DBSVCPMOQ 10 05(Enhanced Mechanical)

8/8/2019 DBSVCPMOQ 10 05(Enhanced Mechanical)

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PM & Operational Qualification Test Protocol

Test System: Procedure Number: Revision: Page:Dissolution Tester System Mechanical Calibration DBSVCPM/OQ-10-05 5.0 1 of 32

Prepared by: Effective Date: Review Due Date:

Ivette Serbia, PerkinElmer LAS 16-SEP-10 16-SEP-12

TESTS SPECIFICATIONS FORTHE DISSOLUTION TESTER SYSTEM MECHANICAL CALIBRATION

VER. 5.0

Equipment Customer ID: ___________________

CONFIDENTIALTHIS DOCUMENT IS THE PROPERTY OF:PERKINELMER, INC.


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1. Pre-approval Signatures

PerkinElmers Issuer

Signature indicates agreement by the ServiceRepresentative that this document, as written,will provide sufficient documented evidencethat the Dissolution Tester System testing canbe executed according to the appropriatemanufacturers specifications.

_________________________________PE Service Representative / Signature

___________Date

PerkinElmers Specialist Review

Signature indicates agreement by the CertifiedService Specialist that this document is clearly

written and is consistent with the systemOperational Qualification requirements.

_________________________________PE Service Specialist / Signature ___________Date

PerkinElmers Approver

Signature indicates agreement by the ServiceManager or Designee that this document isclearly written and is consistent with the systemOperational Qualification requirements andPerkinElmer Policies.

_________________________________PE Service Approver / Signature

___________Date


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2. Publication Record

Revision Date Description

1.0 24-FEB-09 Initial Issue

2.0 22-JUN-09 Table 12.3 divided into two sections, one for paddle resultsand one for basket results.

3.0 26-JUN-09 Basket information was deleted from table 11.1 sections

11.1.6.

Vibration test limit specified as for information only.

Basket depth verification limit changed to 2mm to matchreference requirements.

Bubble level instrument eliminated as an option.

PerkinElmers LabMetrixTM

GLP dissolution calibration systemadded as a testing option.

150 RPM and 250 RPM verifications were added to therotational speed test.

The manual vessel verticality verification procedure was

added to section 12.6Paddle ID information deleted by customer request.

4.0 6-JUL-09 Centering gage minimum resolution changed from 0.2mm to1mm as requested by customer.

5.0 16-SEP-10 Test 12.11 Deleted requirement that none baths must berunning during the test at the same time and added a secondtest with all baths in the same bench running at the same time.


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TABLE OF CONTENTS

1. PRE-APPROVAL SIGNATURES ..................................................................................................... 22. PUBLICATION RECORD ................................................................................................................. 33. INTRODUCTION ............................................................................................................................... 54. PURPOSE ......................................................................................................................................... 55. REFERENCES .................................................................................................................................. 56. DEFINITIONS .................................................................................................................................... 67. ACRONYMS ...................................................................................................................................... 88. RESPONSIBILITIES ......................................................................................................................... 89. SYSTEM DESCRIPTION AND SPECIFICATIONS .......................................................................... 99.1. SYSTEM DESCRIPTION ..................................................................................................................... 99.2. SYSTEM SPECIFICATIONS................................................................................................................. 910. CALIBRATION AND TEST PROCEDURES .................................................................................. 1011. SYSTEM COMPONENTS AND TEST MATERIALS IDENTIFICATION ........................................ 1111.1. SYSTEM COMPONENT IDENTIFICATION FORM................................................................................... 1211.2. CALIBRATION EQUIPMENT IDENTIFICATION FORM............................................................................. 1312. DISSOLUTION BATH TEST CASES ............................................................................................. 1412.1. SYSTEM COMPONENTS VISUAL INSPECTION .................................................................................... 1412.2. SHAFT WOBBLE ............................................................................................................................. 1512.3. PADDLE/BASKET SHAFT VERTICALITY............................................................................................ 1612.4. BASKET WOBBLE (APPARATUS 1)VERIFICATION ............................................................................. 1712.5. VESSEL/SHAFT CENTERING............................................................................................................ 1912.6. VESSEL VERTICALITY ..................................................................................................................... 2112.7. BASKET AND PADDLE DEPTH .......................................................................................................... 2412.8. SHAFT ROTATIONAL SPEED ............................................................................................................ 2612.9. TIMER TEST................................................................................................................................... 2712.10. TEMPERATURE CONTROL ACCURACY TEST..................................................................................... 2712.11. VIBRATION TEST ............................................................................................................................ 2813. DOCUMENT LOG ........................................................................................................................... 3014. POST APPROVAL SIGNATURES & CERTIFICATION ................................................................ 31


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3. Introduction

This test script was written to verify the compliance of Dissolution Tester systems with their designspecifications and USP operational requirements. This helps maintain the system in a readinessstatus, which will provide the user with the required confidence in the system accuracy and precision.

