STP and analysis method of Ammonium Chloride

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STP and analysis method of Ammonium Chloride

Storage Requirements:
Store protected from light and moisture.
Sampling:
Sample equal quantity from each container / bag. Collect a minimum of 5g from each container/bag sample into individual, self –sealing clear polythene bag kept in another clear self sealing polythene bag bearing ‘Sample for Analysis, label. After completion of sampling return rest sample on same container. Collect control sample in Pet Bottle/Glass Bottle.
Quantity of Composite Sample:
10 g
Quantity of individual Identification
0.0100 g from each and every container /bag.
Quantity of Control Sample:
2 X 10 g

Description: Colourless crystals or a white, crystalline powder.

Solubility: Freely soluble in water, sparingly soluble in ethanol (95%).

Identification: It’s gives the reactions of ammonium salts and of chlorides.

pH: 4.5 to 6.0.

Arsenic: Not more than 4 ppm.

Heavy Metals: Not more than 10 ppm

Iron: Not more than 20 ppm

Calcium: Not more than 200 ppm

Sulphate: Not more than 150 ppm

Thyocyanate: No red colour produced.

Sulphated Ash: Not more than 0.1%w/w

Loss on Drying: Not more than 1.0%w/w

Assay: 99.0 % to 100.5 %w/w on dried basis.

Description: Colourless crystals or a white, crystalline powder
Reporting: Report as Complies/Does not comply.
Solubility: Freely soluble in water, sparingly soluble in ethanol (95%).
Reporting: Report as Complies/Does not comply.
Identification: It’s gives the reactions of ammonium salts and of chlorides.
For Ammonium salts
Heat a few mg of the substance under examination with sodium hydroxide solution; ammonia is evolved, which is
recognisable by its odour and by its action on moist red litmus paper, which turns blue.
Reporting: Report as Complies/Does not comply.
For Chlorides:
Dissolve a quantity of the substance under examination equivalent to about 2 mg of chloride ion in 2 ml of water or use
2 ml of the prescribed solution. Acidify with dilute nitric acid, add 0.5 ml of silver nitrate solution, shake and allow to stand; a curdy white precipitate is formed, which is insoluble in nitric acid but soluble, after being well washed with water, in dilute ammonia solution, from which it is reprecipitated by the addition of dilute nitric acid.
Reporting: Report as Complies/Does not comply.
Appearance of solution: A 10.0 per cent solution is clear and colourless.
Reporting: Report as Complies/Does not comply.
pH: Determined in a 5.0 per cent solution.
Reporting: Report as Complies/Does not comply.
Arsenic: Dissolve 2.5 g in 50 ml of water and add 10ml of stannated hydrochloric acid. The resulting solution complies
with the limit test for arsenic (4 ppm).
Procedure: Into the bottle or conical flask introduce the test solution prepared, dissolve 2.5 g add 5 ml of 1 M potassium iodide and 10 g of zinc AsT. Immediately assemble the apparatus and immerse the flask in a water-bath at a temperature such that a uniform evolution of gas is maintained. After 40 minutes any stain produced on the mercuric chloride paper is not more intense than that obtained by treating in the same manner 1.0 ml of arsenic standard solution (10 ppm As) diluted to 50 ml with water.
Reporting: Report as value.

Heavy Metals: 2.0 g complies with the limit test for heavy metals.
Standard solution: Into a 50-ml Nessler cylinder pipette 1.0 ml of lead standard solution (20 ppm Pb) and dilute with water to 25 ml. Adjust with dilute acetic acid or dilute ammonia solution to a pH between 3.0 and 4.0, dilute with water to about 35 ml and mix.
Test solution: Into a 50-ml Nessler cylinder place 25 ml of the solution prepared for the test 2.0g dissolve of the substance under examination in sufficient water to produce 25 ml. Adjust with dilute acetic acid or dilute ammonia solution to a pH between 3.0 and 4.0, dilute with water to about 35 ml and mix.
Procedure: To each of the cylinders containing the standard solution and test solution respectively add 10 ml of freshly prepared hydrogen sulphide solution, mix, dilute to 50 ml with water, allow to stand for 5 minutes and view downwards over a white surface; the colour produced with the test solution is not more intense than that produced with the standard solution.
Reporting: Report as value.
Iron: 2.0 g complies with the limit test for iron (20 ppm).
Procedure: Dissolve 2.0g of the substance under examination in water and transfer to a Nessler cylinder. Add 2 ml of a 20 per cent w/v solution of iron-free citric acid and 0.1 ml of thioglycollic acid, mix, make alkaline with iron-free ammonia solution, dilute to 50 ml with water and allow to stand for 5 minutes. Any colour produced is not more intense than that obtained by treating in the same manner 2.0 ml of iron standard solution (20 ppm Fe) in place of the solution under examination.
Reporting: Report as value.
Calcium: To 0.2 ml of ethanolic calcium standard solution (100 ppm Ca) add 1 ml of a 4 per cent w/v solution of ammonium oxalate. After 1 minute add 1ml of2M acetic acid and 15 ml of a solution made by diluting 5 ml of a 10 per cent solution of the substance under examination with 10 ml of water and shake. Compare any opalescence produced with that of a standard prepared in a similar manner but using a mixture of 10 ml of calcium standard solution (10 ppm Ca)and 5 ml of water instead of the solution of the substance under examination (200 ppm).
Reporting: Report as Complies/Does not comply.
Sulphates: 1.0 g complies with the limit test for sulphates (150 ppm).
Procedure: To 1.0 ml of a 25.0 per cent w/v solution of barium chloride in a Nessler cylinder add 1.5 ml of ethanolic sulphate standard solution (10 ppm SO4 ), mix and allow to stand for 1 minute. Add 15 ml of the solution prepared 1.0g of the substance under examination in 15 ml of water and 0.15 ml of 5 M acetic acid. Add sufficient water to produce 50 ml, stir immediately with a glass rod and allow to stand for 5 minutes. When viewed transversely against a black background any opalescence produced is not more intense than that obtained by treating in the same manner 15 ml of sulphate standard solution (10 ppm S04) in place of the solution under examination.
Reporting: Report as value.

Thiocyanate: Acidify 10 ml of a 10 per cent w/v solution with hydrochloric acid and add a few drops of ferric chloride solution; no red colour is produced.
Reporting: Report as Complies/Does not comply.
Sulphated ash: Not more than 0.1 percent.
Procedure: Heat a crucible to redness for 10 minutes; allow cooling in a desiccator and weighing. Transfer to the crucible 1 g of the substance under examination and weigh the crucible and the contents accurately. Ignite, gently at first, until the substance is thoroughly charred. Cool, moisten the residue with 1 ml of sulphuric acid, heat gently until the white fumes are no longer evolved and ignite at 800° ± 25° until all black particles. have disappeared. Conduct the ignition in a place
protected from air currents. Allow the crucible to cool, add a few drops of sulphuric acid and heat. Ignite as before, allow to cool and weigh. Repeat the operation until two successive weighing do not differ by more than 0.5 mg.
Reporting: Report as value in %.
Loss on drying: Not more than 1.0 percent determined on 1.0 g by drying in an oven at l05°.
Reporting: Report as value in %.
Assay: Weigh accurately about 0.1 g, dissolve in 20 ml of water and add a mixture of 5 ml of formaldehyde solution, previously neutralised to dilute phenolphthalein solution and 20 ml of water. After 2 minutes, titrate slowly with 0.1 M sodium hydroxide using a further 0.2 ml of dilute phenolphthalein solution as indicator.
1ml of0.1 M sodium hydroxide is equivalent to 0.005349 g of NH4Cl.
Calculation: