Calibration of equipments

By: Shravan Kumar

What is Calibration ?
Calibration:

The demonstration that a particular

instrument or device produces results within
specified limits by comparison with those
produced by a reference or traceable
standard over an appropriate range of
measurements .
 OR

Calibration is a comparison between measurements –

one of known magnitude or correctness made or set
with one device and another measurement made in
as similar a way as possible with a second device.
STANDARD DEVICE:
The device with the known or assigned correctness is called the
standard.

UNDER TEST DEVICE:

The second device is the unit under test, test instrument, or any of
several other names for the device being calibrated.
Requirement of Calibration
 •Control of weighing
•Control of measuring

•Control of monitoring and

•Control test equipment

that is critical for assuring the quality of intermediates or

APIs should be calibrated according to written procedures and
an established schedule.
Procedure for Calibration !
1. Equipment calibrations should be performed using
standards traceable to certified standards, if existing.

2. Records of these calibrations should be maintained.

3. The current CALIBRATION status of critical EQUIPMENT

should be known and verifiable.
1. Instruments/equipments that do not meet calibration
criteria should not be used.

2. Deviations from approved standards of calibration on

critical instruments/equipments should be investigated
to determine if these could have had an impact on the
quality of the intermediate(s) or API(s) manufactured
using this equipment since the last successful calibration.
Here we are focusing only on equipment
(Volume) calibration procedures, like:

Reactors

Storage tanks

Vessels
Objective :
To develop a standard procedure for the
equipment (Volume) calibration (e. g.
Reactor, Receiver and Tank)used in
manufacturing.

Responsibility:
1. Production Chemist

2. Production Technician

Shall be responsible for the compliance of SOP.

Procedure For the Calibration :

1.Equipment should be empty & clean.

2.Bottom valve of the equipment should be closed.

3.A DI water flow meter and two clean hose pipe for the performing the
calibration activity.
4.DI water flow meter should be calibrated.

5.Connect the hose pipe with DI water point

6.Connect the DI water flow meter and

7.Than connect the second hose pipe.

8.The water flow meter should be tightly clamped.

9.Put the hose pipe in the equipment.

Types of Equipment Calibration

1. Reactor calibration

2.Tank or Receiver calibration

Reactor calibration

Instrument required for Reactor calibration

1.Calibrated DI water flow meter

2.Calibrated dip rod

REACTOR

Agitator

over flow Thermo Pot

volume

Maximum Working
capacity
(80% of the equipment
volume )

TP
Minimum Touch
stirrable volume
volume Dead
volume
Calibration of equipment can be divide into three
parts

1. Dead volume :

2.Working capacity volume

3.Over flow volume

Dead volume:
A minimum volume of the equipment which is not
stirrable.

Working capacity volume:

Volume between the dead and overflow volume.

Over flow volume:

Volume after the dead and working capacity volume,
Or
the maximum volume after the working capacity, if we
add a single amount of water and the it become out
from the equipment
FOR REACTOR
Procedure for find the dead volume of reactor:
1. Put the hose pipe in the reactor and calibrated dip at the bottom
valve of the reactor.
2. Note the initial reading.
3. Paste a mark on the calibrated dip rod for the identification (where the
leaf of the agitator start)

4. Start the filling of water in the reactor carefully

5. Stop the filling of water as the level of water touch the leaf of the
agitator.
6. Note the second reading.
7. Find the difference between initial and final reading
8. The volume will be as dead volume of the reactor
Procedure for maximum working capacity of the reactor:
1. Put a mark on the dip rod for the dead volume.
2. And again put the second mark after a one centimeter on the dip
rod.
3. Put the dip rod in the reactor at the bottom valve.
4. Fill the DI water till the mark of one centimeter.
5. Note the initial and final reading and find the difference.
6. Than we will get LPCM ( Liter per centimeter)
7. Repeat the activity till the 80% of the equipment volume. (Working
capacity of the equipment)
8. Again fill the water till the neck of the equipment and note the
reading. (Maximum capacity of the equipment)
Procedure for over flow volume of the reactor:

1. After getting the maximum capacity of the equipment.

2. Note the initial reading.

3. Fill the water till the water come out from the manhole .

4. Note the final reading.

5. Find the difference

6. The amount of water will be the over flow volume of the

equipment.
Cross verification Procedure for volume calibration:
1. Note the initial reading.
2. Open the bottom valve and discard the water.
3. Note down the reading .
• For over flow volume.
• For working capacity.
• For LPCM
• For dead volume
Tanks & Vessels calibration

Instrument required for Tanks & Vessels calibration

Calibrated DI water flow meter

 Tanks & Vessels

Line
Over indicator
flow
volume

Visual
capacity

Dead
volume
FOR TANKS & VESSELS
Procedure for find the dead volume of tanks & vessels:

1. Put the hose pipe in the equipment.

2. Note the initial reading.
3. Start the filling of water into the equipment.
4. Stop the filling of water as the level of water shown in line
indicator (LI).
5. Note the second reading.
6. Find the difference between initial and final reading
7. The volume will be as dead volume of the equipment.
Procedure for maximum working capacity of the Tanks
and vessels:

1.After getting the dead volume of the equipment.

2.Note the initial reading

3.Fill the DI water till the level of line indicator reaches at one centimeter
in LI.
4.Note the final reading.

5.Find the difference for LPCM (LPCM-liter per centimeter).

6.Repeat the activity till the LI fill completely (working capacity of the equipment ).
Procedure for over flow volume of the Tanks & Vessels:

1. After getting the maximum capacity of the equipment.

2. Note the initial reading.
3. Fill the water till the water come out from the manhole .
4. Note the final reading.
5. Find the difference
6. The amount of water will be the over flow volume of the equipment.
THANK YOU !!!!