PURIFIED WATER SYSTEM
Raw Water sourced from Borewell is converted into purified water complying with current USP/ BP/ IP/ Ph.Eur. This water is chlorinated by Sodium Hypochlorite Solution (NaOCl) to maintain residual free chlorine. Dosing is done using an electronic metering pump. Chlorinated water is stored in an underground tank and from the tank it is pumped to pass through a Multi Grade Filter (MGF) for removal of suspended solids. A sodium meta-bisulphite (SMBS) dosing system is provided on the outlet discharge pipe of MGF to remove the residual chlorine. Water after de-chlorination is stored storage tank. Water from this tank is pumped to distribute in two loops:
- Feed to the soft water plant
- Treated water distribution
The filtered water then is passed through a softener to reduce Hardness. Softened water is further treated to generate high-purity water as per current USP/ BP/ IP/ Ph. Eur. standards for purified water.
Soft water from the softener is stored in an HDPE storage tank. Soft water from this tank is supplied to different utilities such as Boilers, Cooling towers; Chillers hot water make-up tanks of HVAC and Purified water generation plants. Soft water will be stored in the feed water tank to the RO.
Soft water from softener may form scaling in Reverse Osmosis (RO) membranes, to avoid that special anti-scalant is added to the soft water. the pH of the water is maintained at 7.5-8.5 at the inlet of the Reverse Osmosis unit through the pH correction dosing system
Soft water is further passed through single-stage SDI filtration (with a filter of 5µ) before pumping into the Purified Water Generation System (consisting of RO and EDI units). For protecting the RO membrane in case of accidental entry of free chlorine water ORP meter is installed in the RO feed water. As soon as the ORP meter senses the free chlorine it will trip the system and open the flow divert valve to avoid damage to the RO membrane.
Purified water is stored in an SS Storage Tank Assembly and is distributed through a loop system to various sections. Before final distribution, the purified water is passed through UF/UV purifiers.
PERFORMANCE QUALIFICATION PROTOCOL
OBJECTIVE: To describe the Performance Qualification procedure to be used during the validation of the purified water system to:
a) Ensure the system’s reproducibility over an appropriate period as per user requirement specifications.
b) Ensure that the system is showing consistency in producing water of pre-established specifications.
SCOPE: This procedure applies to the Performance Qualification or Validation of Purified Water System.
RESPONSIBILITY: The validation team shall be responsible for the preparation and checking of the Performance Qualification/Validation protocol.
The Plant Head, quality control & quality assurance shall be responsible for the approval of the Performance Qualification/ Validation protocol.
Head -Quality Control shall be responsible for facilitating the analysis of water samples, evaluations of the test results and compilation of validation data.
Head -Quality Assurance shall be responsible for approval of the Performance Qualification / Validation Report and certification after successful validation of the purified water system
ABBREVIATIONS AND DEFINITIONS
PQ: Performance Qualification; documented verification that the integrated system or subsystem functions as intended, in its normal operating environment.
DQ: Design Qualification.
IQ:Installation Qualification.
OQ: Operational Qualification
Validation Team: Trained representatives from Quality Assurance, Quality Control, Engineering and Production departments participating in validation. For water system validation, the validation team members shall enlist their names & signatures as per Annexure-8
HVAC: Heating, Ventilation and Air-Conditioning
UV: Ultra Violet
TOC: Total Organic Carbon
EDI:Electrodeionization
SDI: Silt Density Index
HDPE: High-Density Polyethylene
PRE-REQUISITES: Before validating the Water system following should be ensured:
- Successful completion of Operational Qualification of Water System as per Protocol
- Availability of Test Protocols for testing water produced at different stages
- Availability of the following Draft SOP(s)
- Operation and Regeneration of MGF & soft water plant, etc
- Operation of the purified water system
- Sanitization (purified water generation system & Distribution system)
- Water Sampling (also describing sampling micro testing)
- Availability of all the relevant Log books of the water system
QUALIFICATION/ VALIDATION PROCEDURE
Qualification/ Validation Strategy : This Validation Study shall be executed in three phases:
- Phase- 1
- Phase – 2
- Phase – 3
Phase- 1: Phase-1 shall last for a minimum of two (2) weeks or unless water of every stage meets the specifications during which preliminary sampling of water shall be done to ensure that the system is ready to go into Phase- 2, the prospective phase of validation. (refer to sampling and testing plan for Phase-1 & Phase-2), During this phase operating, regeneration and sanitization procedures shall be verified & frequencies for sanitization shall be established and fixed.
