validation of volumetric solution 0.1m ammonium thiocyanate

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validation protocol for volumetric solution 0.1M ammonium Thiocyanate

1. Approval:

This document is prepared by the validation and the GMP compliance team
Under the authority of Quality Control Manager. Hence this document before being effective shall be
approved by QA team.

2. Purpose:

To establish documented evidence, on how the quality of a chemical substances or drug product varies with the time

under the influence of a variety of environmental factor such as Temperature, humidity and light during storage.

3. Scope:

This protocol provides a clear explanation of expectations when proposing a retest period or Shelf life and storage conditions

and outlines recommendations for establishing these from Single or multifactor and full reduced- design studies.

4. Reference :

Following documents are referred during preparation of the protocol

Document Name

Document Number

SOP for Volumetric Solution

5. Responsibility:

5.1 Execution:

Quality Control: Executive / Officer is responsible for analysis of physical and chemical Characteristic.

Manager QC: Verification & approval of results.

6. Validation Method:

VALIDATION OF VOLUMETRIC SOLUTION
PREPARATION AND STANDARDIZATION OF MOLAR SOLUTION
Name : ID. No .
STP No.:
Preparation:
Weigh accurately about 7.612g of Ammonium Thiocynate and transfer to a 1000ml volumetric flask. Dissolve in

sufficient purified water and make up to the mark with purified water.
OR
As per requirement (consumption history) prepare suitable amount of volumetric solution accordingly.
Standardization:
Pipette 30ml of 0.1M silver nitrate into a glass-stoperred flask, dilute with 50ml of purified water. Add 2ml of nitric acid

and 2ml of ferric ammonium sulphate solution and titrate with ammonium thiocynate solution until red-brown color appears.

Note down the volume of ammonium thiocynate solution consumed during titration. Repeat the procedure two more times.

Calculate the molarity of the solution by below given formula.
Each ml of 0.1M silver nitrate is equivalent to 0.007612g of NH4SCN

Determine the molarity in triplicate and calculate the average value where the variation is not more than 0.2%.
Preparation:
Weigh accurately about 7.612g of Ammonium Thiocynate and transfer to a 1000ml volumetric flask. Dissolve in sufficient

purified water and make up to the mark with purified water.
OR
As per requirement (consumption history) prepare suitable amount of volumetric solution accordingly.
Standardization:
Pipette 30ml of 0.1M silver nitrate into a glass-stoperred flask, dilute with 50ml of purified water. Add 2ml of nitric acid and

2ml of ferric ammonium sulphate solution and titrate with ammonium thiocynate solution until red-brown color appears.

Note down the volume of ammonium thiocynate solution consumed during titration. Repeat the procedure two more times.

Calculate the molarity of the solution by below given formula.
Each ml of 0.1M silver nitrate is equivalent to 0.007612g of NH4SCN

Validity: 30 day from the date of preparation and Re-Standardization after15 days.

Precaution – Check the physical appearance and fungal growth, sedimentation or change in color.

Storage: Store in glass bottles light-resistant containers. having well fitted, suitable stoppers.

7. Acceptance Criteria:
7.1 The volumetric solution of 0.1M Ammonium Thiocynate validity is 30 day from the date of preparation and

Re standardization every alternate days for validation and deviation should not be more then ±5.0%
7.2 Determine the molarity in triplicate and calculate the average value where the variation (precision) is not more

than 0.2%. This solution must be standardized frequently every month.

validation of volumetric solution molar solution calculation sheet

8. Result Reporting:
Calculation:

Variation (precision) is not more than 0.2%. =

9. Conclusion.
9.1 Normality of solution was found under acceptance criteria up to 35 days hence validity was define 30 days only
9.2 Solution shell be standardize every 15 days interval.
9.3 Solution must not be used after 30 days.
9.4 The validation exercise demonstrates that the Standardization of volumetric solution method of 0.1M Ammonium Thiocynate is stands validated.

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