1.0 PURPOSE:
1.1 To lay down the procedure for operation and calibration malvern mastersizer – 2000.
2.0 SCOPE:
2.1 This SOP is applicable in quality control department.
3.0 RESPONSIBILITY:
3.1 Junior Assistant/Senior Assistant – QC
3.2 Senior Executive – QC
4.0 ACCOUNTABILITY:
4.1 Asst. Manager – QC
4.2 Manager – QC
5.0 OPERATING PROCEDURE:
5.1 Starting the instrument:
5.1.1 Switch on the accessories.
5.1.2 Switch on the instrument, which is placed on the end of the panel.
5.1.3 Switch on the computer and start the software by double click on the Mastersizer Malvern 2000 Icon on the desktop.
5.1.4 Enter the user name and click O.K.
5.2 Creating a new sop for hydro 2000 SM (A):
5.2.1 Go to configure menu and click on the new SOP.
5.2.2 A new SOP creation wizard will appear on the screen and click on the next button.
5.2.3 A sampler selection window will appear on the screen.
5.2.4 Select the sampler-handling unit as Hydro 2000 SM (A) and click on the next button.
5.2.5 Material window appears on the screen. Enter the required material name and select the dispersant name as per the STP.
5.2.6 Click on the models and select the required model and calculation sensitivity and click O.K. Then click on the next button.
5.2.7 Labels window will appear. Enter the sample identification fields. Click on the next button.
5.2.8 The report saving window will appear. Select the required options and click on the next button.
5.2.9 The measurement window appears on the screen. Enter the measurement parameters as per STP and click on the next button.
5.2.10 A sampler settings window will appear. Adjust the stirring speed and other required parameters as per STP. Click on the next button.
5.2.11 Measurement cycles window will appear on the screen. Enter the number of measurement and delay time as required and click on the next button.
5.2.12 Quantities window will appear. Select the required options and click on the next button.
5.2.13 Finished SOP creation window will appear. Click on the finish button.
5.2.14 Save as window will appear. Enter the file name and then click on save button.
5.3 Analyzing a sample using existing methods in hydro 2000 SM (A):
5.3.1 Ensure that the Hydro 2000 SM (A) connected to the main Unit.
5.3.2 Add the specified quantity of dispersant to the tank as per the STP and start the stirring.
5.3.3 Go to Measure menu and click on Start SOP.
5.3.4 Select a required existing SOP and open it.
5.3.5 A SOP-SOP Window will appear on the screen.
5.3.6 Press the start Button.
5.3.7 It will automatically measure the electrical background, align the system and A Documentation window will appear on the screen.
5.3.8 Enter the sample identification and click on the O.K. Button.
5.3.9 Depending on the SOP set up, the following message will be displayed “add a specific quantity or add sample to the tank”.
5.3.10 Now add the specified amount of the sample until the obscuration bar complies with the STP and press the Start Button.
5.3.11 The sample will be measured and the result will be calculated. The measurement data will be automatically saved on the measurement file.
5.3.12 Now a message will displayed as “do you want to run this SOP again”.
5.3.13 If want to continue press O.K. button otherwise click on No. It will come out of the Measurement mode.
5.3.14 Select the record and view the results by selecting one of the report fields.
5.3.15 Go to the File menu click on the print and take the print out.
5.4 Dry method:
5.4.1 Procedure for creating a New SOP in Scirocco – 2000 (A):
5.4.1.1 Go to the Configure menu and select New SOP.
5.4.1.2 New SOP creation wizard appears on the screen.
5.4.1.3 Click on the Next button, a Sampler selection window will appear.
5.4.1.4 Select the Sampler handling Unit as Scirocco-2000 (A) and click on the Next Button.
5.4.1.5 A Material window appears on the screen.
5.4.1.6 Enter the Material name and then click on the Models, a “select result calculation Model” window will appear.
5.4.1.7 Select the required model and calculation sensitivity then click ok.
5.4.1.8 Click on the Next button, a Labels window will appear on the screen.
5.4.1.9 Enter all the required sample identifications and click on the Next button, a Report/Saving window will appear on the screen.
5.4.1.10 Select the required fields and click on the Next button, a Measurement window will appear on the screen.
5.4.1.11 Set the measurement time and snaps as specified in the method of analysis.
5.4.1.12 Click on the Next Button, a sampler settings window will appear.
5.4.1.13 Set the Vibration feed rate and Depressive air pressure and then click on the Next button.
5.4.1.14 A Measurement Cycles window will appear on the screen.
5.4.1.15 Enter the No. of cycles as per the method and Click on the Next button.
5.4.1.16 Finished SOP creation window will appear on the screen and click on the button Finish.
5.4.1.17 A save as window will appear on the screen.
5.4.1.18 Enter the file name and click on save.
5.4.2 Procedure for measuring a sample using existing methods in scirocco-2000 (A):
5.4.2.1 Ensure that the Scirocco 2000 dry cell unit is connected to the main unit. Otherwise replace the wet cell unit with the dry cell.
