Category: QC SOP

SOP Title: Operation, Cleaning and Calibration of Automatic  Refractometer

 

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of Refractometer.

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of Refractometer located in Quality Control Laboratory.

 

3. Responsibility:

• Quality Control: To prepare and review the SOP. To follow the procedures laid down for Operation, Cleaning and Calibration of Refractometer as per this SOP.
• Quality Assurance Department: To review and approve the SOP and Annexures.

 

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department.

5. Procedure

 

5.1	Safety Precautions/Instructions:
5.1.1	Ensure all the electrical connections are properly earthed. Ensure the power plug of the automatic Refractometer is fixed in the socket properly.
5.1.2	Wear personal protective equipments such as safety glasses, hand gloves during operation of instrument.
5.1.3	Ensure that the ON/OFF switch is working properly by switching “ON” the Refractometer.
5.1.4	Clean the Automatic Refractometer with dry lint free duster.
5.1.5	Do not move the automatic Refractometer during cleaning
5.1.6	Do not attempt to do any repairs unless trained.
5.1.7	Keep measuring surface clean. Clean the measuring surface with a wet (with water or isopropyl alcohol), soft, clean cloth or paper towel. For most accurate reading, keep the measuring surface clean and free of residual at all times.
5.1.8	Use only one or two drops of sample. Use a disposable plastic pipette to place the sample on the measuring surface and use the same pipette to suck back up and dispose of it.
5.1.9	Inspect the measuring surface to make sure it is clean and dry with IPA before putting sample on measuring surface.
5.1.10	Do not keep instrument to temperature above 50°C
5.1.11	Keep instrument away from vibration.
5.2	Operation  Procedure:
5.2.1	Check the validity of calibration before starting any operations.
5.2.2	The instrument should be cleaned before operation.
5.2.3	Switch “ON” the mains and switch “ON” Refractometer with on/off switch provided at back side of the instrument. The main screen will display menu as : 1.Escape       2.Menu 3.Zero  4.Print  5.Start
	Introduction to Key:
5.2.4	Escape-Use to exit the current window to return to  previous.
	Menu-The menu key will allow user to access parameter as scale,  temperature and setup.
	Zero-The “zero” is used to perform auto zero of instrument.
	Print-Print key is used to print measured readings.
	Start-Start key is used for measurement of sample.
5.2.5	Click on “MENU” key on main screen, The system will ask for password. Enter  Password , Then screen will show parameters as : 1. Scale                           2.Temperature                    3.Setup
5.2.6	Click on “SCALE” option from menu  key, the screen will display parameters as : 1. Refractive Index         2. Brix                  3.Honey
	Note: Brix and Honey are scale used generally in food industry.
5.2.7	Click on “Refractive index” parameter, then press “Exit” key.
5.2.8	Temperature Control          2.Temperature Correction Click on “TEMPERATURE” parameter, the screen will display sub-parameter
5.2.9	Click on “TEMPERATURE CONTROL” option, the screen will display options as 1. Temperature Control 20ºC           2. Temperature Control 25ºC 3. Temperature Control Off
5.2.10	Select “Temperature control “20ºC or 25ºC” as per standard test procedure and click on “back” option
5.2.11	Click on “TEMPERATURE CORRECTION” from temperature parameter ,  and press “back” key.
5.2.12	Click on “SETUP” menu from main screen “menu” key .   The Screen will display setup parameters as 1.User calibration   2.Operational parameters      3.Measurement Parameters 4.Communication setting   5.system information        6.Service calibration
	Introduction to key:
5.2.13	Service calibration This setup menu is used by outside service                                 engineer during annual maintenance.
	System information   It contains the instrument information.
	Communication setting   It shows setting to print the results.
5.2.14	Click on “OPERATIONAL PARAMETER” setup menu , The screen will display option as 1. Temperature  scale     2.Time/Date  3.Keylock                    4.Password             5.Precision
5.2.15	Click on “Temperature scale” option. The screen will display scale option as 1. Celsius        2. Fahrenheit scale
5.2.16	Select “Celsius” temperature scale and press “Exit” key.
5.2.17	Click on “MEASUREMENT PARAMETERS” from “Setup” menu. The screen will display parameter as 1.Measurement Mode     2.Stability Criteria       3.Sound
5.2.18	Click on “Measurement Mode” parameter. The screen will display the mode as 1. Load & Go        2. Single Measure
	Introduction to Key :
5.2.19	Load & Go- This Mode automatically measure the sample and continue measuring the sample until it has been removed.      Single Measure- This Mode measure the sample 1 time after the sample is placed on the prism and has meet the criteria for temperature and stability.    “Single measure” Mode is used in routine analysis.
5.2.20	Click on “Single Measure” mode. Press on “Done” key.
5.2.21	Click “zero” key on main screen to auto zero the instrument without blank sample i.e. Air Zero. Then the system will display a message “Place pure water on sample dish. Then press zero again.”
5.2.22	Place approximately 1-2 drop of water as blank on measuring surface, such that black circle of measuring surface will cover. Put the lid of Refractometer on sample. Click on “ZERO” Key on main screen to auto zero.
5.2.23	After pressing “ZERO” key, the system will show the message of “Water Zero successful”
5.2.24	Click on “Continue” option. Then system will start to measure Refractive index of water. The measured reading will display on main screen.
5.2.25	Clean measuring surface with paper towel or cloth.
5.2.26	Place sample on measuring surface and put the lid of Refractometer.
	NOTE: Place approximately 1-2 drop of sample or blank such that it should cover black circle of measuring surface. If sample is not sufficient on measuring surface, the system will display a message “Waiting for Sample”
5.2.27	Click on “START” Key on main screen. The measurement reading will display on main screen.
5.2.28	Click on “PRINT” key on main screen. The print taken via RS 232 Port cable which is connected to printer  OR  via  PC connected to Printer.
5.2.29	After measurement clean the measuring surface with wet cloth or paper towel of water or isopropyl alcohol to remove residue particle.
5.3	Calibration procedure :
5.3.1	Update the “Instrument/Equipment Usage Log Book” as per SOP “Calibration of Instruments and Equipments”.
	Frequency:  Quarterly or after carrying out any major maintenance work.
5.3.2	Generate the A. R. No. on the “Instrument/Equipment Calibration Register” as per SOP and give requisition to QA department for calibration formats of instruments on the due date of calibration.
5.3.3	For issuance of calibration report refer SOP “Control of documents, Preparation, Approval, Issuance and Maintenance.
5.3.4	Perform the calibration of instrument as per Annexure and procedure mentioned below.
5.3.5	Determine the refractive index of the following standard materials: 1)     Purified  Water at 20°C 2)     Carbon tetrachloride 3)     Toluene
	User Calibration: (Two Point Calibration)
5.3.6	Click on “User Calibration” setup parameter from “Setup” option.  The screen will show sentence “Prism must be cleaned and covered” then click on “Continue” key.
5.3.7	After clicking  on “continue” option Wait for air zero as shown in figure.
5.3.8	After completion of  air zero, the screen will display parameter as   1. Refractive index        2. Brix
5.3.9	Click on “Refractive index” option. The screen will Display message  as “ Place sample 1 on prism” “Water” is used as sample 1
5.3.10	Click on “Done” key. The screen prompt enter Standard value of Sample 1 E.g. Water –   1.33299
5.3.11	Press “Enter” hence system will start measuring sample-1.
5.3.12	After completion measurement of  sample-1 The system will then proceed  sampe-2 Remove sample -1 from measuring surface. Clean it wet cloth or paper towel so that no any Residue obtained.
5.3.13	Place “sample-2” on measuring surface .
5.3.14	Press “Enter” hence system will start measuring sample-2 After measuring sample-2 the system will return to main screen.
5.3.15	Enter the details in calibration report. Ensure that the results obtained, comply with the acceptance criteria. If instrument fails to meet to acceptance criteria then file an incident and investigate the cause of failure.
5.3.16	Update the “Instrument/Equipment Usage Log Book”, “Annual Calibration Schedule” and “Quarterly Calibration Schedule” as per SOP  “Calibration of Instruments and Equipments”.
5.3.17	Affix the “Calibration Status Label” on the Instrument as per SOP “Calibration of Instruments and Equipments”.
5.3.18	If calibration activity is outsourced, the values are to be transcribed in the Annexure , and external party certificate to be attached.

 

6. Definitions / Abbreviations:

Definitions:

• Calibration: Tests performed to ensure that the instrument is functioning as per set parameters. These tests are performed as per predefined frequency and also after any major repair or replacement of parts.
• Refractometer: Automatic Refractometer automatically measure the refractive index of a sample. The automatic measurement of the refractive index of the sample is based on the determination of the critical angle of total reflection.

 

Abbreviations:

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
0C	Degree Celsius
No.	Number

 

                                          Calibration Report

Sr. No.	Standards	Acceptance Criteria	Observed Values
1.	Purified Water at 20°C	Water     at 20°C ±0.5°C   1.33299  (±0.0001) (1.3329  to 1.3331)
2.	Carbon Tetrachloride at 20°C	Carbon Tetrachloride at 20°C±0.5°C 1.4603 (±0.0003)   (1.4600  to  1.4606 )
3.	Toluene at 20°C	Toluene at 20°C ±0.5°C 1.4969    (±0.0003)  (1.4966  to 1.4972)

 

   Remark: The result Complies/Does not complies as per acceptance criteria.

 

Performed By: ________________     Date:________________       Checked By: ______________           Date: ______________

                                                      

 

*Note – Ready to use SOP available in “DOWNLOAD” Section.

 

SOP Title: Operation, Cleaning and Calibration of Fume Hood

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of Fume hood.

 

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of Fume hood located in Quality Control Laboratory.

 

3. Responsibility:

• Quality Control: To prepare and review the SOP. To follow the procedures laid down for operation, cleaning and calibration of Fume hood as per this SOP.
• Quality Assurance Department: To review and approve the SOP and Annexure.

 

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department

5. Procedure:

 

5.1	Safety Precautions/Instructions:
5.1.1	Ensure all the electrical connections are properly earthed. Ensure the power plug of the Fume hood is fixed in the socket properly.
5.1.2	Wear personal protective equipment’s such as protective hand gloves, nose masks and over gown during operation of the fume hood.
5.1.3	Do not disturb the air flow or switch off the fume hood if analysis are not completed.
5.1.4	Avoid placing head inside fume hood. Close the sash/door as to safe opening height/Minimum Height i.e. 18 cm from the working platform level when working in the fume hood.
5.1.5	Avoid the rapid movement of Sash/door of fume hood. This can cause air currents drawing contaminants out of the fume hood.
5.1.6	Avoid raising the sash/door too quickly. Raise the sash/door slowly and allow the air velocity to increase.
5.1.7	Do not work by opening sash/door higher than the maximum established working height. Close the Sash/Door completely when not working at the fume hood.
5.1.8	Avoid storage of larger amount of chemicals in the fume hood. The storage of chemicals in fume hood may block airflow. Use underneath cabinet designed for chemical storage.
	Note: While working with the chemicals, position the sash/door at safe opening height/minimum height.
5.1.9	Do not place any spark source (i.e. electrical receptacles) inside the hood when flammable liquid or gasses are present e.g. Ether, IPA, Acetonitrile, Ethanol, Methanol, LPG, Hydrogen gas etc.
5.2	Operation  Procedure:
5.2.1	Switch ‘ON’ the main switch of MCB box to supply electricity to the fume hood and blower.
5.2.2	To Start the lights, put ‘ON’ the main switch provided on the side wall and then switch ‘ON’ the button which is provided on the right side of the fume hood. Note: Two power switches are provided for the connection of Instruments.
5.2.3	Start the Air Blower/Air Exhaust by pressing green button on the Starter switch.
5.2.4	Verify the Air Blower/Exhaust system is operating properly before use by checking of current of air flow or by generating smoke in fume hood.
	Note: Back wall of the fume hood is provided with the holes for exhaust.
5.2.5	Keep instruments minimum 15 cm away from the sash/door while using fume hood.
5.2.6	Never work with sash opening higher than the established working height. Sash is provided with mark of minimum and maximum of usage height.
	Note: Do not close sash/Door fully. If sash is fully closed then blower will not get the required air and vacuum will be created in the fume hood.
5.2.7	Left side of the fume hood is provided with the 3 knobs i.e. for water, for air and for gas. Valves can be open/close by rotating Knob left/right side as per the need.
5.2.8	Opening of these valves is provided inside the fume hood.
5.2.9	Fume hood is provided with water tap along with the Basin with drainage connection.
5.2.10	Avoid excessive heat within the fume hood.
5.2.11	Cupboard is provided downside of the fume hood to store the Liquid chemicals and concentrated acids etc.
5.2.12	After the analysis, allow to run the blower at least 5 minutes to remove toxic gas or fumes from fume hood and switch “OFF” the air flow blower.
5.2.13	After cleaning switch “OFF” the light and main switch.
5.2.14	Cleaning should be done as per below mention cleaning procedure.
5.3	Cleaning Procedure:
5.3.1	Cleaning should be done before starting and after the completion of analysis.
5.3.2	Clean the chemical spills on working surface as soon as possible by washing with plenty of water. Clean the dust on sash and side wall with dry cloth.
5.3.3	Minimize the excessive fumes by controlling the process of analysis. For Example- In Sulphated Ash testing, drop wise addition of Sulphuric Acid will avoid excessive fumes.
5.4	Validation:
	Frequency: Once in a year or after carrying out any major maintenance work
5.4.1	Fume Hood shall be validated for Face Velocity/Air Velocity Test.  The face velocity should be checked at different five positions as shown in the Annexure “ Location Chart”
5.4.2	Acceptance Criteria :- Average of five reading should be within   0.4-0.6 m/sec ( i.e. ~  80- 120 fpm) *Note: – Acceptance Criteria reference from ANSI Standard. Record the reading in Annexure.
5.4.3	Validation shall be carried out internally or by external agency. Refer SOP “Calibration of Instruments and Equipment for documentation.
5.5	Preventive Maintenance
	Frequency:  Every Quarterly
5.5.1	Perform the preventive maintenance as per Annexure

6. Definitions/Abbreviations:

• Definitions:
• Breakdown: Any activity leading to operation of fume hood other than the set parameters and/ or unusual sound or vibration observed in the fume hood.
• Calibration: Tests performed to ensure that the equipment is functioning as per set parameters. These tests are performed as per predefined frequency and also after any major repair or replacement of parts.