On completion of Phase 1, a report (Annexure-7) shall be prepared and it shall be checked and approved for further proceeding to Phase 2.
In case there is any deviation in Phase-1, corrective action shall be taken and after corrective action (recording shall be done as per Annexure-4), validation activity shall be continued. Based on Phase-1 data Alert and Action levels for key quality attributes like TOC, Conductivity and Microbial Count shall be established. Criteria for taking alert limit and action limit shall be as follows:
Alert limit = Average Value + 2σ
Action limit = Average Value + 3σ
After Phase-1, sampling shall be continued till the approval of the Phase-1 report as per the Phase-1 schedule and their respective data shall be incorporated in the Phase-2 report.
Phase-2: Phase-2 shall last for Four (4) weeks with sampling frequency similar to Phase-1. (refer to sampling and testing plan for Phase-1 & Phase-2)
This phase shall demonstrate the system consistency concerning desired water quality when operated after sanitization in conformance with SOP(s). During this phase, Alert and Action levels for key quality attributes like TOC, Conductivity and Microbial Count shall be verified. In case there is any deviation in Phase-2, corrective action shall be taken and after correction action (recording shall be done as per Annexure-4)
The purified water system shall be cleared for the production after successful completion of Phase 2
A report (Annexure-7) shall be prepared after the completion of the Phase-2 study
Phase-3: Phase-3 shall last for about eleven (11) months with each sampling point being covered every week (refer to sampling and testing plan for Phase-3), In this concurrent phase of validation, routine monitoring shall be conducted and seasonal variation shall be studied. Scheduled preventive maintenance shall be finalized at this phase of water system validation. A schedule for periodic review of the system performance and re-qualification or revalidation shall also be instituted after the completion of this phase. A report (Annexure 7) shall be prepared after completion of the Phase-3 study. Trending of data shall be done.
The water system shall be evaluated at the following stages through various sampling points and user points:
- Raw water (Stage 1)
- Raw Water after Chlorination (Stage 2)
- Dechlorinated Water after MGF treatment (Stage 3)
- Soft Water after Softener (Stage 4)
- Soft Water after 5-micron filter [Feed water to Purified Water Generation System consisting of Reverse Osmosis (RO) and Electrodeionization (EDI) units] (Stage-5)
- Water after RO treatment (Stage-6 & 7)
- Water after EDI treatment (Stage 8)
- Water after Ultrafiltration (Stage-9)
- Purified Water from a Purified Water Storage Tank (Stage 10)
- Purified water Return from Distribution loop/UV lamp (Stage-11)
- Purified water from all user points (Stage-11)
Description of Sampling Points: The following sampling points shall be defined for validation and monitoring of the purified water system and its distribution during validation through three phases
| S.No | Sampling Point Description | Code |
| 1 | Raw Water (Bore well) | S-1 |
| 2 | MGF-001 Inlet (Multi-grade filter) | S-2 |
| 3 | Dechlorinated Water Storage Tank | S-3 |
| 4 | ISFD-001 Outlet (Softener) | S-4 |
| 5 | MCF-001 Outlet (5Micron Filter) | S-5 |
| 6 | RO-001 Outlet (Reverse Osmosis) | S-6 |
| 7 | RO-002 Outlet (Reverse Osmosis) | S-7 |
| 8 | EDI-001 Outlet (Electro De-Ionizer) | S-8 |