4. Purpose

The procedure is applicable to both basket and paddle systems. This calibration protocol is intended toset the procedure in the use of mechanical calibration as an alternate approach to the use of calibratortablets in calibrating an apparatus used for dissolution testing and to establish the setup, mechanicacalibration, and operation checks for dissolution Apparatus 1 (Basket) and 2 (Paddle).

5. References

5.1 Dissolution Tester Systems Manufacturers Operation/Service Manuals.

5.2 Guidance for Industry, Dissolution Testing of Immediate Release Solid Oral Dosage FormsFDA, August 1997

5.3 USP, General Chapter Dissolution

5.4 Wyeth Division Guidance, QSE #11, Mechanical Calibration and Operational Checks foBasket and Paddle Dissolution Apparatus, Rev 1.0

5.5 Standard Practice for the Qualification of Basket and Paddle Dissolution Apparatus, ASTM E2503-07, 2007


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6. Definitions

6.1. Dissolution TesterThe assembly consists of the following: a vessel, whichmay be covered, made of glass or other inert,transparent material; a motor; a metallic drive shaft; anda cylindrical basket. The vessel is partially immersed in asuitable water bath of any convenient size or heated bya suitable device such as a heating jacket. The waterbath or heating device permits holding the temperatureinside the vessel at 37 0.5 during the test and keepingthe bath fluid in constant, smooth motion. No part of theassembly, including the environment in which theassembly is placed, contributes significant motion,agitation, or vibration beyond that due to the smoothlyrotating stirring element. The vessel is cylindrical, with ahemispherical bottom. Its sides are flanged at the top. Afitted cover may be used to retard evaporation. The shaftis positioned so that its axis is not more than 2 mm atany point from the vertical axis of the vessel and rotatessmoothly and without significant wobble that could affectthe results. A speed-regulating device is used that allowsthe shaft rotation speed to be selected and maintained.Shaft and basket components of the stirring element arefabricated of stainless steel, type 316, or other inert

material. A dosage unit is placed in a dry basket at thebeginning of each test. A second assembly uses apaddle formed from a blade and a shaft is used as thestirring element. The shaft is positioned so that its axis isnot more than 2 mm from the vertical axis of the vesselat any point and rotates smoothly without significantwobble that could affect the results. The vertical centerline of the blade passes through the axis of the shaft sothat the bottom of the blade is flush with the bottom ofthe shaft. The metallic or suitably inert, rigid blade andshaft comprise a single entity. A suitable two-partdetachable design may be used provided the assembly

remains firmly engaged during the test. The paddleblade and shaft may be coated with a suitable coating soas to make them inert. The dosage unit is allowed to sinkto the bottom of the vessel before rotation of the blade isstarted. A small, loose piece of nonreactive material,such as not more than a few turns of wire helix, may beattached to dosage units that would otherwise float.

6.2. LevelMeasures horizontal and vertical (plumb) orientation ofthe assembly. It must be accurate to at least 0.1.


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6.3. Tachometer Measures revolutions per minute. It must be accurate toat least 1RPM. Tachometers may be mechanical oroptical.

6.4. Vibration MeterMeasures displacement, acceleration, and frequency.The sensing device should be able to be placed on bothvertical and horizontal surfaces of the assembly(oriented in x, y, and z directions).

6.5. CaliperMeasures distance between two opposing points orsurfaces. The trueness and precision of measurementby a caliper can be checked using gauge blocks. Gauge

blocks are standardized materials that represent a rangeof distances and are used as reference distances forcalibration of measuring tools.

6.6. CompassTransfers a distance from an otherwise inaccessibleposition to a location where the distance can bedetermined using the caliper. Compasses can haveinward or outward-facing points to allow the transfer ofinner or outer distances. The tips of the compass areadjusted to fit across the points to be measured andfixed, the compass is then removed, and the distancebetween the tips measured.