 

• Abbreviations:

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
No.	Number
PM	Preventive Maintenance
cm	Centi meter
m/sec	Meter Per Second
fpm	Feet Per Minute

 

Fume Hood Calibration/Validation Report

Observed Anemometer Reading at Five different position

 

Position No.	Anemometer Reading at given position(m/sec)	Acceptance Criteria
I		Average of five reading should be within 0.4-0.6 m/sec
II
III
IV
V

 

Average Reading =   Sum of all Anemometer reading

5

 

=     _____________________

5

 

=                             m/sec

 

Remark: The result Complies/Does not complies as per acceptance criteria.

 

 

Performed By: ________________   Date: _______________

Checked By: ______________           Date: ______________

                                                      

               The face velocity should be checked at five different positions as shown below.

 

BACK SIDE

( I )                                                                                               ( II )       (III )       ( IV )                                                                                               ( V )

                                          FRONT   SIDE                              

*Note – Ready to use SOP available in “DOWNLOAD” Section.

                                       

                         

 

SOP Title: Preparation and validation of Excel Calculation Sheet

1. Objective:

To lay down the procedure for Excel Sheet Validation in Quality Control Department.

 

2. Scope:

This procedure is applicable for ascertain the content of sample in Quality Control Department.

3. Responsibility:

• Quality Control Department: To prepare and review the SOP. To follow the procedures laid down in the excel sheet for release of Sampling, in Quality Control Department as per this SOP.
• Quality Assurance Department: To review and approve the SOP and Annexures.

 

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department

5. Procedure:

5.1	Preparation of Excel Sheet :-
5.1.1	Prepare the excel calculation sheet in “Microsoft Excel”.
5.1.2	Prepare separate calculation sheet for individual tests, which can be common for all products or it can be product wise.
5.1.3	The Header of the excel sheet shall consist of  Name of the Organisation, Name of the Department,  Product Name,     Batch No., Stage, Test, A.R. No. and Date of analysis etc.
5.1.4	Wherever applicable but not limited, Main body of the Excel sheet shall generally consist of standard weight, sample weight, dilutions, average weight, standard purity, sample/standard absorbance/area, label claim, final results and calculation formula etc.,
5.1.5	The Footer of the excel sheet consist of  Analysed By & Date, Checked By & Date and Name of the Excel sheet with version Number etc.
5.1.6	In case of Related Substances, include retention time, relative retention time and name of the impurity etc.
5.1.7	For dilutions of standard solution, show weight and diluted to specific volume and the maximum possible dilution in excel sheet.
5.1.8	For dilutions of sample solution, show weight and diluted to specific volume by considering maximum possible dilutions.
5.1.9	Put the calculation formula correctly in the cell where results will appear.
5.1.10	Calculation formula shall be referred from STP/AWR.
5.1.11	Prior to excel validation, calculation formula shall be verified by supervisor.
5.1.12	Results shall be rounded off up to the decimal points. Number of decimal points for results shall be decided by referring product specification.
5.1.13	Protect the full excel sheet except the cells that needs to be filled while calculating the results.
	Note: After protection of the calculation sheet, the cells that are unlocked are open for changes like variables such as area, absorbance, weight, dilution and potency of working standard / reference standard etc.
5.1.14	To protect excel sheet select go to “Review” on the Tool menu of excel and then click Protect Sheet. Type an alphanumeric password and click “OK”, and then retype the password in the Confirm Password dialog box.
5.1.15	Password shall be of eight characters having alphanumerical in nature and one special character. For example:- abc@1234
5.1.16	Password should be known to Administrator/Head QC/IT only.
5.1.17	Master excel calculation sheet shall be stored in separate folder on the computer of administrator.
5.1.18	Only Administrator shall have the rights to create new master Excel calculation sheet.
5.1.19	Only Administrator shall have the rights to modify/delete master Excel calculation sheet after consultation with Head QC.
5.1.20	Fill the unprotected cells that need to be filled while calculating the results.
5.1.21	Give the input cells a color to make the spreadsheet more clear and easier to understand for users.
5.1.22	Prepare a separate excel calculation sheet for respective tests.
5.1.23	Right click option should be deactivated for user.
5.2	Nomenclature of  Excel calculation Sheet :-
5.2.1	Each and every Excel sheet should have unique identification name as mentioned below
5.2.2	“XXXX_YY_ZZ_AA_NN” Where, XXXX-Product Name/Material Name YY- Dosage Form (e.g. Tablet/Capsule/Cream/RM) ZZ-Strength/Type AA-Test Name NN- Version Number For Example:- Paracetamol Tablets 500 mg Assay test should be named as “Paracetamol_Tab_500mg_Assay_00”
5.3	Validation of Excel calculation Sheet
5.3.1	Prepare validation protocol for excel calculation sheet.
5.3.2	Perform calculations using excel calculation sheet and compare the results with same sets of calculations performed using scientific calculator up to pre-determined decimal places.
5.3.3	To validate excel sheet, first perform calculations by putting required values in excel sheet and take the printout of excel sheet.
5.3.4	Then perform same calculations by using scientific calculator. All calculations should be reported on Annexure.
5.3.5	Calculations done by Excel sheet and by calculator shall be compared.
5.3.6	Acceptance criteria: Excel Sheet Calculation results should match with the scientific calculator results.
5.4
5.4.1	Prove that entry in protected cells cannot be made. Screen shot shall be attached with validation documents. To verify the protected cell, double click on the locked excel the display will read as: The cell or chart you are trying to change is protected and therefore read-only.
5.4.2	Prove that, to unprotect the calculation sheet, password is required. Take screen shot. To unprotect the protected calculation sheet click on review on Toolbar select unprotect sheet, enter the password and select ok.
5.4.3	On input of wrong password, system should display warning message of incorrect password applied.
5.4.4	Prove that, entry of alphabets, special character and zero in input cells which are directly involve in calculation results shows invalid results.
5.4.5	Attempt to change Formula/values/text in protected cell. System should disallow change in protected cell.
5.4.6	Attempt to Delete/ Add Row or column in the protected worksheet. System should disallow any deletion/addition of row or column.
5.4.7	Verify the spreadsheet calculations by entering expected values and extreme values and verify the behaviour of the spreadsheet.
5.5	Revalidation of Excel sheet
5.5.1	Excel sheet shall be revalidated in case of change in any formula OR any change in design and templates which will have direct impact on the results. Revalidation shall also be done once in 2 years irrespective of no change.
5.5.2	Any changes in validated calculation sheet shall be made through change control.
5.5.3	Version number of validated calculation sheet shall be updated after changes.
5.5.4	Re-Validation is not required for validated calculation sheet in case of typo graphical correction to be made, which will not have impact on the calculation results. However, impact assessment of changes shall be done through change control.
5.5.5	Maintain list of excel sheet, Product Name, Test Name, version No., validation done on and due date for validation.
5.5.6	Re-validation of Excel Sheet should be done within 30 days from the due date.
5. 6	Calibration of Calculator:-
5.6.1	New calculator shall be calibrated before use.
5.6.2	Before starting calibration of the calculator, check the operation of the calculator as per manufacturer’s manual.
5.6.3	Calibrate the calculator for the functions like Addition (+), Subtraction (-), Multiplication (X), Division (÷) and Square Root (√).
5.6.4	Verify the functions calculated using calculator with manual calculations.
5.6.5	Also verify some complex functions like Multiplication (X), Division (÷) and Square Root (√) by using Logarithmic tables and Antilog tables.
5.6.6	Acceptance criteria: Calculator values should match with the manual calculation values.
5.6.7	Re-calibrate the calculator in case of major repairing.

 

6. Definitions / Abbreviations:

• Definitions:
• Abbreviations:

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
No.	Number
AWR	Analytical Work Report
STP	Standard Testing Procedure

 

 

*Note – Ready to use SOP available in “DOWNLOAD” Section.

 

SOP Title: Operation, Cleaning and Calibration of Analytical weighing Balance

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of Analytical weighing Balance. 

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of Analytical weighing Balance located in Quality Control Laboratory.

 

3. Responsibility:

• Quality Control Department: To prepare and review the SOP. To follow the procedures laid down for Operation, Cleaning and Calibration of Electronic Weighing Balance as per this SOP.
• Engineering Department: To carry out preventive maintenance as per schedule and procedure defined.
• Quality Assurance Department: To review and approve the SOP and Annexures.

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department

 

