Wednesday, October 20, 2021

Identification test of sodium bicarbonate

Learn the identification tests of sodium bicarbonate through a laboratory experiment or practical.

Aim:

To perform identification tests of sodium bicarbonate on a given sample.

Reference: Indian Pharmacopoeia (IP) 2010

Requirements:

Glasswares and miscellaneous:
Test tube, measuring cylinder, pipette, glass rod, volumetric flask, beaker, dropper, rubber stopper, test tube stand, test tube holder, litmus paper, and balance, etc.

Chemicals:
Sodium bicarbonate (NaHCO3), magnesium sulphate (MgSO4), calcium chloride (CaCl2), barium hydroxide (Ba (OH)2), phenolphthalein solution, hydrochloric acid (HCL), potassium carbonate (K2CO3), potassium hydroxide (KOH), and potassium antimonate (K[Sb(OH)6]), etc.

Preparation of reagents:

3% barium hydroxide solution preparation:

Take 03.00 gm of barium hydroxide and dissolve to 100.00 ml of distilled water in a volumetric flask, and properly mix it.

2 M acetic acid preparation:

Take 11.40 ml of glacial acetic acid using a pipette and dissolve to 100.00 ml of distilled water in a volumetric flask, and properly mix it.

1% w/v phenolphthalein solution preparation:

Take 0.1 gm of phenolphthalein and dissolve to 100.00 ml of 95% ethanol in a volumetric flask, and properly mix it.

15% potassium carbonate solution preparation:

Accurately weigh 15.00 g of K2CO3 and pour in 100.00 ml of distilled water and properly mix it.

5 % w/v potassium hydroxide preparation:

Accurately weigh 05.00 g of KOH and pour in 100.00 ml of distilled water and properly mix it.

Dilute HCL preparation:

Click here to get the procedure.

1M NaOH solution preparation:

Take 04.00 gm of sodium hydroxide and dissolve in 70.00 ml of distilled in a volumetric flask and properly mix it. Once it has completely dissolved and cooled, make up the volume to 100 ml.

Potassium antimonate solution preparation:

Take 02.00 gm of potassium antimonate pour into 95.00 ml of water and boil it until dissolved. Cool quickly; add 50.00 ml of prepared KOH solution and 05.00 ml of 1M NaOH solution. Let stand for 24 hours, filter it, and then add enough water to produce 150.00 ml.

Procedure for identification of sodium bicarbonate:

  • Test 1: When a solution of a given chemical is boiling, carbon dioxide is released, turning moist blue litmus paper red. 
  • Test 2: When a substance solution is treated with a magnesium sulphate solution, no precipitate is produced. Boil; A white precipitate is formed.
  • Test 3: Take 0.1 gm of sample to be tested in the test tube and add 02 ml of water. Then add 02 ml 2 M acetic acid, immediately close the tube with a stopper equipped with a glass tube bent at two right angles, gradually heat, and collect the gas in 05 ml barium hydroxide solution. A white precipitate is formed which dissolves on the addition of additional dilute HCL.
  • Test 4: Add 0.1 ml of phenolphthalein solution to 05 ml of a 5 % w/v solution, a light pink color obtains. When the solution is heated, a gas is evolved, and the solution turns red.
  • Test 5: Add 02 ml of a 15 % w/v potassium carbonate solution to 02 ml of a 5 % w/v sodium bicarbonate solution and heat to boiling; no precipitate forms. Add 04 ml of freshly prepared solution of potassium antimonate and heat to boiling. Allow it to cool in ice, then scrape the interior of the test tube with a glass rod if required; a dense, white precipitate will develop.

Observations:

Identification Test

Observation

Inference

Test 1

 

 

Test 2

 

 

Test 3

 

 

Test 4

 

 

Test 5

 

 

Results:

The given sample complies with the tests 1 / 2 / 3 / 4 / 5 and does not comply with the tests 1 / 2 / 3 / 4/ 5 for the identification of sodium bicarbonate as per IP 2010.
It suggests that the given sample is of ………………………...


Identification test of ferrous sulphate

Learn the identification tests of ferrous sulphate through a laboratory experiment or practical.