6.7. Centering GageDetermines centering of the apparatus shaft within thevessel. Distances given by this gauge are checked witha caliper. It must be accurate to at least 0.2mm.

6.8. Dial Test Indicator(Runout Gauge)

Determines the eccentricity of a rotating surface.Trueness and precision are checked with a caliper orgauge blocks. It must be accurate to at least 0.05mm.

6.9. Feeler GaugeThese are small lengths of metal, typically of steel, ofdifferent thicknesses with measurements marked oneach piece used to provide a standard thickness inthe sensitivity test for the level. Gauge blocks typicallyrepresent larger thicknesses and can also be used.

6.10. Digital ProtractorDetermines the angle of a surface relative to horizontalor vertical.

6.11. Executed byDocuments the name and signature of the certifiedperson performing the previous action and itscorresponding documentation.


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6.12. Reviewed by Identifies the name and signature of the certified personin agreement with the information documented by theperson performing the previous action and itscorresponding documentation.

7. Acronyms

7.1. FDA Food and Drug Administration

7.2. LED Light Emitting Diode

7.3. OQ Operational Qualification

7.4. PM Preventive Maintenance

7.5. RPM Revolutions per Minute

7.6. RTD Reference Temperature Detector

7.7. USP United States Pharmacopeia

8. Responsibilities

8.1 Customer Responsibility

8.1.1 It is the responsibility of the Customer to provide accessibility to the instrument and areasonable window of time for the execution of this test script.

8.2 PerkinElmer Responsibility

8.2.1 The individuals executing these tests must be trained in the activities to be performed inthe Dissolution Tester system. The individuals listed in the following table wereinvolved with the execution and review of the Dissolution Tester system TestProcedures.


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8.3 Their signatures or initials will be found throughout this document. Table signatures indicatethat these individuals have read this test specification and will adhere to all specifiedprocedures.

Role Printed Name Signature Initials

Perkin Elmer Service Rep.

Customer Representative

9. System Description and Specifications

9.1. System Description

9.1.1 A dissolution tester comprising: bath/bathless heating system; a head disposed abovethe vessels plate, which moves up and down relative to the base; a cantilever arm forsupporting the head in a cantilevered fashion and for moving the head up and downrelative to the base; a vessel in which a sample and a test liquid are placed, and a test-liquid agitator suspended from the head, for agitating the sample and the test liquidinside the vessel.

9.1.2 The Dissolution bath system consists of a Motor Control Module, a TemperatureControl System, shafts, baskets, paddles, and six to eight vessels.

9.2. System Specifications

9.1.3 The vessel must have cylindrical sides and a hemispherical bottom which must besmooth and without defects. A fitted cover may be used to minimize evaporation. Thevessel conforms to one of the following dimensions and capacities as outlined in Table#1:

Table #1:

Capacity Internal Height Internal Diameter1L 160mm-210mm 98mm-106mm

2L 280mm-300mm 98mm-106mm4L 280mm-300mm 145mm-155mm

9.1.4 The shafts are fabricated of stainless steel, type 316, or other inert material. The shaftis positioned so that the axis is not more than 2mm at any point from the vertical axisof the vessel and rotates smoothly and without significant wobble.

9.1.5 The basket components are fabricated of stainless steel, type 316, or other inertmaterial. The attachment of the basket to the shaft can be done using retention springs


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or other suitable device. When attached to the shaft, the basket must rotate smoothlyand without significant wobble. The critical dimensions to be measured on each basketand shaft should include but not be limited to: shaft diameter, vent hole diameter,thickness of wide portion of the basket-to-shaft-adaptor, total basket height, internaldiameter of the basket, outer diameter of the screen, height of the open screen, outerdiameter of the basket, screen mesh diameter, and wire opening.

9.1.6 The paddle components are fabricated of stainless steel, type 316, or other inertmaterial. The paddle dimensions to be determined on each paddle should include butare not limited to: shaft diameter, blade height, blade thickness, total blade length atthe top of the blade, length of flat portion on bottom of blade, radius of the angle on thetop outer edge of the top of the blade, radius of the outside edge of the blade,difference between the distance from the midline of the shaft to the top outer edge for

the two sides, and difference between the heights of both sides of the paddles at theoutside top.