| 9 | UF-001 Outlet (Ultra filter) | S-9 |
| 10 | T-2101 (Purified water storage tank) | S-10 |
| 11 | UV-2101 outlet | S-11 |
| 12 | Purified water return from distribution | S-12 |
| 13 | Fabrication-1 | S-13 |
| 14 | Fabrication-2 | S-14 |
| 15 | Fabrication-3 | S-15 |
| 16 | Coating-1 | S-16 |
| 17 | Coating-2 | S-17 |
| 18 | Coating-3 | S-18 |
| 19 | Product development lab (PDL) | S-19 |
| 20 | Bin wash area | S-20 |
| 21 | Bin wash machine | S-21 |
| 22 | Ointment wash | S-22 |
| 23 | Warehouse | S-23 |
| 24 | Drain point-1 | S-24 |
| 25 | Drain point-2 | S-25 |
| 26 | Drain point-3 | S-26 |
List of Tests and Acceptance Criteria – Raw Water (Stage-1) Chemical analysis (C1; refer Table-1) of Raw water
Table-1
| Test | Acceptance Criteria |
| Description | Clear, Colourless and Odourless liquid |
| pH | 6.0 to 8.5 at 25ºC |
| Total Hardness | NMT 1000 ppm |
| Total Dissolved Solids | NMT 800 ppm |
| Total Suspended Solids | NMT 1000 ppm |
| Total Alkalinity | NMT 400 ppm |
| Chloride | NMT 250 ppm |
| Sulphates | NMT 500 ppm |
| Heavy Metals | NMT 0.5 ppm |
| Microbiological analysis (M1) of Raw water | |
| Total Aerobic Microbial Count | Informative |
| Yeast and Moulds | Informative |
| Escherichia coli | Informative |
| Salmonella species | Informative |
| Pseudomonas aeruginosa | Informative |
| Staphylococcus aureus | Informative |
After Chlorination (Stage 2): Free chlorine content (FC1) of Raw water after chlorination should range from 0.5-1 ppm
Dechlorinated Water (after MGF treatment; Stage 3) : Chemical analysis (C2; refer Table-2) of dechlorinated water storage tank
Table-2
| Test | Acceptance Criteria |
| Description | Clear, Colourless and Odourless liquid |
| Taste | Agreeable |
| pH | 6.0 to 8.5 at 25ºC |
| Total Hardness | NMT 800 ppm |
| Total Suspended Solids | NMT 500 ppm |
| Residual Free Chlorine | NMT 0.2 ppm (on-line measurement) |
| Microbiological analysis (M2) of dechlorinated water from dechlorinated water storage tank | |
| Total aerobic microbial count | Not More Than 500 CFU/ml |
| Yeast and Mould | Not More Than 10 CFU/ ml |
| Escherichia coli | Should be absent |
| Salmonella species | Should be absent |
| Pseudomonas aeruginosa | Should be absent |
| Staphylococcus aureus | Should be absent |
Soft Water (Stage-4) : Chemical analysis (C3; refer Table-3) of Softened water in the ISFD-001 (sampling point) Outlet (Softener)
Table-3
| Test | Acceptance Criteria |
| Description | Clear, Colourless and Odourless liquid |
| pH | 6.0 to 8.5 at 25ºC |
| Total Hardness (as CaCO3) | NMT 10 ppm |
| Total Dissolved Solids | NMT 500 ppm |
Soft Water after 5 µM filter (Stage-5) : Chemical analysis (C4; refer Table-4) of Softened water in the MCF -001 Outlet (5-micron filter)
Table-4
| Test | Acceptance Criteria |
| Description | Clear, Colourless and Odourless liquid |
| pH | 7.5 to 8.5 at 25ºC |
| Residual Free Chlorine | NMT 0.02 ppm (online measurement) |
RO Water (Stage-6) : Chemical analysis (C5; refer Table-5) of RO-001 Outlet water
Table-5
| Test | Acceptance Criteria |
| Description | Clear, Colourless and Odourless liquid |
| pH | Informative |
| Total Dissolved Solids | Informative |
| Conductivity in µS.cm-1 at 25ºC | Informative (on-line measurement) |
RO Water (Stage-7) : Chemical analysis (C6; refer Table-6) of RO-002 Outlet water
Table-6
| Test | Acceptance Criteria |
| Description | Clear, Colourless and Odourless liquid |
| pH | 5.0 to 7.0 at 25ºC |
| Total Hardness | NMT 1 ppm |
| Total Dissolved Solids | Informative |
