SOP Title: Operation, Cleaning and Calibration of Melting Range Apparatus

SOP Title: Operation, Cleaning and Calibration of Melting Range Apparatus

Objective:

To lay down the procedure for Operation, Cleaning and Calibration of Melting Range Apparatus.

Scope:

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

Responsibility:

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

Accountability:

Head Quality Control Department, Head Quality Assurance Department.

Procedure:

5.1

Safety Precautions/Instructions:

5.1.1

Ensure all the electrical connections are properly earthed. Ensure the power plug of the Melting Range 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 Melting Range Apparatus.

5.1.4

Do not operate the instrument in the presence of flammable gasses or Liquid.

5.1.5

Switch “ON” the Instrument the 15 to 20 min. before the Start of analysis.

5.1.6

Cleaning of the furnace should be done at ambient temperature. Only surface of the furnace is recommended to clean with damp cloth. Do not use organic solvent for cleaning the furnace surface.

5.1.7

While Sample analyzing using capillary preparation, 3 capillaries should be filled about 3 to 5 mm of sample.

5.1.8

For sample whose melting point is not known, use heating RATE: 6.1 to 12.1 °C/MIN.

5.1.9

For ‘Heat & Cool’ Mode, it is recommended to use heating rate 1°C/MIN.

5.1.10

It is recommended to use ‘MANUAL’ operation for coloured samples.

5.1.11

For samples, that shrinks or become transparent during heating process, increase sample size and use heating rates: 6.1 ~ 12.1 °C/MIN.

5.1.12

Ensure the round Cover-slip on the Furnace Lid is clear (not foggy),

5.1.13

Ensure the surface of the Furnace should be clean from any foreign particles for a good thermal contact of the slide.

5.1.14

The presence of foreign particle on slide/cover slip will create the thermal difference and leads to erroneous results.

5.1.15

Ensure that there should not be Direct Air Drift in the furnace direction.

5.2

Front Panel-Keyboard:

5.2.1

Introduction to the soft Keys of Front Panel :

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 directly to main menu.

5.2.7

ENTER- To acknowledge the entered value/parameter.

5.2.8

LAMP- To Switch the Lamp ON/OFF.

5.2.9

STOP-In RUN-MANUAL mode, to hold isothermal condition, while Furnace temperature is raised with the user specified Heating rate.

5.2.10

LOCK- To lock the Start and End Temperature of Melting process in MANUAL mode.

Sample Placement:

5.3

Operation of Melting Range Apparatus:

5.3.1

Check the validity of calibration before starting any operations.

5.3.2

Ensure that the instrument is clean 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 Melting Range Apparatus from back panel.

5.3.5

After instrument is powered “ON”. Press the “RESET” key, it gets initialized and the two line LCD display will read as follows

5.3.6

After 2 to 3 seconds screen will display the Main Menu:

1)Prog 2)Run 3)Print 4)Config T° C: XX

5.3.7

1) ‘Program’ :To Add(create)/,edit, view, copy, delete Programs.

2) ‘Run’ :To Run the desired Program.

3) ‘Print’ :To obtain print copy of Program, Result, Calibration Report, Graph.

4) ‘Config’ : To set Date & time and Data transfer to PC/Printer.

5.3.8

T° C: The screen will display furnace Temperature of Instrument.

1) For Addition of New Program:

5.3.9

Select ‘Prog’ from main menu option by pressing ‘1’. press “ENTER” and the display will show :

1)ADD 2)VIEW

3) COPY 4) DELETE

5.3.10

To create program number 1 press‘1’ and press “ENTER” and the instrument will display as:

Prog No(1-20):

ADD/EDIT Mode

NOTE: Instrument can save upto 20 numbers of program

5.3.11

Press “ENTER” and the display will read :

Sample Name:_______

5.3.12

Use Alphanumeric Keys to Enter Sample Name.

For Example:- Paracetamol

5.3.13

Press “ENTER” and the display will read as :

Sample Preparation: _

1) Slide 2) Capillary

Slide Preparation: Analysis is done by using Slide.