9.1.7 The shaft is positioned so that the axis is not more than 2mm at any point from thevertical axis of the vessel and rotates smoothly and without significant wobble. Thevertical center line of the blade passes through the axis of the shaft so that the bottomof the blade is flush with the bottom of the shaft. The paddle blade and shaft may becoated with a suitable material (e.g., Teflon) so as to make them inert.

9.1.8 Note: A suitable two part detachable design may be used provided the assemblyremains firmly engaged during the test.

10. Calibration and Test ProceduresThis test script shall be executed in accordance with the respective sections of this document.Wherever possible, "Expected Results" information is compared to actual results. Initials will beentered within Initials column of the Results table. Test that met acceptance criteria will bedocumented as Pass and those that does not meet the acceptance criteria will be documented asFail in the corresponding Pass/Fail column. For those Expected Results that include datesand/or times, the actual, observed dates/times used or displayed during the test must also berecorded within the Observed Results column.

Each test procedure entry shall be completed with a waterproof, indelible blue pen. Any mistakes orchanges shall be crossed out with a single line, initialed and dated by the tester. When a test

procedure is completed, the tester shall complete the actual results, Initials and Date cells at theend of each test to indicate its completion. When a testing section has been completed, the reviewershall review the sections completed by the Tester, sign and date the appropriate line.

If a discrepancy from the "Expected Result" occurs during the execution of a test, the tester will notifyimmediately the situation to the Instrument Specialist and to the Laboratory Supervisor who wildetermine actions to take as per companys standard procedure.

If the execution of a test procedure results in the generation of hard copy documentation the testershall log the document(s) into the Document Log of this document. Each document page will benumbered sequentially beginning with page 1 for the first document page. The tester will initial anddate each page. After all of the test scripts have been completed the total number of hard copy


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documentation pages will be determined. This number will then be added to each individual documentpage so that page numbering will read Page 1 of 23, Page 2 of 23, etc.

Perform the following in the order given for mechanical calibration of each apparatus. Perform thesetests every 6 months, after any repair, move, or as specified by the customer. If the instrument is not inroutine use, the mechanical calibration may be performed prior to performing the first dissolution testafter the six month interval.

The following test grid identifies the type of test covered in this test plan:

Tests & Procedures: PM OQ11.1 System Components and Test Materials Identification Form X

12.1 System Components Visual Inspection and Maintenance X

12.2 Shaft Wobble X

12.3 Paddle / Basket Shaft Verticality X

12.4 Basket Wobble Verification X

12.5 Vessel/Shaft Centering X

12.6 Vessel Verticality X

12.7 Basket and Paddle Depth X

12.8 Shaft Rotational Speed X

12.9 Timer Test X

12.10 Temperature Control Accuracy and Timer Test X

12.11 Vibration Test X

11. System Components and Test Materials Identification

The Dissolution Tester System consists of hardware for the dissolution testing of a variety o

pharmaceutical compounds. Perform the following tests to verify that the Dissolution Tester systemmeets the indicated performance specifications. Record the data generated in the appropriate spacefollowing each section.

The following System Identification Form will be used to record system-specific component informationabout the Dissolution Tester system being qualified. The form must be completed before the testing isbegun.


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11.1. System Component Identification Form

11.1.1. Site:

11.1.2. Building/Room:

11.1.3. Manufacturer:

11.1.4. Model Number:

11.1.6. Unit ID:

____________________

SN: ______________ Dissolution Tester System

Vessel #1 ID: _____________ Position: 1

Shaft #1 ID: _________


Shaft #2 ID: _________


Shaft #3 ID: _________


Shaft #4 ID: _________


Shaft #5 ID: _________


Shaft #6 ID: _________

Comments: _________________________________________________________________________________

Signature Date

Executed by:

Reviewed by:


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11.2. Calibration Equipment Identification FormEnter calibration data for equipment used for system functional verification.

DescriptionMinimum

ResolutionManufacturer

ModelNumber

SerialNumber

CalibrationDue Date

CalibrationReference

Digital Thermometer** 0.5C

Stopwatch 1seg

Tachometer** 1RPM

Centering Gauge** 1mm

Depth Gauge** 1mm

Wobble Gauge* ** 0.05mm

0.2 cm Limit Gauge N/A

Level* ** 0.1

Vibration Meter* ** 0.1mil

LabMetrixTM GLP(optional) N/A

QA Station (optional) N/A

* These items are not required when the optional QA station is used.