5. Procedure:

5.1	Safety Precautions/Instructions:
5.1.1	Ensure all the electrical connections are properly earthed. Ensure the power plug of the Electronic Balance is fixed in the socket properly.
5.1.2	Wear personal protective equipments such as safety glasses, hand gloves, nose mask during operation of instrument.
5.1.3	Ensure that the ON/OFF switch is working properly by switching “ON” the Electronic Balance.
5.1.4	Analysts must be familiar with precautions described in respective Material Safety Data Sheet of the materials before weighing it.
5.1.5	Do not unplug the power or shift the balance when ‘CAL’ is Displayed  on display
5.1.6	Check that the balance is kept vibration free table/platform.
5.1.7	Analytical weighing Balance Maximum range is 220 gm and Minimum range is 0.1 gm, do not exceeds the maximum weight limit. Weighing range is 10 mg to 150 gm
5.1.8	Never weigh any material directly on weighing pan, instead use butter paper or any other suitable container.
5.2	Introduction to the Keys of Analytical weighing Balance:
5.2.1	During measurement
5.2.2	Key Pressed Once And Released Pressed And Held For About 3 Seconds [POWER] Switches between the operation and standby modes. Switches the key notification buzzer on/off. [CAL] Enter calibration or menu item selection. Enter calibration or menu item selection. [O/T] Tares the balance. (Displays zero.) *1 NA [UNIT] Switches the units of measurement   NA
5.2.3	Key Pressed Once And Released Pressed And Held For About 3 Seconds [PRINT] Outputs the displayed values to an electronic printer computer, or other external devices.*2,   Outputs  the  date  and  time  to  external devices [1d/10d] Switches display between 1d/10d. (Minimum display is rounded by one digit.)
	During Menu Item Selection:
5.2.4	Key Pressed Once And Released Pressed And Held For About 3 Seconds [POWER] Return to the menu above the current menu level. Returns to mass display. [CAL] Moves to the next menu item. [O/T] Select or set the displayed item, or enter into the displayed menu. [UNIT] Numerical value input, increases the numeric value of the blinking digit by 1. [PRINT] Numerical value input, moves the blinking digit. [1d/10d] No effect.
5.3	Operational  Procedure:
5.3.1	Check the validity of calibration before starting any operations.
5.3.2	Level the balance using levelling feet so that level indicator bubble is centered within the circle of levelling indicator.
5.3.3	Check the cleanliness of the Balance and its surrounding area.
5.3.4	Connect the power supply cord to the switch board and switch on the balance and allow the balance to warm up for about 30 minutes.
5.3.5	Plug The AC adapter to the power outlet
5.3.6	After the balance performs a self check, calibration will be automatically executed, it returns to the mass display and span calibration is complete.
5.3.7	During this process, the display will change as follows. “CAL 2”     “CAL 1”     “CAL 0”       “CAL END”      “OFF”
5.3.8	Press “POWER” key to appears the gram (g) on displays.
5.3.9	Pressing the [POWER] key again turns on the standby symbol and puts the balance in standby (warm up) status.
5.3.10	The current time is display according to the built-in clock setting
	Note: For accurate measurement, perform span calibration again when the balance is moved or when the temperature of the installation site has changed.
	Sample weighing on Balance:
5.3.11	Open one of the glass doors of the weighing chamber, place the weighing vessel (container) on the pan, and close the glass door again. (When using a container)
5.3.12	Wait for the display to stabilize and press the [O/T] key (taring). The appearance of the stability mark (  ) indicates a stable state. The display will read zero.
5.3.13	Open the glass door, place the items to be weighed in the weighing vessel and close the glass door.
5.3.14	After the display stabilizes, read the display.
5.3.15	If beaker/flask/evaporating dish is taken for weighing as the receiver then receiver’s weight plus the material’s weight should not exceed the capacity of the balance.
5.3.16	Butter paper should be used when small amount of materials are to be weighed.
5.3.17	Before weighing any materials which has been heated or stored in refrigerator, they should be brought to the room temperature and weighed.
5.3.18	Printer connected to the Analytical weighing Balance.
5.3.19	After material weigh, display will stabilize, go to printer and Press “ID” key and Press “Date” key. Green light will blow on both keys.
5.3.20	Before going to the “STAT” option, switch off green light by pressing both “ID” key and “Date” key.
5.3.21	Press “STAT” key located on the printer. It will appears on paper print.
5.3.22	Press “PRINT” key located on the Analytical weighing Balance to take weight print on paper print.
5.3.23	After sample weighing finish, Press “STAT” key located on the printer.
5.3.24	Update the “Instrument/Equipment Usage Log Book” as per SOP “Calibration of Instruments and Equipments”.
	Note:1) Except when placing or removing items or calibration weights to and from the weighing chamber, keep the glass doors closed 2) Air convection causes measurement error if the temperatures of the weighed item and the chamber are different. In order to avoid this, equalize the temperatures by leaving the item in the extra space within the chamber before weighing.
	Changing the Unit Display:
5.3.25	Pressing the [UNIT] key switches display between the registered units, piece counting and specific gravity measurement modes.
	Note: The units to be used must be registered in the system
	Menu Item Selection Procedures:
5.3.26	Press the [CAL] key from the mass display. “i-CAL” appears.
5.3.27	After that, pressing the [CAL] key changes the display in the order shown below.
5.3.28	00000	Mass display
	CAL	Execute the preset calibration method
	SET in I	Windows Direct setting (down)
	SET in-	Windows Direct setting (right)
	SE BIE	Settings check display
	Stnd	Standard mode
	PoUr	Pouring mode
	Con Ect	Anti-convection mode
	Hi stb	High-stability mode
	Fu Sel	Entry to second level (application measurement, individual settings menu group)
	SETT  inG	Entry to second level (system settings menu group)
	int FACE	Entry to second level (communication settings menu group)
	00000	Mass display
	Setting the Built-in Clock:
5.3.29	To set the clock From the mass display, press the [CAL] key repeatedly until “SEttinG” appears, press the [O/T] key. “CAL dEF” will appear.
5.3.30	Press the [CAL] key repeatedly until “d-MM.DD” appears (MM and DD are each two digits representing month and date, respectively), and press the [O/T] key. In the upper part of the display, the  mark and the  symbol appear indicating number entry mode. Also, the current date setting
5.3.31	appears as [YY.MM.DD] (YY is the year) with the leftmost digit blinking.
5.3.32	Pressing the [UNIT] key increases the blinking digit by one. Pressing the [PRINT] key moves the blinking digit one place to the right.
5.3.33	Press the [O/T] key when the desired date is shown in the display. The built-in clock will be set.
5.3.34	Press the [POWER] key repeatedly to return to the mass display
	Date Output Style:
5.3.35	The order of the year, the month and the date in the external output can be selected from three styles
5.3.36	From the mass display, press the [CAL] key repeatedly until “SEttinG” appears, press the [O/T] key. “CAL dEF” will appear
5.3.37	Press the [CAL] key repeatedly until “StyL.dAtE” appears.
5.3.38	Press the [O/T] key. The display shows “y-m-d”. After this, pressing the [CAL] key cycles the dis-plays in the order of “y-m-d” → “m-d-y” → “d-m-y” → “y-m-d”. “y-m-d” is for setting YYYY-MM-DD, “m-d-y” is for MM-DD-YYYY and “d-m-y” is for DD-MM-YYYY. When the current setting is displayed, the stability mark (  ) appears. To change the setting, press the [O/T] key when the desired setting is on the display
5.3.39	Press the [POWER] key to return to “StyL.dAtE” without changing the setting
5.3.40	Pressing the [POWER] key again returns to the mass display
	Time:
5.3.41	To set the time, From the mass display, press the [CAL] key repeatedly until “SEttinG” appears. Press the [O/T] key. “CAL dEF” will appear.
5.3.42	Press the [CAL] key repeatedly until “t-HH.MM” appears (HH and MM are each two digits representing hour and minute, respectively), and press the [O/T] key.
5.3.43	In the upper part of the display, the  symbol and the    symbol appear indicating  number entry status. Also, the current time setting appears.
5.3.44	Pressing the [UNIT] key increases the blinking digit by one. Pressing the [PRINT] key moves the blinking digit one place to the right.
5.3.45	Press the [O/T] key when the desired time is shown in the display. The built-in clock will be set.
5.3.46	Press the [POWER] key repeatedly to return to the mass display.
	Changing the Minimum Display:
	A)To change the minimum display by one digit
5.3.47	Press the [1d/10d] key from the mass display. The minimum display digit will be displayed with only three decimal places.
	B)To return the minimum display to the standard setting
5.3.48	Press the [1d/10d] key from the mass display. The minimum display digit will return to the previous setting.
	Note: The decimal point does not move. When the minimum display is changed by one decimal place, the final decimal place remains empty.
	Balance ID Setting:
5.3.49	To set the balance ID No. From mass display, press the [CAL] key repeatedly until “SEttinG” appears. Press the [O/T] key. “CAL dEF” appears.
5.3.50	Press the [CAL] key repeatedly until “id: ∗∗∗∗” appears. (The ∗∗∗∗ is a number.) Press the [O/T] key. In the upper part of the display panel, the  symbol and the  symbol appear in order to indicate numerical input mode. The left-most digit of ∗∗∗∗ blinks. The numeral of the blink-ing digit can be changed.
5.3.51	Press the [UNIT] key to increase the value of the blinking digit by 1. Press the [PRINT] key to set that digit and move the blinking digit one place to the right. When the desired setting is entered, press the [O/T] key to confirm the balance ID number.
5.3.52	Press the [POWER] key to return to “id: ∗∗∗∗”. (No blinking)
5.3.53	Press the [POWER] key again to return to the mass display.
	Settings for Stability and Response:
	A) Standard mode:
5.3.54	Use this mode unless stability or response is affected by environmental factors. From the mass display, pressing the [CAL] key repeat-edly until “Stnd” is displayed. Pressing the [O/T] key here sets the mode to Standard mode
	B) Anti-convection mode:
5.3.55	When ambient temperature changes (such as those due to air-conditioner cycling) are unavoidable during measurements, convection may occur in the weighing chamber and cause display fluctuation after the stabil-ity mark appears
5.3.56	From the mass display, press the [CAL] key repeatedly until “ConvECt” is displayed. Pressing the [O/T] key here sets it to Anti-convection mode.
	C) High-stability Mode:
5.3.57	Function of this is to reduce the effects of vibration or air current even further. The response will slow slightly but the display will be stabilized.
5.3.58	From the mass display, press the [CAL] key repeatedly until “Hi-Stb” is displayed. Press the [O/T] key here to enter High-stability mode
	D) Pouring Mode (fast response):
5.3.59	Press the [CAL] key repeatedly from the mass display until “Pouring” appears.
5.3.60	Pressing the [O/T] key here sets it to Pouring mode and proceeds to “normL.Env” display. the arrow mark indicates that the displayed environmental setting is currently selected. Press [POWER] key to return to the mass display.
5.4	Calibration Procedure:
	A) Daily calibration: Performance check
	Frequency: First half of every day.
	Note: Replace the silica gel on weekly basis (preferably on Monday) or when its appearance changes.
5.4.1	Perform the daily calibration of instrument as per Annexure No. 01 and procedure mentioned below.
5.4.2	Calibration is performed using standard calibrated weight box.
5.4.3	For daily calibration 0.0200 g, 0.1000 g, 1.0000 g, 50.0000 g and 100.0000 g weights are used.
5.4.4	Ensure that the display shows zero reading. If not press ‘[O/T]’ key to zero the display.
5.4.5	Place the standard weights on the weighing pan.
5.4.6	The balance should display the reading within the acceptance criteria specified for each of the standard weight range.
5.4.7	Take weight print of standard weight.
5.4.8	Enter the details in ‘Daily Balance Calibration Record’ as per Annexure No. 01. Ensure that the results obtained, comply with the acceptance criteria.
5.4.9	Update the “Instrument/Equipment Usage Log Book” as per SOP “Calibration of Instruments and Equipments”.
	B) Monthly calibration:
	Frequency:  Monthly or after carrying out any major maintenance work.
5.4.10	Generate the A. R. No. on the “Instrument/Equipment Calibration Register” as per SOP and give requisition to QA Department for calibration formats of instruments on the due date of calibration.
5.4.11	For issuance of calibration report refer QA SOP “Control of documents, Preparation, Approval, Issuance and Maintenance.
5.4.12	Perform the calibration of instrument as per Annexure and procedure mentioned below.
5.4.13	Prepare the “Monthly Calibration Schedule” as per Annexure yearly according to the Validity of weight box.
5.4.14	Calibration of Balance is performed for below parameters: 1. Uncertainty 2. Off Centre and Shift Error 3. Sensitivity check
	1. Uncertainty:
5.4.15	Uncertainty is checked using the standard weight 0.500 g.
5.4.16	Ensure that the display shows zero reading. If not press ‘TARE’ key to zero the display.
5.4.17	Keep the standard weight 0.500 g (xi) on the weighing pan and note down the observed reading (x).
5.4.18	Take 10 replicate readings with the same weight 0.500 g and calculate by using current standard weight (xi – x)2 for every reading.
5.4.19	Take weight print of standard weight
5.4.20	Calculate the Standard Deviation by the formula: SD    =            √  ∑  n ( x i  –  x )2       i=1     n -1 Where, ∑  n ( x i – x)2   = mean of  (xi – x)2  for 10 readings.   n = no. of readings taken.
5.4.21	Calculate uncertainty using the formula: Uncertainty =   3 X SD of 10 Replicate weighing Standard weight SD – Standard Deviation
5.4.22	Enter the details in “Monthly Balance Calibration Record as per Annexure. Ensure that the results obtained, comply with the acceptance criteria.Ο
	2. Off centre and shift error:
5.4.23	To check off centre and shift error the standard weight 0.0500 g is used.
5.4.24	Keep the weight on weighing pan on five different positions as shown below: 2.                                        3.   1.   4.                                           5.
5.4.25	Take weight print of standard weight
5.4.26	Enter the details in “Monthly Balance Calibration Record” as per Annexure No. 02. Ensure that the results obtained, comply with the acceptance criteria.
	3. Sensitivity check:
5.4.27	Place the standard weights on the weighing pan on by one as specified in the “Annexure 02”
	Note: Use current Standard certified weight for sensitivity range
5.4.28	Take weight print of standard weight.
5.4.29	Enter the Calibrated weight and observed weight with its acceptance criteria in excel sheet.
	Linearity Test:
5.4.30	Refer Sensitivity Check test for observed weight and plot the graph on excel sheet and calculate Correlation Coefficient. It should be performed Half yearly. Its acceptance criteria are +1 to -1.
5.4.31	Enter the details in “Monthly Balance Calibration Record” as per Annexure . Ensure that the results obtained, comply with the acceptance criteria.
5.4.32	Update the “Instrument/Equipment Usage Log Book”, “Annual Calibration Schedule” and “Monthly Calibration Schedule” as per SOP “Calibration of Instruments and Equipments”.
5.4.33	Affix the “Calibration Status” on the Instrument as per SOP “Calibration of Instruments and Equipments”.
5.4.34	For out of calibration refer SOP “Calibration of Instruments and Equipments”.
5.4.35	If calibration activity is outsourced, the values are to be transcribed in the Annexure , and external party certificate to be attached.
5.5	Cleaning Procedure:
5.5.1	Cleaning of the Balance should be done daily before calibration and before and after use.
5.5.2	Remove dust and powder with the help of tissue paper or soft nylon brush.
5.5.3	Do not leave anything on the weighing pan after use.
5.5.4	Clean the inside, outside and shutter of the balance with tissue paper or soft cloth soaked and squeezed in IPA to remove any oily substances or spots from the balance.
5.5.5	Then clean the balance with dry tissue paper.
5.5.6	If any breakdown occurs, follow procedure as per SOP “Calibration of Instruments and Equipments”.

 

6. Definitions / Abbreviations:

• Definitions:
• Breakdown: Any activity leading to operation of instrument/equipment other than the set parameters or unusual sound or vibration observed in the instrument/equipment.
• Calibration: Tests performed to ensure that the instrument/equipment is functioning as per set parameters. These tests are performed as per predefined frequency and also after any major repair or replacement of parts.
• Preventive Maintenance: Maintenance activity performed to ensure that the instrument/equipment will function smoothly and to avoid breakdowns. These activities are performed as per predefined frequency.
• Analytical weighing Balanceis a device used to find accurate measurements of weight. It is a class of   balance designed to measure small mass in the sub-milligram range.
• Abbreviations:

 

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
CAL	Calibration
IPA	Isopropyl Alcohol
g	gram
A. R. No.	Analytical Reference Number

 

Daily Balance Calibration Record

 

Performance  Check:                                                                            Acceptance Criteria: + 0.1%

 

Date	Zero Error	Standard Weights					Remark	Done by	Checked by
		0.0200 g	0.1000 g	1.0000 g	50.0000g	100.0000g

 

 

Monthly Balance Calibration Record

 

1. Test for Uncertainty:

Standard Weight as per current certified weight (0.5g):_________g         Limit = NMT 0.001

No. of Observations	Weight in gm observed	( xi–  x )2
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.

√∑  (x_i – x  ) ² =________

SD    =              ∑  ⁿ ( x _i – x)²       =__________

ⁱ⁼¹           n -1

SD =   3 X SD of 10 Replicate weighing = ________________

Standard weight

SD= _________________

 

2. Checks For Off Centre and Shift Error:

    Standard Weight as per current certified weight (0.05g):________g

    Limit = Error NMT 0.5 mg

     

Position of Weight

      2.                        3.

                    1.

   4.                              5.

 

Sr. No.	Weight in gm observed	Error  (NMT 0.5 mg)
1
2
3
4
5

 

3. Sensitivity Check: Acceptance Criteria: + 0.1%

 

Sr. No.	Nominal Weights in  gm	Standard Weights in gm (Certified)	Acceptance Criteria w.r.t std. weights in gm	Observation in gm
1.	100.0000 g
2.	50.0000 g
3.	20.0000 g
4.	10.0000 g
5.	5.0000 g
6.	2.0000 g
7.	1.0000 g
8.	0.5000 g
9.	0.2000 g
10.	0.1000 g
11.	0.0500 g
12.	0.0200 g

 

The results Complies / Does not complies as per acceptance criteria.

Performed By: ________________     Date:___________                 Checked By: ______________          Date: ____________

                                                      

*Note – Ready to use SOP available in “DOWNLOAD” Section.

SOP Title: Operation, Cleaning and Calibration of Moisture Analyzer

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of Moisture Analyzer.

 

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of Moisture Analyzer located in Quality Control Laboratory.

 

3. Responsibility:

• Quality Control Department: To prepare and review the SOP. To follow the procedures laid down for Operation, Cleaning and Calibration of Moisture Analyzer as per this SOP.
• Engineering Department: To carry out preventive maintenance as per schedule and procedure defined.
• Quality Assurance Department: To review and approve the SOP and Annexures.

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department.

