validation protocol
March 13, 2017 | Author: Indústria Petys | Category: N/A
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qualification performance...
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Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 1 / 16
Performance Qualification (PQ) Purified Water System Validation Protocol Multipurpose Synthesis Plant (PMS)
TABLE OF CONTENTS
0- DOCUMENT HYSTORY 1- OBJECTIVE 2- DOCUMETATION 2.1 – Related Documentation 2.2 – Applicable Documentation 3- VALIDATION TEAM 4- SCOPE 5- METHODOLOGY 5.1 – System Validation 5.2 – Description of purified water system 5.3 – Quality Critical Attributes for purified water 5.4 – Qualification strategy 5.5 – Performance Qualification tests 5.5.1 Assessment of compliance with Standard Operating Procedures 5.5.2 Testing of purified water quality 6- ACCEPTANCE CRITERIA 6.1 – Acceptance criteria for compliance with SOPs 6.2 – Acceptance criteria for purified water quality 6.3 – Deviations and conclusions
7- PROTOCOL APPROVAL
Appendix I Site general plan 90-A3-1624 Rev. 12 Appendix II Sampling plan Appendix III Purifying plant and loop sampling points plans
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 2 / 16
0. DOCUMENT HYSTORY Previous document edition: Annex A ERCROS 02/12 Validation Protocol – February 2012 Changes involved: Following FDA recommendations this document is reviewed and updated in order to complete the validation study. The main considerations included are: -
Identification and evaluation of the critical elements for the purified water system. Evaluation of the quality of the water at each step in the purification process Evaluation of the quality of the water at each point of use Complete microbial and endotoxin concentration analysis of purified water.
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 3 / 16
1. OBJECT The aim of this study is to demonstrate the consistent and reliable performance of the purified water production system located in Multipurpose Synthesis Plant (PMS) – Building 54, which ensures that the system produces water appropriate for its intended use in a repetitive manner. This validation study is carried out after Operational Qualification step and is part of the Performance Qualification study. It should be evaluated together with initial study ERCROS PQ 013/10. In addition, this validation study is intended to assess the suitability of production, control and maintenance of the system in the quality management system.
2. DOCUMENTATION 2.1 Related Documentation
Good Manufacturing Practice Guide for Active Pharmaceutical Ingredients (ICH – Q7) USP 35 monograph – Purified Water European Pharmacopoeia 7.0 monograph – Purified Water
2.2 Applicable Documentation
Operating and maintenance handbook – Volume IV. (Afarvi) ERCROS-1697 Purified Water Specification Sheet ERCROS-4104 Process water sampling SOP ERCROS-4111 Process water general testing SOP ERCROS-4303 Process water microbiological testing SOP
3. VALIDATION TEAM Validation team responsible of carried out this qualification step is consisted of responsible persons of each involved department. They are shown in following table as well as their responsibility:
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 4 / 16
Department
PMS Production
Quality Control
Quality Assurance
Responsible / Position
Responsibilities
Assistant of Synthesis Area Production
Process data recording; defining of process critical parameters and their acceptance criteria; defining of SOPs, equipment and other critical information; protocol drafting.
Quality Control Assistant
Analytical data recording; defining of critical quality attributes and their acceptance criteria; defining of SOPs, specifications and other critical information; collaboration in protocol drafting.
Quality Assurance Assistant
Coordinator; supervision of protocol and recorded data; statistical analysis; ensuring of compliance of documentation with current legal requirements; protocol approval and writing of reports.
4. SCOPE Purified water production plant which supplies water to Multipurpose Synthesis Plant (PMS) located in Building 54. Refer to site general plan 90-A3-1624 Rev. 12 provided as Appendix I. This validation protocol considers the performance qualification of production, storage and distribution of the purified water produced in this plant.
5. METHODOLOGY 5.1 System Validation Performance Qualification (PQ) step is performed after the qualification of Design (DQ); Installation (IQ) and Operation of the purified water production plant. These qualification steps have been properly performed and the supported documentation is codified as described below: -
Design qualification: Installation qualification: Operational qualification: Initial Performance Qualification:
DQ – 040/04 and DQ – 041/04 IQ – 040/04 and OQ – 041/04 OQ – 040/04 and PQ – 041/04 PQ – 013/10
For performance requalification purposes, two different steps should be considered: -
First step: during this phase it is demonstrated that the system consistently produces the desired water quality without failure or performance deviation when operates in conformance with the stated SOPs.
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 5 / 16
During this period the system is intensively monitored. The sampling is daily after each step of purification process and at each point of use for three weeks (15 working days). The validation approach includes: -
Undertaking of chemical and microbiological testing. Sampling the incoming feed-water daily to verify its quality. Sampling after each step in the purification process daily. Sampling at each point of use and at other defined sample points daily. Demonstrate consistent production and delivery of water of the required quality and quantity when the system is operated in accordance with SOPs. Use and refine the SOPs for operation, maintenance and sanitization. Verify and confirm stated alert and action levels. Refine test-failure procedure.
