SOP Title: Preparation and Standardisation of Volumetric Solutions
- Objective:
To lay down the procedure for Preparation and Standardisation of Volumetric Solutions.
- Scope:
This SOP is applicable for Preparation and Standardisation of Volumetric Solutions in Quality
Control Department.
- Responsibility:
- Quality Control Department: To prepare and review the SOP. To follow the procedures laid down for Preparation and Standardisation of Volumetric Solutions in Quality Control Department as per this SOP.
- Quality Assurance Department: To review and approve the SOP and Annexures.
- Accountability:
Head Quality Control Department, Head Quality Assurance Department
- Procedure:
| 5.1 | Procedure for Preparation of Volumetric Solutions: | |
| 5.1.1 | Always use personal protective equipments such as Hand gloves, nose masks, and goggles while preparing Volumetric Solutions. | |
| 5.1.2 | Use analytical grade reagents or highly purified salts for preparation of Volumetric Solutions. | |
| 5.1.3 | As per requirement, Volumetric Solutions should be prepared by accurately weighing a suitable quantity of defined chemical specified in respective Standard Testing Procedure or official monograph (IP, BP, and USP) and dissolving it in purified water/solvent to produce a specific concentration. | |
| 5.1.4 | A prior calculation is carried out to estimate the approximate weight of the Primary Standard required to make up the known volume of Volumetric Solution. | |
| 5.1.5 | Weigh accurately the specified quantity of Primary Standard on an electronic balance using a weighing bottle or butter paper. | |
| 5.1.6 | Transfer the solid to the volumetric flask and rinse the butter paper into the volumetric flask with specified solvent. | |
| 5.1.7 | Add specified volume of solvent to the flask and swirl the mixture until all of the solute dissolves and then dilute up to the mark. | |
| 5.1.8 | Invert and shake volumetric flask several times to thoroughly mix the contents.
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| 5.1.9 | Store all the Volumetric Solutions in clean and dry borosilicate glass bottles at room temperature or as specified in the respective Standard Testing Procedure or official pharmacopoeia. | |
| 5.1.10 | Volumetric Solutions which are light sensitive shall be preserved in amber coloured borosilicate glass bottles. | |
| 5.1.11 | Enter all the preparation details in “Volumetric Solution Preparation Record” |
| 5.1.12 | Allocate Reference Number for all the Volumetric Solutions prepared as: VS/ZZZ/XX/YY-NN
Where ‘VS’ stands for ‘Volumetric Solution’ ‘ZZZ’ stands for ‘Volumetric Solution Number as 001, 002’ ‘XX’ stands for ‘Reference Pharmacopeia i.e. IP, BP, USP, EP, IBU, BU, IU, IB or BU’ ‘YY’ stands for ‘Last two digits of the current year’ ‘NN’ stands for ‘Serial number of preparation’ |
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| 5.1.13 | Example: If 0.1 M Sodium Hydroxide which has Volumetric Solution number as VS/022 is prepared as per BP for the first time in the year 2024, then the reference number shall be VS/022/BP/24-01.
If the same solution is prepared for second time in the year 2024, then the reference number shall be VS/022/BP/24-02. |
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| 5.1.14 | If the Volumetric Solution preparation method is same in two or more Pharmacopoeias, then the Reference Pharmacopeia for the Volumetric Solution number shall be denoted by first letter of Pharmacopoeias used. | |
| 5.1.15 | Example: If the Volumetric Solution preparation method is same in IP, BP and USP, then the Reference Pharmacopeia for allocating the Volumetric Solution number shall be ‘IBU’ where ‘I’ stands for ‘IP’, ‘B’ stands for ‘BP’, ‘U’ stands for ‘USP’. | |
| 5.1.16 | All Volumetric Solutions bottles shall be labelled as “Volumetric Solution” indicating the name, concentration of the solution, date of preparation, signature of the person who prepared it, validity and storage conditions as per Annexure. | |
| 5.1.17 | Supervisor should verify that all the Volumetric Solutions are prepared as per STP or Pharmacopeia and check the “Volumetric Solution Preparation Record”.
