CORAL LABORATORIES LIMITED

Plot No. 27-28, Pharmacity

Selaqui Industrial Area
Dehradun – 248197
Uttarakhand, India

PROTOCOL FOR CALIBRATION OF JACKETED

MANUFACTURING TANK

Equipment Name Jacketed Manufacturing Tank

Reason for Qualification Periodic Qualification
Equipment ID No. LV02
Document No. QP-PPQ-LV02-02

Supersede No. Nil

Calibration Frequency Yearly
Effective Date
 PROTOCOL FOR CALIBRATION OF MANUFACTURING TANK

Equipment Name: Jacketed Manufacturing Tank Equipment ID No.: LV02

Coral Laboratories Ltd.
Document No.: QP-PPQ-LV02-02 Page No.: 2 of 7
Location: Dehradun

1.0 PROTOCOL APPROVAL:

1.1 This protocol is prepared by validation task force member:

Department Quality Assurance

Sign

Name Rajvar
Designation Chemist
Date

1.2 This protocol is reviewed by validation core committee:

Quality Engineering &

Department Production Quality Control
Assurance Maintenance

Sign

Name Puja Aswal Nilesh Patel Rajesh Suthar Nand Kishor

Designation Executive Manager Manager Incharge Utility
Date

1.3 This protocol is approved for implementation by Head-QA:

Sign

Name Sunil Kumar Gupta

Designation Manager
Date

1.4 This protocol is authorized for implementation by Plant -Head:

Sign

Name B.H. Patel

Designation Plant Head
Date
 PROTOCOL FOR CALIBRATION OF MANUFACTURING TANK

Equipment Name: Jacketed Manufacturing Tank Equipment ID No.: LV02

Coral Laboratories Ltd.
Document No.: QP-PPQ-LV02-02 Page No.: 3 of 7
Location: Dehradun

2.0 TABLE OF CONTENT:

SR. NO. CONTENT PAGE NO.

1.0 PROTOCOL APPROVAL 2

2.0 TABLE OF CONTENT 3

3.0 OBJECTIVE 4

4.0 SCOPE 4

5.0 RESPONSIBILITIES 4

6.0 DOCUMENTATION 5

7.0 MATERIAL REQUIREMENT FOR CALIBRATION 5

8.0 PROCEDURE 5

9.0 OBSERVATION 7

10.0 CONCLUSION 7
 PROTOCOL FOR CALIBRATION OF MANUFACTURING TANK

Equipment Name: Jacketed Manufacturing Tank Equipment ID No.: LV02

Coral Laboratories Ltd.
Document No.: QP-PPQ-LV02-02 Page No.: 4 of 7
Location: Dehradun

3.0 OBJECTIVE:

To establish evidence that the manufacturing tank is calibrated for the volume with dip rod marking, equipment ID
No-LV02 is acceptably verified in liquid manufacturing area at CORAL LABORATORIES LTD, Dehradun.

4.0 SCOPE:
This is applicable at the time of calibration of manufacturing tank ID No-LV02 Liquid manufacturing area at
CORAL LABORATORIES LTD, Dehradun.
The details are given below:

Sr. No. Equipment Name Equipment ID Parameter

1 Jacketed Manufacturing Tank LV02 Calibration

5.0 RESPONSIBILITIES:
5.1 RESPONSIBILITIES :

5.2.1 Quality Assurance: -

5.2.1.1 Preparation and review of Protocol and report.

5.2.1.2 Execute the protocol as per procedure.

5.2.1.3 Approval of Protocol and report.

5.2.2 Quality Control: -

5.2.2.1 Providing the equipment for validation.

5.2.2.2 Review the protocol and Report.

5.2.3 Engineering & Maintenance: -

5.2.3.1 Providing the utility services.

5.2.3.2 Review the protocol and report.

5.2.4 Production Department:-

5.2.4.1 Check the calibration protocol

5.2.4.2 Provide the materials used during calibration

5.2.5 Store Department:-Dispensing of material for the calibration of tank
 PROTOCOL FOR CALIBRATION OF MANUFACTURING TANK

Equipment Name: Jacketed Manufacturing Tank Equipment ID No.: LV02

Coral Laboratories Ltd.
Document No.: QP-PPQ-LV02-02 Page No.: 5 of 7
Location: Dehradun

6.0 DOCUMENTATION

All Calibration work will be performed as defined in the protocol. This will include the information, data
and analysis of Calibration results. All required documentation (Approved Protocol & Report) would be filled. Any
deviation or abnormality observed during the execution of the protocol will be documented. Upon completion of the
Calibration process, a final summary report will be prepared, that summarizes the Calibration of the Manufacturing
tank. The summary report will be reviewed and approved by Head-QA .

