Dissolution apparatus Calibration SOP


1.0  OBJECTIVE:
To lay down the calibration procedure of Dissolution apparatus.
2.0  SCOPE:
This shall be applicable to the Dissolution apparatus of Quality Control Instrument Laboratory.
3.0  RESPONSIBILITY:
3.1  Technical Assistant/ Helper.
3.2  Q.C Analyst.
4.0  ACCOUNTABILITY:
4.1  Manager-Quality Control.
5.0  MATERIAL AND EQUIPMENT:
5.1  Dissolution apparatus.
5.2  Calibrated thermometer.
5.3  Purified water.
6.0  PROCEDURE:
6.1  Switch ON the mains.
6.2  Operate the apparatus according to SOP.
6.3  Calibration of RPM:
6.3.1        Enter the required RPM value in the range of 30 to 200.
6.3.2        Press ENTER key to terminate. The SET RPM key LED will now be put off. If the RPM value is not in the range error message Er is displayed on the RPM display.
6.3.3        If the error message is displayed then go back to resetting. If the error message “Er” is displayed on the RPM display and the ENTER key is pressed then the last correctly set value of RPM for that step will be accepted and the SET RPM LED will be put off.
6.3.4        Suppose the RPM VALUE 100 is to be entered. First press the SET-RPM key. The SET-RPM key LED will be illuminated. Next press no. 1 key once following by 0 key twice. Then press ENTER key. The SET-RPM key LED will go OFF. Then the RPM DISPLAY will show 100.
6.3.5        Record the RPM manually & enter in the calibration log.
6.4  Calibration of Temperature:
6.4.1        Press the SET key. The SET TEMP key LED will be illuminated TEMP.
6.4.2        Enter the required temperature value in the range of 30oC to 100oC.
6.4.3        Press ENTER key to terminate. The SET TEMP key LED will now be put off. If the TEMP value is not in the range error message Er is displayed on the TEMP display. If the error message is displayed then go back to resetting.
6.4.4        If the error message “Er” is displayed on the TEMP display and the ENTER key is pressed then the last correctly set value of TEMP for that step will be accepted and the SET TEMP LED will be put off.
6.4.5        Set the temp. 35oC, 37oC & 40oC and check the temperature of bowl with the thermometer & record the data in calibration log.
6.4.6        To view the set temperature presses the SET TEMP key again. Then the TEMP DISPLAY will show set TEMP in oC.
6.4.7         If the calibration is not found within the specified limits immediately inform to QC head.
6.4.8        Affix the calibration label on the instrument.
6.5  Calibration of Apparatus suitability:
6.5.1        Calibration for Disintegrating Type:
6.5.1.1  Prepare standard solution of Prednisone:
6.5.1.1.1        Prepare the standard solution by dissolving the 25mg of prednisone to 50.0ml of purified water.
6.5.1.1.2        Further dilute 5.0ml from this solution to 50.0ml with purified water.
6.5.1.1.3        Again make dilution of this 5.0ml to 25.0ml with purified water.
6.5.1.1.4        And take absorbance at 242nm against the purified water.
6.5.1.1.5        NOTE: If the standard is not dissolve first add not more than 2.5ml of alcohol.
6.5.1.2  Dissolution calibration by using Prednisone tablet:
6.5.1.2.1        Ensure that mains of instrument and supply are “ON”.
6.5.1.2.2        Set the time program for 30 min, temperature 37oC±0.5oC and for 50 RPM.
6.5.1.2.3        Fit the required apparatus paddle.
6.5.1.2.4        Place 900.0ml of deaerated water. De-aerate the purified water according to SOP for de-aeration of dissolution media.
6.5.1.2.5        After achieving the temperature place one tablet in each bowl and start the time program.
6.5.1.2.6        After completion of time program withdraw the sample solution from each bowl and filter through the filter paper in individual tubes. Discard first 50.0ml filtrate, take 5.0ml of filtrate and dilute with purified water to 25.0ml and take the absorbance at 242nm against the purified water.
6.5.2        Calculate the content of prednisone.
6.5.3        Also carry out above procedure for 100 RPM.
6.5.4        Enter the data in the calibration record.
6.5.5        Also carry out above procedure by changing the basket apparatus for 100 RPM and enter the data in calibration log.
6.5.6        Precautions:
6.5.6.1  If the calibration is not found within the specified limits immediately inform to QC head.
6.5.6.2  Record the result on the “Calibration Record”, “Calibration Log Book” & paste the “Calibration Status Sticker” on Dissolution apparatus.
6.5.6.3  In case of noticing any malfunctioning of instrument, inform the maintenance dept. and Head of dept.
6.6  Checking of physical parameters for the apparatus:
6.6.1        Basket:
6.6.1.1  Make identity of each basket which is in use and make the inventory.
6.6.1.2  Check the physical parameters for the each basket like appearance, opening, height, total height of basket, ID of basket, external diameter of basket, external diameter of ring, vent hole diameter, height of coupling disk.
6.6.1.3  All parameters should be fall within the limit as given in the calibration log.
6.6.2        Paddle:
6.6.2.1  Make identity of each paddle which is in use and make the inventory.
6.6.2.2  Check the physical parameters for the each paddle like appearance, height, shaft diameter, blade upper chord, lower chord, height, radius (disk), thickness, and distance from bottom, distance shaft axis and vertical axis of vessel.
6.6.2.3  All parameters should be fall within the limit as given in the calibration log.
6.7  Checking of wobbling, rotations & distance parameters for the apparatus:
6.7.1        Wobbling:
6.7.1.1  Fix the paddle/ basket apparatus to the instrument, lower the apparatus.
6.7.1.2  Fix the wobbling meter on the top of the bowl.
6.7.1.3  The needle of wobbling meter should touch to the surface of the apparatus.
6.7.1.4  Measure the wobbling on the meter.
6.7.2        Rotations:
6.7.2.1  Fix the paddle/ basket apparatus to the instrument.
6.7.2.2  Set the RPM 50/100.
6.7.2.3  The needle of tachometer should touch to the surface of the apparatus.
6.7.2.4  Press the “Start” key of tachometer to start.
6.7.2.5  Fix the tachometer with apparatus.
6.7.2.6  Start the rotation.
6.7.2.7  The tachometer will show result on display.
6.7.3        Distance from the apparatus:
6.7.3.1  Fix the paddle/ basket apparatus to the instrument, lower the apparatus.
6.7.3.2  Insert the vernier calipers between the bottom of the apparatus and the bottom of the bowl.
6.7.3.3  Measure the reading on the display.
7.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

