SOP for Calibration of Dissolution Test Apparatus (Make: LAB INDIA)

OBJECTIVE

The purpose of this SOP is to lay down a procedure for the Calibration of Dissolution Test Apparatus.

SCOPE

This SOP is applicable for the Calibration of Dissolution Test Apparatus of Make: LABINDIA, Model No: DS8000 & Model No: DS14000 installed at the Quality Control Laboratory of PharmaInfo Ltd.

RESPONSIBILITY

The analyst / Section Head or his designee shall be responsible for following the SOP.

The Head of the Quality Department or his designee shall be responsible for and implementation of the SOP.

PROCEDURE

Calibration Frequency: Physical Calibration: Monthly

Carry out the calibration check for the following physical parameters on a monthly basis:

1. Rotational speed
2. Water bath temperature
3. Timer
4. Shaft wobbles
5. Distance from paddle/basket to the bottom of the jar.
6. Distance between the shaft axis and vertical axis of the vessel.
7. Head coplanarity.
8. Integrity checks and mesh size of the basket.

Revolution Check

• Select any one paddle or basket and check the number of revolutions using a tachometer. 
• Repeat the same procedure for the other eleven paddles/baskets.
• The above result should fall within the limits specified below:

Acceptance criteria:

Number of Revolutions (RPM)	Limits (RPM)
50	48 – 52
100	96 – 104
125	120 – 130

Temperature Check

• Set the temperature to 37°C and wait for the display to show 37°C at both the bath and individual jars. 
• Record the temperature in all jars by keeping the thermometer in the jars.

Acceptance criteria:

The observed temperature in each position of jars in normal in the range of 36°C to 37.5°C/

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Calibration of Timer

• Adjust the ‘SET TIME’ to 30 minutes, press the start button, and simultaneously start the stopwatch. 
• When the alarm starts, check the time on the stopwatch.
• Follow the procedure for 60 minutes as above.

Acceptance criteria:

Set time Tolerance

1. 30 minutes: Between 29 min 24 Seconds and 30 min. 36 Seconds.
2. 60 minutes: Between 58 min 48 Seconds and 61 min. 12 Seconds.

Wobble Check

• Check the calibration for the wobble of the paddle and basket using the wobble meter.
• Empty all the jars and keep them without the jar lid in their respective positions.
• Lower the stirrer unit so that the blabs of blades of the paddle/basket just enter the jars. Ensure that the paddle or basket rod is properly tightened on the spindle.
• Use the key provided to tighten it. Fix the wobble meter in the stand and attach it to the jar in such a way that the sensor of the dial gauge just touches the body of the paddle without any obstruction. Start the rotation of the paddle/basket rod.
• Check the maximum deviation of the pointer of a device on both sides of ‘0’ and add the reading. Carry out this procedure for 50 and 100 rpm and measure the wobble (in mm) from the dial gauge

Acceptance criteria

1. The tolerance for wobble is not more than 0.5 mm for paddles and 1 mm for baskets.
2. Check the wobble of all paddles and baskets.

Measurement of distance from paddle/basket bottom to jar

• Keep all the jars empty and remove all jar lids. Clamp all the jars using the jar holder
• Provided on jar plate and lower the stirrer unit to the bottom-most position till it stops automatically. 
• Hold the vernier vertically and touch parallel to the paddle shaft. 
• Touch the reference bracket of the vernier vertical and touching parallel to the paddle. 
• Slide the vernier scale down till the point of the stylus touches the jar bottom. Lock the vernier at this position and note the reading repeat the procedure for the remaining paddles. 
• The correction factor for paddle Measurement is 0.4 mm.
• Actual reading – Vernier Reading + Correction Factor

Acceptance criteria:

The distance should be 25 mm ± 2mm.

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Head co-planarity

• A spirit level should be used to ensure that both the head plate and base plate are perfectly horizontal.
• A spirit level should be kept on the head plate to check that the head plate is perfectly horizontal. If it is not horizontal, the bath should be removed and the base plate under the bath should be checked with the spirit level.
• A base plate should be brought to the planarity and then the bath should be kept in its place and the head plate should be checked for the planarity.

Integrity check of the basket

• Check the integrity of the SS wire mesh by holding the basket under an illuminated magnifier in seven baskets.

Note: If SS wire mesh is found to be damaged, discard the basket

Acceptance criteria: The mesh should be intact.

Mesh size of basket

• Use a magnifying lens provided with a bracket of one inch (distance between a to b) half inch(distance between c to d) and a quarter inch (distance between e to f) to check the number of openings of a mesh of the basket.
• Keep the basket in a vertical position. Place the lens on the portion of the mesh of which the mesh number is to be determined, such that the bracket is resting on the mesh.
• Ensure that the bracket and the wire mesh are aligned. Observe the lens and count the number of openings in a linear half-inch portion. Multiply the number by 2 to determine the number of openings per linear inch. Place the basket in the horizontal position. Take two observations.

Calculation:

1. Number of openings per linear inch = Number of openings of the wire mesh per linear half x 2.
2. Repeat the procedure for the remaining baskets.

Acceptance criteria: The number of openings should be 40 per linear inch.

Maintenance

1. Replace the water in the water bath once in 8 days or whenever it is found to be turbid and clean the water bath before adding the fresh water.
2. Do not pull or force the paddle or basket.
3. Check the integrity of the basket prior to use.
4. Baskets and paddles must be controlled for any damage prior to use. Deformed baskets or dented paddles must be taken out of use and discarded.
5. If the lifting arrangement is jammed, make it free by using the lifting screw adjustment located at the side of the motorized unit.
6. Oil the lifting arrangement regularly and smooth operation.

ANNEXURE

Annexure-I: Calibration Datasheet for physical calibration DS 14000

Annexure-II: Calibration Datasheet for physical calibration DS 8000

REFERENCES

Instrument Manual

REVISION HISTORY

Nil

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