7.0 MATERIAL REQUIREMENT FOR CALIBRATION

7.1 Test Equipment/Instrument Calibration Verification:

1. Manufacturing tank to be calibrated – I.D. No: LV02

2. Dip rod for marking of calibrated points

3. Sodium Chloride IP

4. Calibrated 50 Ltr SS container.

8.0 PROCEDURE:

For the calibration of the tank, maintain the manufacturing area with 25°C. Confirm that there are no traces of
chloride in the Purified water used and weigh 49.801 kg of Purified water in the SS container which is
equivalent to 50 Lts of water considering the specific gravity of 0.99602. Mark the container with permanent
marker at the water level.

Weigh the Purified water of 49.801 Kg x 10 and transfer it to the manufacturing tank. Take exact weight of
4.5kg NaCl (Sodium chloride) in calibrated 50 ltrs SS tank & complete dissolve in purified water, make
volume up to 50 Ltrs. And transfer it in to manufacturing tank. Now the total volume in the tank is 500 ltr. Stir
for 5 minutes.
After stirring take out 15 ml of Sodium chloride solution & titrate for content of Sodium chloride content.
Based on the content of Sodium chloride calculate the actual volume of purified water content in the tank.

If the volume of purified water is within the acceptance criteria as stated in the volume verification chart,
permanent mark on Dip rod for 500 ltr.

The above same procedure shall followed for calibration point for 1000, 1500, 2000, 2500 and finally 3000

Justification for Addition of Sodium Chloride:

The purpose of use of tank is for manufacturing of Oral liquid batches at different batch sizes with
appropriate Active Pharmaceutical Ingredients. Hence for to ensure it is essential to determine whether the
actual input are getting at different batch size accurately at calibrated points.

Hence 0.9%w/v of Sodium Chloride Solution is used as active Pharmaceutical Ingredient in Calibration
activity
 PROTOCOL FOR CALIBRATION OF MANUFACTURING TANK

Equipment Name: Jacketed Manufacturing Tank Equipment ID No.: LV02

Coral Laboratories Ltd.
Document No.: QP-PPQ-LV02-02 Page No.: 6 of 7
Location: Dehradun

Procedure for Estimation of Sodium Chloride:

Titrate the water sample with the 0.1N silver nitrate solution using Potassium chromate indicator and note
the burette reading for the amount of 0.1N Silver nitrate consumed by NaCl available in the water. Content of
Sodium Chloride:

Assay = BR X 0.1N Normality of Ag No3 X 0.005844 X 1000 = X gm/ltr

For example if we want of verify the volume of purified water for 500 Ltrs :-

1 X Exact wt. of Sodium Chloride in gms = Y Ltr of water in the tank

X gms /Ltr.
Y – 500 = + Z ltrs of actual difference of Purified water in tank. (Limit: Difference ± 1%)

Determination of % of difference of Purified water in the tank.

Z (Actual Difference in Volume) x 100 = W % of Difference)

Calibrated Volume (500)

Repeat the same procedure at different water level listed below in the Observation chart
Volume verification

Sr.No. Volume of water Burette Reading Factor Assay (g/Ltr)

1 500
2 1000
3 1500
0.005844
4 2000
5 2500
6 3000

Normality of 0.1N AgNO3 =

9.0 OBSERVATION:

Sr. No. To be Wt. of water Volume NaCl Assay Actual Limit Result
calibrated added in Kg of water Added (%w/w) Water (± 1.0%)
 PROTOCOL FOR CALIBRATION OF MANUFACTURING TANK

Equipment Name: Jacketed Manufacturing Tank Equipment ID No.: LV02

Coral Laboratories Ltd.
Document No.: QP-PPQ-LV02-02 Page No.: 7 of 7
Location: Dehradun

at volume added in volume Ltr.

(Ltr.) Ltr
1 500 49.801 x 10 500 4.5kg 495-505
2 1000 49.801 x 10 1000 4.5kg 990-1010
3 1500 49.801 x 10 1500 4.5kg 1485-1515
4 2000 49.801 x 10 2000 4.5kg 1980-2020
5 2500 49.801 x 10 2500 4.5kg 2475-2525
6 3000 49.801 x 10 3000 4.5kg 2970-3030

10.0 CONCLUSION :

After calibration at different point of manufacturing vessel shall verify and it should be within the 1% of the
verification as specified in the Observation table. Than only the tank can be used for the routine commercial
batch preparation at calibrated points only.