** These items are included in the LabMetrixTM GLP system.

Comments: _______________________________________________________

____________________________________________________________

Signature Date

Executed by:

Reviewed by:


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12. Dissolution Bath Test Cases12.1. System Components Visual Inspection

12.1.1. Perform general instrument verification

12.1.2. Inspect all system components.

Table 12.1 General System Verification Results:

Expected Results Results Initials Date

Inspect the vessels for any apparent damage.All vessels are free of defects

Defective vessels were replaced Inspect the baskets for any apparent damage.All baskets are free of defects

Defective baskets were replaced Inspect the paddles for any apparent damage.

All paddles are free of defects Defective paddles were replaced

Inspect the temperature sensors and shafts forany apparent damage.

All temperature sensors and shafts

are free of defects Defective temperature sensors and

shafts were replaced Ensure that all vessel centering arms and pivotposts are securely installed as per manufacturerspecifications.

Yes Not Required

Each paddle must be visually examined fordefects such as rusting of loose pieces ofcoating sticking out from the paddles.

All paddles are free of defects Defective paddles were replaced

Comments: ________________________________________________________________________________

Signature Date

Executed by:

Reviewed by:


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Table 12.1 General System Verification Results:

Expected Results Results Initials Date

Check that the release lock mechanism on thedrive head works as expected. Adjusted

No Adjustment Required Check the hydraulic actuator for smooth up anddown motion. Adjusted

Not Required

Comments: ________________________________________________________________________________

Signature Date

Executed by:

Reviewed by:

12.2. Shaft Wobble

1. A runout gauge is placed on top of the vessel plate, and the drive module is

positioned so that the gauge probe touches the shaft about 2 cm above the topof the paddle blade or basket.

2. The gauge is placed so that the probe slightly presses in on the turning shaft. Ifa mechanical gauge is used, the gauges pointer should read slightly more thanzero.

3. The pointer will vary from a minimum to a maximum reading, and the differenceis called the wobble. The specification is 1.0 mm total runout. The digital oanalog dial must be accurate to 0.05mm. Repeat for each shaft.

4. Upon removal and reinsertion, recalibration would not be required as long as

appropriate procedures for re-insertion and alignment are maintained, whichinclude numbering and specific location identification.


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Table 12.2 Shaft Wobble Test Result:SpindleNumber

Shaft ID Wobble (mm) Expected Result Pass / Fail Initials Date

Paddle

1

1.0mm

2

3

4

5

6Basket

1

1.0mm

2

3

4

5

6

Comments: ________________________________________________________________________________

Signature Date

Executed by:

Reviewed by:

12.3. Paddle / Basket Shaft Verticality

1. Ensure that the system is fitted with a stirring element in all spindle positions.

2. Lower the drive unit to where it would be during an actual dissolution test. Inecessary the shaft verticality may be checked with the shafts raised above thedrive unit. Place an accurate digital leveling device on the front edge of each ofthe shafts. Rotate the level 90 so it is on the side of the shaft to determine thatthe shafts are vertical in two directions 90 apart around the vertical axis whilethe drive unit is in the operating position.

3. If the shafts are not vertical adjust the feet of the apparatus until they arevertical.

4. The shaft must be 0.5 from vertical. The digital or analog levels must be


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accurate to 0.1.Table 12.4.1 Paddle Verticality Test Result:

ShaftNumber

Paddle ID From Vertical @

Point 1 From Vertical @

Point 2Expected Result

Pass /Fail

Initials Date

1

Shaft must bevertical. The levelshould read 0.5

from vertical.

2

3

4

5

6

Table 12.4.2 Basket Verticality Test Result:Shaft

NumberBasket ID

From Vertical @Point 1

From Vertical @Point 2

Expected ResultPass /

FailInitials Date

1

Shaft must bevertical. The levelshould read 0.5

from vertical.

2

3

4

5

6

Comments: ________________________________________________________________________________

Signature Date

Executed by:

Reviewed by:

12.4. Basket Wobble (Apparatus 1) Verification

1. Raise the drive head upwards and lock.

2. Remove all vessels and identify the position # on each of them to ensure theyare returned to the same position. The shafts should remain as-is.

3. Bring down the drive head and lock in position so that the tip of the meter andthe baskets lowerrim are very close.

4. A runout gauge is placed on top of the vessel plate and the drive unit ispositioned so that the gauge probe touches the bottom rim of the basket.

