laboratory. It ensures accuracy, consistency, and compliance with GMP and regulatory requirements.

2. Scope

This SOP applies to all analysts involved in preparing, handling, and using aqueous and non-aqueous reagents, buffer solutions, and volumetric titrants in the AMD laboratory of API and formulation development.

3. Responsibilities

• Analytical Chemist: Prepares and labels reagents and solutions as per SOP.
• Reviewer/Analyst II: Verifies preparation and standardization procedures.
• QA: Reviews records, audits preparation logs, and approves new titrant batches.
• Head – AMD: Ensures compliance with traceability, safety, and storage guidelines.

4. Accountability

The Head of AMD is accountable for ensuring all reagents and solutions are prepared as per approved procedures, verified for quality, and used within assigned validity periods.

5. Procedure

5.1 General Guidelines

1. Use only AR/LR grade chemicals and deionized water unless otherwise specified.
2. Use clean, dry glassware or calibrated volumetric flasks for solution preparation.
3. All preparations must be done under proper ventilation or fume hood (where required).

5.2 Preparation of Reagents

1. Calculate required weight/volume using stoichiometric formulas.
2. Dissolve solutes completely before making up the volume.
3. Label each container with:
   • Name of reagent
   • Concentration
   • Date of preparation
   • Use before date
   • Prepared by and checked by initials
4. Document all details in Annexure-1: Reagent Preparation Log.

5.3 Preparation of Volumetric Solutions

1. Prepare titrants such as NaOH, HCl, H₂SO₄ by:
   • Weighing or diluting stock solutions
   • Allowing to stand (e.g., NaOH for 24h) before standardization
2. Standardize using primary standards:
   • NaOH with potassium hydrogen phthalate (KHP)
   • HCl with sodium carbonate
3. Calculate normality using titration formula and record in Annexure-2: Volumetric Solution Standardization Record.

5.4 pH Buffer Preparation

1. Use freshly prepared solutions or commercially available certified buffers.
2. Calibrate pH meter daily using pH 4.01, 7.00, and 9.21 buffers before testing.

5.5 Storage and Validity

1. Assign validity based on reagent type:
   • Aqueous reagents: 1 month
   • Volumetric titrants: 1 week (unless stability is validated)
   • Non-aqueous reagents: up to 3 months
2. Store labeled containers in chemical cabinets away from heat and light.
3. Document inventory and disposal of expired reagents in Annexure-3: Reagent Usage and Disposal Register.

5.6 Safety and Hygiene

1. Wear PPE: gloves, goggles, lab coat during preparation.
2. Label all solutions with hazard symbols where applicable (acid, base, flammable).
3. In case of spill or exposure, refer to MSDS and report to QA.

6. Abbreviations

• AMD: Analytical Method Development
• AR: Analytical Reagent Grade
• LR: Laboratory Reagent Grade
• MSDS: Material Safety Data Sheet
• PPE: Personal Protective Equipment
• SOP: Standard Operating Procedure

7. Documents

1. Reagent Preparation Log – Annexure-1
2. Volumetric Solution Standardization Record – Annexure-2
3. Reagent Usage and Disposal Register – Annexure-3

8. References

• USP General Chapters <821>, <1225>, <1226>
• ICH Q2(R1) – Validation of Analytical Procedures
• WHO TRS 970 Annex 2 – Quality Risk Management
• 21 CFR Part 211 – Subpart I: Laboratory Controls

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Reagent Preparation Log

Date	Reagent Name	Concentration	Prepared By	Checked By	Use Before
02/05/2025	Ammonia Solution	10% v/v	Ajay Verma	Sunita Reddy	02/06/2025

Annexure-2: Volumetric Solution Standardization Record

Date	Titrant	Primary Standard	Volume Used	Normality	Checked By
03/05/2025	NaOH	KHP	25.00 mL	0.0998 N	QA Officer

Annexure-3: Reagent Usage and Disposal Register

Date	Reagent	Used In	Disposed By	Remarks
10/05/2025	Sulfuric Acid	Titration (Lot 002)	Rajesh Kumar	Expired – neutralized and discarded

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
04/05/2025	2.0	Added standardization and safety sections with updated annexures	Audit Observation