PROTOCOL No.

:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

REQUALIFICATION PROTOCOL
FOR
PURIFIED WATER STORAGE &
DSITRIBUTION SYSTEM
 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

S.No. Item description Page No.

1.0 PROTOCOL APPROVAL 3
2.0 OVERVIEW 4
2.1 Objective 4
2.2 Purpose 4
2.3 Scope 4
2.4 Responsibility 4
2.5 Execution Team 5
3.0 ACCEPTANCE CRITERIA 6
4.0 REQUALIFICATION CRITERIA 6
5.0 REQUALIFICATION PROCEDURE 6
5.1 System Description 6
5.2 Instruction for filling the checklist 6
5.3 Procedure For Power Failure Study 7
5.4 Sampling Plan 8
5.5 Sampling Point & Sampling Frequency 8-10
5.6 Sanitization Procedure 11
5.7 Sanitization Process 11
5.8 Acceptance Criteria 12
5.9 Action in case of Failure 13
6.0 DEFICIENCY & CORRECTIVE ACTION 14
7.0 SUMMARY AND CONCLUSION 15
7.1 Summary 15
7.2 Conclusion 15
7.3 Final Report approval 16
 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

1.0 PROTOCOL PRE APPROVAL:

Signing of this approval page of Protocol indicates agreement with the requalification approach described in
this document. If modification to the requalification approach becomes necessary. The protocol cannot be used
for execution unless approved by the following authorities.
This Requalification protocol of Purified water Storage & Distribution System been reviewed and approved by
the following persons:

FUNCTION NAME DEPARTMENT SIGNATURE DATE

QUALITY
PREPARED BY
ASSURANCE

PROJECTS /
REVIEWED BY
ENGINEERING

REVIEWED BY PRODUCTION

QUALITY
REVIEWED BY CONTROL
(MICRO)

QUALITY
REVIEWED BY
CONTROL

QUALITY
APPROVED BY
ASSURANCE
 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

2.0 OVERVIEW:
2.1 OBJECTIVE:
The objective of this protocol is to perform & evaluate the power failure study of all user point of distribution
loop of purified water distribution system. The power failure study of water system is available which was
performed during PQ stage for 5 min. Now it is planned to perform the power failure study for 12 hours.

2.2 PURPOSE:
The purpose of this protocol is to execute & evaluate the power failure study which is planned to execute in
water system.

2.3 SCOPE:
This document is applicable to power failure study of purified water storage & distribution system at service
floor.

2.4 RESPONSIBILITY:

The following shall be responsible:

Quality Assurance officer/ Executive-Preparation of protocol its execution and support

Execution team –for execution of protocol

Projects / Engineering – For execution support and review of protocol/report

Production – For execution support and review of protocol/report

Quality Assurance Head – For adequacy and final approval
 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

2.5 EXECUTION TEAM:

The satisfactory power failure study of the purified water storage & distribution system shall be verified by
executing the requalification studies described in this protocol. The successfully executed protocol documents
that the purified water storage & distribution system is working satisfactorily.
Execution team is responsible for the execution of power failure study of purified water storage & distribution
system, Execution team comprises of:

NAME DEPARTMENT DESIGNATION SIGNATURE DATE

PROJECTS/
ENGINEERING

PRODUCTION

QUALITY
CONTROL

QUALITY
CONTROL
(MICRO)

QUALITY
ASSURANCE
 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

3.0 ACCEPTANCE CRITERIA:

3.1 All SOPs for the equipment shall be available
3.2 All the functionality of equipment & components to shall be available.
3.3 The validity of the calibration of tests instruments shall be within calibration status with tag.
3.4 Capacity of equipment shall be verified.

4.0 REQUALIFICATION CRITERIA:

The purified water storage & distribution system shall be re qualified if
 There are any major changes in system components which affect the performance of the system.
 After major breakdown maintenance is carried out.
 After change in the location
 As per revalidation date and schedule

5.0 REQUALIFICATION PROCEDURE:

5.1 SYSTEM DESCRIPTION:

Equipment Name : Purified Water Storage & Distribution System
Supplier/Manufacturer :
Capacity : 7.5 KL
Location :
Equipment id :

5.2 INSTRUCTION FOR FILLING THE CHECKLIST:

5.2.1 In case of the compliance of the test actual observation should be written in specified location.
5.2.2 Actual observation of the component should be written in specified location
5.2.3 For identification of utilities actual observation should be written in specified location.
5.2.4 Give the detailed information in the summary and conclusion part of the Requalification report.
5.2.5 Whichever column is blank or not used ‘NA’ shall be used.
 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