 

5. Procedure:

5.1	Safety Precautions/Instructions:
5.1.1	Ensure all the electrical connections are properly earthed. Ensure the power plug of the Moisture Analyzer is fixed in the socket properly.
5.1.2	Ensure that the ON/OFF switch is working properly by switching “ON” the Moisture Analyzer.
5.1.3	Analysts must be familiar with precautions described in respective Material Safety Data Sheet of the materials before weighing it.
5.1.4	Moisture Analyzer Maximum range is 60 gm and Minimum range is 0.001 gm, do not exceeds the maximum weight limit. Weighing range is 0.5 gm to 40 gm.
5.1.5	Do not place flammable materials near the moisture Prohibitions analyzer.
5.1.6	Check the cleanliness of the Balance and its surrounding area.
5.1.7	The moisture analyzer includes a heater that heats samples to dry them off during measurement. The heater becomes hotter than the preset heating temperature. Incorrect handling may cause fire, explosion, burn injury.
5.1.8	Level the balance using levelling feet so that level indicator bubble is centered within the circle of levelling indicator
5.2	Front Panel-Keyboard:
5.2.1	Introduction to the Keys of Moisture Analyzer :
5.2.2	The front panel of the instrument keys are functional keys as follows:
5.2.3
	MENU   To enter the main menu.
	“►“                        To select the items.
	“▼”                       To move to the lower level.
	“▲”                       To move to the upper level.
	ENTER-  To accept the selection.
	ESC-To return to the standby state from the menu.
5.3	Operational  Procedure:
5.3.1	Check the validity of calibration before starting any operations.
5.3.2	Connect the power supply cord to the switch board and switch “ON” the balance and allow the balance to warm up for about 30 minutes.
5.3.3	When the power switch is turned on, the version number “*1” is displayed and the internal system is checked automatically. Then, “oFF” appears on the display panel. !!!!!!!!!—CHECK—OFF—-1.0000
5.3.4	The device enters the standby state i.e. it shows Main Measurement Display. PROGRAM                                           M/W 0.000 g
	Setting Measuring Condition
5.3.5	There are five types of drying modes (Standard drying automatic ending mode, Standard drying timed ending mode, rapid drying mode, slow drying mode, and stepped drying mode) for measurement conditions.
	A)    Setting the temperature and the amount of change in moisture content (▲M) as measurement condition(AUTO: Standard drying automatic ending mode):
5.3.6	In this mode, it dries a sample at the set temperature. When the amount of change in the moisture content take place below the set value, It terminates the measurement automatically.
5.3.7	The instrument can create 9 different program, before starting an run check the program number. Program parameter can be checked by selecting required program no.
5.3.8	Press “Menu” key, the display will show “program”. Press “►” to enter the program No., further Press “▲” or “▼” to create or edit the program number For example PNO.1
5.3.9	After enter the program No.  Press “▲” or “▼” to select “AUTO” mode for measuring condition and Press “Enter” key.
5.3.10	After selection of “AUTO” mode, Press “▲” or “▼” to select the temperature within the range from 50 °C to 200 °C in 1-degree increments.
5.3.11	After selection of temperature, Press “▲” or “▼” to select the moisture change rate per 30 seconds within the range from 0.01 % to 0.1 % in 0.01-percent increments.
5.3.12	To return the previous step Press “◄” key.
5.3.13	Press “Enter” key to save the programme and Press “ESC” key to return to the standby state.
	B)    Setting Temperature and Time as Measuring Conditions (TIME: Standard drying timed ending mode):
5.3.14	In this mode, it dries a sample at the set temperature. When the time set as the ending condition is reached, it terminates the measurement automatically.
5.3.15	This mode is suitable for measurements to be completed within a limited time.
5.3.16	Press “Menu” key, the display will show “program”. Press “►” to enter the program No.
5.3.17	After enter the program No.  Press “▲” or “▼” to select “TIME” mode for measuring condition and Press “Enter” key.
5.3.18	After selection of “TIME” mode, Press “▲” or “▼” to select the temperature within the range from 50 °C to 200 °C in 1-degree increments and followed by selection of drying time.
5.3.19	Press “▲” or “▼” to select the drying time within the range from 1 minutes to 4 hours in one minute increment or 4 hours to 12 hours in one hour increments.
5.3.20	To return the previous step Press “◄” key.
5.3.21	Press “Enter” key to save the programme and Press “ESC” key to return to the standby state.
	C)     Measuring Samples by Raising Temperature Rapidly (RAPID: Rapid drying mode):
5.3.22	In this mode, it raises the temperature rapidly until the amount of change in moisture content per 30 seconds drops below the set value. It dries a sample at the set temperature.
5.3.22	As the ending condition, select either the amount of change in moisture content per 30 seconds or the time.
5.3.23	When the amount of change in moisture content per 30 seconds drops below the set value, or the time reaches the set value, the measurement terminates automatically.
5.3.24	This mode is suitable for measuring liquid or other samples that take time to be dry.
5.3.25	Press “Menu” key, the display will show “program”. Press “►” to enter the program No.
5.3.26	After enter the program No.  Press “▲“ or “▼” to select “RAPID DRYING” mode for measuring condition and Press “Enter” key.
5.3.27	After selection of “RAPID DRYING” mode, Press “▲“ or “▼” to select the moisture change rate per 30 seconds within the range from 0.1 % to  9.9 % in 0.01-percent increments.
5.3.28	For selection of temperature Press “▲“ or “▼” to select the temperature within the range from 50 °C to 200 °C in 1-degree increments and followed by selection of drying time.
5.3.29	As the ending condition, select either the amount of change in moisture content per 30 seconds or the time.
5.3.30	If moisture change rate is selected, specify the value within the range from 0.01% to 0.1% in 0.01% increment and if Time is selected, specify the time within the range from 1 minutes to 4 hours in one minute increment or 4 hours to 12 hours in one hour increments.
5.3.31	To return the previous step Press “◄” key.
5.3.32	Press “Enter” key to save the programme and Press “ESC” key to return to the standby state.
	D)    Measuring Samples by Raising Temperature Gradually (SLOW: Slow drying mode):
5.3.33	In this mode, it raises the temperature more gradually than measurements in normal conditions, taking about five minutes from the time the measurement begins until the temperature reaches the preset level.
5.3.34	As the ending condition, select either the amount of change in moisture content per 30 seconds or the time.
5.3.35	When the amount of change in moisture content per 30 seconds drops below the set value, or the time reaches the set value, the measurement terminates automatically.
5.3.36	Sample that change in composition take place when exposed in rapid temperature and it burn dry. Slow drying mode is suitable for such sample to measure their moisture content.
5.3.37	This mode is suitable for measuring samples such as protein and high molecular compound that change when heated in a high temperature.
5.3.38	Press “Menu” key, the display will show “program”. Press “►” to enter the program No.
5.3.39	After enter the program No.  Press “▲“ or “▼” to select “Slow drying mode” mode for measuring condition and Press “Enter” key.
5.3.40	After selection of “Slow drying mode ” mode, Press “▲“ or “▼” to select the temperature within the range from 50 °C to 200 °C in 1-degree increments .
5.3.41	As the ending condition, select either the amount of change in moisture content per 30 seconds or the time.
5.3.42	If moisture change rate is selected, specify the value within the range from 0.01% to 0.1% in 0.01% increment and if Time is selected, specify the time within the range from 1 minutes to 4 hours in one minute increment or 4 hours to 12 hours in one hour increments.
5.3.43	To return the previous step Press “◄” key.
5.3.44	Press “Enter” key to save the programme and Press “ESC” key to return to the standby state.
	e)Measuring Samples by Setting Temperature Step by Step (STEP: Stepped drying mode):
5.3.45	If the crystal of hydrate is dried off, heat changes its composition. As a result moisture content measured differently depending on the drying temperature.
5.3.46	In Stepped drying mode, the drying temperature of sample in maximum three steps, which is suitable for measuring moisture content at different temperatures.
5.3.47	In the Stepped drying mode, the drying temperature and time in one to three steps for measurement purpose.
5.3.48	As the ending condition, select either the amount of change in moisture content per 30 seconds or the time.
5.3.49	After measuring a sample by changing drying temperature in two or three steps, when the amount of change in moisture content per 30 seconds drops below the set value, or the time reaches the set value, the measurement terminate automatically.
5.3.50	Set the temperature and time of the first step, second step and the third step.
5.3.51	Press “Menu” key, the display will show “program”. Press “►” to enter the program No.
5.3.52	After enter the program No. Press “▲” or “▼” to select “Stepped drying mode” for measuring condition and Press “Enter” key. Followed by the selection of temperature of the first step.
5.3.53	Press “▲” or “▼” to select the temperature of the first step within the range from 50 °C to 200 °C in 1-degree increments.
5.3.54	After select the temperature, Press “▲” or “▼” to select the time of the first step within the range from 1 minutes to 240 minutes in 1 minutes increments.
5.3.55	Press “▲” or “▼” to select the temperature of the second step within the range from 50 °C to 200 °C in 1-degree increments.
5.3.56	After select the temperature, Press “▲” or “▼” to select the time of the second step within the range from 1 minutes to 240 minutes in 1 minutes increments.
5.3.57	If the Measurement ends at the second step, then select the rate of moisture value within the range from 0.01 % to 0.1 % in 0.01-percent increments.
5.3.58	Press “Enter” key to save the programme and Press “ESC” key to return to the standby state.
5.3.59	If the measurement proceeds to the third step, select the time and specify the value within the range from 1 minutes to 240 minutes in 1 minute increment.
5.3.60	As the ending condition, select either the amount of change in moisture content per 30 seconds or the time. If moisture change rate (∆M) is selected, specify the value within the range from 0.01 % to 0.1 % in 0.01-percent increments.
5.3.61	If TIME is selected, set a time between 1 and 240 minutes, in one minutes increment.
5.3.62	To return the previous step Press “◄” key.
5.3.63	Press “Enter” key to save the programme and Press “ESC” key to return to the standby state.
	Moisture Analyzer Setting:
	Measurement Standard:
5.3.64	Change in the moisture analyzer setting can be done by setting a sample code or by setting a moisture analyser ID.
5.3.65	Press “Menu” key, the display will show “program”. Further Press “▲” or “▼” to Select “UNIT” from the menu.
5.3.66	Select the type of unit as per requirement. [M/W]    –     Moisture content (Wet Base) [D/W]    –      Dry content (Wet Base) [M/D]     –     Moisture content (Dry Base) [GRAM] –     Mass
5.3.67	Press “▲” or “▼” and select the type of unit.
	Method to Start Measurement:
5.3.68	After setting measuring condition for different types of drying mode mentioned at no. 5.3.5, “Easy” and “Normal” option shall be used to perform moisture content.
5.3.69	Generally “Easy” option shall be used for routine testing.
5.3.70	Ensure that Select the method to start measurement before placing a sample.
5.3.71	Press “Menu” key, the display will show “program”. Further Press “▲” or “▼” to Select “START” from the menu and “Enter” to select the method to start measurement.
5.3.72	Select the method to start measurement from the following two types:
5.3.73	Easy: Place a sample and close the heater cover, and the measurement will start automatically without pressing “START” key.
5.3.74	Normal: Press “START” key to start the measurement. Start the measurement even by keeping open heater cover. This is useful when the weight of a volatile sample is measure before it is dried.
5.3.75	If the stability mark (      ) is shown while “Easy” method appears, it indicate “Easy” method is set.
5.3.76	If only “Easy” method appears on screen without stability mark then it shall be considered as “Normal” method is set.
5.3.77	Press “Enter” key to move towards other parameters.
	Setting Sample Codes:
5.3.78	Set sample codes to identify the sample (object) from measurement results.
5.3.79	The sample code consists of four digits. The first and second digits allow “0 to 9”, “- (hyphen)”,”A to Z”, or “_ (underscore)” to be entered, and the third and fourth digits only allow “0 to 9”. For example for an Paracetamol API set the code as PA01.
5.3.80	Program no. and sample code are correlated. For example for program no.1 sample code is PA01. Then same code will be applied for Program no. 1 for all future testing.
5.3.81	Press “Menu” key, the display will show “program”.
5.3.82	Further Press “▲“ or “▼” to Select “Code” and press “Enter”.
5.3.83	In “Code” option a 4-digit number appears and the first digit flashes.
5.3.84	Press “▲“ or “▼” to enter a sample code.
5.3.85	Press “Enter” key to return to the standby state.
	Setting the Date and Time:
5.3.86	Press “Menu” key, the display will show “program”.
5.3.87	Further Press “▲“ or “▼” to Select date setting “Date” and press “Enter”.
5.3.88	Select the date format by pressing “▲“ or “▼” keys and Press”►“move to the next step.
5.3.89	Enter the year, month and day by pressing “▲“ or “▼” keys. Press “Enter” key to save the settings and Press”►“move to the next step.
5.3.90	Enter the hour and minute by pressing “▲“ or “▼” keys. Press “Enter” key to save the settings and Press”►“move to the next step.
5.3.91	Press “ESC” key to return to the standby state.
	Restricting the Menu Display:
5.3.92	Restrict the menu display so that the moisture analyser setting cannot be changed without authorization.
5.3.93	Press “Menu” key, the display will show “program”.
5.3.94	Further Press “▲” or “▼” to Select “Lock” and press “Enter”.
5.3.95	Enter the password by using “▲” or “▼” keys. When “Lock” is displayed, Press “ESC” key to return to the standby state.
	Setting the Password:
5.3.96	Restrict the menu display by setting the password. The password consists of four digits, and each digit allows “0 to 9” to be entered.
5.3.97	Press “Menu” key, the display will show “program”.
5.3.98	Further Press “▲” or “▼” to Select “PASS” and press “Enter”.
5.3.99	Enter the password by using Pressing “►” keys.
5.3.100	Press “ESC” key to return to the standby state.
5.3.101	Setting the Moisture Analyzer ID:
5.3.102	Set the moisture analyzer IDs, to identify which unit is responsible for measured data when the data check.
5.3.103	The ID consists of four digits, and each digit allows “0 to 9”, “- (hyphen)”, “A to Z”, or “_ (underscore)” to be entered.
5.3.104	Press “Menu” key, the display will show “program”.
5.3.105	Further Press “▲“ or “▼” to Select “ID” and press “Enter”.
5.3.106	Enter the ID by using Pressing “►” keys.
5.3.107	Press “ESC” key to return to the standby state.
	Actual Procedure to Measure Moisture Content:
5.3.108	Confirm that the device is in the standby mode. If it is not, Press “ESC” key to return to the standby state refer point no. 5.3.4
5.3.109	Enter the Program Number which already exist or create Programme as per sample requirement refer point no. 5.3.8
5.3.110	Press “Menu” key, the display will show “program” and press “Enter”. Press “▲“or”▼” to Select the drying modes as per sample requirement refer point no. 5.3.5 to 5.3.63.
5.3.111	Press “ESC” key to return to the standby state.
5.3.112	Press “▲“or”▼” to select measurement standards refer point no. 5.3.64 to 5.3.67
5.3.113	Further Press “▲“or”▼” to select the method to start the measurement refer point no. 5.3.68 to 5.3.77
5.3.114	Further Press “▲“or”▼” to set sample code refer point no. 5.3.78 to 5.3.85
5.3.115	Further Press “▲“or”▼” to set date and time refer point no. 5.3.86 to 5.3.91
5.3.116	Hold the handle of heater cover and carefully open the cover.
5.3.117	Place a sample pan on the pan supporter.
5.3.118	Placing a sample on the warmed sample pan may cause evaporation of moisture from the sample before starting measurement.
5.3.119	Before using sample pan ensure that it is in room temperature when measuring another sample.
5.3.120	Be sure that the Stability mark (     ) is displayed, it indicates that instrument is ready for analysis.
5.3.121	If the Stability mark is not displayed then press “O/T” to adjust the zero point.
5.3.122	Place a sample (object) on the sample pan and sample weight will appear on display.
5.3.123	Ensure that the sample placed should be as flat as possible and spread uniformly on the pan so that heat is applied evenly to the sample during measurement.
5.3.124	Place a sample with at least 0.5 grams on the sample pan.
5.3.125	After placing the sample, immediately close the sample pan with the heater cover.
5.3.126	If the instrument is in “Easy” method then RUN process will start Automatically.
5.3.127	For manual start, press “START” key to RUN process and the display will show “ΔM value“.
5.3.128	The heater fan will get start.
5.3.129	If the printer is connected, after Press “START” immediately Printer will print initial information such as Make, Model, Serial No., ID No., Code, Date, Time, Program No., Unit, Mode, Temperature and time or Moisture change rate, sample initial weight etc.
5.3.130	Press”▼” key to return to the previous display.
5.3.131	After completion of process a short beep sounds is heard, it indicate that the measurement is completed.
5.3.132	The display panel shows the measurement result and the measurement completed indicator ” “.
5.3.133	If the printer is connected to the instrument, Printer will print final information such as Moisture content in %, Time taken to complete the run and Dry sample weight. It will print the data automatically.
5.3.134	After completion of run the heater fan will stop automatically.
5.3.135	Press “ESC” key to return to the standby state.
5.3.136	After the measurement of a sample is completed, sample pan and the sample are hot after measurement.
5.3.137	Open the heater cover with the help of side holder. Take precaution, the heater cover is hot during and immediately after measurement.
5.3.138	Wait until heater cover and sample pan are cooled to room temperature. Remove sample pan with the help of sample holder and dispose the sample as laboratory waste. Ensure that heater cover and sample pan has attain room temperature, before performing next measurement.
5.3.139	Hold an edge of the sample pan with the handler to dispose a sample.
5.3.140	After the disposal, return the sample pan onto the pan supporter.
5.3.141	Update the “Instrument/Equipment Usage Log Book” as per SOP  “Calibration of Instruments and Equipments in Quality Control”.
	Aborting Measurement:
5.3.142	To abort the measurement while process is run mode, Press “STOP” key, a long beep sound is heard and Instrument will display “ABORT”.
5.3.143	Press “ESC” key to return to the standby state without Printing the measurement result or Press “STOP” key again, the measurement completed indicator ” ” is displayed, the measurement results will print and the device enters the standby state.
	Print
5.3.144	Press “Menu” key, the display will show “program”. Press “▲“or”▼” to Select “Print”. Further press “►” keys to select “Memory”. By selecting “Memory” option it will print all moisture data report starting from installation till upto the date.
5.4	Calibration Procedure:
	1) Day of use Calibration 2) Quarterly Calibration
	A)Day of use Calibration:
5.4.1	Frequency: Before starting an analysis on moisture Analyser, calibrate the instrument with Standard Weight as specified in the “Annexure ”.
	B)Quarterly Calibration
5.4.2	Frequency: Quarterly or after carrying out any major maintenance work.
5.4.3	Generate the A. R. No. on the “Instrument/Equipment Calibration Register” as per SOP and give requisition to QA Department for calibration formats of instruments on the due date of calibration.
5.4.4	For issuance of calibration report refer SOP “Control of documents, Preparation, Approval, Issuance and Maintenance.
5.4.5	Perform the calibration of instrument as per Annexure and procedure mentioned below.
	1. Sensitivity check:
5.4.6	Place the standard weights on the weighing pan one by one as specified in the “Annexure”.
5.4.7	Enter the details in calibration report. Ensure that the results obtained, comply with the acceptance criteria.
	2. Moisture  Content
5.4.8	Take a 5 gm of primary standard Sodium Tartarate Dihydrate in the sample pan and set the temperature at 120° C to perform moisture content test for the calibration of moisture analyser.
5.4.9	After use of primary standard Sodium Tartarate Dihydrate, enter its usage in Primary Standard Receipt and Usage Record.
5.4.10	Repeat the same operation procedure from point no. 5.3.108 to 5.3.141
5.4.11	After completion of moisture content, Enter “Print” key to take print of result or if printer is connected Automatically printer will print the result.
5.4.12	Enter the details in calibration report, Ensure that the results obtained, comply with the acceptance criteria.
5.4.13	Update the “Instrument/Equipment Usage Log Book” as per SOP “Calibration of Instruments and Equipments in Quality Control” .Update the “Annual Calibration Schedule” as per SOP “Equipment’s/Instruments Calibration“
5.4.14	Affix the “Calibration Status” on the Instrument as per SOP “Calibration of Instruments and Equipment’s in Quality Control”.
5.4.15	If calibration activity is outsourced, the values are to be transcribed in the Annexure, and external party certificate to be attached.
5.5	Cleaning Procedure:
5.5. 1	Cleaning of the Moisture Analyzer should be done before and after use.
5.5. 2	Remove dust and powder with the help of tissue paper or soft nylon brush.
5.5. 3	Do not leave anything on the weighing pan after use.
5.5. 4	Clean the inside, outside and shutter of the balance with tissue paper or soft cloth soaked to remove any oily substances or spots from the balance.
5.5. 5	Clean the Moisture Analyzer with dry tissue paper.
5.5. 6	If any breakdown occurs, follow procedure as per SOP “Calibration of Instruments and Equipments”.