Aim:

To perform identification tests of ferrous sulphate on a given sample.

Reference: Indian Pharmacopoeia (IP) 2010

Requirements:

Glasswares and miscellaneous:
Test tube, test tube stand, test tube holder, measuring cylinder, pipette, glass rod, dropper, rubber stopper, volumetric flask, and balance, etc.
Chemicals:
Sulphuric acid (H2SO4), hydrochloric acid (HCL), 1,10-phenanthroline (C12H8N2), sodium hydroxide (NaOH), ceric ammonium sulphate ((NH4)4Ce(SO4)4), iodine (I2), potassium iodide (KI), stannous chloride (SnCl2), lead acetate (Pb(C2H3O2)2), barium chloride (BaCl2), ammonium acetate (C2H7NO2).

Preparation of chemicals:

Dilute H2So4 preparation:

Take 57.00 ml of concentrated H2So4of using a pipette and dilute to 1000.00 ml of distilled water in a volumetric flask, and properly mix it.

0.1% w/v 1,10-phenanthroline solution preparation:

Take 0.1 gm of 1,10-phenanthroline and dissolve to 100.00 ml of distilled water in a volumetric flask, and properly mix it.

0.1M ceric ammonium sulphate preparation:

In a mixture of 30.00 ml H2SO4 and 500 ml distilled water, dissolve 65.00 g ceric ammonium sulphate with the help of mild heat. Once cooling, dilute to 01 liters by distilled water and filter it. Filter the solution, if turbid,

Dilute HCL preparation:

Take 10.00 ml of concentrated hydrochloric acid (Approximately 10% w/w of HCL) using a pipette and dilute to 100.00 ml of distilled water in a volumetric flask, and properly mix it.

25 % w/v barium chloride solution preparation:

Take 25.00 gm of BaCl2 and dissolve to 100.00 ml with the same solvent in a volumetric flask, and properly mix it.

Iodine solution preparation:

Weigh accurately 02.00 gm of I2 and 03.00 gm of KI dissolve to 100.00 ml with the distilled water in a volumetric flask and properly mix it.

Stannous chloride solution preparation:

Accurately weigh 330.00 g of SnCl2 and pour in 100.00 ml of concentrated HCl, adding enough water to make 1000 ml.

Ammonium acetate solution preparation:

Weigh accurately 150.00 gm C2H7NO2 dissolve to 200.00 ml with the distilled water and add 03.00 ml of glacial acetic acid and add enough water to make 1000 ml. Make sure you are using a freshly prepared solution.

Procedure for identification of ferrous sulphate:

  • Test 1: In 02.00 ml of water, dissolve a quantity of the substance under study containing 10 mg of iron. Then add 02.00 ml of dilute H2SO4 and 01.00 ml of a 0.1 % 1, 10-phenanthroline solution, an intense red color is formed, which discharged with adding a small amount of 0.1 M ceric ammonium sulphate is produced.
  • Test 2: Take 50 mg of the sample and dissolve in 05.00 ml of water. Add 01.00 ml of dilute HCL and 01.00 ml of prepared BaCl2 solution; a white precipitate is formed.
  • Test 3: Add 0.1 ml of iodine solution to the suspension produced in Test 2. The suspension stays yellow however is decolorized by dropwise adding prepared stannous chloride solution. Boil the mixture; no colored precipitate is formed.
  • Test 4: Dissolved 20 mg of the sample substance in 02.00 ml of water and add 01.00 ml of prepared lead acetate, by which a white precipitate is formed that is soluble in ammonium acetate and sodium hydroxide solutions.

Observations:

Identification Test

Observation

Inference

Test 1

 

 

Test 2

 

 

Test 3

 

 

Test 4

 

 

Results:

The given sample complies with the tests 1 / 2 / 3 / 4 and does not comply with the tests 1 / 2 / 3 / 4 for the identification of ferrous sulphate as per IP 2010.
It suggests that the given sample is of ………………………...


FAQ (Frequently Asked Questions):


What is the assay of ferrous sulphate?
The assay of ferrous sulphate is to find out the percentage purity, click here to get the procedure.


