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.

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(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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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:

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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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.

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:

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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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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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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Volumetric Analysis: Principle, Types, Procedure & Applications

Learn about the principle, types, procedures, and applications of the volumetric technique which is used to determine the concentration of a substance using the known volume of a known substance.

Chemical analysis is an important part of the study of different materials or substances. It is broadly classified into two forms: qualitative analysis and quantitative analysis. Qualitative chemical analysis is a branch of chemistry that that deals with the identification of elements or grouping of elements present in a sample.

Quantitative analysis is any technique used to determine the concentration of a substance in a sample. It is further divided into gravimetric analysis and volumetric analysis.

Titration, also called titrimetry, is a type of quantitative analysis that is used to determine the amount of a specific substance in an unknown given sample. Since measuring volume is the most important part of this analysis, it is also called volumetric analysis.

In the process, the titrant is added to the analyte until a certain endpoint or equivalence point is reached. The reaction's endpoint is identified using an indicator. The indicator causes the color of the solution when the endpoint is reached.

Table of Contents: Definition of volumetric analysis What is volumetric analysis? History of volumetric analysis Example of volumetric analysis Principle of volumetric analysis Types of volumetric analysis Procedure of volumetric analysis Applications of volumetric analysis

Definition of volumetric analysis:

"The process of titrating a solution to find out how much of a substance is in it, by volume"

What is volumetric analysis?

Volumetric analysis, also known as titration, is a quantitative chemical analysis technique that is used in laboratories to determine the concentration of an analyte by measuring the volume that it occupies or, more broadly, the volume of a second substance that combines with the first in known proportions, also known as titrimetric analysis.

In other words, volumetric analysis or titration refers to the process of measuring the volume of a second substance that combines with the first in known proportions. It is used in laboratories which allows us to determine the concentration of analyte. 

The titrant is a reagent that produced a standard solution with a specific volume and concentration. The titrant reacts with an analyte solution to determine the concentration of the analyte.

History of volumetric analysis:

The French chemist Jean-Baptiste-Andre Dumas derived and found the first volumetric analysis method while attempting to quantify the proportion of nitrogen with other elements in organic compounds.

To assure the conversion of the chemical into pure gas, the nitrogen compound was burned in a furnace and passed through the furnace in a stream of carbon dioxide (CO2) that is passed into a strong alkali solution. The mass of the nitrogen is calculated, which occupies the sample under conditions of pressure and volume that are already known.

Example of volumetric analysis:

Volumetric analysis refers to any method of quantitative analysis in which the quantity of a substance is determined by measuring the volume that it occupies the volume of a second substance that combines with the first substance in known proportions.

For example, acid-base titration, preparation, and standardization of sodium hydroxide (NaOH) solution.

Principle of volumetric analysis:

The following are some of the fundamentals of volumetric analysis:

• The solution that needs to be examined must have an unknown number of chemicals.
• To show the end-point of the reaction a chemical with an unknown amount reacts with a substance of unknown concentration in the presence of an indicator (E.g. phenolphthalein/methyl orange). The endpoint is the point at which a chemical process is complete.
• The titration procedure, which measures the volumes, is used to complete the reaction between the titrant and titrand.
• The amount of reagent and solution is represented by the volume and concentration of the reagent used in the titration.
• The mole fraction of the equation determines the quantity of an unknown substance in a given volume of solution.

When the reaction reaches its endpoint, the volume of reactant consumed is measured and used to calculate the volumetric analysis of the analyte (molarity or normality) using the formula Ca= Ct Vt M / Va.

Types of volumetric analysis:

The volumetric analysis can be classified into the following three types:

1. Simple titration
2. Back titration
3. Double titrations

1. Simple titration: 

A simple titration is a method of determining the concentration of an unknown solution using a solution of known concentration. The simple titration can be subdivided into the following four categories:

• Acid-base titration
• Redox titration
• Precipitation titration
• Complexometric titration

2. Back titration:

In a back titration, the concentration of an analyte is determined by reacting it with a known amount of excess reagent, whereas in a direct titration, the concentration of an unknown compound is examined directly. Back titration is also known as indirect titration in which excess reagents are not added.

3. Double titration:

These types of titrations are carried out to find out the percentage content of an acid or alkali mixture. Gilson's titration method is also known as double titration, which determines the concentration of organometallic compounds in hydrocarbon solvents.

In the first step, the base concentration in the solution is determined. The concentration of the metal-organic complex can be calculated in the second stage by determining the residual amount of alkali after the organometallic compound and halide react.

Procedure of volumetric analysis:

Common apparatus required to perform volumetric titration are burette, conical flask, beaker, pipette, funnel, volumetric flask, wash bottle, etc. Following are the steps used for volumetric analysis:

1. All glassware should be cleaned and dried according to standard laboratory procedures.
2. Remove air bubbles from the burette and adjust the reading to zero.
3. By precisely weighing the chemicals, accurately prepare the standard solution and a sample of the material to be measured in the solution.
4. A common titration begins with the placement of a conical flask underneath a burette, which contains the solution of analyte/sample and a few drops of suitable indicator (such as methyl orange or phenolphthalein).
5. Then, the titrant is dropwise added to the analyte until a change in the indicator's color is observed, showing that the endpoint of the titration has been reached. This indicates that the amount of titrant present equals the amount of analyte present due to their interaction.
6. Depending on the desired endpoint, a single drop of the titrant can cause either a temporary or permanent change in the color of the indicator.
7. To get accurate results, repeat the titration three times, and properly record the readings of the burette. Take their mean and calculate the molarity/normality of the sample.

Applications of volumetric analysis:

Volumetric analysis is one of the fundamental analytical techniques in chemistry and is applied for quantitative analysis in life sciences, pharmaceuticals, clinical chemistry, cosmetic industry, water pollution, wastewater management, food industry, wine industry, etc.

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References:

• Textbook of modern analytic chemistry, Harvey David, 1956, 1st edition. Avialable Here
• Wikipedia contributors. "Titration." Wikipedia, The Free Encyclopedia. Wikipedia, The Free Encyclopedia, 18 Jul. 2022. Available Here: 

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Why is titration known as volumetric analysis?

Titration, also known as volumetric analysis or titrimetry, is a method that is used to determine the concentration of an unknown solution. It is a quantitative method in which an reaction between the titrant and the titrand occurs. The titrant is the substance whose concentration is known, and the titrand (also known as analyte) is the compound that is analyzed.

An indicator is used to determine the endpoint of the reaction. When the endpoint has been reached, this indicator changes the color of the solution. However, sometimes the reactants themselves can act as an self indicator in which no indicator is needed.

There are different types of titration, including acid-base, redox, complexometric, and precipitation titrations, which are employed in chemistry and for pharmaceutical applications.

Why titration is also called volumetric analysis?

Due to the measurement of volume plays a key role in titration, it is also known as "volumetric analysis." It is a method of quantitative chemical analysis used in laboratories to detect the unknown concentration of an identified analyte.

Volumetric Analysis: Volumetric analysis is a practical method in which reactive volumes are used to analyze and calculate a range of unknown values.

Titrations: A titration is a technique used for determining the concentration of an unknown solution.

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What is the process of titration?
Definitions and basic terms used in titration
Volumetric Analysis: Principle, Types, Procedure & Applications
Sources of error in titration
What solution usually goes in the burette in titration?
Preparation and standardization of oxalic acid using sodium hydroxide
Standardization of NaOH with oxalic acid
Standardization of NaOH with KHP
Standardization of HCl solution