Standard Operating Procedure for Preparation, Standardization and Stability of Volumetric Solution

1.0 Purpose:

To lay down a procedure for Preparation, Standardization and Stability of Volumetric Solution.

2.0 Scope:

The scope of this SOP is to provide a procedure for Preparation, Standardization and Stability of Volumetric Solution in quality control department at [Company name].

3.0 Responsibility:

3.1 QC-Personnel:

– Prepare and standardize the volumetric solution.

– To Evaluate Stability of Volumetric Solution.

3.2 Section Head QC/ Designee: To review the report.

3.3 Head QC/ Designee:

– To approve the report.

– Ensure the compliance of SOP.

4.0 Definitions:

Not applicable

5.0 Procedure:

5.1 Use purified water for preparation of volumetric solution.

5.2 Use calibrated glassware and balance.

5.3 Analytical Research (AR) Grade or Guaranteed Reagent (GR) grade reagents shall be used for preparation.

5.4 Separate Molarity/ Normality register shall be prepared for IP, BP, USP, EP & IH volumetric solutions.

5.5 If any precipitation is found in volumetric solution during the validity period, the solution should be discarded and freshly prepared solution shall be used.

5.6 Always use cleaned and dried glassware for dispensing of volumetric solution.

5.7 The Volumetric Solution should be stored at 25 ± 2°C temperature.

5.8 Volumetric solution shall be used up to its validity date i.e., 15 days from the date of preparation, after which it shall be discarded in the running tap water.

5.9 Freshly prepared solution shall be used in case of Stability Evaluation.

5.10 Use freshly prepared solution for standardization.

5.11 The solution shall be prepared as per respective Pharmacopoeia or as specified in specification.

5.12 Preparation of volumetric solution:

– Use purified water for preparation of volumetric solution which complies as per requirement of specification of Purified water.

– Print the Worksheet from LIMS for required volumetric solution preparation..

– Prepare volumetric solution according to the respective Pharmacopoeia and fill data in worksheet.

– Numbering system for volumetric solution is VS/IP/00X, VS/BP/00X, VS/USP/00X, VS/EP/00X and VS/IH/00X.

Where, X – Denotes serial number 1, 2, 3…. etc for respective volumetric solution.

– Volumetric solution preparation number to be generated in the following manner.

XXX…YYZZZZZ

Where,

XXX… = Prefix given for VS name during registration.

Note:  Number of Characters may be very upon strength and Pharmacopoeia status.

YY= Last two digits of VS preparation year.

ZZZZZ= VS preparation serial number for each volumetric solution.

– Volumetric solution preparation will be approved by Head QC.

– After preparation of volumetric solution store the solution in a glass stoppered bottle and as specially specified in procedure.

– Label the bottle as per respective format in which volumetric solution kept.

– Enter the details in Molarity/ Normality register as per respective format.

5.13 Volumetric solution standardization:

– Print the worksheet from LIMS for Volumetric solution standardization.

– Carry out the standardization of volumetric solution with reference document number, VS/IP/00X, VS/BP/00X, VS/USP/00X, VS/EP/00X and VS/IH/00X.

Where, X – Denotes serial number 1, 2, 3…. etc for respective volumetric solution.

– Standardize the solutions using primary standards of high purity. Store the primary standards in a desiccator designated for the purpose with a silica gel in bottom.

– Before standardization mix the solution carefully.

– Carry out the standardization in triplicate.

– Record the observations during standardization in work sheet print out taken.

– Document the Batch No. of reagent indicators and primary standard or the value for reference volumetric solution number of equinormal or equimolar solution used in standardization in respective record.

– The result will be calculated for each set of values provided and the final values are displayed against the respective parameters.

– Volumetric solutions should not differ from the prescribed strength by more than ± 5 % (95 to 105 % of its prescribed strength) and the molarity is determined with a relative standard deviation of 0.2 %.

– The final decision Pass or Fail will be based on the acceptance criteria.

– Standardization results will be approved by Supervisor / Manager – QC.

– Enter the details in Molarity/ Normality log.

– Discard the solution after validity period in running tap water.

5.14 Usage of Volumetric solution: For using the volumetric solution usage, enter the details LIMS.

5.15 Preparation & Maintenance of Molarity/ Normality Register:

– Prepare the index of all the volumetric solution on the first page of register.

– Refer the method of preparation, standardization and calculations for each volumetric solution.