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| 5.1.18 | All the Volumetric Solutions shall be kept on the racks of the working table provided in wet chemistry area. | |
| 5.1.19 | Unless otherwise specified, all the Volumetric Solutions should be used within one month from the date of preparation or earlier depending on the solution stability. | |
| 5.1.20 | Example: If 0.1 M Sodium hydroxide solution is prepared on 01/06/24, then the date of preparation shall be 01/06/24 and the validity shall be 30/06/24. | |
| 5.2 | Procedure for Standardisation of Volumetric Solutions: | |
| 5.2.1 | Volumetric Solutions shall be standardized by titration against a primary standard or by titration with a standard solution that has been recently standardized against a primary standard as per the method given in respective specification or pharmacopeia in triplicate. | |
| 5.2.2 | After use of Primary Standards, enter its usage in Primary Standard Receipt and Usage Record. | |
| Take the mean of three readings for reporting. | ||
| 5.2.3 | Acceptance Criteria:
1) The % RSD for three replicate readings should not be more than 0.2% 2) The actual concentration/ strength of the volumetric Solution should be within 10% of its theoretical value. |
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| Example: 1 M NaOH Solution has to be prepared then actual molarity should be within 0.9 M to 1.1 M | ||
| 5.2.4 | If any solution does not comply within above mentioned criteria then investigate the cause by filling incidence. Discard the solution if necessary and prepare fresh solution. | |
| 5.2.5 | Enter all the standardisation details in “Volumetric Solution Standardisation Record”. | |
| 5.2.6 | All Volumetric Solution Standardisation records shall be counter checked by second analyst or supervisor. | |
| 5.2.7 | All Volumetric Solution Standardisation | |
| 5.3 | Procedure to perform Solution Stability Study: | |
| To assign validity, solution stability study shall be performed every week up to 5 week or it can also be established based on the available historical data. | ||
| Procedure to perform Solution Stability Study Based on Real Time Data:-
Prepare three different standard solutions on three different days. Standardize these volumetric standard solutions every week up to 5 week. Record all the preparations and result as per Annexure; |
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| 1) If all three volumetric solutions are stable for 5 week as per given acceptance criteria then validity shall be assigned one month from the date of solution preparation.
2) If all three volumetric solutions are stable up to 4 week as per given acceptance criteria then validity shall be assigned 21 days from the date of solution preparation. 3) If all three volumetric solutions are stable up to 3 week as per given acceptance criteria then validity shall be assigned 15 days from the date of solution preparation. 4) If all three volumetric solutions are stable up to 2 week as per given acceptance criteria then validity shall be assigned 7 days from the date of solution preparation. 5) If all three volumetric solutions are stable up to 1 week as per given acceptance criteria then validity shall be assigned 3 days from the date of solution preparation. 6) If all three volumetric solutions are not stable up to 1 week as per given acceptance criteria then every time fresh solution shall be prepared and shall be used for analysis.
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| Procedure to Establish Solution Stability Study Based on Historical Data:-
For three different solutions prepared on three different days. Based on evaluation of data conclusion shall be made. |
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| Acceptance Criteria:
1) The % RSD for three replicate readings should not be more than 0.2% 2) The actual concentration/ strength of the volumetric Solution should be within 10% of its theoretical value. |
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| 5.2.8 | All the Volumetric Solutions that show evidence of deterioration, e.g. sedimentation, discoloration or crystallization, shall be discarded regardless of validity. Record for discard shall be recorded in Annexure. | |
| 5.2.9 | All the Volumetric Solutions shall be destroyed as per SOP “Destruction of Laboratory waste”. | |
- Definitions / Abbreviations :
- Definitions :
- Abbreviations :
| Abbreviation | Expansion |
| SOP | Standard Operating Procedure |
| QC | Quality Control |
| QA | Quality Assurance |
| STP | Standard Testing Procedure |
| No. | Number |
| % | Percentage |
| M | Molar |
*Note – Ready to use SOP available in “DOWNLOAD” Section.