8.0  REFERENCES:
8.1  Not Applicable.
9.0  ANNEXURES:
Annexure 1: Calibration of RPM of Dissolution apparatus.
Annexure 2: Calibration of Temperature of Dissolution apparatus.
Annexure 3: Calibration Log of Suitability of Dissolution apparatus (by disintegrating type).
Annexure 4: Checking of Physical parameters of Basket/ Paddle.
Annexure 5: Checking of wobbling, rotation & distance parameters of apparatus.


Annexure: 1
Calibration of RPM of Dissolution Apparatus
Calibration of RPM of Dissolution apparatus
Calibration date
Date of last calibration done
Next due for calibration



INSTRUMENT DETAILS:
Model no.
Make
Instrument code no.:



OBSERVATIONS
Sr.#

Set values
Observed value
Limits
1
2
3
4
5
6

1.
Calibration of RPM
50






48-52
100






96-104
150






144-156

Conclusion: Satisfactory/ Not satisfactory.

Done by/date
Checked by/date










Annexure: 2
Calibration of Temperature of Dissolution apparatus
Calibration of Temperature of Dissolution apparatus
Calibration date
Date of last calibration done
Next due for calibration



INSTRUMENT DETAILS:
Model no.
Make
Instrument code no.:
Thermometer code no.:


OBSERVATIONS
Sr.#

Set values
Observed value
Limits
1
2
3
4
5
6

1.
Calibration of temperature
35oC






34.5oC-35.5oC
37oC






36.5oC-37.5oC
40oC






39.5oC-40.5oC

Conclusion: Satisfactory/ Not satisfactory.