| Conductivity | NMT 30µS.cm-1 at 25ºC (on-line measurement) |
| Sulfide | NMT 0.01 ppm |
| Silica(SiO2) | NMT 1 ppm |
EDI Water (Stage-8) : Chemical analysis (C7; refer Table-7) of EDI-001 Outlet water
Table-7
| Test | Acceptance Criteria |
| Conductivity | NMT 1.3 µS.cm-1 at 25ºC (on-line measurement) |
Water after Ultra Filtration/ (Stage-9) : Chemical analysis (C8; refer Table-8) of Ultra filter(UF-001) Outlet water
Table-8
| Test | Acceptance Criteria |
| Description | Clear, Colourless and Odourless liquid |
| pH | 5.0-7.0 at 25ºC |
| Conductivity | NMT 1.3 µS.cm-1 at 25ºC |
Purified Water from the Storage Tank outlet (Stage 10) : Chemical analysis (C9; refer Table-9) of Purified Water from the Storage Tank outlet
Table-9
| Test | Acceptance Criteria |
| Description | Clear, Colourless and Odourless liquid |
| pH | 5.0-7.0 at 25ºC |
| Conductivity | NMT 1.3 µS.cm-1 at 25ºC |
| Acidity or Alkalinity | a) Should not produce red colour with 10 ml of sample quantity using 0.5ml methyl red solution. b) Should not produce blue colour with 10 ml of sample quantity using 0.1ml bromothymol blue solution. |
| Ammonium | NMT 0.2 ppm |
| Calcium and Magnesium | To 100 ml add 2 ml of ammonium chloride buffer solution pH 10.0, 50 mg of mordant black 11 triturate and 0.5 ml of 0.01 M sodium edetate. A pure blue colour is produced. |
| Heavy metals | NMT 0.1 ppm |
| Chloride | No change in the appearance of the solution up to 15 min |
| Sulphate | No change in the appearance of the solution up to 60 min |
| Nitrate | NMT 0.2ppm |
| Oxidisable substances | Pink colour should be retained, for 100 ml of sample + 10 ml of H2SO4 + 0.1 ml of 0.02 M KMnO4 |
| Carbon Dioxide | Should produce a clear mixture |
| Residue on Evaporation | NMT 0.001% w/v |
| Microbiological analysis (M3) | |
| Total Aerobic Bacterial Count | NMT 100 CFU /ml |
| Yeast and Moulds | NMT 1.0 CFU /ml |
| Escherichia coli | Should be absent |
| Salmonella species | Should be absent |
| Pseudomonas aeruginosa | Should be absent |
| Staphylococcus aureus | Should be absent |
Purified Water Returns from Distribution Loop (Stage-11): Chemical analysis (C9) of Purified Water return from Distribution Loops, UV Lamp and User Points. Refer to Table-9 for specifications and acceptance criteria.
Operational Checks during Validation: The following operating parameters for the Purified water system shall be monitored every 1 hour during running conditions and shall be summarized along with Phase-wise reports.
Table-10
| Parameter | Acceptance Criteria |
| MGF-001 Inlet water pressure | Not less than 3.5 kg/cm2 |
| ISFD-001 Inlet water pressure | Not less than 3.5 kg/cm2 |
| RO-I Inlet water flow rate | Not less than 5.23 m3/h |
| RO-II.Inlet water flow rate | Not less than 3.66 m3/h |
| RO-I Operating pressure | Not more than 7.7 kg/cm2 |
| RO-II Operating pressure | Not more than 6.8 kg/cm2 |
| EDI Inlet water flow rate | Not less than 2.93m3/h |
| EDI Operating pressure | Not more than 3.0 kg/cm2 |
| UF Inlet water flow rate | Not less than 2.64 m3/h |
| UF Inlet water pressure | 2 to 3 kg/cm2 |
| TOC( In the loop) | NMT 500ppb |
This parametric recording shall be recorded in the format.
Other operational parameters like UV light consumption, pressure differential for all the filters, etc shall also be monitored and recorded in respective log books during validation studies.
Sampling Plan and Testing Plan
Sampling and testing plan for Phase-1 & Phase-2
The following table indicates the sampling and testing plan for Phase 1 & Phase 2.
