SOP Title: Operation, Cleaning and Calibration of KBr Press Apparatus

 SOP Title: Operation, Cleaning and Calibration of KBr Press Apparatus

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of KBr Press Apparatus.

 

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of KBr Press 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 KBr Press Apparatus 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	Wear personal protective equipments such as safety glasses, hand gloves during operation of equipment.
5.2	Operational  Procedure:
5.2.1	Check the validity of calibration before starting any operations.
5.2.2	Check and ensure that the KBr Press is clean and suitable for use.
5.2.3	Take approximately 1 to 3 mg of the sample and 100 to 300 mg of potassium bromide (dried for 105oC for 1 hour) in clean and dried granite mortar and pestle.
5.2.4	Grind the potassium bromide with the sample in order to mix it thoroughly.
5.2.5	Insert the small shiny stainless steel round disc into the barrel with the polished side up.
5.2.6	Assemble the dye by inserting the barrel into the base.
5.2.7	Transfer the powder from the mortar into the barrel with the help of clean and dry stainless steel spatula or butter paper in such a way that the surface of the powder in the barrel is levelled and uniformly spread over the barrel.
5.2.8	Now insert the plunger slowly and carefully.
5.2.9	Place the dye assembly in the centre of the KBr press.
5.2.10	Rotate the wheel on top of the KBr press in clockwise direction until it holds the dye assembly tightly.
5.2.11	Ensure that the dye assembly is tightly placed between the top and bottom of the KBr press.
5.2.12	Close the valve present at the side of the pressure gauge in the clockwise direction and increase the pressure by moving the piston to about 10 tons and wait for about 2 minutes.
5.2.13	Check the pressure on the pressure gauge.
5.2.14	Release the pressure gently by opening the same valve in the anticlockwise direction.
5.2.15	Rotate the wheel on top of the KBr press in anti clockwise direction until the dye assembly can be easily removed.
5.2.16	Remove the sample pellet by separating the barrel from the base.
5.2.17	Gently tap the plunger on the inverted side so that the small round disc and sample pellet can be removed from the top.
5.2.18	Check that the sample pellet prepared is transparent and uniform.
5.2.19	For preparation of blank KBr pellet follow the same procedure without the sample from point no. 5.2.3 to 5.2.18.
5.2.20	The KBr or sample pellet is now ready to be scanned.
5.3	Cleaning Procedure:
5.3.1	Clean the granite mortar and pestle with lint free cloth or tissue paper before and after use.
5.3.2	Clean the barrel and base of the dye assembly with lint free cloth or tissue paper before and after use.
5.3.3	Clean the small round disc and plunger first with tissue paper and then apply grease on all sides of the disc and plunger.
5.3.4	Wrap the disc and plunger in aluminium foil and keep in desiccator.
5.3.5	Remove the grease of disc and plunger before use with dry tissue paper and then with carbon tetrachloride solvent.
5.3.6	Clean the KBr press equipment with lint free cloth before and after use.
5.4	Calibration Procedure:
	Frequency: Once in a Year
5.4.1	Calibration is carried out by external agency as per SOP “Calibration of Instruments and Equipments”.
5.4.2	Refer Annexure for calibration test to be performed and acceptance criteria. Sr. No. Tests Set value in Tons Acceptance Criteria 1. Pressure Verification 0 ± 2 % 2 ± 2 % 4 ± 2 % 6 ± 2 % 10 ± 2 % 14 ± 2 %
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/equipments 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	Update “Annual Calibration Schedule” and “Monthly Calibration Schedule” as per SOP “Calibration of Instruments and Equipments”.
5.5	Preventive Maintenance:
5.5.1	Perform the preventive maintenance as per Annexure.
5.5.2	If preventive maintenance activity is outsourced, the observations are to be transcribed in the Annexure and external party certificate to be attached.
5.5.3	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.
• Abbreviations:

 

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
PM	Preventive Maintenance
KBr	Potassium Bromide
mg	milligram
No.	Number
A.R.No.	Analytical Reference Number

 

 

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