5.4.2.2 Switch on the Instrument, which is placed on the end panel of the instrument.
5.4.2.3 Connect the tube between dry cell and the sample feeder.
5.4.2.4 Connect the vacuum line on the rear side of the dry cell.
5.4.2.5 Connect the vacuum monitor tube to the rear side of the dry cell.
5.4.2.6 Switch on the dry powder sample feeder on the rear side of the feeder.
5.4.2.7 Switch on the Air Compressor.
5.4.2.8 Switch on the Vacuum pump.
5.4.2.9 Place the sample on the sample feeder and close the lid.
5.4.2.10 Switch on the computer and double click on the Mastersizer 2000 icon.
5.4.2.11 Enter the User Name and click Ok.
5.4.2.12 Go to the Measure menu and start SOP.
5.4.2.13 A Open dialogue box will appear on the screen and open the required existing SOP.
5.4.2.14 A Documentation window appears on the screen.
5.4.2.15 Enter the sample identifications and click Ok, a SOP window will appear on the screen.
5.4.2.16 The system will automatically checks the Vacuum pressure, Air pressure and measures the electrical background, align the system and then measures the optical background.
5.4.2.17 The measurement data will automatically saved to a measurement file.
5.4.2.18 Select the record and view the results by selecting one of the report fields.
5.4.2.19 For print out, go to the File menu and click on the print.
5.4.2.20 After completing the analysis exit from the software then switch off the Accessories and the Instrument.
6.0 CALIBRATION PROCEDURE:
6.1 To calibrate the Malvern 2000 using Scirocco – 2000 accessory:
6.1.1 Connect the Scirocco-2000 dry unit to the main unit.
6.1.2 Switch on the System, Scirocco dry cell and the data handling system.
6.1.3 Create a SOP with the following settings:
6.1.3.1 Material tab:
Display shows |
Enter the Details |
Glass beads |
Typical |
Refractive index |
1.52 |
Absorption |
0.00 |
Model |
General purpose, Fine powder |
Calculation sensitivity |
Enhanced |
6.1.3.3 Measurement tab:
Display shows |
Enter the Details |
Back ground/measurement time |
15 seconds |
Measurement Time |
15 seconds |
Obscuration limits |
0.5 & 6 |
6.1.3.4Sample settings tab:
Display shows |
Enter the Details |
Sample tray |
General purpose |
Air pressure |
3.5 bar |
Typical feed rate |
40% |
6.1.3.5 Cycle tab:
6.1.3.5.1 Select single aliquot and 1 measurement cycle.
6.1.4 Ensure that the cell windows and lenses are clean and free from scratches.
6.1.5 Start the instrument as per the SOP.
6.1.6 Place the QAS 2003 glass micro spheres in the sample tray.
6.1.7 Measure the sample.
6.1.8 Note down the test results of Dv10, Dv50 and Dv90.
6.1.9 The limits should be
3% on the median value for the Dv50 and
6% on the median value for the Dv10 & Dv90.
|
Dv10 |
Dv50 |
Dv90 |
Lower limit |
27.18 |
46.52 |
74.19 |
Median values |
28.91 |
47.96 |
78.92 |
Upper limit |
30.65 |
49.40 |
83.66 |
6.2 To calibrate the Malvern 2000 using hydro 2000 SM (A) accessory:
6.2.1 Connect the Hydro 2000 SM (A) wet unit to the main unit.
6.2.2 Switch on the Instrument, Hydro2000 SM (A) and the data handling system.
6.2.3 Pour water to the dispersant tank. Add 4 drops of 5% Nonidet P40 surfactant to the tank.
6.2.4 Adjust the rpm to 3000.
6.2.5 Setup a SOP with the following settings:
6.2.5.2 Measurement tab:
Display shows |
Enter the Details |
Back ground/measurement time |
12 seconds |
Measurement Time |
12 second |
6.2.5.3Sample settings tab:
Display shows |
Enter the Details |
Pump / Stirrer speed |
3000 rpm |
6.2.5.4 Cycles tab: Select single aliquot and 3 measurement cycles.
6.2.6 Start the instrument as per the SOP.
6.2.7 Add the QAS 2001 glass micro spheres to the tank.
6.2.8 Measure the sample.
6.2.9 Take the print out and Note down the test results of Dv10, Dv50 and Dv90.
6.2.10 The limits should be
2% on the median value for the Dv50 and
3% on the median value for the Dv10 & Dv90.
Dv10 Dv50 Dv90
Lower limit 27.58 45.86 74.89
Median values 28.43 46.80 77.00
Upper limit 29.28 47.74 79.31
6.3 If it does not comply with the specification requirement put the status label as UNDER MAINTENANCE and call the Service engineer. After the rectification recalibrate the instrument.
6.4 Record the details as per Format No. xxxxx
6.5 Calibration frequency:
6.5.1 Once in six months.
Mastersizer, malvern, calibration, stirring, electrical background