 

6. Definitions/Abbreviations:

• Definitions:
• Breakdown: Any activity leading to operation of instrument/equipment other than the set parameters or unusual sound or vibration observed in the instrument/equipment.
• Calibration: Tests performed to ensure that the instrument/equipment is functioning as per set parameters. These tests are performed as per predefined frequency and also after any major repair or replacement of parts.
• Preventive Maintenance: Maintenance activity performed to ensure that the instrument/equipment will function smoothly and to avoid breakdowns. These activities are performed as per predefined frequency.
• Moisture Analyzer: Itcovers a variety of methods for measuring moisture content in both high level and trace amounts in solid. Moisture in percentage amounts is monitored as a specification in Drugs.

 

• Abbreviations:

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
CAL	Calibration
°C	Degree celecius
g	gram
A. R. No.	Analytical Reference Number

  

Day of Use Calibration Record (Daily)

Note: Carry out the calibration of the instrument as per SOP for the following parameters:

Standard Weights	Certified value	Sensitivity Range
0.1000 g
0.5000 g
5.0000 g
10.0000 g

 

Performance Check:                                                                              Acceptance Criteria: +   0.1%

Date	Zero Error	Standard Weights				Remark	Sign
		0.1000 g	0.5000 g	5.0000 g	10.0000 g

 

Calibration Report (Quarterly)

1. Sensitivity Check: Acceptance Criteria: + 0.1%

Sr. No.	Standard weight	Certified value	Sensitivity Range	Observation in gm
1.	0.1 g
2.	1  g
3.	5  g
4.	10 g

 

2. Moisture Content

Sr. No.	Test	Specification Limit	Sample Weight (gm)	Temperature	Observation	Remarks
1.	Sodium Tartarate Dihydrate.

 

Standard Equipments used:

Sr. No.	Name of standard	Batch No.	Valid upto
1.	Sodium Tartarate dihydrate

 

The results Complies / Does not complies as per acceptance criteria.

 

Performed By: ________________ Date:________________        Checked By: ______________         Date: ______________

                                                      

*Note – Ready to use SOP available in “DOWNLOAD” Section.

SOP Title: Operation and Maintenance of Emergency Eyewash and Safety Shower

1. Objective:

To lay down the procedure for Operation and Maintenance of Emergency Eyewash and Safety Shower.

2. Scope:

This procedure is applicable for Operation and Maintenance of Emergency Eyewash and Safety Shower for accidental spillage of chemicals on the personnel of Quality Control Department.

 

3. Responsibility:
   • Quality Control: To prepare and review the SOP. To follow the procedures for Operation and Maintenance of Emergency Eyewash and Safety Shower.
   • Engineering Department: To carry out preventive maintenance as per schedule and procedure defined.
   • Quality Assurance Department: To review and approve the SOP and Annexure.

 

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department

 

5. Procedure:

5.1	Safety Precautions/Instructions:
5.1.1	Always keep the water supply valve in ON position.
5.1.2	Ensure that adequate supply of water must be available at any given time.
5.1.3	Provide medical attention after flushing the areas of contact for at least 15 minutes.
5.1.4	When chemical spillage occurs, remove contaminated clothing under the shower.
5.1.5	Eye wash nozzles must be protected from airborne contaminants by flushing or running it periodically.
5.1.6	The 2014 ANSI standard recommends that the water temperature should be between 16-38°C.
5.2	Procedure for Handling of Eyewash and Safety Shower
5.2.1	Ensure that all employees who may need to use the emergency eyewash and safety shower equipment are trained on its location and use.
5.2.2	Conduct periodic checks to ensure that emergency eyewash station and shower equipment satisfactory.
5.2.3	Update periodic checking status label after flushing/testing activities for emergency eyewash and safety shower equipment.
5.2.4	Eye wash nozzles must be protected from airborne contaminants by flushing or running it periodically.
5.2.5	If incident occur immediately inform concern supervisor.
5.2.6	If effect of a hazard may be limited to the worker’s face and eyes immediately remove goggle or contact lenses to avoid any delays caused injury to eyes.
5.2.7	Bring  the person under the eyewash shower, flush the eye with fluid by turning the handle downward
5.2.8	Because of intense pain the person may not always be able to flush their eyes on their own.
5.2.9	On such occasion trained helpers should be prepared to assist with holding the eyelids open and roll the eye ball continuously so water will flow on surface of eye.
5.2.10	Other helpers may need to assist with keeping the person under the flushing fluid for at least 15 minutes or till irritation in the eye reduced.
5.2.11	To stop flow of water, push handle upward or back to the position.
5.2.12	Seek medical attention after flushing the areas of contact for at least 15 minutes or till irritation in the eye reduced.
5.2.13	If spillage of chemicals is in the eyes and on the body then initially eye wash treatment should be given and followed by shower treatment on the body.
5.2.14	Immediately bring the person under the shower and pull safety shower handle towards right hand side.
5.2.15	If chemical spillage on the body is serious in nature, immediately remove contaminated clothing under the shower.
5.2.16	Nature of incident assistant may use a fire blanket or uncontaminated article of clothing as a shield to provide privacy, under emergency for body coverage while seeking medical attention.
5.2.17	Seek medical attention after flushing the areas of contact for at least 15 minutes or till irritation reduced.
5.2.18	To stop flow of water, push handle back to the position.
5.2.19	Inform the supervisor as soon as the emergency has subsided.
5.3	Testing:
	Testing Frequency: Fortnightly
5.3.1	Equipments required are: 1. Bucket 2. Tray with wheels and handle to transport bucket.
5.3.2	Align bucket with valve under Emergency Shower.
5.3.3	Start safety shower by pulling handle and run for 2 minutes.
5.3.4	Record total volume of water collected.
5.3.5	To stop flow of water, push handle back to the upward position
5.3.6	Record testing and flushing on the inspection Annexure, affix label on the emergency eyewash and Safety shower.
5.4	Preventive Maintenance:
5.4.1	Perform the preventive maintenance as per Annexure.
5.4.2	If preventive maintenance activity is outsourced, the observations are to be transcribed in the Annexure and external party certificate to be attached.

 

5. Definitions / Abbreviations:

• Definitions:

 

• Abbreviations:

 

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
PM	Preventive Maintenance
ANSI	American National Standard of Inspection

 

*Note – Ready to use SOP available in “DOWNLOAD” Section.

SOP Title: Operation, Cleaning and Calibration of  Tablet  Hardness Tester

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of Hardness Test Apparatus.

 

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of Hardness Test Apparatus located in Quality Control Laboratory.

 

3. Responsibility:

• Quality Control: To prepare and review the SOP. To follow the procedures laid down for Operation, Cleaning and Calibration of Hardness Test Apparatus as per this SOP.
• Quality Assurance Department: To review and approve the SOP and Annexures.