5. The gauge is placed so that the probe slightly presses in on the bottom rim othe turning basket. If a mechanical gauge is used, the gauges pointer should


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read slightly more than zero.6. The pointer will vary from a minimum to a maximum reading and the difference

is called the wobble. The specification is 1.0 mm total runout. The digital oanalog indicator must be accurate to 0.05mm. Repeat for each basket.

Table 12.4.1 Basket Wobble Verification Results-Basket:

SpindleNumber

Basket IDWobble @ bottom rim

of basket (inch) Expected ResultPass / Fail Initials Date

1

1.0mm

2

3

4

5

6

Comments: _________________________________________________________________________________

Signature DateExecuted by:

Reviewed by:


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12.5. Vessel/Shaft Centering

1. The vessel plate of an apparatus may warp or bend or the thickness of a vesselip or centering collar lip may not be perfectly uniform. If either of these occurseven though the shafts are vertical and the vessel plate is level, the vessel wallsmay not be vertical.

2. Use centering tools which measure centering inside the vessel. Two centeringtools are used to center the vessels around the paddle or basket shafts and toalign the vessels so that their sides are vertical.

3. For the paddle method, the bottom of one centering tool is placed 2 mm above

the top of the paddle blade and the bottom of the second centering tool isclamped on the shaft 80 mm above the blade with the probes positioned in thesame direction towards the glass vessel wall.

4. For the basket method, the bottom of one centering tool is placed 2 mm abovethe top of the basket and the bottom of one centering tool is placed 60 mmabove the top of the basket with the probes positioned in the same directiontowards the glass vessel wall.

5. Carefully lower the shaft and centering tools into the vessels so that the paddleblade or basket bottom is about 2.5 cm above the bottom of the vessel.Manually rotate the shaft slowly and check the centering at both levels. If the

vessel is not centered at either level, adjust the vessel to center it. Adjustmentscan be made by rotating the vessel or the vessel with the centering collar insidethe vessel plate, moving the vessel sideways within the vessel plate or placingshims (such as tape) under one side of the lip of the vessel or vessel centeringcollar.

6. Repeat this process until both bottom and top positions are centered within 1.0mm from the center line. The digital or analog centering/verticality tool must beaccurate to 0.2mm.

7. An alternative procedure is to use a mechanical or digital centering device thacenters the inside of the vessel around the shaft or a surrogate shaft. The

centering is measured at two positions inside the vessel in the cylindricaportion, one near the top but below the rim and one just above the bottomportion of the vessel just above the basket or vessel blade. The shaft osurrogate shaft must be centered within 1.0 mm from the center line.

8. Perform the measurements and document for each position sequentially.


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Table 12.5.1 Vessel/Shaft Centering Result:

SpindleNumber Shaft ID Vessel ID

Centerline MeasurementDistance from Vertical Axis

measured at lower position (mm)Acceptance

CriteriaPass /

Fail Initials Date

Position 1

1

1.0 mmfrom

centerline

2

3

4

5

6

Position 2

1

1.0 mmfrom

centerline

2

3

4

5

6

Comments: _________________________________________________________________________________

Signature Date

Executed by:

Reviewed by:


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12.6. Vessel Verticality

1. The vessel verticality can be calculated using the centering measurements andthe difference in height between the two measurements or it can be determinedusing a digital leveling device placed on the inside wall of the vessel.

2. The verticality should be determined at two positions 90 apart. Adjustments canbe made by placing shims (such as tape) under one side of the lip of the vesselor vessel centering collar. The vessel must be 1.0 from vertical at bothpositions. The digital or analog centering/verticality tools

3. After each vessel has been centered and made vertical, each vessel and vesse

plate opening must be numbered and a mark must be placed on the lip of eachvessel and on the vessel plate directly next to the mark on the vessel lip.

4. Each vessel must be returned to the same vessel plate opening and positionedin the exact same position inside the vessel plate opening for all futuredissolution tests.

5. Using a Digital Level:

a. A small digital level can be used to measure vessel verticality. This isdone by placing it on the straight inside wall of the vessel above thespherical bottom and below the lip of the vessel.

b. This is then repeated at a second position on the inside vessel surfacethat is approximately 90 from the first measurement. The vessel musbe 1.0 from vertical. The digital or analog centering/verticality toolsmust be accurate to 0.2mm.

c. There are automated digital levels that are connected to a controller thaallow the degrees to read directly from the display.