Monday, October 18, 2021

Working Principle and Procedure of pH Meter

Learn the principle, types, and procedure of pH meter which is used to measure hydrogen-ion activity (acidity or alkalinity) in solution.

What is a pH meter?

A pH meter is an automated measurement tool used to determine the pH of the liquid. It is also known as a potentiometric pH meter since it determines the difference in electrical potential between a pH electrode and a reference electrode.

A rough idea of pH can be achieved using indicators, pH papers, or litmus papers that change color based on the pH level. Such types have limits on their precision, and it can be difficult to interpret correctly. Hence a pH meter is broadly used to determine the exact pH of the sample solution.

A pH meter consists of an electrode that is attached to an electronic meter that monitors and displays the correct pH reading. A glass electrode made of a specialized glass membrane is sealed at the end to forming a bulb. An internal standard acidity solution, generally 0.1 M hydrochloric acid (HCl), and an internal reference electrode, REin (often an Ag/AgCl wire electrode), are included within the glass. This solution is referred to as the reference solution, which has a pH of 07.00.

A second electrode, REext, is inserted into potassium chloride (KCl)-soaked external tube. Around the first enclosed glass tube containing the 0.1 M HCl, this external tube forms a concentric enclosure. This setup is known as a combination pH electrode.

Working principle of pH meter:

principle of pH meter
The pH meter mainly works on the assumption that the interface between two liquids produces an electric potential that can be determined. The working principle of the pH meter relies on the exchange of ions from the liquid sample through the glass membrane to the inner solution of a glass electrode. The porosity of the glass membrane decreases with constant use, which reduces the probe's performance.

It detects the difference in voltage between the two electrodes i.e. glass electrode and reference electrode. When both electrodes are present, the electrode is referred to as a combination electrode, and it is placed into the solution to be tested.

These two electrodes are immersed in a solution, and after that, the H+ ions in the test solution exchange for other positively charged ions present on the glass ball. So there is an action between these plus ions of the solution and the H+ ions or positively charged ions present on the glass bulb.

The difference in electric potential between the two electrodes is detected by the amplifier. The pH unit is the difference between these potentials. The difference in electric potential between the two electrodes is detected by the amplifier. The difference of this potential is known as the pH unit.

Types of pH meter:

The pH meter ranges from easy and economical pen-like apparatus with computer interfaces and complex and costly laboratory apparatus, in which many inputs are recorded for indicators and temperature measurements to manage the variation in pH due to temperature. The display may be digital and the systems may be operated by batteries or depend on the electric power.

There are special pH meters that can be used in particular applications that allow pH determination colorimetrically. Commercial pH meters are available based on solid-state electrodes, instead of traditional glass electrodes.

Procedure of pH meter:

Before beginning a pH meter process, we must recognize the various parts essential to perform the process. A pH meter consists of three major parts such as pH electrode or glass electrode or combined electrode, a temperature probe, and electronic control unit.

pH Electrode:

Glass electrodes are the most widely used pH electrodes made of special glass. Silver/silver chloride (Ag / AgCl) is the most regular reference electrode form used today.

Temperature probe:

For accurate determination of pH, some pH meters automatically compensate for temperature. This is achieved by a meter, temperature probe, which, along with the electrode, is submerged in the sample solution.

Electronic control unit:

To produce a chemical signal, the electrode responds to the concentration of hydrogen ions in the sample solution. This signal is then transformed into pH values shown on the screen.

Procedure for pH measurement:
  • The pH meter should be calibrated with the appropriate buffer solution such as pH 07.00, 04.00, and 09.20 to confirm the performance of the pH electrode before pH measurement. The process may look a little variation depending on the pH meter used and the electrode used however in most cases the pH determination process is very similar.
  • Clean the electrode and temperature probe with deionized water and wipe gently with soft tissue paper.
  • Immerse the electrode in the sample solution.
  • Press the pH mode key which is on the board.
  • The instrument will display the pH.
  • Save the reading or print the reading if the printer is connected.
  • Reset the instrument and again clean the electrode and temperature probe with distilled water and wipe gently with soft tissue paper.