 

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department

 

5. Procedure:

Sr. No.	Procedure
5.1	Safety Precautions/Instructions:
5.1.1	Ensure all the electrical connections are properly earthed. Ensure the power plug of the Tablet Hardness Tester is fixed in the socket properly.
5.1.2	Wear personal protective equipments such as safety glasses, hand gloves during operation of instrument.
5.1.3	Ensure that the ON/OFF switch is working properly by switching “ON” the Tablet Hardness Tester.
5.1.4	During the test do not put Fingers between movable test jaw and Fixed jaw, it can be squeezed.
5.1.5	During breaking the test samples fragments of the samples can spring   off. Use only protective glasses.
5.2	Front Panel-Keyboard
	Introduction to the Keys of Disintegration Tester :
5.2.1	Left hand side keys on the front panel of the instrument are alphanumeric keys having dual functions are (A-Z, 1-9), Zero (0) with Dash (-), Dot (.), Slash (/), Decimal point (.) and Clear Entry (CE) Key.
5.2.2	Right hand side keys are functional keys as follows:
5.2.3	RESET- To Reset instrument.
5.2.4	BACK-To go backward for previous function display screen.
5.2.5	ESCAPE To go back to main menu.
5.2.6	ENTER-To acknowledge the entered value.
5.2.7	START-  To start the direct measurement.
5.2.8	STOP-To stop the direct measurement.
5.3	OPERATION  OF TABLET  HARDNESS TESTER:
5.3.1	Check the validity of calibration before starting any operations.
5.3.2	Ensure that the instrument should be cleaned before operation.
5.3.3	Connect the power cord to 230 VAC/50 Hz stabilized power supply.
5.3.4	Switch ON the mains of Tablet Hardness Tester.
5.3.5	Allow 15 minutes warm up time before operation of Tablet Hardness Tester.
5.3.6	After instrument is powered “ON”. Press the “RESET” key, it gets initialized and the 2 line LCD display will read.
5.3.7	V3.03 indicates the firmware version of the system.
5.3.8	If instrument is not calibrated display shows: Perform calibration for Hardness, Length/Diameter/Width/Thickness
5.3.9	Press “ENTER” key to select main menu function.
5.3.10	The display shows: 1)Prog    2)Run   3)Print   4)Disp 5)Function  6)Configuration   J=40mm
5.3.11	1)‘Program’         :To Add(create)/, edit, view, copy, delete Programs. 2)‘Run’                 :To Run the desired Program. 3)‘Print’                :To obtain a hard copy of Program, Result, Calibration Report, Validation  report, Template.  4)‘Disp’                :To display the result. 5)‘Function’         :To set Clock & Date. To perform Calibration, Clear the calibration, Edit Run No., Cal. Reminder 6)‘Configuration’:To select Weight transfer, Data transfer to  pc/ printer ,to                                       set Password , to set System setting , to set Report Setup.
	1)PROGRAM  ENTRY:
5.3.12	Select   ‘PROG’ from main menu option by pressing ‘1’. press “ENTER” and the display shows : 1)ADD      2)VIEW 3) COPY   4) DELETE
5.3.13	To create program no. 1 press ‘1’ and press  “ENTER” and  the instrument will display as: Prog No(1-20): 1 ADD/EDIT Mode
5.3.14	Press “ENTER” and the display will read : Product Name:___
5.3.15	Use Alphanumeric Keys to Enter Sample Name.
5.3.16	Press “ENTER” and the display will read : No. of Table (1-99):_
5.3.17	Enter value and press “ENTER”, the   display will read: % Length/Diameter Limit (0.01-100):-_
5.3.18	Select % Length/Diameter Limit and press “ENTER”, the   display will read: Length Sensitivity: (10-30)———-
5.3.19	Select Length Sensitivity  and press “ENTER”, the   display will read: Breaking Sensitivity (30-250) :————–
5.3.20	Select Breaking Sensitivity  and press “ENTER”, the   display will read: Speed:1)0.2    2)0.4    3)0.6    4)0.8 5)1.0       6)1.2      7)1.4       8)1.6:
5.3.21	Enter speed  and press “ENTER”, the   display will read: Program No. 1 Stored———–
	b) To select tolerance limit in Value:
5.3.22	Select Hardness limit and press “ENTER”, the   display will read: Nominal Length/Diameter (0.1-40 mm):
	2)  RUN  Process :
5.3.23	Note: 1) During the test, part of the body like fingers etc. can be squeezed between the movable test jaw and fixed jaw. 2) Please place the sample tablets with tweezers or a similar tool. 3) To remove the remaining test pieces use the supplied brush. 4) During breaking the test samples fragments of the samples can  spring off. Use only protective glasses.
5.3.24	To Run the instruments, 1st Check & Clean the Sample tablet Carousel base for fragments of earlier test sample, Clean the fragments by the brush.
5.3.25	To Run the instrument, press ‘2’ and the display shows : Login: 1)Admin  2)User
5.3.26	To run through User,press‘2’ and Press ‘ENTER’ and the display shows : User (1- 25) :
5.3.27	Enter User No. press “ENTER” and it will Display: Enter User Password —-
5.3.28	Password is in numeric for ( minimum 4 digit And maximum 8 digit).
5.3.29	Enter password and  Press “ENTER” and the display will show: Enter User Password————–
5.3.30	To Run program  press ‘2’ refer point no.5.3.11 and  and  the instrument will display as: Program No(1-99): RUN  Mode
5.3.31	Enter Program No. and Press “ENTER” and the display will read : Product Name:______
5.3.32	Use Alphanumeric Keys to Enter All the data.
5.3.33	Press “ENTER” and the display will read : Batch No:—————
5.3.34	Enter batch No. and Press “ENTER” and the display will read : Stage:
5.3.35	Enter Stage  and Press “ENTER” and the display will read : Press Details:
5.3.36	Enter Press Detail  and Press “ENTER” and the display will read : Comment:
5.3.37	Enter Comment  and Press “ENTER” and the display will read : Weight 1 (0.01-99999.9 mg):
5.3.38	For manual weight entry set in the ‘Configuration’ option then, Enter the Weight manually by keyboard for 1st Tablet in mg.
5.3.39	Continue entering weights of remaining tablets, one by one, as per No. of tablets entered in program.
5.3.40	Press Print Key of Balance to Xfer Wt. Note: When Weight Transfer is in AUTO mode from Balance, Balance should be ‘ON’ & connect to the instrument to transfer the weight press “PRINT” key of balance after stable display, and Display will show:
5.3.41	If  the tablet Wt. entry selection is No., then display will show: Initialized to home Load Sample  & press ‘Enter’
5.3.42	Place tablet in proper position to measure Width & press ‘Enter’ Keep the weighed tablets on the Tablet Base positioning towards the fixed Jaw  and display will show:
5.3.43	Press “ENTER” and the display will read : Wait…. Measuring Width
5.3.44	Movable jaw will start moving towards fixed jaw with high speed until it reaches to pre-calculated distance (width + limit + 1.0 mm), Display show: Place tablet in proper position to measure Width & press ‘Enter’ Width  = x.xxmm
5.3.45	Keep the tablet on the Tablet Base positioning towards the fixed Jaw.
5.3.46	Press “ENTER” and the display will read : Thickness  = x.xxmm Wait…. Measuring Thickness
5.3.47	Keep the tablet on the Tablet Base positioning towards the fixed Jaw, and the display will read : Place tablet in proper position to measure Width & press ‘Enter’
5.3.48	Press “ENTER” and the display will read : Length diameter =xx.xmm Hardness = x.xxN Wait…. Measuring Length/Hardness
5.3.49	Repeat this operation until all the tablet measurement are over, Press ‘ENTER’ to continue.
	Note: if Tablet is not detected, display shows ‘No Tablet’.
5.3.50	After completion of RUN, Display will show : Run Over
	To perform ‘START’/‘STOP’ Key function:
5.3.51	Press ‘START’ Key  and the display Show  as: 1)Hardness   2)Length / Diameter  3)Width 4) Thickness  5)All
5.3.52	To measure only Hardness Select ‘1’ To measure only Length / Diameter Select ‘2’ To measure only Width Select ‘3’ To measure only Thickness Select ‘4’ To measure all three parameters sequentially Select ‘5’
	1) To Measure Hardness:
5.3.53	Press ‘1’  and  “ENTER” and the display will read : 1) Measure   2)Print
5.3.54	To measure Hardness, press ‘1’  and  “ENTER” and the display will read : Product Name:
5.3.55	Enter product Name by using alphanumeric Key  and Press “ENTER” and the display will read Batch No. :
5.3.56	Enter Batch No. by using alphanumeric Key  and Press “ENTER”  and the instrument will read : Nominal length /Dia. (0.1-40.0):
5.3.57	Enter value and press ‘ENTER’, the display  read as: Length/Dia/Thick/Width Sensitivity (10 -30): % Limit(L/D):
5.3.58	Select Sensitivity  and press “ENTER”, the   display will read: Breaking Sensitivity: (30-250)
5.3.59	Select Sensitivity  and press “ENTER”, the   display will read: Speed: 1)0.2    2)0.4    3)0.6    4)0.8 5)1.0       6)1.2      7)1.4       8)1.6:
5.3.60	Enter Speed and press ‘ENTER’, the display  read as: Initialized to Home Load Sample & press “ENTER”,
5.3.61	Keep the tablet at the Hardness measurement area and display will show: Place tablet in proper position to measure Hardness & press ‘Enter’
5.3.62	Moveable jaw will start moving towards fixed jaw with High Speed until it reaches to pre-calculated distance (i.e. nominal length + 1mm) & continuous to move further with displacement speed as per selection, until the tablet breaks & giving hardness of tablet.
5.3.63	Note: 1) If Tablet is not detected, display shows ‘No Tablet’. 2) Eye protection is required when operating the Hardness Tester. Wear approved safety glasses. 3) There is pinch hazard between the sensing jaw and the power jaw.
5.3.64	Hardness = xx.xxN Wait…. Measuring Hardness Press “ENTER” and the display will read : Press “ENTER” or “STOP”
5.3.65	Wait…. Measuring Length &Hardness Hardness = xx.xxN If no. of tablet are 2 or more,To continue hardness measurement, Press “ENTER” and the display will read :
5.3.66	Repeat the above operation until all the tablet measurements are over.
	2) To Measure Length / Diameter :
5.3.67	Press ‘2’ refer point no. 5.3.51  and  “ENTER” and the display will read : 1) Measure   2)Print
5.3.68	To measure Length /Diameter, press ‘1’  and  “ENTER” and the display will read : Product Name:————
5.3.69	Enter product Name by using alphanumeric Key  and Press “ENTER” and the display will read Batch No. :————-
5.3.70	Enter Batch No. by using alphanumeric Key  and Press “ENTER”  and the instrument will read : Nominal length /Dia. (0.1-40):
5.3.71	Enter value and press ‘ENTER’, the display  read as: Length/Dia/Thick/Width Sensitivity (10 -30):   % Limit(L/D):
	Note: The jaw advance speed is set to default value 0.8mm/sec.
5.3.72	Press ‘ENTER’, the display  read as: Initialized to Home Load Sample & press “ENTER”,
5.3.73	Keep the tablet at the Hardness measurement area and display will show: Place tablet in proper position to measure Length & press ‘Enter’
5.3.74	Moveable jaw will start moving towards fixed jaw with High Speed until it senses the tablet for Length /Diameter.
5.3.75	Press “ENTER” and the display will read : Press ‘Enter’ or ‘STOP’ Wait Length / Diameter =x.xx mm Wait…… Measuring Length
5.3.76	To continue Length /Diameter measurement, Press “ENTER”
5.3.77	Repeat the above operation until all the tablet measurements are over.
	3) To Measure Width :
5.3.78	Press ‘3’  and  “ENTER” and the display will read : 1) Measure   2)Print
5.3.79	To measure Width, press ‘1’  and  “ENTER” and the display will read : Product Name:———-
5.3.80	Enter product Name by using alphanumeric Key  and Press “ENTER” and the display will read Batch No. :
5.3.81	Enter Batch No. by using alphanumeric Key  and Press “ENTER”  and the instrument will read : Nominal Width (1-15mm):
5.3.82	Enter value and press ‘ENTER’, the display  read as: Length/Dia/Thick/Width Sensitivity: (10 -30) % Limit(L/D):
	Note: The jaw advance speed is set to default value 0.8mm/sec.
5.3.83	Press ‘ENTER’, the display  read as: Initialized to Home Load Sample & press “ENTER”,
5.3.84	Keep the tablet at the Hardness measurement area and display will show: Place tablet in proper position to measure Width & press ‘Enter’
5.3.85	Moveable jaw will start moving towards fixed jaw with High Speed until it senses the tablet for Width.
5.3.86	Press “ENTER” and the display will read : Wait Width =x.xx mm   Press ‘Enter’ or ‘STOP’   Wait…… Measuring Width
5.3.87	To continue width, Press “ENTER”
5.3.88	Repeat the above operation until all the tablet measurements are over.
	4) To Measure Thickness :
5.3.89	Press ‘4’  refer point no.5.3.124 and  “ENTER” and the display will read : 1) Measure   2)Print
5.3.90	To measure Thickness, press ‘1’  and  “ENTER” and the display will read : Product Name:
5.3.91	Enter product Name by using alphanumeric Key  and Press “ENTER” and the display will read Batch No. :
5.3.92	Enter Batch No. by using alphanumeric Key  and Press “ENTER”  and the instrument will read : Nominal Thickness (1-15mm):
5.3.93	Enter value and press ‘ENTER’, the display  read as: Length/Dia/Thick/Width Sensitivity: (10 -30)   % Limit(L/D):
	Note: The jaw advance speed is set to default value 0.8mm/sec.
5.3.94	Press ‘ENTER’, the display  read as: Initialized to Home Load Sample & press “ENTER”,
5.3.95	Keep the tablet at the Hardness measurement area and display will show: Place tablet in proper position to measure Thickness & press ‘Enter’
5.3.96	Moveable jaw will start moving towards fixed jaw with High Speed until it senses the tablet for Thickness.
5.3.97	Press “ENTER” and the display will read : Press ‘ENTER’ or ‘STOP’ Wait……. Measuring Thickness Wait….. Thickness = x.xxmm
5.3.98	To continue Thickness measurement, Press “ENTER”
5.3.99	Repeat the above operation until all the tablet measurements are over.
	5) To Measure Width/Thickness/Length/Hardness parameters sequentially :
5.3.100	Please note: Measurement parameter sequence is Width / Thickness / Length/Diameter/ Hardness
5.3.101	Press ‘5’ refer point no.5.3.124 and  “ENTER” and the display will read : 1) Measure   2)Print
5.3.102	To measure all parameters, press ‘1’  and  “ENTER” and the display will read : Product Name:———–
5.3.103	Enter product Name by using alphanumeric Key  and Press “ENTER” and the display will read Batch No. :–
5.3.104	Enter Batch No. by using alphanumeric Key  and Press “ENTER”  and the instrument will read : Nominal Length /Dia.(0.1-40.0):
5.3.105	Enter Nominal Length /Dia by using alphanumeric Key  and Press “ENTER”  and the instrument will read : Nominal Thickness (0.1-15mm):
5.3.106	Enter Thickness by using alphanumeric Key  and Press “ENTER”  and the instrument will read : Nominal Width (1-15mm):
5.3.107	Enter value and press ‘ENTER’, the display  read as: Length/Dia/Thick/Width Sensitivity (10 -30): % Limit(L/D):
5.3.108	Select Sensitivity  and press “ENTER”, the   display will read: Breaking Sensitivity: (30-250)
5.3.109	Select Breaking Sensitivity  and press “ENTER”, the   display will read: Speed: 1)0.2    2)0.4    3)0.6    4)0.8 5)1.0       6)1.2      7)1.4       8)1.6:
	Note: The jaw advance speed is set to default value 0.8mm/sec.
5.3.110	Enter Speed and press ‘ENTER’, the display  read as: Initialized to Home Load Sample & press “ENTER”,
5.3.111	Keep the tablet at the Hardness measurement area and display will show: Place tablet in proper position to measure Width & press ‘Enter’
5.3.112	Keep the tablet on the base of positioning towards fixed jaw.
5.3.113	Press “ENTER” and the display will read : Place tablet in proper position to measure Thickness & press ‘Enter’ Wait….. Width = x.xxmm Wait……. Measuring Width
5.3.114	Press Enter and the display will read: Place Tablet in proper position To measure Thickness and ‘ENTER’ Wait….. Thickness =x.xxmm Wait….. Measuring Thickness
5.3.115	Length =x.xxmm Hardness=x.x N Press Enter and the display will read: Wait…… Measuring Length &Hardness
5.3.116	To continue measurement, Press “ENTER”
5.3.117	Repeat the above operation until all the tablet measurements are over.
	To  STOP the RUN:
5.3.118	Press ‘STOP’ Button and the display will read : Press ENTER or STOP
5.3.119	Press ‘STOP’ Button  and the display will read : 1) Measure   2)Print
5.3.120	Press ‘2’ and the display will read : Printing…….    Printing Over
	3)To Print program parameters / Result / Calibration Report / Template / Verification Report :
5.3.121	·   Ensure the Printer is properly connected, powered On and is online with A4 size paper is loaded in it.
5.3.122	Select Print option from main menu by pressing ‘3’, and the display will read as: 1) Program Parameters 2) Result  3)Template 4) Calibration Report  5)System parameter Report
	1) To Print Program Parameter :
	2) To Print Result :
5.3.123	Press ‘2’ refer point no. 5.3.195 and ‘ENTER’ and the display will read as: 1)All: 2)Skip out of Limit
5.3.124	To print all tablet results select ‘1’ & to print only tablets result which are in limits select ‘2’ and press ‘ENTER’  the instrument will display: Printing….
5.3.125	To continue the printing, Press ‘1’and to discontinue the Run, Press ‘2’
5.3.126	No Data B) If calibration data is not available display reads,
	1) Clock :To enter Date & Time (this setting is available for Admin only)
5.3.127	Enter Admin Password – Press ‘1’and the display will read as:
5.3.128	Enter Admin Password and Press ‘ENTER’ and the display will read as:  Press ‘Enter’ to Edit 05/08/08        10.10
5.3.129	To edit Date & Time, press ‘ENTER’
	2) To Calibrate the instrument :
5.3.130	To ensure the precision of the Instrument it must be calibrated at regular time intervals and when the measuring results are in doubt.
5.3.131	On completion of a calibration and verification cycle, calibration report can be printed.
5.3.132	Press ‘2’and the display will read as: Login : 1)Admin    2)User
5.3.133	Enter Admin Password Press ‘1’and the display will read as:
5.3.134	Enter Admin Password and Press ‘ENTER’ and the display will read as: 1)Hardness  2)Length/Dia/Width/Thickness
	a) To Perform Hardness Calibration
	Note: TH1050 M provides 3 point hardness calibration by using standard calibrated weights. We suggest weight from 5 – 30kg.
5.3.135	Press ‘2’and the display will read as: Login : 1)Admin    2)User
5.3.136	Press ‘ENTER’ and the display will read as: Remove L-jaw, Connect Pan, Remove all Weight, Press ‘ENTER’
5.3.137	The moving jaw arm will be moved forward & stops midway. Remove the L jaw from the moving jaw arm by removing screws by using PH Screw Driver & fix the hardness calibration bracket assembly (Pan) on the moving jaw by using the same screws by using PH Screw Driver.
5.3.138	Once the bracket is fixed on the moving jaw, place the instrument carefully on its right side so that the calibration pan is pointing vertically upward.(Do not hold the carousel top assembly & the Pan assembly.
5.3.139	Press ‘ENTER’ and the display will read as: Press ‘ENTER’ if stable reading Pan weight (Kg)=x.xx
5.3.140	Press ‘ENTER’ and the display will read as: Enter Weight W1( 1-50Kg) :
5.3.141	Keep 5 Kg Weight and press ‘ENTER’ and the display will read as: Measured Weight (Kg) = xx.xx Press ‘ENTER’
5.3.142	After stable reading ,press ‘ENTER’ and the display will read as: Enter Weight W2( >5-50Kg) : –
5.3.143	Keep 10 Kg Weight and press ‘ENTER’ and the display will read as: Measured Weight (Kg) = xx.xx Press ‘ENTER’
5.3.144	After stable reading ,press  ‘ENTER’ and the display will read as: Enter Weight W3( >10-50Kg) :
5.3.145	Keep 20 Kg Weight and press ‘ENTER’ and the display will read as: Measured Weight (Kg) = xx.xx Press ‘ENTER’
5.3.146	After stable reading ,press  ‘ENTER’ and the display will read as: Remove Pan & all weight,Fix L-Jaw press  ‘ENTER’
5.3.147	Now place the instrument carefully on its base. Remove the hardness calibration bracket assembly (Pan) fixing screws & refit the L jaw. (Do not hold the carousel top assembly & pan assembly).
5.3.148	While fixing ensure that there is no gap (Flush mounted) left between the L jaw & moving arm.
	Note: After every calibration of hardness, a calibration of Length / Diameter is necessary.
5.3.149	Now the moving arm will advances further to touch the fixed jaw and the display will read as: Tighten the L-Jaw srew and press  ‘ENTER’
5.3.150	Now slightly loosen the L Jaw screws and re-tighten them to ensure they are parallel, press  ‘ENTER’, and the display will read :   Perform Length /Diameter Calibration For Correct measurement   Verification Over
	Note: If calibration reminder function is enabled.
5.3.151	Enter Due Date : dd / mm / yy After few seconds ,and display will read as :
5.3.152	1) Hardness  2)Length/Dia/Width/Thickness Enter new calibration Due date, and display will read as :
	b) To Perform  Length Calibration:
5.3.153	1) Hardness  2)Length/Dia/Width/Thickness Press‘2’, and display will read as :
5.3.154	To enter Length sensitivity and Press‘ENTER’, and display will read as : Place Gauge & Press ‘ENTER’
5.3.155	Clean the movable jaw and fixed jaw using the brush.Now position the gauge close to fixed jaw orienting it in the centered  axis between the fixed & moveable jaw. and display will read as : Enter Length/Diameter (1-40 mm) =
5.3.156	Length Gauge for 25.1-65mm Jaw Length  Gauge for                                               0.1-40mm  Jaw
5.3.157	Wait….. Place 5 mm gauge, by pressing key “1” & “5” from the keyboard. Press ‘ENTER’ and display will read :
5.3.158	Moveable flat jaw will start moving towards fixed jaw until it senses the gauge for length & displays the Raw values of length with offset and returns to home position.
5.3.159	Same procedure to be followed  for measured raw value length of 10mm and 20mm from point no. 5.3.239 to 5.3.241
5.3.160	Display will show: Measured Length/Diameter = xx.xx mm Place standard for verification Press‘ENTER’ Calibration Over
	c) To Verify Length Calibration
5.3.161	Enter Length/Dia/Thickness/Width( 1-40 mm )= Clean the movable jaw and fixed test jaw using the brush. Press‘ENTER’and display will read as:
5.3.162	Place 5 mm Length gauge,  Enter  Value 5mm and Press ‘ENTER’
5.3.163	Enter Length/Dia /Thickness/Width( 1-40 mm )= To verify with 2nd standard and Press ‘ENTER’ display will read as:
5.3.164	Place 10 mm Length gauge,  Enter  Value 10 mm and Press ‘ENTER’
5.3.165	Enter Length/Dia /Thickness/Width( 1-40 mm )= To verify with 3rd standard and Press ‘ENTER’ display will read as:
5.3.166	Place 20 mm Length gauge,  Enter  Value 20 mm and Press ‘ENTER’
5.3.167	After few seconds ,and display will read as : Enter Due Date : dd / mm / yy
5.3.168	Enter new calibration Due date, and display will read as : 1) Hardness  2)Length/Dia/Width/Thickness
5.4	Calibration Procedure:
	Frequency:  Every Quarterly or after carrying out any major maintenance work.
5.4.1	Refer Annexure for calibration test to be performed and acceptance criteria.
5.4.2	Generate the A. R. No. on the “Instrument/Equipment Calibration Register” as per SOP number and give requisition to QA department for calibration formats of equipment/instruments on the due date of calibration.
5.4.3	For issuance of calibration report refer SOP  “Control of documents, Preparation, Approval, Issuance and Maintenance.
5.4.4	Same procedure to be followed  For Calibration of  Tablet Hardness Tester from point no. 5.3.130 to 5.3.168.
5.4.5	Calibration parameters are as follows: 1) Hardness 2) Length
5.4.6	Enter the details in calibration report. Ensure that the results obtained, comply with the acceptance criteria.
5.4.7	Update the “Instrument/Equipment Usage Log Book” and “Monthly Calibration Schedule” as per SOP “Calibration of Instruments and Equipments”. Update the “Annual Calibration Schedule” as per SOP i.e. Equipment’s/Instruments Calibration.
5.4.8	Up to date “Calibration Status” on the Instrument as per SOP  “Calibration of Instruments and Equipments”.
5.4.9	If calibration activity is outsourced, the values are to be transcribed in the Annexure, and external party certificate to be attached.
5.5	Cleaning Procedure:
5.5.1	Before cleaning the instrument unplug the power cord from the power source.
5.5.2	It is good laboratory practice to wipe away any spillage.
5.5.3	The exterior surface can be cleaned with soft cloth.
5.5.4	Do not use solvents like Chloroform, toluene.
5.5.5	Before and After use, clean the apparatus by removing tablet particles and powder from the platform using a brush and finally clean with lint free dry cloth.
5.5.6	If any breakdown occurs, follow procedure as per SOP “Calibration of Instruments and Equipments”.

