August 17, 2022

Standardization of NaOH with KHP

Learn about the preparation and standardization of NaOH solution through a laboratory experiment or practical.

To prepare and standardize 0.1N sodium hydroxide solution with potassium hydrogen phthalate by acid-base titration.


Requirements:

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

Chemicals: LR grade potassium hydrogen phthalate (C8H5KO4), sodium hydroxide (NaOH), phenolphthalein indicator, etc.

Apparatus: Digital/analytical balance

Theory for standardization of NaOH:


When sodium hydroxide is weighed, it takes moisture from the air because it is hygroscopic. Because of this water, we will not be able to find out the exact mass of NaOH. Therefore to determine the exact concentration of prepared sodium hydroxide solution, titration with a solid acid that is not hygroscopic is required.

KHP, also known as potassium hydrogen phthalate, is an acidic salt compound. It is used as the primary standard because it has high purity, is non-toxic, has a high molecular weight, is non-hygroscopic, and is easy to weigh. For the purpose of determining the concentration of a solution containing sodium hydroxide, we will use this primary standard.

It is an acid-base titration in which sodium hydroxide is a strong base and potassium hydrogen phthalate is a weak acid. By direct titration, we standardize the 0.1 N NaOH solution (the titrant) with potassium hydrogen phthalate (KHP, KC8H4O4H) using phenolphthalein as an indicator.

KHP is a weak acid, and its reactions with bases are as follows:

Standardization of NaOH

Preparation of 0.1N NaOH solution:

Weigh accurately 0.2 gm of sodium hydroxide and dissolve in 40 ml of distilled water in a volumetric flask, and properly mix it. Once it has completely dissolved, make up the volume to 50 ml with distilled water.

Preparation of 0.1N KHP solution:

Weigh accurately 1.02 gm of potassium hydrogen phthalate and dissolve in 40 ml of distilled water in a volumetric flask, and properly mix it. Once it has completely dissolved, make up the volume to 50 ml with distilled water.

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 05.00 ml of prepared KHP solution and pour it into a conical flask.
  • Add 2-3 drops of phenolphthalein indicator.
  • Titrate the sample solution with the sodium hydroxide (NaOH) solution until the color of the solution is discharged.
  • To get accurate results, repeat the titration three times.
  • Properly record the readings of the burette.

Observation table:

Sr. No.

Content in conical flask

Burette reading

Volume of titrant used (ml)

Initial

Final

1

 

 

 

 

2

 

 

 

3

 

 

 

 

Mean:

Calculations:

Calculate the normality and % of NaOH.

meq. NaOH = meq KHP

(N * V)NaOH = (N * V)KHP

Wt./ Eq.Wt * 1000 = ( N * V) KHP

Wt./40*1000 = 0.1 x V1 X V2 X V3/3

% NaOH = Wt./Wt. of sample X 100


Result:

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




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Tuesday, August 16, 2022

Standardization of NaOH with oxalic acid

Learn about the preparation and standardization of Sodium hydroxide through a laboratory experiment or practical.

Aim:

To prepare and standardize sodium hydroxide standard solution with oxalic acid by acid–base titration.

Requirements:

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

Chemicals: LR grade oxalic acid (C2H2O4), sodium hydroxide (NaOH), phenolphthalein indicator, etc.

Apparatus: Digital/analytical balance

Principle:

It is an acid-base titration in which sodium hydroxide is a strong base and oxalic acid is a weak acid. When oxalic acid reacts with sodium hydroxide, sodium oxalate and water are formed. The phenolphthalein (HPh) indicator is used to determine the endpoint of this titration. The endpoint is when the color changes to pale pink and persists for 30 sec.

Standardization of NaOH with oxalic acid

Because oxalic acid compliance with all primary standard requirements (Properties), it is use as a primary standard and can later be used to standardize other solutions.

Preparation of 0.1M NaOH solution:

Weigh accurately 04.00 gm of sodium hydroxide and dissolve in 500 ml of distilled water in a volumetric flask, and properly mix it. Once it has completely dissolved, make up the volume to 1000 ml.

Preparation of oxalic acid solution:

Weigh accurately 0.63 gm of oxalic acid and dissolve in 50 ml of distilled water in a volumetric flask, and properly mix it. Once it has completely dissolved, make up the volume to 100 ml with distilled water.

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 20.00 ml of prepared oxalic acid solution and pour it into a conical flask.
  • Add 2-3 drops of phenolphthalein indicator.
  • Titrate the sample solution with the sodium hydroxide (NaOH) solution until the pink color appears.
  • Properly record the readings of the burette.
  • To get accurate results, repeat the titration three times.

Observation table:


Sr. No.

Content in conical flask

Burette reading

Volume of titrant used (ml)

Initial

Final

1

 

 

 

 

2

 

 

 

3

 

 

 

 

Mean:


Calculations:


The following equation can be used to determine the molarity of a NaOH solution.

N 1V 1=N 2V 2

N 2 = N 1V 1/ V 2

Result:


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


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Preparation and standardization of oxalic acid using sodium hydroxide

Learn about the determination of the concentration (strength) of a given sodium hydroxide solution by titrating it against a standard solution of oxalic acid through a laboratory experiment or practical.