Applications of pH meter:

  • The basic application of the pH meter allows us to determine if any liquid sample is acidic or basic or neutral.
  • The pH is used mainly in the pharmaceutical, beverage, chemical, and food industries.
  • It is commonly used in chemistry to determine the acidity or basicity of a substance.
  • It is used in production to ensure product quality.
  • The pH is widely used in the development and research in many fields.
  • The pH is very significant for checking the consistency of water, soil, and pesticides in the agricultural sector.
  • The pH meter is an improved version for pH determination than traditional methods, providing simple, accurate pH.

Advantages of pH meter:

  • This makes pH measurement quick and simple.
  • The advantage of the pH meter is that they are compact and portable (Pen pH meter) you can use at a different location.
  • It can be used for a wide variety of applications.
  • This indicator gives an accurate pH value compared to pH paper, and indicators.
  • It covers the entire range of pH i.e. 01 to 14.
  • With a standard buffer solution, you can calibrate the pH meter to improve consistency.

Disadvantages of pH meter:

  • Deposition on the electrode membrane can cause an error in the results.
  • Because of fragile glass electrodes, there is a risk of breakage.
  • It is often necessary to calibrate the pH meter.
  • To calibrate the pH meter you need buffer solutions that make it expensive.

FAQ (Frequently Asked Questions):


What is pH meter?
A pH meter is an apparatus used to determine the acidity or alkalinity of a solution. The pH is a measure of hydrogen ion concentration.

What is the basic principle pH meter?
A pH meter gives information for how acidic or alkaline a solution is. Measuring the concentration of hydrogen ions in the basic principle of the pH meter.

Why do you need to calibrate a pH meter?
To prevent drift and maintain the accuracy of the pH meter, it is necessary to periodically calibrate the pH.

Why are buffer solutions used to calibrate the pH meter?
The buffer solutions are used to calibrate a pH meter as they avoid changes in pH. You can adjust the value of pH by using the standard buffer solution of known pH.



Sunday, October 17, 2021

Difference between pH meter and conductivity meter

The major difference between pH meter and conductivity meter is that the pH meter uses to measure the hydrogen ion concentration of a solution (pH) and conductivity meter used to determine the conductance (electric current) in a solution. The unit of conductance is Siemens/cm (S/cm), generally the more impurities in the sample solution, the higher the value of conductivity.

The pH and conductance, both are significant factors in various fields. These are generally classified as physical tests, although they generally, depending on the chemical characteristics of the sample or solution. 

Both processes are quick and simple to perform and are usually done immediately after obtaining a sample. It is also used to check the stability of the compound; constant changes in these parameters indicate that the basic conditions are changing.

What is pH meter:

A pH meter is an electronic apparatus that determine hydrogen ion activity in solutions, or in other words, it measures the acidity or alkalinity of a solution. The pH meter is also referred to as a "potentiometric pH meter" as it detects the difference in electrical potential between a pH electrode and a reference electrode. 

It consists of a special measuring probe (glass/combine electrode) connected to an electronic meter that displays the pH measurement in decimal form.

The pH scale is usually measured in the scale of pH 01 to 14. The value below the pH 07 considered as acidic and above 07 considered as a basic value. We determine pH using dyes or indicator solutions, pH papers, and pH meters. 

But the indicator indicates that the solution is acidic or basic, pH paper gives a rough idea regarding the pH of the solution, but the pH meter gives an exact pH value of the sample. The pH meter consists of a glass/combine electrode, temperature sensor, display, and measurement keys.

What is conductivity meter:

A conductivity meter is an electronic device that measures the amount of electrical current or conductance in a solution. A conductivity meter consists of a conductivity cell or probe. A small electrical current runs between two electrodes that are set a certain distance by about one centimeter. 

The conductance of a solution with a high concentration of ions is high, resulting in a rapid current. When there is a lower concentration of ions, the electrical current is slower and the reading is smaller.

A conductivity meter used to determine the amount of conductance or electric current in a solution. The current is carried almost whole by dissolved ions. The capacity of an ion to carry current is a function of its charge and its size or mass, hence more charged ions conduct more current and larger ions conduct less current. The conductivity meter consists of a conductance cell, temperature sensor, display, and measurement keys.