After this initial step critical sampling points are confirmed as it. After this initial study and whenever no critical deviation or failure of the system occurs, the second step can address. -
Second step: during this phase it is demonstrated that when the water system is operated in accordance with stated SOPs over a long period of time. The sampling is daily from a minimum of two critical points, with at least all points of use tested weekly, for a full year worth of data. The validation approach includes: - Demonstrate extended reliable performance. - Ensure that seasonal variations are evaluated. - The sample locations, sampling frequencies and routine monitoring. After this validation step, final routine water monitoring program will be stated. As appendix II is included a spreadsheet in which it is shown the samples to be taken in both steps as well as it frequency.
5.2 Description of purified water system The facility consists of a purified water production plant (pretreatment; reverse osmosis and water purifying systems); a storage tank and a loop that supply purified water to the points of use. Steps of water purifying and distribution are described as follows. In addition cleaning and sanitization of the system is described too:
WATER PURIFYING PLANT
-
Pretreatment
This step is considered as critical since the objective is to treat in the first instance the incoming potable feed water in order to avoid fluctuations of physic-chemical characteristics of water that could affect the reverse osmosis system. Consist of the following steps: a) Silex / anthracite filter In this step particles in suspension larger than 30 microns are retained and colloidal matter is minimized. b) Duplex decalcification unit In this step calcium and magnesium ions are retained in ion-exchange resins. c) Microfiltration 10 microns This additional filtration ensures the protection of reverse osmosis membranes.
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 6 / 16
d) Addition of bisulphite By means of bisulphite addition, chlorine from the water system is neutralized, which prevents reverse osmosis membranes with polyamide composition can be damaged. Bisulphite remove other oxidants dissolved in water by means of its reduction power and has a bacteriostatic effect since oxygen dissolved is minimized. This process is automatically controlled and performed. In addition, this production plant is provided with a sanitization and cleavage tank and additional microfiltration system that ensures the suitable flow conditioning and pressure and supports the cleaning and sanitization procedures. Sanitization and cleavage tank After previous microfiltration, water is storage in the cleavage tank. From this tank water is pumping to the reverse osmosis membranes. In addition, the tank fulfils the following functions: -
Feeding tank: whenever the water after electrodesionization system has not the desired quality, it is returned to this tank. The system automatically makes the feeding of subsequent equipment independent of flow and pressure.
-
Cleaning of membranes: periodically, in order to avoid the potential blockage of membranes, the tank pumps water at low pressure when the production has stopped.
-
Sanitization: the tank is provided with an element that can heat the water at 80 ºC for sanitization purposes. The loop is provided with a heat exchanger that heats the water to more than 80 ºC in order to sanitize the complete system.
-
Chemical cleaning: cleaning products are dissolved in this tank.
Microfiltration 1.5 microns This additional filtration ensures the remove of particles in suspension and the additional protection of reverse osmosis membranes. The system is controlled by means of a redox-meter that checks the level of chlorine in water and sends the corresponding signals to the system in order to allow water recirculation again in case of its presence is too higher. The potential influence of this treatment on membranes and final quality of water justifies that system Performance Qualification includes sampling before and after this pre-treatment in order to verify the correct operation. -
Reverse osmosis
By means of this treatment, water is subjected to pressure and forced to pass through a semipermeable membranes across which salts or impurities cannot pass. These membranes remove 90 – 98 % of inorganic ions, non-ionic contaminants and organic molecules with a weight more than 200 (colloidal matter, bacteria, pyrogens…), which makes that this step is considered critical. The system is provided with a high pressure pump that forces the water to flow through the membrane surface. Two different and complementary steps with two membranes per step compose the system.
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 7 / 16
The potential influence of this treatment on membranes and final quality of water justifies that system Performance Qualification includes sampling before and after reverse osmosis in order to verify the correct operation. -
Purifying system
This step is considered as critic since by means of this treatment, water is subjected to an electrodes-ionization E-cell system in order to perform a chemical polishing of osmotic water. The application of electric power in the system removes salts dissolved in water by means of conventional ionic exchange resins. In addition, the bactericidal action is carried out by a UV lamp which treats the water after E-cell system. In order to verify the correct performance of the purifying system and final quality of water Performance Qualification includes sampling before and after electro-des-ionization E-cell system and UV-lamp.
STORAGE AND DISTRIBUTION
Alter purifying system, water is storage in a storage tank and distributed to every point of use in the PMS manufacturing plant by means of a loop. 3 Purified water is maintained in the loop under constant flow at 1m /h which avoids point of stagnant water. In addition and in order to ensure and avoid the microorganism presence the system is provided with a UV lamp which treats the water after storage tank and prior to its distribution to the points of use.
In order to verify the correct control of microorganism presence and the potential contamination of storage tank, Performance Qualification includes sampling after storage tank and before and after UV-lamp. -
Points of use
The loop feeds every point of use in the manufacturing plant. In order to verify the correct distribution of the purified water and identify potential sources of contamination, Performance Qualification includes sampling in every point of use. In addition, to ensure the correct recirculation of water and no influence of the loop in water quality, sampling at return hose is performed too.
