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SOP for Operation of Malvern Particle Size Analyzer

The technique of laser diffraction is based on the principle that particles passing through a laser beam will scatter light at an angle that is directly related to their size: 
  • Large particles scatter at low angles
  • Small particles scatter at high angles. 
The laser diffraction is accurately described by the Fraunhofer Approximation and the Mie theory, with the assumption of spherical particle morphology.
PURPOSE
The purpose of this SOP is to describe the Operation and Maintenance of the Malvern Particle Size Analyzer (Model: APA 2000 /AWA 2001-SR /ADA 2000).

SCOPE
This SOP is applicable to the Malvern Particle Size Analyzer (Model: APA 2000 /AWA 2001-SR /ADA 2000).

RESPONSIBILITY
Analyst: Operation of the Malvern Particle Size Analyzer as per the SOP
Quality Control Head or Designee: 
  • Providing training to all the concerned persons before the implementation of SOP.
  • Ensuring the operation and performance check of the Malvern Particle Size Analyzer as per SOP.
  • Ensuring proper documentation as per SOP

PROCEDURE
Operational Procedure for Dry Analysis:
  • Ensure that system is connected with the main power supply.
  • The system contains three modules.
  1. MASTERSIZER2000 (Detector),
  2. SCIROCCO2000 (Dispersion Unit),
  3. SCIROCCO2000 (Sample Cell Compartment)
  • Switch “ON” the power supply of MASTERSIZER2000 provided on the righthand side of the panel.
  • Switch “ON” the power supply of SCIROCCO2000 provided on the backside of the panel.
  • Ensure the tubing connection of the vacuum cleaner and air compressor to the system.
  • Switch “ON” the vacuum cleaner and the air compressor. (vacuum cleaner and air compressor can Active only through the software named “Mastersizer2000”).
  • Click on the “Mastersizer2000” icon on the PC.
  • Login to the software with the user name.
  • Go to the File menu and create the new measurement file if the sample is analyzing for the first time or open the existing measurement file.
  • Click on the “Measure” option and then select the “Manual” option in that.
  • Now “Measurement Display” window will appear.
  • The laser intensity will display in a red bar and a graph of Laser Energy versus Number of detectors will be displayed.
  • Then click on the “Options” tab, the “Measurement Option” window will appear.
  • Select the first tab “Material” then click on “Sample Material Name” (according to Sample Method) in the optical property section.
  • If the sample material name is not in the given list then click the “Materials” option in the same window.

The “Sample material list” window will appear.
  • In that window click the “Add” option then enter the Name, Refractive Index value, Absorption Index value, and Density of the sample as per given in the method and click OK.
  • Then the model – general purpose should be selected in the result calculation section.
  • Click on the “Documentation” option in that “Measurement Display” window and select “Labels”.
  • Enter the sample Details (Sample Name, Batch No, Notes). Then click OK.
  • Now select the second tab “Measurement”.
  • Enter the values for “Sample Measurement Time” and “Background Measurement Time”(according to the sampling method) in the “Measurement Times” section.

And click on “Measurement” in the “Advanced” options section.
  • Enter the value for “Obscuration limits” and “Obscuration filtering”. (Select obscuration range filter, So The Particle Size Analyzer (Malvern) will only measure the particle size of the sample when the obscuration comes within the desired range.)(according to Sample Method). Then click OK.
  • Ensure the Air compressor and Vacuum are not active during filling the tray with the sample in Sample Dispersion Unit (SCIROCCO2000).
  • If you want to perform more than one analysis of the same sample, From the “Measurement Option” window, select the third tab “Measurement Cycles” and enter the values for “Repeat Measurement” and tick mark on the average result. Then click OK.
  • Click “Start” on the “Measurement Display” window.
  • The system will start and will perform the self-alignment.
  • During that period system will show the status of the yellow-colored highlighted portion.
  • Click on the “Accessory” option from the “Measurement display” window, the “Dry Accessory” window will appear.
  • In that same window, set the “Air pressure” and “Feed rate” in the “Controls” section as per method and start the airflow.
  • The air pressure and vacuum will start simultaneously.
  • If Air pressure or Vacuum is not achieved, then Error will be indicated in the Error section of the “Dry Accessory” window with red color.
  • In the “Measurement Display” window, the sample obscuration range will be displayed in the red and green bar to ensure that sample is in the obscuration range.
  • Start the analysis by simultaneously clicking on the “Feed” option in the “Dry Accessory” window and clicking on the “start” tab of the “Measure Sample” option in the “Measurement Display window.
  • The system will start the analysis.
  • After completion of the Analysis, the result will be saved on the main window “Mastersizer2000”.