6. Manual Calculations:

a. Before determining vessel verticality, ensure that the paddle or baskeshaft is vertical. Make measurements at two vertical positions. There aretwo options for these measurements: either two tools are positioned onthe shaft with the probes positioned in the same direction forsimultaneous measurements or the measurement can be conductedsequentially by repositioning the tool.

b. The difference in the readings at the two vertical positions is the amounthat the vessel is out of verticality over the distance between the twoprobes. From this measurement and the vertical distance between thetwo gauge probes, the verticality can be determined in degrees.

c. Degrees out of verticaliy = Arctan (X/Y)


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Where:

X: is the Deflection (mm), (=XA/XB) between the two gauges

Y: is the distance (mm) between measurement points

Arctan: is the principle value of the inverse tangent of the ratio of the rise(Y) over run (X) and calculates the angle in degrees (See figure below.)

Figure #1: Arctan Measurement for Vessel Verticality


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Table 12.6.1 Vessel Verticality Result:

Basket

SpindleNumber

Vessel ID Straight portion ofvessel at position 1 ()

Straight portion ofvessel at position 2 ()

AcceptanceCriteria

Pass /Fail Initials Date

1

1.0 fromvertical

2

3

4

5

6

Paddle

1

1.0 fromvertical

2

3

4

5

6

Comments: _________________________________________________________________________________

Signature Date

Executed by:

Reviewed by:


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12.7. Basket and Paddle Depth

1. The actual distance between the bottom of the vessel and bottom of the baskeor paddle is determined. If the depth of the basket/paddle is adjustable, first adepth gauge is used to set the distance between the bottom of the paddle bladeor basket and the bottom of the vessel.

2. The depth gauge is set at 25 mm and placed on the bottom of the vessel. Eachshaft is raised into the apparatus drive module. The drive unit is then lowered toits operating position.

3. The paddle or basket is then lowered into the vessel until it touches the top o

the depth gauge. The shafts are locked into this height.

4. This is repeated for each shaft. The specification is 25 mm 2 mm.


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12.8. Shaft Rotational Speed

1. Set the RPM to the required RPM value. Remove the plug in the back center ofthe drive head cover to expose the location for RPM measurement. Bring the tipof the tachometer probe in contact with the recessed portion on top of the shaftin one any position and hold it as close to vertical as possible. If an opticaltachometer is used, place a piece of reflective tape around any shaft at aconvenient height to be able to comfortably aim the light beam from thetachometer but not in a section of the shaft which would come in contact withthe medium during a run.

2. After approximately one minute, measure the spindle speed.

3. A tachometer should be used to measure the rotational speed of the paddle orbasket. The shafts should be rotating smoothly at 2 rpm or 2%, whichever islarger, of the target value.

4. The digital or analog rotational tools must be accurate to 1 RPM.

5. Change the RPM to the next required setting and repeat the measuremenprocedure.

6. If the system is not capable of achieving the specified speed skip that testRecord the results in table below and compare the results with the RPMtolerance.

Table 12.8.1 Shaft Speed Test Results:

Set SpeedRPM

Current Speed ExpectedRPM

Pass / Fail Initials Date

50 48-52

100 98-102

150 147-153

250 242-258

Comments: _________________________________________________________________________________

Signature Date

Executed by:

Reviewed by:


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12.9. Timer Test

1. The timing is measured by simultaneous activation of a calibratedtimer/stopwatch and an action on the unit, which then results into anaudible/visible signal on the unit at the appropriate time. Since all the tankswould have to be executed/monitored by the same person, these measurementsdepend on the precision of the coordination. Setup a 3 min step procedure. Theacceptance criterion of 4 seconds takes into account the degree of difficulty toprecisely coordinate all actions.

2. Follow the display prompts and start the calibrated timer/stopwatchsimultaneously with the starting of the run. Follow the display prompts and star

the run. Document the time it takes to complete a sequence versus the timer.

Table 12.9.1 Timer Accuracy Result:

Test Task ExpectedResults

Observed Results Pass /Fail

Initials Date

1Programmed Sample Time =3 min

4 seconds(mm:ss) = ___________

Comments: _________________________________________________________________________________

Signature Date

Executed by:

Reviewed by:

12.10. Temperature Control Accuracy Test

1. Ensure each vessel is filled with 900mL of DI water. Lower the drive head inposition and cover each vessel.

2. First, using a calibrated thermometer (reference), sequentially measure thetemperature in each vessel and simultaneously compare with the temperaturevalue displayed for the respective vessel.