Table-11
| Sampling point Description | Sampling Point code | Stage | Weekdays | ||||||
| Sun | Mon | Tue | Wed | Thu | Fri | Sat | |||
| Raw Water (Bore well) | S-1 | 1 | C1 M1 | C1 M1 | C1 M1 | C1 M1 | C1 M1 | C1 M1 | C1 M1 |
| MGF-001 Inlet (Multi-grade filter) | S-2 | 2 | FC1 | FC1 | FC1 | FC1 | FC1 | FC1 | FC1 |
| Dechlorinated Water Storage Tank | S-3 | 3 | C2 M2 | C2 M2 | C2 M2 | C2 M2 | C2 M2 | C2 M2 | C2 M2 |
| ISFD-001 Outlet (Softener) | S-4 | 4 | C3 | C3 | C3 | C3 | C3 | C3 | C3 |
| MCF-001 Outlet (5Micron Filter) | S-5 | 5 | C4 | C4 | C4 | C4 | C4 | C4 | C4 |
| RO-001 Outlet (Reverse Osmosis) | S-6 | 6 | C5 | C5 | C5 | C5 | C5 | C5 | C5 |
| RO-002 Outlet (Reverse Osmosis) | S-7 | 7 | C6 | C6 | C6 | C6 | C6 | C6 | C6 |
| EDI-001 Outlet (Electro De-Ionizer) | S-8 | 8 | C7 | C7 | C7 | C7 | C7 | C7 | C7 |
| UF-001 Outlet (Ultra filter) | S-9 | 9 | C8 | C8 | C8 | C8 | C8 | C8 | C8 |
| T-2101 (Purified water storage tank) | S-10 | 10 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 |
| UV-2101 outlet | S-11 | 11 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 |
| Purified water return from distribution | S-12 | 11 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 |
| Fabrication-1 | S-13 | 11 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 |
| Fabrication-2 | S-14 | 11 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 |
| Fabrication-3 | S-15 | 11 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 |
| Coating-1 | S-16 | 11 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 |
| Warehouse | S-23 | 11 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 |
| Drain point-1 | S-24 | 11 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 | C9 M3 |
Sampling and testing plan for Phase 3: The following table indicates the sample plan for Phase 3.
Table-12
| Sampling point Description | Sampling Point code | Stage | Weekdays | |||||||
| Sun | Mon | Tue | Wed | Thu | Fri | Sat | ||||
| Raw Water (Bore well) | S-1 | 1 | C1 /M1 | |||||||
| ISFD-001 Outlet (Softener) | S-4 | 4 | C3 | C3 | C3 | C3 | C3 | C3 | C3 | |
| Purified water storage tank) | S-10 | 10 | C9/M3 | C9/M3 | C9/M3 | C9/M3 | C9/M3 | C9/M3 | C9/M3 | |
| Fabrication | S-13 | 11 | C9 /M3 | C9/M3 | ||||||
| Coating- | S-16 | 11 | C9/M3 | C9/M3 | ||||||
| Product development lab (PDL) | S-19 | 11 | C9/M3 | C9/M3 | ||||||
| Bin wash area | S-20 | 11 | C9/M3 | C9/M3 | ||||||
| Bin wash machine | S-21 | 11 | C9/M3 | C9/M3 | ||||||
| Ointment wash | S-22 | 11 | C9/M3 | C9/M3 | ||||||
RECORDING/ DATA COMPILATION: During the validation study the Data from each phase shall be compiled by the Validation Team Representative from Quality Control in the following formats
- Tabulated Data- Date-wise evaluations
- Analytical Testing -Raw Data Sheet
DEVIATIONS AND INVESTIGATIONS: In case there is any deviation followed during any stage of validation, corrective action shall be taken after proper investigation. Deviations shall be recorded.
QUALIFICATION/ VALIDATION REPORT PREPARATION: After completion of validation, a report based on all phase-wise evaluations shall be prepared by the validation team members supported with tabulated data and statistical analysis (trending and graphical presentation of data). The water System Validation Report shall include various components compiled in the following sequence:
- Validation Report cover page (Annexure-1)
- Index page for Validation Report
- Approval Sheet (Annexure-2)
- Conclusion/ Summary (Report format: Annexure-3) on validation detailed with trending and graphical presentation of data along with and phase-wise sampling & testing plan followed as per protocol.
- Deviations and Investigations, if any (Annexure-4)
- Tabulated data (Annexure-5), Analytical Testing-Raw Data Sheet (Annexure-6) & Parametric Recording (Annexure-9)
- Phase-wise Validation Reports (Annexure-7)
- Name of validation team members (Annexure-8)
- Certification of completion of validation (Annexure-10)
- P & I Diagram for Generation and P.W. Storage & Distribution System (Annexure-11)
RE-VALIDATION/ RE-QUALIFICATION OF WATER SYSTEM
After completion of the three-phase validation study, the frequency of re-qualification or re-validation of the purified water system shall be fixed. Moreover, the water system shall invite revalidation as and when any major modification(s) is/ are done. Any change in the water system shall be executed through a change control procedure as per SOP titled ‘Change Control’
REFERENCES
- SOP ‘Sampling and Analysis of Ground Water and Drinking Water
- User Requirement Specifications
- Design Qualification
- Installation Qualification,Operational Qualification