Aim:

Determination of the concentration (strength) of a given sodium hydroxide solution by titrating it against a standard solution of oxalic.

Requirements:

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

Chemicals: LR grade oxalic acid (C2H2O4), sodium hydroxide (NaOH), phenolphthalein indicator, etc.

Apparatus: Digital/analytical balance

Theory:

It is based on alkalimetry titration, at the point in the titration of a strong acid with a strong base, the amount of acid and base becomes chemically equivalent, and the chemical reaction is referred to as a neutralization reaction.

The pH of the solution suddenly changes near the end point. Even a small volume of base or acid added after the end point would become slightly alkaline or acidic respectively. When oxalic acid (a weak acid) is titrated with sodium hydroxide (a strong base), the following reaction happens:

Preparation and standardization of oxalic acid

In this titration the endpoint is detected using the phenolphthalein HPh indicator.

Preparation of 0.1M oxalic acid solution:

Weigh accurately 12.67 gm of oxalic acid and add 500 ml of distilled water. Once it has completely dissolved, make up the volume to 1000 ml.

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 prepared 10 mL of oxalic acid solution and pour it into a conical flask.
  • Add 2-3 drops of phenolphthalein indicator.
  • Titrate the acid with sodium hydroxide solution (NaOH) till a very faint permanent pink colour is obtained.
  • Properly record the readings of the burette.
  • To get accurate results, repeat the titration three times.
  • The following equation can be used to determine the molarity of a NaOH solution.

Observation table:


Sr. No.

Content in conical flask

Burette reading

Volume of titrant used (ml)

Initial

Final

1

 

 

 

 

2

 

 

 

3

 

 

 

 

Mean:

Calculations:

a1 M1V1 = a2 M2V2


where M1 and V1 are the molarity and volume of the oxalic acid solution.

M2 and V2 are the molarity and volume of the sodium hydroxide solution.

 

Result:

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



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Wednesday, August 10, 2022

What solution usually goes in the burette in titration?

The titrant is a known concentration solution that is placed in the burette, and the analyte is a solution of unknown concentration that is poured into a conical flask. In an acid-base titration, the base, such as sodium hydroxide (NaOH), is often taken in a burette, whereas the acid, such as hydrochloric acid (HCl), is typically taken in a conical flask.

Titration, also known as titrimetry, is a type of quantitative analysis used to determine the concentration of a substance. To determine the endpoint an indicator is used that changes the color of the solution after the endpoint or equivalence point is reached. Based on chemical reactions, there are four types of titrations: acid-base, redox, precipitation, and complexometric titrations.

Which solution is in burette in titration?

When performing titrations, the solution is often placed in a burette, known as a titrant. In analytical chemistry, the titrant is a solution with a known concentration that is added to another solution to measure the concentration of analytes.

The known (concentration) solution is taken in a conical flask, and the solution whose concentration or strength you are trying to determine, i.e., titrant, is taken in a burette.

Titration is performed between two interacting solutions. The purpose is to determine the precise volume of a solution that reacts with a known concentration of other solutions.

Typically, a pipette that can only measure a single fixed volume, such as 10 ml or 20 ml, is used to take the known volume. A small amount of the other solution is taken into the burette and added dropwise into the solution, which is taken in a conical flask. That's why we use a burette in the titration.



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Tuesday, August 9, 2022

Sources of error in titration

Titration also known as volumetric analysis or titrimetry is a method of determining the concentration of an unknown solution. It is a quantitative technique in which a reaction between the titrant and titrand takes place. The titrant is the substance whose concentration is known, and the titrand or analyte is the compound to be tested.

The endpoint of the reaction is detected using an indicator; this indicator changes the color of the solution. In chemistry, different types of titrations, such as acid-base, precipitation complexometric, and redox titrations, are used for various purposes and pharmaceutical research.

Titration is a highly sensitive analytical technique that allows us to determine the concentration of an unknown sample in solution by introducing a compound with a known concentration. Therefore, it must be carried out precisely to get the desired results.

Possible sources of errors in titration:

There are two different kinds of titration errors: random errors and systematic errors. Errors in titration can be caused by several different things, including human error and some of the other things that are listed below.
  • Misinterpretation of colors
  • End Point Error
  • Misreading the volume
  • Use of contaminated solutions
  • Using solutions with the incorrect concentration
  • Using the wrong amount of indicator
  • Improper use of equipment
  • Use of contaminated glassware
  • Inaccurate weight of material (Balance/weighing error)
  • Using the wrong solution to rinse the pipette and/or burette
  • Incorrectly filling the burette with liquid
  • Not transferring all solids or liquids while preparing samples
  • Transferring excess or less volume of liquid
  • Use of wrong chemicals or reagents
  • Performing the titration at the wrong temperature
  • Leakage in Burette
  • Use of the wrong procedure
  • The accuracy of volumetric glassware
  • Use of the same glassware for two different substances


Frequently Asked Questions (FAQ):

What do you mean by percentage error?

A percentage error represents the difference between the estimated value and the actual value, represented as a percentage. In other words, the percent error is the relative error multiplied by 100.

What is a titration error?

An error in titration is the difference between a titration's endpoint and an equivalence point. The volume of the endpoint that is higher or lower than the equivalence point is referred to as the titration error. The endpoint of the titration is the color change observed at the end of the reaction.



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