WATER PURIFYING PLANT
-
Sanitization
For sanitization purposes the system is provided with a heat exchanger that allows raising the loop temperature to 80 – 85 ºC. The procedure is automatically controlled once it is starting. The frequency converter that controls the feeding pump (SW-P-001) as well as opening and closing of the other valves is automatically controlled. Osmotic water is storage in the sanitization and cleavage tank and heated to 80 – 85 ºC. Once the temperature is reached (controlled by means of a TT-001 probe) it is distributed though the
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 8 / 16
purifying system and the loop and maintained under recirculation. During this procedure all the points of use should be open in order to ensure that opening valves are sanitized too. The whole sanitization procedure takes approximately 90 – 120 minutes. Once the recirculation has finished, water is cooled by means of a default cooling gradient. Once the water is at operation temperature, it is drained and the usual production cycle starts. This procedure should be performed after a planned long stoppage (holiday period), after a break whenever the repairs takes more than 24 hours and/or whenever an analytical parameter is out of specifications. In addition as part of preventive maintenance program, this procedure could be performed quarterly. -
Chemical Cleaning
The aim of this procedure is to remove the damaging substances and materials that cold be accumulated in the reverse osmosis membranes (colloids, metals, organic matter, biological compounds…) in order to avoid an irreversible damage. Some evidences that could appear as it or together with other/s show that membranes should be cleaned, these are for instance: -
Loosing of load (10 - 15%) Water conductivity is increased in 15% Nominal flow decrease (at standard Tª 20ºC) in 15% Accumulation of salts Accumulation of organic and inorganic materials Biological contamination in equipments or pipes
Cleaning procedure is performed in the usual operating and acid or base solution could be used. The procedure takes the following steps: 1. 2. 3. 4. 5. 6.
Preparation of Cleaning solution Pumping at low pressure Recirculation of cleaning solution Draining Pumping at high flow Removing of cleaning solution
Once the cleaning has finished, the rejected water and treated water is removed until conductivity parameter decrease and operating parameters are as usual operating.
5.3 Critical Quality Attributes (CQAs) for Purified Water According to ICH Q7 Good Manufacturing Practice Guide for Active Pharmaceutical Ingredients, water used in the manufacture of APIs should be demonstrated to be suitable for its intended use. In this context and in our specific case, water should comply with requirements as laid down in current edition of official USP and European Pharmacopoeia monographs for purified water. The parameters established in the monograph are considered as Critical Quality Attributes. In addition, and taking into account that the product can be used in the production of sterile drug products, microbial and endotoxin content should be assessed and considered as Critical Quality Attributes. In following table are summarized the CQAs and their limits. Reference to internal code for methods of analysis is included too:
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 9 / 16
PURIFIED WATER TEST 1
Appearance
2
Nitrates
UNITS
SPECIFICATIONS*
INTERNAL SOP
-
Clean liquid, transparent, colorless and odorless
ERCROS-4111
NMT 0.2
ERCROS-4111
S – cm
NMT 1.3 (at 25 ºC)
ERCROS-4111
mg / l
NMT 0.5
ERCROS-4260
mg / l -1
3
Conductivity
4
TOC
5
Total Germs Viable
Germs / ml
NMT 100
ERCROS-4303
6
Bacterial Endotoxin
IU/ml
NMT 0.25
ERCROS-4047
NMT: No more than * According to official USP / European Pharmacopoeia monographs.
5.4 Qualification Strategy The qualification strategy is based on the system validation described in section 5.1. The main objective is to check and verify that the critical production steps identified in section 5.2 for purified water system fulfill their functions correctly. In a first instance, it should be ensured that incoming water is suitable for the system feeding and from this point, the following topics should be considered for assessing: -
Correct using of SOPs for operation, maintenance and sanitization. Performance of pretreatment step. Performance of reverse osmosis step. Performance of storage and distribution steps. Quality of water in points of use and return hose.
5.5 Performance Qualification Tests Two different approaches should be taken into account for qualification purposes: 1- Assessment of compliance with Standard Operating Procedures 2- Testing of purified water quality
5.5.1 Assessment of compliance with Standard Operating Procedures 5.5.1.1 Objective The aim of this test is to ensure by writing evidences that the Operating and Maintenance SOP described properly the production and distribution of purified water. In addition alarm system will be verified. In this context, whenever al alarm is detected and informed by the system, it should be recorded in appropriate section of Annex B. The cause of every alarm should be properly investigated according to ERCROS 4008 Investigation of Deviation internal SOP. The SOPs will be checked by means of verification of every item described in the corresponding check-list. Every check-list has been drawn up on the basis of the procedures and steps described in internal SOPs and taking into account the worst-case in every situation.
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 10 / 16
Worst-case: -
Production step: starting the production after a stoppage which involves a cleaning of membranes and sanitization treatment.
-
Storage and distribution step: starting the system after a stoppage which involves a sanitization treatment.