 

6. Definitions / Abbreviations:

• Definitions:
• Breakdown: Any activity leading to operation of instrument/equipment other than the set parameters or unusual sound or vibration observed in the equipment.
• Calibration: Tests performed to ensure that the instrument/equipment is functioning as per set parameters. These tests are performed as per predefined frequency and also after any major repair or replacement of parts.
• Hardness Test: This test is performed to measure of the mechanical integrity of tablets is their breaking force, which is the force required to cause them to fail (i.e.,break) in a specific plane.
• Abbreviations:

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
A. R. No.	Analytical Reference Number
kgf	Kilo gram force
NLT	Not less than
NMT	Not more than
±	Plus or Minus

 

Calibration of Hardness Test Apparatus

1) Hardness Calibration:

 

Sr. No.	Parameters	Set Value (Kg)	Acceptance Criteria	Measured Value (Kg)	Complies / Does Not Complies
1	Hardness	5	±0.1Kg
		10	±0.1Kg
		20	±0.1Kg

 

2) Length Calibration:

Sr. No.	Parameters	Set Value (mm)	Acceptance Criteria	Measured Value (mm)	Complies / Does Not Complies
1	Length	5	± 0.06mm
		10	± 0.06mm
		20	± 0.06mm

 

Remark: The result Complies/Does not complies as per acceptance criteria.

 

Performed By: ________________      Date:________________     Checked By: ______________           Date: ______________

                                                    

 *Note – Ready to use SOP available in “DOWNLOAD” Section.

SOP Title: Operation, Cleaning and Calibration of Tablet Friability Tester

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of Friability Test Apparatus.

 

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of Friability Test Apparatus located in Quality Control Laboratory.

 

3. Responsibility:

• Quality Control: To prepare and review the SOP. To follow the procedures laid down for operation, cleaning and calibration of Friability Test Apparatus as per this SOP.
• Quality Assurance Department: To review and approve the SOP and Annexures.