– Prepare a table on second page of every solution giving details as per respective format.

– Attach the balance printout with analytical protocol.

5.16 Stability of Volumetric Solution:

– After preparation the Volumetric Solution shall be stored in a stoppered clear or amber coloured bottle as per respective Pharmacopoeia or as per specified in specification. Label the bottle properly.

– Standardization of Volumetric Solution shall be done as per the procedure given in the respective standard analytical procedure or pharmacopoeia.

– Standardization shall be carried out in triplicate each time. Find out the % RSD. It should not be more than 0.2 %.

– In case new Volumetric Solution is prepared, it shall be Standardize initially (before use) and in the interval of 5 days up to 15 days to check / evaluate the validity / stability of the Volumetric Solution. In case the new volumetric solution is prepared with different concentration (Normality) stability of volumetric solution is established.

– Volumetric solutions which are light sensitive, solution stability is not performed.

– Find out the % of all observations. It should be between 98.0 to 102.0 % of its actual first-time determined strength.

5.16.7 Record the observation in the Format (Refer details in respective format).

6.0 Acceptance Criteria:

6.1 Standardization:

– Volumetric solutions should not differ from its prescribed strength by more than ± 5 % (95 % to 105 % of its prescribed strength).

– Molarity or Normality is determined with a relative standard deviation of 0.2 %.

6.2 Volumetric Solution Stability:

– All observations (interval of five days – for four times) should be between 98.0 % to 102.0 % of it’s actual first-time determined strength, considering initial value as 100 %.

– % RSD of for all observations (interval of five days – for four times) should be within NMT 0.2%.

7.0 Frequency:

7.1 Volumetric solutions, which have a stability data, should be standardizing as per frequency given in respective volumetric solution’s methods in register.

7.2 In absence of stability data standardize the volumetric solution before use.

7.3 As and when stability evaluation of new Volumetric Solution is required.

8.0 Format for recording:

– Format for Preparation and Standardization with Primary standard.

– Format for Preparation and Standardization without Primary standard.

– Format for Volumetric solution Label.

– Format for Water content Determination in Perchloric acid.

– Format for Standardization of Perchloric acid.

– Format for Stability of Volumetric Solution.

8.1 Format for Preparation and Standardization with Primary standard

Sr. No.

Date of Preparation

Manufacturer Batch No. of solute

Wt. of solute Qty. Prepared

A.R. No. of Purified water for Preparation

Prepared By / Date

Manufacturer Of Primary Std.

Date of standardization

Batch No. of Primary std.

Wt. of Primary standard

Burette Reading

Molarity / Normality

Mean Molarity / Normality

% RSD (NMT 0.2 %)

Valid up to

Batch No.

Standardized by Checked By

8.2 Format for Preparation and Standardization without Primary standard.

Sr. No.

Date of Preparation

Manufacturer Batch No. of solute

Wt. of solute Qty. Prepared

A.R. No. of Purified water for Preparation

Prepared By / Date

Date of standardization Volume Taken

Molarity / Normality of

Burette Reading

Molarity / Normality

Mean Molarity / Normality

% RSD (NMT 0.2 %)

Valid up to

Batch No.

Standardized by

Checked By

8.3 Lable – Standardization of Volumetric Solution

Solution :

Strength :

Storage Condition :

Batch No.:

Date of Prep.

Date of Stand.

Molarity

Valid up to

Analyst

8.4 Format for Water content Determination in Perchloric acid.

Sr. No.

Date of Preparation

Weight of Disodium Tartrate

Batch No. of Disodium Tartrate

Manufacturer and Batch No. of Karl Fischer Reagent

Burette Reading Factor (mg/ml)

Mean Factor

% RSD (NMT 1.5 %)

Weight of Sample Burette Reading

% Water (0.02 To 0.05 %)

Analyzed By

Checked By

8.5 Format for Standardization of Perchloric acid.

Sr. No.

% Water Content

Opening Date

Manufacturer and Batch No. of 0.1 N Perchloric acid

Date of Standardization

Manufacturer of Primary Standard

Batch No. of Primary Standard

Wt. of Primary standard

Blank Reading

Burette Reading

Difference Molarity / Normality

Mean Molarity / Normality

% RSD

Valid up to [15 Days]

Batch No.

Standardized by

Checked By

8.6 Format for “Stability of Volumetric Solution”