The tests should be performed by PMS Plant staff since they are usually who operates in the Water Purifying Plant and supervised by PMS Manager. 5.5.1.3 Records The following check-list should be fulfilled: -
Annex B Water Purifying; Distribution and Sanitization of the system data check-list
5.5.2 Testing of Purified Water Quality 5.5.2.1 Objective The aim of this test is to ensure by writing evidences that the purified production system produces in a consistent and repetitive way purified water of the desired quality and only this water is distributed to the loop. In addition, it will be verified that the loop has no influence in water quality and bacteriostatic level in maintained. 5.5.2.2 Methodology Taking into account the critical production steps considered in section 5.2 Description of Purified Water System, water quality will be tested as follows. The first step of this performance qualification study should be considered all the sampling point described below. After this step, critical point (defined below and remarked in bold with “*”) will be sampled during the second step during a whole year of worth data. As Appendix III is provided a sketch of the purifying plant and loop which includes sampling points and the desired quality of water in each one.
A – Purifying plant: a) Water pretreatment checking: 1. Sampling of incoming feed water. (VHB 001) 2. Sampling at the end of pretreatment (VHD 003) b) Reverse osmosis checking: 1. Sampling at the end of pretreatment (VHD 003). This sampling point is the same mentioned above. 2. Sampling at the end of reverse osmosis treatment (VHD 007) c) Purifying system checking. 1. Sampling at the end of reverse osmosis treatment (VHD 007). This sampling point is the same mentioned above. 2. Sampling after electrodeionization treatment (VHD 010) 3. Sampling after UV lamp (VHD 011)
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 11 / 16
B – Storage and distribution a) Storage tank checking: 1. Sampling before storage tank (VHD 011). This sampling point is the same mentioned above. 2. Sampling after storage tank (SV 541 001) b) UV lamp checking: 1. Sampling after storage tank (SV 541 001). This sampling point is the same mentioned above. 2. Sampling after UV lamp (SV 541 002) c) Points of use checking: 1. Sampling at every point of use (refer to table below)* d) Water recirculation checking: 1. Sampling at return hose*. In table below is summarized all considered sampling points; their location their identification and the water quality desired in each one. Sampling points marked with “*” are those considered as critical and they should be sampled in the second step of this performance qualification during a whole year of worth data.
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 12 / 16
Sampling sketch
Sampling point
Identification
Location
Quality
a1) VHB 001
VHB 001
Incoming feed water
Potable water
a2) VHD 003
VHD 003
After 1.5 mc microfiltration unit
Potable water
b2) VHD 007
VHD 007
After reverse osmosis system
Osmotic water
c2) VHD 010
VHD 010
After electrodesionization system
Purified water
c3) VHD 011
VHD 011
After UV lamp UVA
Purified water
Purifying Plant (A)
Storage and Distribution (B) a2) SV 541 001
SV 541 001
After storage tank and before UV lamp
Purified water
b2) SV 541 002
SV 541 002
After UV lamp
Purified water
d1) SV 541 003
SV 541 002
At return hose
Purified water
c1) Points of use DC-0502-00 Reactor
PU-5
DC-0501-00 Reactor
PU-4
DC-0504-00 Reactor
PU-3
DC-0507-00 Reactor
PU-2
DC-0508-00 Reactor
PU-1
DF-0532-02 DF-0532-03 Dissolution Tanks DF-0532-00 DF-0532-01 Dissolution Tanks
PU-8 PU-9
JL-0512-00 Centrifuge
PU-6
Laboratory
PU-11
DF-0531-00 DF-0531-01 Dissolution Tanks
PU-10
JL-0511-00 Centrifuge
PU-7
EI-0521-00 Drier
PU-12
Level 2. Intake drainage valve at DC-0502-00 reactor Level 2. Intake drainage valve at DC-0501-00 reactor Level 2. Intake drainage valve at DC-0504-00 reactor Level 2. Intake drainage valve at DC-0507-00 reactor Level 2. Intake drainage valve at DC-0508-00 reactor Level 2. Intake common drainage valve at auxiliary tanks Level 2. Intake common drainage valve at auxiliary tanks Level 1. Intake drainage valve at JL-0512-00 centrifuge Level 1. Laboratory Level 0. Intake common drainage valve at auxiliary tanks Level 0. Intake drainage valve at JL-0511-00 centrifuge Level 0. Drier room
Purified water Purified water Purified water Purified water Purified water Purified water Purified water Purified water Purified water Purified water Purified water Purified water
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 13 / 16
5.5.2.2.1 Analytical test and methods In following tables are summarized the tests performed for every quality of water and reference to internal SOPs.
PURIFIED WATER TEST 1
Appearance
2
Nitrates
UNITS
SPECIFICATIONS*
INTERNAL SOP
-
Clean, transparent, colorless and odorless liquid
ERCROS-4111
NMT 0.2
ERCROS-4111
S – cm
NMT 1.3 (at 25 ºC)
ERCROS-4111
mg / l
NMT 0.5
ERCROS-4260
mg / l -1
3
Conductivity
4
TOC
5
Total Germs Viable
Germs / ml
NMT 100
ERCROS-4303
6
Bacterial Endotoxin
IU/ml
NMT 0.25
ERCROS-4047
NMT: No more than * According to official USP / European Pharmacopoeia monographs.
