SHINIL Pharma Ltd.

B K Bari, Mirzapur, Gazipur.

Standard Test Procedure (Active Ingredient)

Material Name Ammonium Bicarbonate BP Material Code RA- A02
Revision No. 01 STP No. STP-RA-A02
Effective Date July 05, 2021 Review Date July 04, 2024

1.0 APPEARANCE :
Take 1 g of test sample in a watch glass and observe visually with white background.
2.0 IDENTIFICATION :
A. Bicarbonates
i) Introduce into a test tube 0.1 g of the substance being examined suspended in 2 ml of water or
use 2 ml of the prescribed solution. Add 3 ml of 2M acetic acid, close the tube immediately using a
stopper fitted with a glass tube bent at two right angles. The solution or suspension effervesces. Heat
gently and collect the gas in 5 ml of a 4.73% w/v solution of barium hydroxide. A white precipitate is
produced which dissolves on addition of an excess of 7M hydrochloric acid.

ii) Treat a solution of the substance being examined with a solution of magnesium sulfate; no
precipitate is produced (distinction from carbonates). Boil; a white precipitate is produced.

iii) A solution liberates carbon dioxide when boiled.

B. Ammonium Salts
To the prescribed solution add 0.2 g of magnesium oxide R. Pass a current of air through the mixture
and direct the gas that escapes just beneath the surface of a mixture of 1 ml of 0.1 M hydrochloric
acid and 0.05 ml of methyl red solution R. The colour of the indicator changes to yellow. On addition
of 1 ml of a freshly prepared 100 g/L solution of sodium cobaltinitrite a yellow precipitate is formed.
3.0 SOLUBILITY :
Take 1.0 g and 10 mg of test sample in two different test tubes. Add 10 ml of water and 100 ml of
ethanol (96 %) into these test tubes respectively. Shake properly.

4.0 APPEARANCE OF SOLUTION :

Solution S

Dissolve 14.0 g in 100 ml of distilled water R. Boil to remove the ammonia, allow to cool and dilute to
100.0 ml with distilled water.
Procedure:
Using Identical tubes of colorless, transparent, neutral glass with a flat base and an internal diameter
of 15 mm to 25 mm, compare the solution to examine with water.
5.0 CHLORIDES :
Dilute 5 ml of solution S to 15 ml with water.
To 15 ml of the prescribed solution add 1 ml of dilute nitric acid and pour the mixture as a single
addition into a test-tube containing 1 ml of silver nitrate solution. Prepare a standard in the same
manner using 10 ml of chloride standard solution (70 ppm Cl) R and 5 ml of water. Examine the tubes
laterally against a black background.

Prepared By Checked By Approved By

Md. Rasheduzzaman Bejoy Karim Md. Mahabub Alam

Officer, Quality Control Senior Officer, PD Manager, Quality Assurance
Page no. 1 of 2
 SHINIL Pharma Ltd.
B K Bari, Mirzapur, Gazipur.

Standard Test Procedure (Active Ingredient)

Material Name Ammonium Bicarbonate BP Material Code RA- A02
Revision No. 01 STP No. STP-RA-A02
Effective Date July 05, 2021 Review Date July 04, 2024
After standing for 5 min protected from light, any opalescence in the test solution is not more intense
than that in the standard.
6.0 SULFATES:
Determined on solution S. All solutions used for this test must be prepared with distilled water.

Add 3 ml of a 250 g/L solution of barium chloride to 4.5 ml of sulfate standard solution (70 ppm SO4).
Shake and allow to stand for 1 min. To 2.5 ml of this suspension, add 15 ml of the solution to be
examined and 0.5 ml of acetic acid. Prepare a standard in the same manner using 15 ml of sulfate
standard solution (70 ppm SO4) instead of the solution to be examined.

After 5 min, any opalescence in the test solution is not more intense than that in the standard.
7.0 IRON:
Dissolve the prescribed quantity of the substance to be examined in water and dilute to 10 ml with the
same solvent or use 10 ml of the prescribed solution. Add 2 ml of a 200 g/L solution of citric acid and
0.1 ml of thioglycollic acid. Mix, make alkaline with ammonia and dilute to 20 ml with water. Prepare a
standard in the same manner, using 10 ml of iron standard solution (40 ppm Fe).

After 5 min, any pink colour in the test solution is not more intense than that in the standard.

8.0 ASSAY :

Dissolve cautiously 0.500 g in 50.0 ml of carbon dioxide-free water R. Titrate with 1.0 M hydrochloric
acid, Determining the end-point potentiometrically using 0.1 ml of methyl red solution as indicator.

1 ml of 1.0 M hydrochloric acid is equivalent to 79.1 mg of NH4HCO3.

Calculation :

V X F X 79.1 X 100
Result = = % (As it is)
Wu
Here,
V = Volume required for titration
F = Factor of 0.1 M Sodium Hydroxide solution
Wu = Sample weight taken in mg

List of Distribution
1) Quality Assurance
2) Product Development
3) Quality Control
4) Commercial
Prepared By Checked By Approved By

Md. Rasheduzzaman Bejoy Karim Md. Mahabub Alam

Officer, Quality Control Senior Officer, PD Manager, Quality Assurance
Page no. 2 of 2