FAQ (Frequently Asked Questions):


What is the difference between pH and conductivity?
pH is a measurement of hydrogen ion concentration in a sample that is used to determine a compound's acidity or alkalinity, whereas electrical conductivity is a determination of the ions concentration present within a sample solution.

Is there a relationship between electrical conductivity and pH?
There is no relationship between the conductivity and pH, because pH is related to the number of hydrogen ions per molecule of an acid or base, while conductivity is dependent on free electrons. The presence of hydrogen ions in a substance will affect the pH level and, most likely, the conductivity levels.


You may also like this

Difference between spectrophotometry and colorimetry

The major difference between spectrophotometry and colorimetry is that the colorimeters use fixed wavelengths in the visible range (about 400–800 nm), whereas spectrophotometers use wavelengths in the UV/visible range (around 200–800 nm).


Spectrophotometers and colorimeters both are used to measure the absorption and transmittance of components based on their wavelength. The Tristimulus colorimeter has color filters and a light source which works on color sample only, whereas the spectrophotometer work with tungsten lamp, deuterium lamp, and monochromator for select the fixed wavelength as well as the range of UV/VIS.


What is spectrophotometry?

A spectrophotometer is an analytical device that measures the transmission or reflection of UV/visible/IR (infrared) light in a quantitative manner. The spectrophotometry measures the light intensity of a sample compound by passing a light beam through it. These apparatus are used to measure color and monitor color accuracy throughout the manufacturing process and different disciplines such as chemistry, biochemistry, physics, and molecular biology, etc.

Single and dual beam spectrophotometers are the two types of spectrophotometers. A single-beam spectrophotometer determines the absolute light intensity, whereas a double-beam spectrophotometer measures the ratio of light intensities on two independent light pathways, the reference standard, and the sample.

What is colorimetry?

A colorimeter is light-sensitive equipment that determines the amount of transmittance and absorbance of light that passes through a liquid sample. It measures the intensity or concentration of the color that emerges when a particular reagent is added to a solution.

The spectrophotometer and tristimulus colorimeter are the two types of colorimeters are used for color measurement. It determines the color intensity of the analyte and correlates it with the sample concentration. In colorimetry, the sample color is compared with the color of the standard in which the color is known.

Difference between spectrophotometry and colorimetry


Difference between spectrophotometer and colorimeter:

  • The basic difference between spectrophotometer and colorimeter is that spectrophotometry can use wavelengths from a wider range, while colorimetry uses fixed wavelengths that are only observable in the visible spectrum.
  • The light source in the spectrophotometer is a UV lamp (Tungsten, Xenon, and Deuterium) which works at wavelength, while the light source in colorimeter is LED which works at a fixed wavelength.
  • The particular wavelength is selected in a spectrophotometer by using a monochromator, while the particular wavelength is selected in colorimetry by using a color filter.
  • A spectrophotometer consists of a sensor, data processor, and a computer that gives data as per the given format, whereas a colorimeter typically consists of a sensor and a data processor.
  • The spectrophotometer can serve for research, development, and quality control, while the colorimeter is typically used for inspection and quality control purposes.
  • Spectrophotometry uses a wide range of wavelengths i.e., Ultraviolet and visible regions, whereas colorimetry uses a fixed wavelength in the visible range.
  • The obtained data of spectrophotometry indirectly provide psychophysical information, while the obtained colorimetric data provides tristimulus values.
  • Spectrophotometry is a more expensive and complex instrument than a colorimeter, while colorimetry is a robust and less expensive and complex instrument than a spectrophotometer.
  • The spectrophotometer can recognize the strength and metamerism of color, whereas the colorimeter cannot identify the strength and metamerism of color.
  • The spectrophotometer determines the amount of light, whereas the colorimeter determines the absorption of light that passes through a sample solution.
  • A spectrophotometer is more sensitive than a colorimeter, while a colorimeter is less sensitive than a spectrophotometer.
  • The approach of the spectrophotometer is a physical analysis, while the approach of colorimetry is psychophysical analysis.
  • A spectrophotometer measures color in human-visible light wavelengths, while a colorimeter measures the three major color components of light such as red, green, and blue.
  • In spectrophotometry, data is shown in a computer equipped with the appropriate software, while in colorimetry data is displayed on a digital or analog output.


FAQ (Frequently Asked Questions):


Which is better spectrophotometer or colorimeter?
The spectrophotometer is better than the colorimeter in terms of precision and adaptability. It is also better for more complicated color analysis because it can determine the spectral reflectance at each wavelength.

Is a colorimeter a spectrophotometer?
The colorimeter and spectrophotometer are similar as they are both used to measure the absorbance sample to determine analyte concentrations.


You may also like this

Saturday, October 16, 2021

Limit test for chlorides in sodium bicarbonate

Learn the limit test for chlorides in sodium bicarbonate through a laboratory experiment or practical.

Aim:

To perform the limit test for chlorides for the given sample and report its compliance /non-compliance with standards of I.P.

Sample: Sodium bicarbonate

Requirements:

Glasswares and miscellaneous: Nessler cylinders, measuring cylinder, pipette, pipette bulb, dropper, test-tube stand, glass rod, volumetric flask, and balance.
Chemicals: Sodium bicarbonate (NaHCO3), silver nitrate (AgNO3), nitric acid (HNO3), and sodium chloride (NaCl).

Principle:

We already discuss the principle of the limit test for chloride in the previous article. Click here to get the detailed reaction involved in this test.

Preparation of reagents:

Preparation of dilute HNO3:

Click here to get the procedure.

Preparation of 0.1M AgNO3:

Click here to get the procedure.

Preparation of 25 ppm standard NaCl solution:

Click here to get the procedure.


Procedure:

Standard opalescence:
  • Take 10.00 ml of 25 ppm chloride standard solution using a pipette into a Nessler cylinder and label it as standard.
  • Add 05.00 ml of water.
  • Add 10.00 mL of dilute HNO3 solution to the above preparation and dilute to 50 ml with water.
  • Then add 01.00 ml of prepared 0.1 M silver nitrate solution.
  • Stir immediately with a glass rod and let stand for five minutes by protecting from light.
  • Observe this standard preparation under a black background.

Test opalescence:

  • Take 01.20 gm of sodium bicarbonate into a Nessler cylinder and label it as a test.
  • Add 02.00 ml of dilute HNO3 solution to the above preparation and dilute to 50 ml with water.
  • Then add 01.00 ml of prepared 0.1 M silver nitrate solution.
  • Stir immediately with a glass rod and let stand for five minutes by protecting from light.
  • Observe this standard preparation under a black background.

Observations:

The test solution produces less or same or more opalescence than the standard solution.


Results:

The sample passes/fails the limit test as per Indian Pharmacopoeia.



FAQ (Frequently Asked Questions)


Which precipitate is obtained in the limit test for chloride?
The reaction of the Cl- with AgNO3 in the presence of weak HNO3 produces a silver chloride precipitate as a limit test for chloride.

Which acid is used in the limit test of chloride?
Nitric acid is used in the chloride limit test, which makes the solution acidic and aids silver chloride precipitation, which causes the solution to become turbid at the end of the process.

Which standard solution is used for the limit test of chloride?
Standard sodium chloride solution of specific concentration (PPM) is used for limit test of chloride.


Limit test for chlorides for water insoluble substances

Learn the limit test for chlorides for water-insoluble substances through a laboratory experiment or practical.

Aim:

To perform the limit test for chlorides for water insoluble activated charcoal

Sample: Activated charcoal

Requirements:

Glasswares and miscellaneous: Nessler cylinders, measuring cylinder, pipette, pipette bulb, dropper, test tube stand, glass rod, volumetric flask, and balance.
Chemicals: silver nitrate (AgNO3), nitric acid (HNO3), and sodium chloride (NaCl).

Principle:

The test opalescence produced by chloride impurities reacting with AgNO3 is compared to the standard opalescence produced by a known amount of chloride reacting with silver nitrate. If other impurities are present, a dilute HNO3 solution is used to dissolve them.