OSMOTIC WATER TEST 1
Appearance
2
Nitrates
UNITS
SPECIFICATIONS*
INTERNAL SOP
-
Clean, transparent, colorless and odorless liquid
ERCROS-4111
NMT 5
ERCROS-4111
S – cm
NMT 200 (at 25 ºC)
ERCROS-4111
mg / l
NMT 3
ERCROS-4260
mg / l -1
3
Conductivity
4
TOC
5
Total Germs Viable
Germs / ml
NMT 100
ERCROS-4303
6
Bacterial Endotoxin
IU/ml
-
**
ERCROS-4047
NMT: No more than * According to internal established specifications. ** No specification is established for endotoxins in osmotic water. Obtained result is only for information and it should be taken into account for checking the capacity of purified water system for endotoxins removing.
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 14 / 16
POTABLE WATER TEST
UNITS
SPECIFICATIONS*
INTERNAL SOP
-
Clean, transparent, colorless and odorless liquid
ERCROS-4111
1
Appearance
2
Calcium
mg / l
NMT 500
ERCROS-4111
3
Chlorides
mg / l
NMT 250
ERCROS-4111
4
Sulfates
mg / ml
NMT 250
ERCROS-4111
5
Nitrates
mg / l
NMT 50
ERCROS-4111
6
Ammonium
mg / l
NMT 0.5
ERCROS-4111
7
pH
pH
6.5 – 9.5
ERCROS-4111
8
Total Solids
mg / l
NMT 1000
ERCROS-4111
9
Heavy metals (Pb)
μg / l
NMT 0.25
ERCROS-4111
mg / l
NMT 1.3
ERCROS-4111
S – cm-1
NMT 2500
ERCROS-4111
mg / l
NMT 5
ERCROS-4260
Germs / ml
NMT 100
ERCROS-4303
-
Absence
ERCROS-4303
IU/ml
-
**
ERCROS-4047
10 Organic matter 11 Conductivity 12 TOC 13 Total Germs Viable 14 Escherichia coli 15 Bacterial endotoxins
NMT: No more than * According to internal established specifications. ** This test will be performed only at point identified as VHB 001 with the aim of knowing the endotoxin burden of incoming water. Endotoxins test at point VHD 003 has not been considered since any treatment to remove or minimize endotoxins content has been performed at this point. No specification is established for endotoxins in potable water. Obtained result is only for information and it should be taken into account for checking the capacity of purified water system for endotoxins removing. Detailed description of method of analysis to be performed for each sample is described in the corresponding internal SOPs. (Refer to section 2.2. Applicable Documentation). 5.5.2.2.2 Sampling method Sampling should be performed once the purified plant and loop are normally working. Sampling during this validation step will be daily for 15 working days. It should be recorded date and time (in sample label) of sampling in every sample. Sampling date should be recorded as follows: Sampling point / day / month (two digits) / year (two digits) Example: sample taken at VHD 007 on July 14th, 2012, should be identified as follows: VHD 007 / 14 / 07 /12 Two different labels are available depending on the test. Label model is as follows:
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 15 / 16
Chemical Tests Purified Water
Microbiological Control Purified Water
Sampling Point / Date
Sampling Point / Date
Analyst
Analyst
Initials / Signature
Initials / Signature
The label should be fulfilled just before sampling and stick to the bottle immediately. The sampling should be performed according to the instructions given in ERCROS-4104 Process water sampling internal SOP. A brief summary of this procedure is provided below: Process water sampling should be carried out by Quality Control Laboratory staff. It should be taken into account the test to be performed and prepare the material needed for sampling and testing according to this. In this context, sampling material for endotoxins test should be prepared in non-pyrogenic conditions by Quality Control staff and material for microbiological analysis should be prepared and maintained in sterile conditions. For other chemical analysis is enough that the material is properly clean. The general operating procedure is as follows: 1. Check that the drain or faucet is clean. Otherwise, clean them. 2. Open the drain or the faucet and let the water run a few minutes (5 minutes). 3. Open the bottle where it will take the sample and rinse with the same water to be taken. Pull the water. Sample for TOC and conductivity should be approximately 500 mL in non-sterile bottle and sample for total viable germ should be approximately 200 mL in sterile bottle. 4. Fill the bottle completely and cover it perfectly. Label the form unequivocally dated, internal code and plant. 5. Transfer the sample to the laboratory as soon as possible. 5.5.2.3 Records Analytical data should be recorded in Annex C of this validation study and in ERCROS 4111 Process water general testing record data sheet.
6.
ACCEPTANCE CRITERIA
6.1 Acceptance criteria for compliance with SOPs Acceptance criteria for this test is that check lists provided as Annex B and Annex C are fulfilled following the tested SOP and every item is recorded as positive. The procedure is considered valid if quality water meets established specifications after tests described in section 5.5.2.
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 16 / 16
6.2 Acceptance criteria for purified water quality Acceptance criteria for this test is that every sample taken and tested as described in section 5.5.2 meets established specifications for its quality.
6.3 Deviations and conclusions Deviations occur during validation should be recorded in the deviation sheet provided at the end of the corresponding annex. Results and conclusions will be summarized in the Validation Report.
7.