Capillary Preparation: Analysis is done by using Capillaries.

5.3.14

After Selection of sample preparation mode, Press “ENTER” and the display will read as :

Method: _

1) Stand 2) USP-1a

Standard method: Need to set parameters Externally.

USP-1a method: Method is set by default as per USP

5.3.15

Press ‘1’ for Stand or press ‘2’ for USP-1a and press ‘ENTER’ the display will read as:

NOTE: In method USP-1a the instrument will run with heating rate 1°C/Minute once the furnace temperature is reached to below 5°C of set temperature. Example: Set Temperature is 100°C then heating will start at 1°C/Minute once it reaches to 95°C.

I) Standard Method

5.3.16

Mode: _

1) Heat 2) Heat & cool

After Selection of standard method the display will read as:

Mode: _

1) Heat 2) Heat & cool

Heat mode: AUTO / MANUAL detection of Melting Point can be used with this mode

Heat & Cool mode: Only manual detection of Melting Point can be done by this mode.

5.3.17

Press ‘1’ for Heat and press ‘2’ for Heat & Cool mode as per requirement

NOTE: If ‘Heat & Cool’ Mode is selected, the Only ‘MANUAL’ detection is possible since the User has to Lock the Start & End temperature by pressing the LOCK key.

Heat Mode:

5.3.18

In Heat mode the display will read as :

Operation: _

1) Auto 2) Manual

Auto Operation: Auto operation used in case of known sample/Colorless sample.

Manual Operation: Manual operation is mostly used for coloured sample/ unknown sample.

5.3.19

Press ‘1’ Auto press ‘2’ for Manual operation as per requirement and press ‘ENTER’

Auto Operation

5.3.20

While operation with Auto Mode the display the will read as:

Set Temp ° C: __

5.3.21

Set Temperature is generally melting point of the Sample

5.3.22

After setting of temperature press Enter, the display will read as:

Rate: °C/MIN

Please enter RATE

5.3.23

Enter the desired temperature at which it should rise the temperature in °C/min. The temperature will rise at specified desired rate when it reaches 10° C below the set temperature For Example: Suppose X sample set temperature is 100°C and rate of temperature increment is 1°C/ min then the temperature will rise 1°C /min only after it has reached to 90°C.

5.3.24

After selection of Rate press ‘ENTER’. The programme will get saved as a 1 number programme.

5.3.25

If set Temperature is not in the limit the display will read as:

Invalid Entry

RANGE: 8 to 350

5.3.26

Re-enter the valid Set temperature to continue the program.

NOTE: The Furnace Temperature Cut-off Limit will be automatically calculated as Set Temp +15 °C for Heating Rates 0.2 to 6.0°C/Min.

Example: Set Temperature is 100°C then Furnace Temperature Cut-off Limit will be 115°C.

5.3.27

For Heating Rates 6.1 to 12.1°C/Min, the by default cut-off limit is at 365°C.

Manual Operation

5.3.28

While adding program with manual operation the display the will read :

Set Temp ° C: __

5.3.29

After setting of the Temperature press ‘ENTER’ the display will read as:

Furnace temperature

Cutoff Limit: __

5.3.30

The Furnace temperature cut-off limit is the limit at which the instrument run will get abort. The cut off limit should be about 10°C more than the sample Melting point.

NOTE: If the start and end temperature of melting are not locked manually, then the furnace will heat till CUT-OFF Temperature. ‘MANUAL’ operation recommended to use for colored/unknown samples.

5.3.31

After the selection of the furnace temperature the display will read as:

Rate: __ °C/MIN

Please enter RATE

5.3.32

After selection of Rate press ‘ENTER’. The programme will get saved as a 1 number programme.

5.3.33

If the Furnace Temperature Cut-off limit is less than SET Temperature or more than 365°C then the instrument gives an error message as below,

Invalid Entry!….

Limits: AB + 5 – 365 °C

Where AB is set temperature value.

5.3.34

Re-Enter the Furnace Temperature Cut-off limit to continue the program.