Limit test for chlorides for water insoluble substances

The precipitate formed is AgNO3 insoluble in dilute HNO3 solution and provides opalescence. The key objective here is to determine chloride impurities in charcoal rather than actual charcoal. Chloride salts are generally water-soluble. Chloride salt dissolves when charcoal is treated with H2O, however charcoal does not. As a result, the suspension filtrate is used for the limit test for chloride.

Preparation of reagents:

Preparation of dilute HNO3:

Take 10.60 ml of concentrated HNO3 using a pipette, dilute in 100 ml of distilled water in a volumetric flask, and properly mixing it.

Preparation of 0.1M AgNO3:

Take 17.00 gm of silver nitrate 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 with distilled water to 100 ml. Light-resistant containers should be used for storage.

Preparation of 0.0824% w/v standard NaCl solution:

Take 0.0824gm of sodium chloride 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 with distilled water to 100 ml.

Preparation of 25 ppm standard NaCl solution:

Take 05 volumes of 0.0824% w/v sodium chloride solution using a pipette and dilute to 100 volumes of distilled water in a volumetric flask.

Procedure:

Standard opalescence:
  • Take 10.00 ml of 25 ppm chloride standard solution using a pipette into a Nessler cylinder and label it as standard.
  • Add 05.00 ml of water.
  • Add 10.00 mL of dilute HNO3 solution to the above preparation and dilute to 50 ml with water.
  • Then add 01.00 ml of prepared 0.1 M silver nitrate solution.
  • Stir immediately with a glass rod and let stand for five minutes by protecting from light.
  • Observe this standard preparation under a black background.
Test opalescence:
  • Take 03.00 gm of activated charcoal in 75.00 ml distilled water, boil it for 5 minutes then cool.
  • Make up the volume with distilled water to 100 ml and filter.
  • Take 06.00 ml of the filtrate using a pipette into a Nessler cylinder and label it as a test.
  • Add 10.00 mL of dilute HNO3 solution to the above preparation and dilute to 50 ml with water.
  • Then add 01.00 ml of prepared 0.1 M silver nitrate solution.
  • Stir immediately with a glass rod and let stand for five minutes by protecting from light.
  • Observe this standard preparation under a black background.

Observations:

The test solution produces less or same or more opalescence than the standard solution.

Results:

The sample passes/fails the limit test as per Indian Pharmacopoeia.



FAQ (Frequently Asked Questions):


What is the inference for the chloride test?
When compared to a standard solution, the provided substance passes or fails the chloride limit.

Limit test of chloride is based on which reaction?
The chloride limit test is based on the reaction of soluble chloride with AgNO3 in the presence of dilute HNO3 to form AgNO3, which appears in the solution as solid particles.


Wednesday, October 13, 2021

Limit test for lead

Learn the limit test of lead through a laboratory experiment or practical.

Aim:

To perform the limit test for lead of the given samples.

Requirements:

Glasswares and miscellaneous:
Separating funnel, separating-flask ring, measuring cylinder, pipette, dropper, beaker, volumetric flask, rubber stopper, test tube, glass rod, and balance, etc.
Chemicals:
Ammonium citrate (C6H5+4yFexNyO7), ammonium cyanide(CH4N2), potassium cyanide (KCN), ammonia solution (NH4OH), hydroxylamine hydrochloride (HONH2·HCl), phenol red (C19H14O5S), nitric acid (HNO3), chloroform(CHCl3), and dithizone (C13H12N4S), etc.

Principle of limit test for lead:

The reaction of lead and diphenyl thiocabazone in an alkaline solution produces a lead dithizone complex, which has color-red.

Because dithizone is green in chloroform and the lead-dithizone complex is violet, the final color at the end of the process is red.

Preparation of chemicals:

Preparation of 0.1 % lead standard solution:

In a volumetric flask, dissolve 0.400 gm of lead nitrate in 250.00 ml of distilled water containing 02.00 ml of nitric acid, properly mixing it.

Preparation of 100 ppm lead standard solution:

Take 01 volume of 1% lead standard solution using a pipette and dilute to 10 volume of distilled water in a volumetric flask, and properly mixing it.