PROTOCOL APPROVAL
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Appendix II
APPENDIX II
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Appendix II
-
First Step Frequency Sampling Point
Day 1
Day 2
Day 3
Day 4
Day 5
Day 6
Day 7
Day 8
Day 9
Day 10
Day 11
Day 12
Day 13
Day 14
Day 15
VHB 001
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
VHD 003
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
VHD 007
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
VHD 010
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
VHD 011
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
SV 541 001
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
SV 541 002
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
SV 541 002
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
PU-5
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
PU-4
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
PU-3
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
PU-2
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
PU-1
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
PU-8
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
PU-9
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
PU-6
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
PU-10
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
PU-7
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
PU-11
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
PU-12
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Appendix II
-
Second Step
Even-numbered weeks:
Day 1
Sampling Point
Chemical
SV 541 002
x
PU-5
x
PU-4
x
PU-3
x
Day 2
Microbiological
Chemical
Day 3
Microbiological
Chemical
Day 4
Microbiological
Day 5
Chemical
Microbiological
PU-6
x
x
PU-10
x
PU-7
x
Chemical
Microbiological
x
x
PU-2
x
PU-1
x
x
PU-8
x
PU-9
x
x
x
PU-11
x
PU-12
x
x
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Appendix II
Odd-numbered weeks:
Sampling Point SV 541 002 PU-5 PU-4 PU-3 PU-2 PU-1 PU-8 PU-9 PU-6 PU-10 PU-7 PU-11 PU-12
Day 1
Day 2
Chemical
Microbiological
x
x
Day 3
Chemical
Microbiological
x
x
Day 4
Chemical
Microbiological
x
x
Chemical
Day 5
Microbiological
Chemical
Microbiological
x
x
x x
x
x
x
x x x
x
x
x
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Appendix III
APPENDIX III
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Appendix III
Water Purifying System
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Appendix III
Points of use
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Appendix III
Annex A ERCROS 02/12 Validation Protocol – Rev. 1 Appendix III
Annex B ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 1 / 8
Compliance with Standard Operating Procedures Check-list
TABLE OF CONTENTS
1- TABLE 1 – Purifying step 2- TABLE 2 – Distribution and sanitization steps
PREPARED BY:
Date and signature
SUPERVISED BY:
Date and signature
APPROVED BY:
Date and signature
Annex B ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 2 / 8
TABLE 1 Starting and operating of purifying system after stoppage Step
Operation
Results
Bisulphite removing
Press button: Proceso después de parada de larga duración
Manual
Bisulphite removing
Send Bisulphite Solution to sewage
Manual
Bisulphite removing
PLC shows: CONECTAR LAS CONEXIONES DE LIMPIEZA DE PERMEADO Y RECHAZO CON DRENAJE.
Automatic
Bisulphite removing
Connect and press ACCEPT
Manual
Bisulphite removing
Decalcified water loading starts
Automatic
Bisulphite removing
High and low pressure pumping start
Automatic
Bisulphite removing
Stop pumps
Automatic
Bisulphite removing
Bisulphite removing E-cell system regeneration E-cell system regeneration E-cell system regeneration E-cell system regeneration E-cell system regeneration
PLC shows: VOLVER A CONECTAR CLAMP CIEGO EN LAS CONEXIONES DE LIMPIEZA. Connect the Clamp and press ACCEPT Opening of valves: VHB-010, VHB-011, VHD-012 and VHD-008. Close VPD-008 and open VPD-009 Starting the preosmosis and reverse osmosis for this valve Stabilize the inlet flow Starting the concentrate recirculation pump
Yes No
Yes No
Yes No
Yes No
Yes No
Yes No
Yes No
Yes No
Manual
Yes No
Manual
Yes No
Yes No
Manual
Manual
Manual
Manual
Supervised by
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Yes No
Automatic
Performed by:
Yes No
Yes No
Annex B ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 3 / 8
Step
Operation
E-cell system regeneration
Stabilize the flow of concentrate: Inlet Pressure from 0.3 to 0.6 bars Outlet Pressure from 0.3 to 0.6 bars
Manual
E-cell system regeneration
Adjust the flow of purge concentrate
Manual
E-cell system regeneration
Verification of suitability of flow rates and pressures
E-cell system regeneration E-cell system regeneration
Normal Start Normal Start
Normal Start
Normal Start Normal Start Normal Start Normal Start Normal Start Normal Start
Starting the rectifier Water quality and flow (parameters shown at PLC) are suitable Press button: NORMAL OPERATION Enter Password Confirm the password for the computer and the screen Message appears: NORMAL OPERATION Operation of UV Lamp Correct Pretreatment Cycle Correct Osmosis Cycle Correct Water Cycle of Refinement Correct water return to sanitization and cleavage tank
Results
Yes No
Yes No
Manual
Yes No
Manual
Yes No
Manual
Manual Automatic
Yes No
Yes No
Yes No
Automatic
Yes No
Manual
Yes No
Automatic
Yes No
Automatic
Automatic
Yes No Yes No
Yes No
Automatic
Supervised by
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Date / Sign.
Yes No
Manual
Performed by:
Annex B ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 4 / 8
Alarms Detected:
Date / Signature:
Remarks:
Date / Signature:
Results and conclusion: Number of Positive responses: Number of Negative responses: Conclusion*: *The test is considered valid only if all the questions are positive.