Heat & Cool Mode:

5.3.35

While adding Program with Heat & cool Mode the display will read as:

Set Temp ° C: __

5.3.36

After selection of the required temperature press ‘ENTER’ the display will read as:

Furnace temperature

Cutoff Limit: __

5.3.37

Rate: __ °C/MIN

Please enter RATE

Select the Furnace temperature cut-off Limit and press ‘ENTER’ , the display will read as:

5.3.38

After selection of Rate press ‘ENTER’. The programme will get saved.

II) USP-1a Method:-

5.3.39

While adding Program with USP-1a Method (From Point no.5.3.14)

5.3.40

After Selection of USP-1a method press ‘ENTER’ the display will read as :

Operation: _

1) Auto 2) Manual

5.3.41

Press ‘1’ for Auto and press ‘2’ for Manual operation as per requirement. And press ‘ENTER’

i) Auto Operation

5.3.42

While operation with Auto Operation the display the will read as :

Set Temp ° C: __

5.3.43

Enter the required temperature and press ‘ENTER’ to save the programme.

ii) Manual Operation

5.3.44

While operation with Manual Operation the display the will read :

Set Temp ° C: __

5.3.45

After selection of set temperature the display will read as:

Furnace temperature

Cutoff Limit: __

5.3.46

The instrument will set by default cut-off limit above 15°C of Set temperature OR can be set Cut-off limit manually as per requirement. Press ENTER to save the programme.

Note: If program parameters are already stored at a particular program number then, to modify the desired parameters, follow the same procedure as mentioned from point number 5.3.9 to 5.3.32 for modification of existing program. The previously stored parameters are displayed, which may be acknowledged by pressing ‘ENTER’ or may be modified as per requirement.

I) EXPLANATION OF MODE :

5.3.47

Modes are two types i.e. Heat Mode and Heat & Cool Mode

HEAT MODE:

5.3.48

In Heat mode, the furnace will heat till the end temperature of melting range is detected or till the Furnace cut-off temperature is attained.

HEAT & COOL MODE:

5.3.49

Only MANUAL operation is to be carried out with this mode

II) EXPLANATION OF OPERATION :

5.3.50

Operation are of two types i.e. ‘Auto operation’ and ‘Manual operation’

AUTO OPERATION:

5.3.51

The lamp will automatically adjust to optimum intensity depending on the brightness of the sample, in standard mode, below 5°C of the SET temperature & in USP-1A mode, 10°C below the set temperature. The system will then continue to heat with SET RATE. The start temperature will be automatically logged in, on the basis of slope changes. The end point is also detected automatically to give the melting range for the particular sample.

2) Procedure to RUN Programme :

5.3.52

Before Running the instruments, check the cleanliness of the instrument.

5.3.53

To Run the instrument, press ‘2’ from main menu 5.3.6 and the display will show :

Prog No.: _

Inst. Calibrated

5.3.54

For Example To run program no. 4.

5.3.55

Enter Program No. and Press “ENTER” and the display will read as :

Prog No.: 4 R_N0.: 1

1) Run 2) View: _

NOTE: R. No. indicates the run number for particular day.

5.3.56

If entered program no. does not exist then display will read as:

Prog No.:4

Prg does not exist!.

5.3.57

If program does not exists then display will returns to the main menu

5.3.58

Press ‘2’ i.e. View to check the Program details.

5.3.59

To Run the program press ‘1’ i.e. Run and press “ENTER” the display will read as :

Sample No: _

5.3.60

Enter Sample Number/Batch Number if it is available or else keep it as 1 number by using alphanumeric keys and Press “ENTER” and the display will read as:

Id. No.:_

NOTE: Maximum 10 character sample no. and I.D can enter.

5.3.61

Enter Id. No. by using alphanumeric keys and Press “ENTER” to run the program. Furnace will start heating.

5.3.62

The furnace temperature start rising fast till the Sample Insertion Temperature arrives.

Note:- The sample insertion temperature is the temperature below 15°C of set temperature. If the set Temperature is below 100° C then the sample insertion temperature will be 10° C below the set temperature.