Procedure for Result Printout
  • After completion of the Analysis, click on the “Result Analysis” option on the main (Mastersizer2000) window.
  • The result table and graph will appear. Take the printout of that.
  • For the analysis parameter, click on the “Parameter Report” in the main window. Then take the printout.

Precaution during Handling of Malvern Particle Size Analyzer:
  • Ensure the cell compartment should be of “Dry” type (SCIROCCO2000).
  • Before putting the cell compartment into Mastersizer2000, visually observe the lenses of the cell, wipe out the dust with fiber tissue paper provided with Kit, and observe the lenses for scratches.
  • If any scratch is found, replace the lenses. Dust and scratches on lenses can cause false measurements.
  • Ensure the tubing connection between the outlet of SCIROCCO2000 (Dispersion module) and the inlet of the Cell compartment.
  • The vacuum tubing connection at the outlet of the cell compartment.
  • Ensure the locking of the cell compartment by moving its handle in an anticlockwise direction (cell compartment can be unlocked by moving its handle in a clockwise direction).
  • Ensure the Air compressor outlet tubing (blue in color) to the inlet of the Dispersion module (SCIROCCO2000).
  • Check the Air Compressor it should be between 4 to 6 kgf.
  • Discharge the Air regulator of Air compressor by pressing the knob located at bottom of the regulator on daily basis to vent condensed water from Air.
  • Ensure the sample should be in a dry state & should be free-flowing.
  • Good pouring characteristic indicates a non-cohesive powder which usually disperses well, whereas highly cohesive material tends to stick and clump together, and gives false Measurement.
  • Sample clumping can often be overcome by drying the sample properly in an Oven.


Operational Procedure For Wet Analysis at Malvern Particle Size Analyzer:
  • Ensure the System is connected with the main power supply.
  • The system contains four modules.
  1. MASTERSIZER2000 (Detector),
  2. Dispersion Unit Pump,
  3. Dispersion Unit Controller,
  4. Hydro2000SM (Sample Cell Compartment)
  • Switch “ON” the power supply of “MASTERSIZER2000” provided on the Right-hand side of the panel.
  • Switch “ON” the power supply of the Dispersion Unit Controller.
  • Ensure the cell compartment is of Wet type (Hydro2000SM).
  • Ensure the tubing connection of the Sample Dispersion unit (Connect outlet of sample dispersion unit to the inlet of the cell compartment.
  • Connect the yellow tube with a red ring.
  • Connect the outlet of the cell compartment to the inlet of the sample dispersion unit.
  • Then Connect the yellow tube with a blue ring.)
  • Ensure the drain valve of the Sample dispersion Unit is closed (lever in vertical direction).
  • Then Fill the sample dispersion Unit with a suitable solvent for washing then open the drain valve (lever in the horizontal direction).
  • Again fill the sample dispersion unit with a suitable solvent after closing the drain valve.
  • Then set 2000 rpm (or as per requirement) by stirrer speed knob on the Dispersion unit controller.
  • Stir for 10 mins for washing (or as per requirement).
  • Then open the drain valve to drain out the solvent from the sample dispersion unit.
  • Now close the drain valve.
  • Before the analysis of the sample, the drain valve of the sample dispersion module should be closed and the rpm of the Dispersion unit controller should be zero.
  • Fill the Sample dispersion module with Sample (sample which is to be measured.
  • It should be in the suspended condition in suitable dispersion media)
  • Now increase the rpm gradually (sudden change in rpm generates bubbles in the sample) to the predefined value(specified in Method) of the sample dispersion pump from the Dispersion Unit Controller.
  • Ensure that, no leakage should be there in the system.
  • Now start the Analysis by clicking on the “MASTERSIZER2000” icon on PC.
  • Login to the Software with the user name.
  • Go to file menu and create the new measurement file if the sample is analyzing for the first time or open the existing measurement file.
  • Click on “Measure” option and then select “Manual” option in that.
  • Now “Measurement Display” window will appear.
  • The laser intensity will display in red bar and Graph of Laser Energy versus Number of Detector will be displayed.
  • Then Click on “Options” tab, the “Measurement Option” window will appear.
  • Select the first tab “Material” then click on “Sample Material Name” (according to Sample Method) in optical property section.
  • If the sample material name is not in the given list then click “Materials” option in same window.
  • “Sample material list” window will appear .
  • In that window click “Add” option then enter the Name, Refractive Index value, Absorption Index value, and Density of the sample as per given in the method and click OK.
  • Then model – general purpose should be selected in result calculation section.
  • Click on “Documentation” option in that “Measurement Display” window and select “Labels”.
  • Enter the “Sample Details” (Sample Name, Batch No, Notes). Then click OK.
  • Now select second tab “Measurement”.
  • Enter the values for “Sample Measurement Time” and “Background Measurement Time” (according to Sample Method) in “Measurement Times” section. And click on “Measurement” in “Advanced options” section.
  • Enter the value for “Obscuration limits” and “Obscuration filtering”.
  • Select obscuration range filter, so instrument will only measure the particle size of sample when the obscuration come within the desired range (according to Sample Method ) then click OK.
  • If you want to perform more then one analysis of same sample. In the “Measurement Option” window, select third tab “Measurement Cycles” and enter the values for :Repeat Measurement” and tick mark on average result then click OK.
  • Click “Start” on the “Measurement Display” window. System will start and will perform the self alignment. During that period system will show the status on yellow colored highlighted portion.
  • In the “Measurement Display” window the sample obscuration range will be displayed in red and green bar to ensure that sample is in obscuration range.
  • Start the Analysis by clicking “Measure Sample” option in “Measurement Display” window. System will start the Analysis.
  • After completion of the analysis, the result will be saved on main window “Mastersizer2000”.