Performed by: Date / Signature
Supervised by: Date / Signature
Annex B ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 5 / 8
TABLE 2
Starting and operating of distribution and sanitization after stoppage Step Starting
Starting
Starting
Operation Verify that all the points of use are closed. Verified that storage tank valve is closed. Verify that all the pumping and intaking valves are closed.
Starting
Verify that purifying system is operation.
Starting
Verify the availability of comprised air.
Starting
Verify the availability of electric power.
Starting
Starting
Starting
Starting Starting
Starting
Turn off the general switch in the electric frame. Release emergency stop. Connect all the switches and fuses in electric frame. Verify screen is on. Press button: CONSIGNAS. Verify that operating parameters shown in the screen are correct and no alarms are shown.
Starting
Press button: AUTOMATICO.
Starting
Press button: MARCHA LOOP.
Starting
Verify that water is entering in storage tank.
Results Manual
Manual
Manual
Manual
Manual
Manual
Manual
Yes No
Yes No
Yes No
Yes No
Yes No
Yes No Yes No
Manual
Yes No
Manual
Manual
Yes No Yes No
Manual
Yes No
Manual
Manual
Automatic
Supervised by
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Yes No
Manual
Performed by:
Yes No
Yes No
Yes No
Annex B ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 6 / 8
Step
Starting
Operation Verify the correct level of water for pumping starts.
Starting
Pumping system starts.
Starting
Speed of water return is regulated.
Starting
Starting
Starting
Sanitization
Sanitization
Sanitization
Sanitization
Sanitization
Sanitization Sanitization
Sanitization
Sanitization
UV lamp starts. Valves at points of use operate correctly. Valves at sampling points operate correctly. Verify the operating program is: AUTOMATICO Verify the system is operating. Verify that no consume is any point of use. Verify availability of cool water and steam. Verify valves at steam entrance; condenser returns; cool water entrance and cool water return are open. Start sanitization program. Confirmation. Storage tank draining. Valve in storage tank is in draining position. UV lamp starts.
Results
Automatic
Yes No
Automatic
Yes No
Automatic
Yes No
Automatic
Yes No
Automatic
Manual
Manual
Manual
Manual
Manual
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Yes No Yes No
Yes No
Date
Yes No
Supervised by
Yes No
Automatic
Performed by:
Yes No
Yes No
Manual
Yes No
Automatic
Yes No
Automatic
Yes No
Automatic
Yes No
Annex B ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 7 / 8
ETAPA Sanitization Sanitization
Sanitization
Sanitization Sanitization Sanitization Normal operation
ACCIÓN Purge Heating Water is maintained hot during sanitization. Purge. Cooling. Water is at operating temperature. Water is available at every point of use.
CONFORMIDAD Automatic
Automatic
Yes No Yes No
Automatic
Yes No
Automatic
Automatic
Yes No Yes No
Automatic
Yes No
Yes No
Automatic
REALIZADO
VERIFICADO
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Date
Annex B ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 8 / 8
Alarms Detected:
Date / Signature:
Remarks:
Date / Signature:
Results and conclusion: Number of Positive responses: Number of Negative responses: Conclusion*: *The test is considered valid only if all the questions are positive.
Performed by: Date / Signature
Supervised by: Date / Signature
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 1 / 29
Sampling Control and Data Record
TABLE OF CONTENTS
1. Introduction
2. Sampling record template
3. Analytical data record template
PREPARED BY:
Date and signature
SUPERVISED BY:
Date and signature
APPROVED BY:
Date and signature
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 2 / 29
1.
INTRODUCTION
A very important part of Performance Qualification step of this purifying water system involves sampling and testing of water along the whole production and distribution. This annex covers and compiles sampling, codification of samples, acceptance criteria and obtained results. In table below is summarized considered sampling points; their location their identification and the quality desired in each one. During the first step of this qualification study, every point listed below should be sampled during 20 days. After this step and whenever no critical deviation or failure of the system occurs, only critical points (marked in bold) will be tested during a whole year of worth data.
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 3 / 29
Sampling sketch
Sampling point
Identification
Location
Quality
VHB 001
VHB 001
Incoming feed water
Potable water
VHD 003
VHD 003
After 1.5 mc microfiltration unit
Potable water
VHD 007
VHD 007
After reverse osmosis system
Osmotic water
VHD 010
VHD 010
After electrodesionization system
Purified water
VHD 011
VHD 011
After UV lamp UVA
Purified water
SV 541 001
SV 541 001
After storage tank and before UV lamp
Purified water
SV 541 002
SV 541 002
After UV lamp
Purified water
SV 541 003
SV 541 002
At return hose
Purified water
Purifying Plant
Storage and Distribution
Points of use DC-0502-00 Reactor
PU-5
DC-0501-00 Reactor
PU-4
DC-0504-00 Reactor
PU-3
DC-0507-00 Reactor
PU-2
DC-0508-00 Reactor
PU-1
DF-0532-02 DF-0532-03 Dissolution Tanks DF-0532-00 DF-0532-01 Dissolution Tanks
PU-8 PU-9
JL-0512-00 Centrifuge
PU-6
Laboratory
PU-11
DF-0531-00 DF-0531-01 Dissolution Tanks
PU-10
JL-0511-00 Centrifuge
PU-7
EI-0521-00 Drier
PU-12
Level 2. Intake drainage valve at DC-0502-00 reactor Level 2. Intake drainage valve at DC-0501-00 reactor Level 2. Intake drainage valve at DC-0504-00 reactor Level 2. Intake drainage valve at DC-0507-00 reactor Level 2. Intake drainage valve at DC-0508-00 reactor Level 2. Intake common drainage valve at auxiliary tanks Level 2. Intake common drainage valve at auxiliary tanks Level 1. Intake drainage valve at JL-0512-00 centrifuge Level 1. Laboratory Level 0. Intake common drainage valve at auxiliary tanks Level 0. Intake drainage valve at JL-0511-00 centrifuge Level 0. Drier room
Purified water Purified water Purified water Purified water Purified water Purified water Purified water Purified water Purified water Purified water Purified water Purified water
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 4 / 29
2.