5.3 Procedure for Power failure study:

Perform the power failure study in distribution loop to evaluate the impact of power failure on Purified Water
quality after Power OFF of the purified water distribution pump for 12 hours.
Collect water samples from all the sampling points at interval of 04 hours i.e. sampling from all sampling points
shall be performed at 04 hours, 08 hours and 12 hours after switching off the distribution pump and same shall
be analyzed as per specification. The power failure study shall be performed after Power OFF of the purified
water distribution pump

Note: Purified water distribution loop shall not be started during sampling of power failure study.
On successful completion of sampling for power failure study drain the water from distribution loop and
sanitization shall be carried out as per current SOP & observation shall be recorded below table-II

Power failure study

Table – I
Purified water distribution loop off time: __________
Sampling Checked by
S.No. Sampling Interval Done by (Sign/Date)
(Sign/Date)
04 hours
1. Date:
Time:
08 hours
2. Date:
Time:
12 hours
3. Date:
Time:
 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

5.4 Sampling Plan:

After completion of sampling from all user points and return loop shall performed for 4 hr, 8 hr,12 hr time and
trend shall be made and evaluate the impact. After successful completion of the activity routine monitoring of
purified water user points shall be carried out as per define frequency in SOP.

5.5 Sampling points and Sampling frequency:

The sampling points and their sampling frequencies are mentioned as below.
Sampling
Sampling points Description Frequency
point No.
SP-13B RM store Janitor room ground floor 4 hours,8 hours,12 hours

SP-14B RM store wash area ground floor 4 hours,8 hours,12 hours

SP-15B Wash area ground floor 4 hours,8 hours,12 hours

SP-16B IPQA ground floor 4 hours,8 hours,12 hours

SP-17B Janitor room first floor 4 hours,8 hours,12 hours

SP-18B IPQA first floor 4 hours,8 hours,12 hours

SP-19B Wash room first floor 4 hours,8 hours,12 hours

SP-20B Coating-VIII First floor 4 hours,8 hours,12 hours

SP-21B Coating Solution prepration-1(first floor) 4 hours,8 hours,12 hours

SP-22B Coating-IX first floor 4 hours,8 hours,12 hours

SP-23B Coating –X First floor 4 hours,8 hours,12 hours

SP-24B Coating-XI first floor 4 hours,8 hours,12 hours

SP-25B Coating Solution Prep-II (FIRST FLOOR) 4 hours,8 hours,12 hours

SP-26B Pilot Plant FBD (Second Floor ) 4 hours,8 hours,12 hours

SP-27B Pilot Plant RMG (Second Floor ) 4 hours,8 hours,12 hours

SP-28B Granulation-VI second floor 4 hours,8 hours,12 hours

SP-29B Sifting and milling area-VI second floor 4 hours,8 hours,12 hours

SP-30B Paste preparation – I second floor 4 hours,8 hours,12 hours

SP-31B Sifting and milling area-III second floor 4 hours,8 hours,12 hours

SP-32B Granulation-VII second floor 4 hours,8 hours,12 hours

 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

Sampling
Sampling points Description Frequency
point No.
SP-33B Paste preparation –II second floor 4 hours,8 hours,12 hours

SP-34B FBP solution preparation second floor 4 hours,8 hours,12 hours

SP-35B Granulation-VIII second floor 4 hours,8 hours,12 hours

SP-36B Bin washing service floor 4 hours,8 hours,12 hours

SP-37B Unclean Bin Room Area 4 hours,8 hours,12 hours

SP-38B Janitor room second floor 4 hours,8 hours,12 hours

SP-39B IPQA second floor 4 hours,8 hours,12 hours

SP-40B FBP –III second floor 4 hours,8 hours,12 hours

SP-41B FBP-III Second floor 4 hours,8 hours,12 hours

SP-42B Blender VI 4 hours,8 hours,12 hours

SP-43B FBP-V Second floor 4 hours,8 hours,12 hours

SP-44B Blender –IV second floor 4 hours,8 hours,12 hours

SP-45B Roll compactor V (Second Floor ) 4 hours,8 hours,12 hours

SP-46B Sifting and milling area- I Second floor 4 hours,8 hours,12 hours

SP-47B Granulation –V second floor 4 hours,8 hours,12 hours

SP-48B Return Loop 4 hours,8 hours,12 hours

SP-49B Coating Area -XIII 4 hours,8 hours,12 hours

SP-50B Solution Preparation (Inspection –X) 4 hours,8 hours,12 hours

SP-51B Feed up Water to PSG 4 hours,8 hours,12 hours

SP-52B FBD-6 Area 4 hours,8 hours,12 hours

SP-53B Granulation Area -IX 4 hours,8 hours,12 hours

SP-54B FBP Machine WIP 4 hours,8 hours,12 hours

SP-55B Solution Preparation -III 4 hours,8 hours,12 hours

SP-56B Solution Preparation -IV 4 hours,8 hours,12 hours

SP-57B PSG-III 4 hours,8 hours,12 hours

 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

5.6 Sanitization procedure:

Sanitize the system with hot water as per current sanitization SOP for distribution system. After completion of
sanitization the purified water may be supply to distribution loop for routine activity.

