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

over flow

volume

TP Touch volum

e

Minimum stirrable volume

Maximum Working capacity (80% of the equipment

volume )

Dead volume

Agitator

Thermo Pot

REACTOR

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 REACTORProcedure 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 carefully5. 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 reading8. 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

Line indicator

Dead volume

Visual capacit

y

Over flow

volume

Tanks & Vessels

FOR TANKS & VESSELSProcedure 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 reading7. 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 reading3.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 difference6. The amount of water will be the over flow volume of the equipment.

THANK YOU !!!!