Example: If SET Temperature is 114° C then the Furnace Temperature will rise fast till 99.0° C

5.3.63

The display will read as:

T°C: 26.5 SET: 114.0

Wait Heating! 99.0

NOTE: The furnace Lid should be placed on the furnace before start the analysis.

5.3.64

If furnace temperature is more than the Sample Insertion temperature, then the furnace cooling fan will turn “ON” internally until its temperature reaches below sample insertion temperature and the display will read as:

T°C: 100.1 SET: 114.0

Wait cooling! 99.0

5.3.65

After the Furnace reaches Sample Insertion Temperature the instrument will give beep sound and the display will read as:

T°C: 99.0 SET: 114.0

Keep Sample & ‘ENTER’

NOTE: If ‘ENTER’ key is not pressed within 5 minutes, furnace will cool down to room temperature for the purpose of power saving and safety.

5.3.66

Prepare sample as per required method i.e. Slide and Capillary method

Sample Preparation for Slide method:

5.3.67

Required Accessories for Slide method

1) Clear Glass slide

2) Clear Round Cover slip

3) Clear dry mortar and pastel

4) Small Spatula

5) Finely crushed sample powder.

5.3.68

SAMPLE

POWDER

22 DIA.

COVER

SLIP

MICRO –SLIDE

1 MM THICK

5.3.69

Place the finely powdered sample on the one side of the glass slide. Finely spread the sample with the help of spatula. Place the round cover slip on the sample. Check for the sample is homogeneously spread in a circle.

Sample Preparation for Capillary method:

5.3.70

Required Accessories for Slide method

1) Clear dry mortar and pastel.

2) One sealed Capillary tube

3) Sample Filling Tube

4) Tissue paper

NOTE: Place a round cover slip for Slide method & square cover slip for Capillary method on the furnace lid. In between the Runs, the furnace lid should be sufficiently cooled.

5.3.71

Put the sample and press ‘ENTER’ the display will read as:

T°C: 104.5 SET: 114.0 Heating! 109.0

5.3.72

The furnace will heat up to 5 °C below Set temperature and the Lamp will be switched ON automatically as soon as the Furnace temperature reaches 5°C below Set Temperature and the display will read as:

Switching Lamp On…

NOTE:

i. Instrument checks the light level & adjusts the illuminator intensity automatically for the optimum sensitivity level of Photo sensor.

ii. In AUTO operation, if the sample is not placed properly / sample quantity is less / sample preparation is not correct, a message will display accordingly error messages .

5.3.73

Now the Furnace temperature rises as per specified rate and the display will read as:

T°C: 109.0 ST°C: ____

AUTO ET°C: ____

NOTE: For MANUAL operation, ‘MANUAL’ will appear in left corner of the display instead of ‘AUTO’

5.3.74

While Program running with AUTO operation, when the sample start melting, the photo sensor will detects start of the melting temperature and will record it automatically and display will show recorded temperature as “ST” as shown below:

T°C: 114.5 ST°C: ____

AUTO ET°C: ____

5.3.75

Furnace temperature will rise as per the specified Heating Rate. When the sample melts completely instrument will record the end temperature i.e. ‘ET’ and the display will read as:

T°C: 115.5 ST°C: 114.5

AUTO ET°C: 115.5

NOTE: While sample running with MANUAL operation Start temperature ‘ST’ and End temperature ‘ET’ is recored manually by using ‘LOCK’ key.

5.3.76

After completion of melting point, press ‘ESC’ the display will return to Main menu.