Done by/date
Checked by/date










Annexure: 3
Calibration Log of Suitability of Dissolution apparatus (by disintegrating type)
Calibration Log of Suitability of Dissolution apparatus (by disintegrating type)
Calibration date
Date of last calibration done
Next due for calibration



INSTRUMENT DETAILS:
Model no.
Make
Instrument code no.
Lot no. of tablet




OBSERVATIONS
Standard preparation:
Transferred ______mg to 50.0ml in volumetric flask, dissolved and diluted to 50.0ml with purified water.
Diluted _______ml to 50.0ml with purified water and mix.
Diluted _______ml to 25.0ml with purified water and mix.
Weight of tablet
Dissolution time
Diluted to
(5ml to 50ml)
Diluted to
(5ml to 25ml)
UV reading at 242nm
Remarks
From
To
1.






2.






3.






4.






5.






6.









Sr.#
Set apparatus
Observed value
50 RPM
100 RPM
Limits
1.
Apparatus I
Min.



Max.



Mean.



2.
Apparatus II
Min.



Max.



Mean.




Conclusion: Satisfactory/ Not satisfactory.

Done by/date
Checked by/date

















Annexure: 4
Checking of Physical parameters of Basket/ Paddle
Checking of Physical parameters of Basket
Calibration date
Date of last calibration done
Next due for calibration



INSTRUMENT DETAILS:
Model no.
Make
Instrument code no.



OBSERVATIONS
Sr.#
Parameter
Specifications 
Observed value
Remarks
1
2
3
4
5
6
Mean
1.
Total height of basket
37.0±3.0mm








2.
Height of screen
27.0±1.0mm








3.
ID of screen
20.2±1.0mm








4.
External diameter screen
22.2±1.0mm








5.
External diameter of ring
25.0±0.02mm








6.
Hole diameter
2.0±0.5mm








7.
Height of coupling disk
5.1±0.5mm








8.
Distance from bottom
25.0±2.0mm








Conclusion: Satisfactory/ Not satisfactory.
Done by/date
Checked by/date



Checking of Physical parameters of Paddle
Calibration date
Date of last calibration done
Next due for calibration



INSTRUMENT DETAILS:
Model no.
Make
Instrument code no.



OBSERVATIONS
Sr.#
Parameter
Specifications 
Observed value
Remarks
1
2
3
4
5
6
Mean
1.
Shaft diameter
9.4±10.1mm








2.
Blade upper chord
74.5±0.5mm








3.
Blade lower chord
42.0±1.0mm








4.
Paddle height
19.0±0.5mm








5.
Thickness
4.0±1.0mm








6.
Distance from bottom
25.0±2.0mm








Conclusion: Satisfactory/ Not satisfactory.
Done by/date
Checked by/date











Annexure: 5
Checking of wobbling, rotation & distance parameters of apparatus
Checking of wobbling, rotation & distance parameters of apparatus
Calibration date
Date of last calibration done
Next due for calibration



INSTRUMENT DETAILS:
Model no.
Make
Instrument code no.



OBSERVATIONS
Test unit
Paddle wobble
Basket wobble
Paddle rotation
D1
(mm)
D2
(mm)
USP standards
(2.0mm)
(2.0mm)
(4% of set rpm)
(25.0±2.0mm)
(25.0±2.0mm)
50 RPM
100 RPM
1.






2.






3.






4.






5.






6.






D1
Distance between the bottom edges of the blade to the lowest inner surface of the vessel.
D2
Distance between the bottom edges of the basket to the lowest inner surface of the vessel.
Conclusion: Satisfactory/ Not satisfactory.
Done by/date
Checked by/date





10.0    ABBREVIATIONS:
Abbreviation
Expanded Form
SOP
Standard operating procedure
&
And
No.
Number  
Ltd.
Limited
Q.C
Quality control
Q.A
Quality assurance
QCEB
Quality control equipment calibration
F
Format
g
Grams
mm
Millimeters
%
Percentage
Sr.#
Serial number
RPM
Rotation per minute
oC
Degree centigrade
ml
Milliliter
mg
Milligram
nm
Nanometer
ID
Identification
UV
Ultra violet
Max.
Maximum
Min.
Minimum
min
Minutes


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