SAMPLING RECORD TEMPLATE
Purifying Plant
Sampling Point: Sampling Date VHB 001 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 5 / 29
Sampling Point: Sampling Date VHD 003 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 6 / 29
Sampling Point: Sampling Date VHD 007 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 7 / 29
Sampling Point: Sampling Date VHD 010 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 8 / 29
Sampling Point: Sampling Date VHD 011 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 9 / 29
Storage and Distribution
Sampling Point: Sampling Date SV 541 001 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 10 / 29
Sampling Point: Sampling Date SV 541 002 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 11 / 29
Sampling Point: Sampling Date SV 541 003 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 12 / 29
Points of use
Sampling Point: Sampling Date PU-5 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 13 / 29
Sampling Point: Sampling Date PU-4 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 14 / 29
Sampling Point: Sampling Date PU-3 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 15 / 29
Sampling Point: Sampling Date PU-2 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 16 / 29
Sampling Point: Sampling Date PU-1 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 17 / 29
Sampling Point: Sampling Date PU-8 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 18 / 29
Sampling Point: Sampling Date PU-9 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 19 / 29
Sampling Point: Sampling Date PU-6 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 20 / 29
Sampling Point: Sampling Date PU-11 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 21 / 29
Sampling Point: Sampling Date PU-10 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 22 / 29
Sampling Point: Sampling Date PU-7 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 23 / 29
Sampling Point: Sampling Date PU-12 Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 Day 7 Day 8 Day 9 Day 10 Day 11 Day 12 Day 13 Day 14 Day 15 Day 16 Day 17 Day 18 Day 19 Day 20
Sample taken by: (Initials and signature)
Verify by: (Initials and signature)
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 24 / 29
Deviations Description
Affect the validation study:
Date / Sign.
□Yes □ No
Remarks
Conforms
Non conforms
Final result:
Performed by:
Signature:
Date:
Verify by:
Signature:
Date:
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 25 / 29
3.
ANALYTICAL DATA RECORD TEMPLATE
Complete the following record data sheet per taken sample and enclose copy of raw data record:
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 26 / 29
POTABLE WATER
Sampling Point:
Sampling date:
Test
Specification
Appearance
Clean, transparent, colorless and odorless liquid
Calcium
NMT 500 mg / l
Chlorides
NMT 250 mg / l
Sulfates
NMT 250 mg / ml
Nitrates
NMT 50 mg / l
Ammonium
NMT 0.5 mg / l
pH
6.5 – 9.5 pH
Total Solids
NMT 1000 mg / l
Heavy metals (Pb)
NMT 0.25 μg / l
Organic matter
NMT 1.3 mg / l
Conductivity
NMT 2500S – cm-1
TOC
NMT 5 mg / l
Total Germs Viable
NMT 100 Germs / ml
Escherichia coli
Absence
Bacterial endotoxins*
(informative) IU/ml
Result
* Only to be tested at point identified as VHB 001 Remarks
Analysis Date
Analyzed by:
Verify by:
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 27 / 29
OSMOTIC WATER
Sampling Point:
Sampling date:
Test
Specification
Appearance
Clean, transparent, colorless and odorless liquid
Nitrates
NMT 5 mg / l
Conductivity
NMT 200 (at 25 ºC) S – cm-1
TOC
NMT 3 mg / l
Total Germs Viable
NMT 100 Germs / ml
Bacterial Endotoxin
(informative) IU/ml
Remarks
Result
Analysis Date
Analyzed by:
Verify by:
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 28 / 29
PURIFIED WATER
Sampling Point:
Sampling date:
Test
Specification
Appearance
Clean, transparent, colorless and odorless liquid
Nitrates
NMT 0.2 mg / l
Conductivity
NMT 1.3 (at 25 ºC) S – cm-1
TOC
NMT 0.5 mg / l
Total Germs Viable
NMT 100 Germs / ml
Bacterial Endotoxin
NMT 0.25 IU/ml
Remarks
Result
Analysis Date
Analyzed by:
Verify by:
Annex C ERCROS 02/12 Validation Protocol – Rev. 1 Pag. 29 / 29
Deviations Description
Affect the validation study:
Date / Sign.
□Yes □ No
Remarks
Conforms
Non conforms
Final result:
Performed by:
Signature:
Date:
Verify by:
Signature:
Date:
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