5.7 Sanitization process:

Table II
Date of Sanitization Start Sanitization Done By Checked By
Sanitization On Completed On (Sign/Date) (Sign/Date)

Inference:-------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------

Reviewed by
(Sign & Date)
 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

5.8 Acceptance Criteria:

Water, which is collected from different locations from distribution system, shall meet the specified acceptance
limits mentioned in given below table.
Acceptance criteria for Purified water:

S.No. Test Specification

1. Description Clear color less and odorless liquid
2. pH Between 5.0 to 7.0
1. *For online monitoring
Not more than 1.25 S/cm
3. 2. #For offline monitoring
Conductivity at 25°C (S/cm )
Stage 1: NMT 1.3 S/cm
Stage 2: NMT 2.1 S/cm
Stage 3: NMT 4.7 S/cm
Acidity/ Alkalinity For acidity, the resulting solution should not be red
4.
For alkalinity, the resulting solution should not be blue.
5. Nitrate (ppm) Not more than 0.2
6. @Nitrite content (µg/ml) (by HPLC) Not more than 0.1
7. Heavy Metals (ppm) Not more than 0.1
*Total Organic Carbon (ppb)
NMT 500 ppb
8. (Alternative Test)
**Oxidisable Substances The solution should remain faintly pink
9. Total Viable Count (cfu/ml) NMT 100
10. Test for specified microorganism
A. Escherichia coli, Should be Absent
B. Stapylococcus aureus Should be Absent
C. Pseudomonas aeroginosa Should be Absent
D. Salmonella species Should be Absent
E. Burkholderia cepacia Should be Absent
* Online measurement.
** In case of instrument breakdown, perform oxidisable substance in place TOC.
# In Case of instrument breakdown, perform offline conductivity measurement.
@ shall be performed only on return loop point.
 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

5.9 Action in case of Failure:

In case of any failure, investigation shall be carried out and rectification or modification shall be done if
required. Based upon the data recommendation shall be given. During this period no production activity shall be
carried out.
 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

6.0 DEFICIENCY AND CORRECTIVE ACTION (S) REPORT (S):

Following deficiency was verified and corrective actions taken in consultation with the Engineering
Department.
Description of Deficiency: -----------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
--------------------------------------------------------------------- -----------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
-----------------------------------------------------------------------------------------------------------------------------------
Corrective Action(s) taken: ---------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
----------------------------------------------------------------------- ---------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
------------------------------------------------------------------------------------------------------------------------------------

Reviewed by
Sign & Date
 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

7.0 Summary & Conclusion:

The requalification final summary & conclusion shall be written in below given space.

7.1 Summary: --------------------------------------------------------------------------------------------------------------

---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
-------------------------------------------------------------------------------------------------------------------------------------

7.2 Conclusion :-------------------------------------------------------------------------------------------------------------

---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
---------------------------------------------------------------------------------------------------------------------------------------
-------------------------------------------------------------------------------------------------------------------------------------

Reviewed By
Sign & Date
 PROTOCOL No.:
PHARMA DEVILS
QUALITY ASSURANCE DEPARTMENT

PHARMA DEVILS
REQUALIFICATION PROTOCOL FOR PURIFIED WATER STORAGE & DSITRIBUTION
SYSTEM

7.3 FINAL REPORT APPROVAL:

It has been verified that all tests required by this protocol are completed, reconciled and attached to this protocol
or included in the requalification summary report. Verified that all amendments and discrepancies are
documented, approved and attached to this protocol, (if applicable).
Signatures in the block below indicate that all items in this requalification report of Purified water storage &
distribution system have been reviewed and found to be acceptable and that all variations or discrepancies have
been satisfactorily resolved.

NAME DESIGNATION DEPARTMENT SIGNATURE DATE

PROJECTS /
ENGINEERING

PRODUCTION

QUALITY
CONTROL
(MICRO)

QUALITY
CONTROL

QUALITY
ASSURANCE