3) Procedure to Print Reports and programmes :

5.3.77

To Print the data like Program, Result, Calibration Report, Graph, press ‘3’ from main menu refer point number 5.3.6

The display will show :

1) View Prev.Result

2) Print: _

5.3.78

Press ‘1’ and press ‘ENTER’, to view the previous result. The Display will read the complete Set of parameters and Results in Screen by screen,

5.3.79

Press ‘2’ and press “ENTER” to obtain a hard copy of Program, Result, Calibration Report, and Graph the display shows :

1) Prg Para 2) Rpt: _

3) Cal Rpt 4) Graph

5.3.80

For the hardcopy of last RUN report Press ‘2’ and ‘ENTER

5.3.81

1) Select 2) All: _

To print Hardcopy of program parameter Press ‘1’ & press “ENTER” the display will show :

5.3.82

Select ‘1’ to print the hard copy of single selected Program parameter and select ‘2’ to print hard copy of all saved program parameter.

5.3.83

Prog No. (1-20):

To print the hard copy of single program press ‘1’ and ‘ENTER’, the Display will read as:

5.3.84

Select the required program number and press ‘ENTER’.

5.3.85

3) Cal Rpt:-To print the Instrument Calibration report done in Factory press ‘3’ & ‘Enter’.

5.3.86

To print the hardcopy of last run sample graph press ‘4’ & ‘Enter’.

Note: The ‘Graph’ option will be displayed only if last sample RUN was performed in AUTO operation. No graph is available for MANUAL Operation and serial transfer mode.

5.3.87

While Printing data the display will show:

PRINT MODE…

5.3.88

While printing is in Progress the display will show:

WAIT… PRINTING DATA

and after printing the display will show below screen and will return to main menu

PRINTING OVER….

If printer is not connected then the display will show below screen and will return to main menu.

PRINTER NOT READY!.

NOTE: Only Last run result can be viewed or printed.

Note: For invalid Entry, the entry position gets blank/clear and cursor returns to start of the entry

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

Perform the calibration of instrument as per Annexure No. 01 and procedure mentioned below.

5.4.4

Determine the melting points of the following standard materials:

1) Vanillin

2) Sulphanilamide

3) Caffeine

4) Benzoic Acid

5.4.5

Follow the same procedure from point no. 5.3.52 to 5.3.76

5.4.6

Enter the details in calibration report Annexure No. Ensure that the results obtained, comply with the acceptance criteria.

5.4.7

Update the “Instrument/Equipment Usage Log Book”, and “Calibration Schedule” as per SOP “Calibration of Instruments and Equipments in Quality control”. Update the “Annual Calibration Schedule” as per SOP,“Equipment’s / Instruments Calibration”

5.4.8

Affix the “Calibration Status Label” 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 No. 01, and external party certificate to be attached.

5.4.10

For Out of calibration/breakdowns, follow procedure as per SOP “Calibration of Instruments and Equipments”.

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 with dry cloth.

5.5.3

The exterior surface can be cleaned with soft dry cloth.

5.5.4

Do not use solvents like Chloroform, toluene.

5.5.5

Before and After use, clean the apparatus by removing sample particles powder from the platform using a brush and finally clean with dry cloth.

5.5.6

Use damp cloth or tissue paper to clean the lens. Do not adjust camera aperture since it is factory setup. The lens cleaning activity is recommended weekly. Always put lens cap when instrument is not in operation. User should not try to remove camera from Instrument since its alignment is factory adjusted.

Definitions / Abbreviation:

Definitions:
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.
Melting point: The temperature at which the solid and liquid forms of a pure substance can exist in equilibrium.
Melting Range: The temperature range from which the crystals of the substance
Principle: Melting point is the temperature at which a solid becomes a liquid at standard atmospheric pressure; at this point, solid and its liquid are in an equilibrium state at a certain pressure. Melting point is one of the physical properties of a compound by which it is identified.
Abbreviation:

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control

QA	Quality Assurance
A. R. No.	Analytical Reference Number
° C	Degree Celsius
MIN	Minutes
Temp	Temperature

Calibration Report

Sr. No.	Standards	Acceptance Criteria	Observed Values	Complies / Does Not Complies
1.	Vanillin	81^°C – 83^°C
2.	Benzoic Acid	121°C -123°C
3.	Sulphanilamide	163°C – 165°C
4.	Caffeine	234^°C – 237^°C

Remark: The result Complies/Does not complie’s as per acceptance criteria.

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

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

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