INSTRUMENT CALIBRATION

DISSOLUTION APPARATUS
 HORIZONTALITY:

Place the spirit level on the long side of bench top, base of the
instrument, vessel support plate and observe the bubble of the spirit
level.

Similarly place the spirit level on the short side of bench top, base of the
instrument, vessel support plate observe the bubble of the spirit level.

Acceptance Criteria: The bubble should be within the lines of spirit

level.
 TIMER:

Prepare the program as per procedure with sampling time of 15

min, 30 min and 1 hour.

Start the run and at the same time start the calibrated stop watch.

Note down the time in which the sample drawing starts by syringe

Acceptance criteria: The observed value should be ± 2% for time

interval i.e. 15mins ± 18secs, 30mins ± 36secs and 60mins ± 72secs.
 CENTERING OF THE VESSEL:
Place the two hemisphere blocks of the centering device at the mouth
of the jar, with the paddle connected.

Fix the paddle in position and lower it in the bowl not more than 2 cm
below the vessel flange.

Place the wobble check meter on the bowl. Adjust the wobble check
meter such that the sensor just touches the shaft of the paddle. Adjust
the zero point on the dial of the wobble meter.
Slowly rotate the wobble check meter on the periphery of the bowl
for 360° and note the number of units deflected from zero in
clockwise and anti-clockwise direction.

Evaluation of the centering of stirring element shaft from centre:

 CENTERING OF THE VESSEL:
Evaluation of the centering of stirring element shaft from centre:

(A+B) X LC
D = ----------------
2
D = Centering of stirring element shaft from centre (mm)
A = number of units deflected from zero in clockwise, on the dial gauge during
360° rotation
B = number of units deflected from zero in anti-clockwise, on the dial gauge
during 360° rotation
LC= Least count of wobble check meter in mm

Acceptance criteria:
The value obtained for centering of stirring element shaft (D), should be not
more than 2.0 mm.
 PADDLE WOBBLE:
Attach the paddle apparatus and lower the central unit till half way.
Place the wobble check meter on the Bowl

Adjust the wobble check meter such that the sensor just touches the shaft of the paddle
about 1 cm above the blade.

Adjust the zero point on the dial of the wobble meter.

Set the paddle speed to 50 rpm and note the number of units deflected from zero in
clockwise and anti-clockwise direction.

Evaluation of paddle wobbles:

Paddle wobble in mm = (A + B) x LC
A = number of units deflected from zero in clockwise, on the dial gauge
B = number of units deflected from zero in anti-clockwise, on the dial gauge
LC= Least count of wobble check meter in mm

Acceptance criteria: Shaft wobble should be NMT 0.5 mm.

Note: Limit For basket: NMT 1.0
 DISTANCE FROM PADDLE / BASKET BOTTOM TO BOWL:

Place all empty jars in the tester and lock the jars.

Attach the paddles and lower the central unit till its lower end
limit.
Measure the distance between the inside bottom of the vessel
and bottom of the paddle blade, by means of a depth gauge

Repeat for baskets

Acceptance criteria: Distance from paddle/basket bottom to

bowl should be 25 mm ±2 mm.
 ROTATIONS PER MINUTE:

Attach the paddle apparatus and lower the central unit.

Set the rotations per minute as 25.

Measure the rotations of each shaft using a calibrated

tachometer.

Repeat step by setting RPM at 50, 100 and 150.

Acceptance criteria: Observed RPM should be ± 4 % of set RPM.

 TEMPERATURE:

Pour 500 mL purified water as dissolution medium in each jar.

Set the temperature control of the instrument to achieve 37°C
Connect paddles at all positions and insert the temperature
probe in a jar.
Set the RPM as 50 and start the stirrer.
Note down the temperature of each vessel using a calibrated
thermometer and dissolution system.

Acceptance criteria: Observed temperature should be 37°C ±

0.5°C.
 CHEMICAL CALIBRATION-PERFORMANCE VERIFICATION TEST (PVT):

Apparatus : USP-I(Basket)or USP-II (Paddle)

Dissolution medium : 499.0g (corresponding to 500 mL)
deareated water or as per certificate of Prednisone tablets.
Temperature: 37ºC  0.5ºC, RPM: 50 rpm
Time: 30 minutes , Ref Product: Prednisone tablets

Acceptance criteria: Compare the GM and % CV of single-

stage acceptance criteria given in the certificate of the
current lot of USP Prednisone Tablets RS for PVT. The GM
must not fall outside the limits, and the % CV must not be
greater than the limit.