 

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department

 

5. Procedure:

5.1	Safety Precautions/Instructions:
5.1.1	Ensure all the electrical connections are properly earthed. Ensure the power plug of the Friability Test Apparatus is fixed in the socket properly.
5.1.2	Wear personal protective equipment’s such as safety glasses, hand gloves during operation of instrument.
5.1.3	Ensure that the ON/OFF switch is working properly by switching “ON” the Friability Test Apparatus.
5.1.4	For safety reasons and to ensure sufficient cooling in the electronic compartment, the side walls of the instrument must be kept at least 30cm away from the walls or other objects.
5.1.5	No containers, chemicals or other appliances should be placed behind the instrument.
5.2	Front Panel-Keyboard:
5.2.1	Introduction to the Keys of Tablet Friability Tester:
5.2.2	Left hand side keys on the front panel of the instrument are alphanumeric keys having dual functions are (A-Z, 1-9), Zero (0) with Dash (-), Dot (.), Slash (/), Decimal point (.) and Clear Entry (CE) Key.
5.2.3	Right hand side keys are functional keys as follows:
5.2.4	RESET- To Reset instrument.
5.2.5	BACK- To go backward for previous function display screen.
5.2.6	ESCAPE- To go back to main menu.
5.2.7	ENTER-To acknowledge the entered value.
5.2.8	START- To start the program.
5.2.9	STOP-To stop the run program.
5.3	Operation  of Tablet  Friability Tester:
5.3.1	Check the validity of calibration before starting any operations.
5.3.2	Ensure that the instrument should be cleaned before operation.
5.3.3	Connect the power cord to 230 VAC/50 Hz stabilized power supply.
5.3.4	Switch ON the mains of Tablet Friability tester.
5.3.5	Allow 15 minutes warm up time before operation of Tablet Friability tester.
5.3.6	After instrument is powered “ON”. Press the “RESET” key,it gets initialized and the 2 line LCD display will read as follows.
5.3.7	Press “ENTER” key to select main menu function.
5.3.8	The display shows: 1)Prog    2)Run   3)Print 4)Disp   5)Funct   6)Cfg
5.3.9	1)‘Prog’               : To Add(create)/edit, view, copy, delete Programs. 2)‘Run’                 :To Run the desired Program. 3)‘Print’                :To obtain a hard copy of Method,Result and Validation report. 4)‘Disp’                :To display the result. 5)‘Function’         :Toset Clock & Date.To perform Validation. 6)‘Configuration’:To select Drum,Weight transfer,Data transfer & Password entry.
	1)PROGRAM  ENTRY:
5.3.10	Select   ‘PROG’ from main menu option  by pressing ‘1’. press “ENTER” and the display shows 1)ADD      2)VIEW 3) COPY   4) DELETE
	1) Adding a New Program:
5.3.11	To ADD/Modify a new /existing program, press‘1’. press “ENTER” and it will Display: Login: 1)Admin   2)User
5.3.12	Password is in only numeric form, Entry required is minimum 4 digit And maximum 8 digit.
5.3.13	For User password Press‘2’ and  “ENTER” and thedisplay will show: Enter User Password ————
5.3.14	Enter password  required and press “ENTER” and The display reads  : Enter User Password- xxxx
5.3.15	To create program no.1 press‘1’and press  “ENTER” and  the instrument will display as: Prog No(1-20): 1 ADD/EDIT Mode
5.3.16	Press “ENTER” and the display will read : Sample Name:___________
5.3.17	Use Alphanumeric Keys to Enter Sample Name.
5.3.18	Press “ENTER” and the display will read : Mode: _ 1>Time    2>Count
	To select Time Mode:
5.3.19	Press “1” and “ENTER” and the display will display as : Time (00:01-99:00) 00:00 (hh:mm)
5.3.20	Select time and Press “ENTER”
	2) RUN Process :
	Note:Do not touch / hold the drum during Run process.
5.3.21	To Run the instrument, press ‘2’
5.3.22	Drum gets initialized,  and display  will read: Prog. No. (1-20) :__
5.3.23	Select Prog. No. and Press ‘ENTER’
	·     To Run in Single Drum:
5.3.24	Press‘1’and ‘ENTER’ and the display shows: Identification No. 1: _
5.3.25	Enter ID No. by using alphanumeric Key( Maximum 10 digit).
5.3.26	Press “ENTER” and the display will read as: Initialized to home Load Sample 1 & Enter
5.3.27	Dedust the tablets carefully and weigh accurately the required number of tablets as per standard testing procedure on the balance and note down the weight.
5.3.28	Put the Tablets in drum, Press “ENTER” and the display will read as: Initial Wt.1 (gms) :__
5.3.29	Enter Wt. of Tablets by using alphanumeric Key.
5.3.30	If the Mode is ‘Time Mode’ Press “ENTER” and the display shows, Running Prg : 1 00:00:00
5.3.31	If the Mode is ‘Count Mode’ Press “ENTER” and the display shows, Running Prg : 2 Count: _
5.3.32	Tablet Dropped Final Wt.1 (gms) :__ After end of the run, instrument will rotate the drum in reverse direction and the display will read: Tablet Dropped Final Wt.1 (gms) :
5.3.33	Enter Tablet Final Wt. by using alphanumeric Key.
5.3.34	Press “ENTER” and the display shows: % Loss 1 =
	·     To Run in Dual Drum:
5.3.35	Press‘1’and ‘ENTER’ and the display shows: Identification No. 1:_
5.3.36	Enter ID No. for Drum 1.by using alphanumeric Key( Maximum 10 digit).
5.3.37	Press ‘ENTER’ and the display shows: Identification No. 2:_
5.3.38	Enter ID No. for Drum 2, by using alphanumeric Key( Maximum 10 digit).
5.3.39	Press “ENTER” and the display will read as: Initialized to home Load Sample 1 & Enter
5.3.40	Put the Tablets in drum 1, Press “ENTER” and the display will read as: Initial Wt.1 (gms) :__
5.3.41	Enter initial Tablets Wt. of Drum 1,by using alphanumeric Key.
5.3.42	Press “ENTER” and the display will read as: Initialized to home Load Sample 2 & Enter
5.3.43	Put the Tablets in drum 2, Press “ENTER” and the display will read as: Initial Wt.2 (gms) :__
5.3.44	Enter initial Tablets Wt. of Drum 2, by using alphanumeric Key.
5.3.45	If the Mode is ‘Time Mode’ Press “ENTER” and the display shows, Running Prg : 1 00:00:00
5.3.46	If the Mode is ‘Count Mode’ Press “ENTER” and the display shows, Running Prg : 2 Count: _
5.3.47	Tablet Dropped Final Wt.1 (gms) :__ After end of the run, instrument will rotate the drum in reverse direction and the display will read: Tablet Dropped Final Wt.1 (gms) :
5.3.48	Take the Wt. Of Tablets from tray 1 & Enter the Wt. And  Press “ENTER” and the display will read as: Final Wt.2 (gms) :__
5.3.49	Take the Wt. Of Tablets from tray 2 & Enter the Wt. And  Press “ENTER” and the display will read as: % Loss 1= % Loss 2=
5.3.50	Press “ENTER” and the display will read as: % Loss 1= % Loss 2=
	To perform ‘START’/‘STOP’ Key function:
5.3.51	Press ‘START’ Key,Drum will get initialised to home position and the display will read as: Initialized to home Load Sample  & Enter
5.3.52	Take the Wt. and Load  Tablet,Press “ENTER” and the display will show: Time :00:00:00       Count:XYZ
5.3.53	To STOP the Run, press “STOP” and the display will show: Tablets Dropped   Wait……
5.3.54	Take the Wt. of Tablets from tray & dothe calculation manually.
	Note: In START’/‘STOP’ Key function Print option is not available.
	1) Run data is available during power failure / interruption. Instrument will restart automatically.
	·     For Count Mode:
5.3.55	Continue Run 1)Y 2)N From‘X’ Count Display will show:
5.3.56	1 Count ‘X’ To Continue Run, press ‘1’ and it will display:
5.3.57	Tablet dropped To discontinue Run, press ‘2’ and it will display:
	·     For Time Mode:
5.3.58	Display will show: Continue Run 1)Y 2)N From‘00:XY:XY’
5.3.59	To Continue Run, press ‘1’ and it will display: 1 ‘00:XY:XY’
5.3.60	To discontinue Run, press ‘2’ and it will display: Tablet dropped
5.3.61	After few Seconds display reads, 1)Prg.    2)Run    3)Prn 4)Disp   5)Funct  6)Cfg
	2) If Run data is interrupted by pressing ‘ESC’ Key.
5.3.62	Display will show: 1)Prg.    2)Run    3)Prn 4)Disp   5)Funct  6)Cfg
	·     For Count Mode:
5.3.63	Continue Run 1)Y 2)N From‘X’ Count To Continue Run, press ‘2’ and it will display:
5.3.64	1 Count ‘X’ To Continue Run, press ‘1’ and it will display:
5.3.65	Tablet dropped To discontinue Run, press ‘2’ and it will display:
	·     For Time Mode:
5.3.66	To Continue Run, press ‘2’ and it will display: Continue Run 1)Y 2)N From‘00:XY:XY’
5.3.67	To Continue Run, press ‘1’ and it will display: 1 ‘00:XY:XY’
5.3.68	To discontinue Run, press ‘2’ and it will display: Tablet dropped
5.3.69	After few Seconds display reads, 1)Prg.    2)Run    3)Prn 4)Disp   5)Funct  6)Cfg
	3)  PRINT :
5.3.70	Select Print option from main menu by pressing ‘3’,to obtain a hard copy of Method, Result &Validation Report and the display will read as: 1) Program   2) Result 3) Validation Report
	2)To Print Result :
5.3.71	Press ‘2’and ‘ENTER’ and the display will read as: Printing….
	3)To Print Validation report
5.3.72	Press ‘3’and ‘ENTER’ and the display will read as: Printing…..
	4)  DISPLAY:
5.3.73	% Loss 1 = To Display result for single Drum , press ‘4’ from Main Menu option and the instrument will display:

 

5.3.74		% Loss 1 = % Loss 2 = To Display result for Dual Drum , press ‘4’ from Main Menu option and the instrument will display:
5.3.75		Enter 25 Counts and Press ‘ENTER’, After complition 25 count and display will show:  Counts1:25 RPM:_
5.3.76		Similarly for 50 Counts,75 Counts,100 Counts and 125 Counts, same procedure to be followed for Validation.
5.3.77		Instrument can do validation with 5 different counts OR to discontinue press ‘ESC’ Key
5.4	Calibration Procedure:
	Frequency:Every Quarterly or after carrying out any major maintenance work.
5.4.1	Generate the A.R.No. on the “Instrument/Equipment Calibration Register” as per SOP and give requisition to QA Department for calibration formats of instruments on the due date of calibration.
5.4.2	For issuance of calibration report refer SOP “Control of documents, Preparation, Approval, Issuance and Maintenance.
5.4.3	Check the number of Countscompleted on the display. For operation of stop watch refer SOP “Operation of Stop watch”. Note: Start the stop watch and cycle at once.
5.4.4	Perform the calibration of instrument as per Annexure and procedure mentioned below.
5.4.5	Switch ON the mains of FriabilityTestapparatus.
5.4.6	Select ‘Function’ from Main Menu option by pressing ‘5’ and the display will read as: 1)Clock   2)Validation
5.4.7	Login: 1)Admin  2)User Press ‘2’and the display will read as:
5.4.8	Enter User Password xxxxx To enter User password, press ‘2’and Enter Password (Minimum 4 digit & Maximum 8 digit) the display will read as: Enter User Password- xxxxx
5.4.9	Calibration parameters are as follows: 1) 25 Counts 2) 50 Counts 3) 75 Counts 4) 100 Counts 5) 125 Counts
5.4.10	Enter Counts1:_ (10-999) Press ‘ENTER’,Drums moves to count position and the display will read as:
5.4.11	Set the 25 Counts andPress ‘ENTER’, After completion 25 count and display will show:  Counts 1:25 RPM:_
5.4.12	Note down the Rotation by Tachometer and time by using Calibrated Stop watch.
5.4.13	After completion of Counts, stop the Stop Watch; Check the time taken to complete Entered Counts.
5.4.14	Same procedure to be followed  For 50 Counts,75 Counts,100 Counts and 125 Countsfrom point no. 5.4.10 to 5.4.13
5.4.15	Enter the details in calibration report.Ensure that the results obtained, comply with the acceptance criteria.
5.4.16	Update the “Instrument/Equipment Usage Log Book”,“Annual Calibration Schedule” and “Monthly Calibration Schedule” as per SOP “Calibration of Instruments and Equipments”.
5.4.17	Up to datethe “Calibration Status” on the Instrument as per SOP “Calibration of Instruments and Equipments”.
5.4.18	If calibration activity is outsourced, the values are to be transcribed in the Annexure, and external party certificate to be attached.
5.5	Cleaning Procedure:
5.5.1	Before cleaning the instrument unplug the power cord from the power source.
5.5.2	It is good laboratory practice to wipe away any spillage.
5.5.3	The exterior surface can be cleaned with soft cloth.
5.5.4	Do not use solvents like Chloroform,toluene.
5.5.5	Clean the drums with soft brush or free nylon cloth before and after completion of the test.
5.5.6	If any breakdown occurs, follow procedure as per SOP “Calibration of Instruments and Equipments”.

 

6. Definitions/Abbreviations:

• Definitions:
• Breakdown: Any activity leading to operation of instrument other than the set parameters and/ or unusual sound or vibration observed in the instrument.
• Calibration: Tests performed to ensure that the instrument is functioning as per set parameters. These tests are performed as per predefined frequency and also after any major repair or replacement of parts.
• Friability test: It is designed to evaluate the ability of the tablet to withstand abrasion in packaging, handling and shipping.

 

• Abbreviations:

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
±	Plus or Minus
No.	Number

 

Calibration Report

Sr. No.	Parameters	Acceptance Criteria	Observed counts	Acceptance Criteria	Observed Times(sec)	Complies / Does Not Complies
1.	25 Counts	25 ± 1		60±2 sec
2.	50 Counts	50 ± 2		120 ± 4 sec
3.	75 Counts	75 ± 3		180 ± 6 sec
4.	100 Counts	100 ± 4		240 ± 8 sec
5.	125 Counts	125±5		300±10 sec

 

Remark: The result Complies/Does not complies as per acceptance criteria.

 

Performed By: ________________   Date:________________       Checked By: ______________         Date: ______________

                                               

*Note – Ready to use SOP available in “DOWNLOAD” Section.