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 3
 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 HEAVY METALS :

Dissolve cautiously 2.5 g in 25 mL of 1 M hydrochloric acid. 12 mL of the solution complies with test A.
Prepare the reference solution using lead standard solution (10 ppm Pb).
Reagents:
1) Acetate Buffer pH 3.5 (Buffer solution pH 3.5): Dissolve 25 g of ammonium acetate in 25 ml of
water and add 38 ml of 7M hydrochloric acid. Adjust the pH to 3.5 with either 2M hydrochloric acid or
6M ammonia and dilute to 100 ml with water.
2.Thioacetamide Reagent: Add 1 ml of a mixture of 15 ml of 1M sodium hydroxide, 5 ml of water and
20 ml of glycerol (85%) to 0.2 ml of thioacetamide solution, heat in a water bath for 20 seconds, cool
and use immediately.
3) Lead Standard Solution (0.1% Pb): Dissolve 0.400 g of lead (II) nitrate in sufficient water to
produce 250.0 ml.
4) Lead Standard Solution (100 ppm Pb): Dilute 1 volume of lead standard solution (0.1% Pb) to 10
volumes with water immediately before use.
5) Lead Standard Solution (10 ppm Pb): Dilute 1 volume of lead standard solution (100 ppm Pb) to
10 volumes with water immediately before use.
6) Lead Standard Solution (1 ppm Pb): Dilute 1 volume of lead standard solution (10 ppm Pb) to 10
volumes with water immediately before use.
Test Solution: Dissolve 2.0 g a mixture of 2 ml of hydrochloric acid and 18 ml of water in carbon
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 3
 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
dioxide-free water. Take 12 ml of this solution to be complies with following limit test for heavy metals.
Reference Solution (Standard): A mixture of 10 ml of lead standard solution (1 ppm pb) or lead
standard solution (2 ppm pb) as prescribed and 2 ml of the prescribed aqueous solution of the
substance to be examined.
Blank Solution: A mixture of 10 ml of water and 2 ml of solution to be examined.
To each solution, add 2 ml of buffer solution pH 3.5. Mix and add to 1.2 ml of thioacetamide
reagent .Mix immediately. Examine the solutions after 2 min.
System Suitability: The reference solution shows a slight brown colour compared to the blank
solution.
Result: Any brown color in the test solution is not more intense than that in the reference solution.

9.0 ASSAY :
Dissolve cautiously 1.0 g in 20.0 mL of 0.5 M sulfuric acid and dilute to 50 mL with water R. Boil, cool
and titrate the excess of acid with 1.0 M sodium hydroxide, using 0.1 mL of methyl red solution as
indicator.

1 mL of 1.0 M sodium hydroxide is equivalent to 79.1 mg of NH4HCO3.

Calculation :
Vol. of 0.5 M sulfuric acid (20 ml) x Factor of 0.5 M sulfuric acid solution = A ml
Vol. of 1.0 M sodium hydroxide x Factor of 1.0 M sodium hydroxide = B ml

(A-B) X 79.1 X100

Result = = % (As it is)
Sample weight taken (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. 3 of 3