3. Next, compare each of the recorded values for the thermometer reference withthe set temperature of 37.0C. The measured value for each vessel shouldagree with the set temperature within 0.5C. This will verify the accuracy of thecalibration.


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Table 12.10.1 Temperature by Vessel Result:A B C

VesselVessel

ID

SetTemp.( C )

DisplayTemp.(C )

ReferenceTemp.( C )

[A-B]( C )

[B-C]( C )

[A-C]( C )

Acceptancecriteria( C )

Pass /Fail

Initials Da

1 37.0 0.5

2 37.0 0.5

3 37.0 0.5

4 37.0 0.5

5 37.0 0.5

6 37.0 0.5

Comments: _________________________________________________________________________________

Signature Date

Executed by:

Reviewed by:

12.11. Vibration Test

1. Ensure that each vessel contains 900mL of DI water.

2. Set the drive head in the operating position and lock.

3. Set the RPM at 50 and run.

4. Measure the base plate vibration with a vibration meter. Repeat procedure a100 RPM.

5. The maximum should be 0.1 mls vertical displacement.

6. Repeat the test with all baths in the same bench running at the same time.


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Table 12.11.1 Vibration Result:Standard Test

Base Plate Vibration @ 50RPM in mils Acceptance Criteria Pass / Fail Initials Date

0.1 mls verticaldisplacement



Test with all dissolution baths running at the same time





Comments: _________________________________________________________________________________

Signature Date

Executed by:

Reviewed by:


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13. Document LogEvery page of hard-copy testing documentation must be logged onto this form, following the directionsset forth in Test Procedures. When all testing is completed, all hard-copy documentation must be affixedto the back of this log.

Attachment # Page(s) Description Initials / Date


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14. Post approval Signatures & Certification

Instrument Preventive Maintenance & Calibration Certification

This is to certify that the tests in procedure DBSVCPM/OQ-10-05 have been performed and the configuration testedmeets / does not meet the tests specifications listed on this protocol. This certificate does not modify

PerkinElmer's standard terms and conditions of sale, including warranty terms. PerkinElmer assumes no liability fortest results. Any test non-conformance must be accepted by the customer with the agreement of both parties thatthe system will perform in an acceptable manner while this non-conformance is fixed.

Instrument: Dissolution Tester System Mechanical Calibration

ID Number: _____________________________________

Manufacturer: ____________________________ Model: ___________________

Calibration Equipment used:

Instrument Type Instrument ID/Serial #Calibration

DateExpiration

Date

Customer: __________________________________ Location of calibration: ________________________

Date of calibration: ______________________

Service Engineer Name / Signature: ____________________________________________ Date: _______________

Customer Representative Name / Signature: _____________________________________ Date: _______________

This certificate is composed of 2 pages. This is page 1 of 2.


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Instrument Preventive Maintenance & Calibration Certification (Continued.)

Instrument: Dissolution Tester System Mechanical Calibration

ID Number: __________________________ Model: ______________

This certifies that the above product was calibrated in compliance with a quality system registered to

ISO9001:2000 using applicable PerkinElmer LAS procedures.

Released conditions: At the completion of the calibration, measured values were IN-SPECIFICATION.

Remarks or special requirements:

____________________________________________________________________________________________

_______________________________________________________________

The calibration procedures are designed to provide measurement uncertainty of less than or equal tospecifications included in the corresponding test protocol. The test limits stated in the report correspond tothe published specifications of the equipment, at the points tested.

The User should determine the suitability of this instrument for its intended use. This is page 2 of 2. Basedon the manufacturer recommended or user requested calibration interval, the next calibration is due on________________________.

Service Representative

Signature indicates agreement by the ServiceRepresentative that this test plan has beenexecuted as written, providing sufficientdocumented evidence that the instrument inquestion performs according to the appropriatemanufacturers specifications.

_________________________________Service Representative / Signature

___________Date

Customer Representative

Signature indicates agreement by theCustomer Representative that this test plan hasbeen executed as written, providing sufficient

documented evidence that the instrument inquestion performs according to the appropriatemanufacturers specifications

_________________________________

Customer Representative / Signature

___________

Date

DBSVCPMOQ 10 05(Enhanced Mechanical)

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