Procedure for Result Printout
  • After completion of the analysis, click on “Result Analysis” option on main (Mastersizer2000) window. The result table and graph will appear. Take the printout of that.
  • For the Analysis Parameter, click on “Parameter Report” on main window.
  • Then Take the printout.

Precaution during handling of Wet Analysis on Malvern Particle Size Analyzer:
  • Ensure the Cell Compartment should be of “Wet” type (Hydro2000SM) Before putting the Cell compartment into Mastersizer2000, visually observe the lenses of cell, wipe out the dust by fiber tissue paper provided with Kit and observe the lenses for scratches.
  • If any scratch is found, replace the lenses.
  • Dust and scratches on lenses can cause false measurement.
  • Ensure the tubing connection of Sample Dispersion unit (connect outlet of sample dispersion unit to inlet of Cell compartment.
  • Connect yellow tube with red ring.
  • Connect the outlet of cell compartment to inlet of sample dispersion unit.
  • Yellow tube with blue ring.
  • Ensure the locking of Cell Compartment by moving its handle in anticlockwise direction (Cell compartment can be unlocked by moving its handle in clockwise direction)
  • The change in RPM of sample dispersion unit should be done very gradually by the dispersion unit controller. 
  • Sudden change in RPM can form bubbles in sample which will give false measurement.
  • RPM of sample dispersion unit must be kept to zero during draining of dispersion media.
  • Ensure the proper dispersion of sample. The sample should neither dissolve nor float on dispersion Media. It should be in suspended condition.
  • Choose appropriate dispersion media (According to Method) Flush the system with dispersion media (sample suitable) after every Analysis.
  • Follow suitable solvent sequence to flush the system at the end of working day if it has been used for analysis on that day.
  • Flush with solvent sequence means If our dispersion media is liquid paraffin and the dispersion module contains water then don’t put liquid paraffin directly but for changing media from water to liquid paraffin, follow the sequence like,
Water—Methanol—Hexane—Chloroform—Liquid paraffin
  • If media changes from liquid paraffin to water then follow the sequence like,
Liquid paraffin—Chloroform—Hexane—Methanol—Water
  • Flush the solvent system, sample Cell Compartment (HYDRO 2000SM) and Dispersion Unit Pump with appropriate solvent or dispersion media by checking it’s solubility with previously used dispersion media.

ABBREVIATIONS
QC – Quality Control

REVISION HISTORY
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