Preparation of 10 ppm lead standard solution:


Take 01 volume of 100 ppm lead standard solution using a pipette and dilute to 10 volume of distilled water in a volumetric flask, and properly mixing it.

Preparation of 01 ppm lead standard solution:

Take 01 volume of 10 ppm lead standard solution using a pipette and dilute to 10 volume of distilled water in a volumetric flask, and properly mixing it.

Preparation of 1% v/v nitric acid:

Take 01 volume of nitric acid using a pipette and dilute to 100 volume of distilled water in a volumetric flask, and properly mixing it.

Preparation of ammonium citrate solution:

Take 40.00 gm of citric acid in 90.00 ml of distilled water, add 2 drops phenol red solution, followed by gradual addition of strong ammonia solution until the solution turns a reddish color.

Remove any lead from the solution by extracting it with 30.00 ml increments of dithizone extraction solution until the dithizone solution retains its orange-green color.

Preparation of dithizone extraction solution:

Take 30.00 mg of dithizone in a 1-liter volumetric flask, add 05.00 ml of 95% ethanol, and make up the volume with chloroform. The solution should be kept in the refrigerator. Shake an appropriate volume of the solution with about half the volume of a 1 percent v/v HNO3 before using, and then discard the acid.

Preparation of dithizone standard solution:

Take 10.00 mg dithizone and dissolve to 1000 ml of distilled water in a volumetric flask, and properly mixing it.

Procedure of limit test for lead:

Standard:
  • Take the desired amount of lead standard solution in the separating funnel, which is equivalent to the amount of lead allowed in the substance being tested.
  • Add 06.00 ml of prepared ammonium citrate solution.
  • Add 02.00 ml hydroxylamine hydrochloride and 02.00 ml potassium cyanide.
  • Then add 2 drops of phenol red.
  • Add ammonia solution to make the solution alkaline.
  • Extract instantly with numerous volumes of dithizone extraction solution, each of 05.00 ml, until it becomes green.
  • Combine the dithizone extracts with 30.00 ml of nitric acid solution (1 % v/v), shake for 30 seconds, and discard the chloroform layer. (Dithizone remains in the layer of chloroform and lead nitrate is in the aqueous layer)
  • Add 05.00 ml of standard dithizone solution to this acid solution.
  • Add 04.00 ml of ammonium cyanide solution.
  • Shake well for a half-hour, and observe the color of the chloroform layer after separation.
Test:
  • Take the desired amount of sample in the separating funnel.
  • Add 06.00 ml of prepared ammonium citrate solution.
  • Add 02.00 ml hydroxylamine hydrochloride and 02.00 ml potassium cyanide.
  • Then add 2 drops of phenol red.
  • Add ammonia solution to make the solution alkaline.
  • Extract instantly with numerous volumes of dithizone extraction solution, each of 05.00 ml, until it becomes green.
  • Combine the dithizone extracts with 30.00 ml of nitric acid solution (1 % v/v), shake for 30 seconds, and discard the chloroform layer. (Dithizone is remains in the layer of chloroform and lead nitrate is in the aqueous layer)
  • Add 05.00 ml of standard dithizone solution to this acid solution.
  • Add 04.00 ml of ammonium cyanide solution.
  • Shake well for a half-hour, and observe the color of the chloroform layer after separation.

Observation:

Test color of the chloroform layer is more/not more intense than the standard color of the chloroform layer.

Results:

The given sample passes/fails the limit test for lead.


FAQ (Frequently Asked Questions):


What is the role of ammonium citrate, potassium cyanide, and hydroxylamine hydrochloride in the limit test for lead?
Ammonium citrate, potassium cyanide, and hydroxylamine hydrochloride are used to adjust the pH to the optimum, removing interference and effects of other impurities.

How many methods are there for the limit test of heavy metals?
The four different methods are used for the limit test of heavy metals; generally, it is based on the reaction of metallic impurities with H2S in an acidic medium to form a colored solution.

Why phenol red is used in the limit test for iron?
Phenol red is used as an indicator, which produces the color at the end of the process.