Malvern Instruments Mastersizer X, Manual

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©Malvern Instruments Ltd. 1995, 1997

Malvern Instruments makes every effort to ensure that this document is correct. However, due to
Malvern Instruments policy of continual product development we are unable to guarantee the accuracy
of this, or any other document after the date of publication. We therefore disclaim all liability for any
changes, errors or omissions after the date of publication.

No reproduction or transmission of any part of this publication is allowed without the express written
permission of Malvern Instruments Ltd.

Head Office:
Malvern Instruments Ltd.
Spring Lane South,
Malvern.
Worcestershire.
WR14 1XZ U.K.

Tel + [44] (0) 1684-892456

Fax + [44] (0) 1684-892789

Printed in England

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Summary of Contents for Mastersizer X

Page 1: ...QS Small Volume Sample Dispersion Unit QS Small Volume Sample Dispersion Unit M A N 0 1 6 1 I s s u e 1 1 A p r i l 1 9 9 7...

Page 2: ...ny other document after the date of publication We therefore disclaim all liability for any changes errors or omissions after the date of publication No reproduction or transmission of any part of thi...

Page 3: ...tion 1 3 Other reading 1 5 Chpater 2 Health safety Introduction 2 1 Site requirements 2 1 Laser safety 2 2 General laser safety 2 2 Laser Warnings 2 2 Electrical safety warnings 2 3 Sample handling 2...

Page 4: ...ller Unit rear panel 4 3 The Malvern software 4 4 Qspec MS1 macro 4 4 Chapter 5 How the Accessory works Introduction 5 1 What does the Accessory do 5 1 How does the Accessory do it 5 1 Operating princ...

Page 5: ...ntroduction 9 1 Replacing the sample tubing 9 1 Replacing the fuse 9 2 Cleaning the Accessory 9 2 Disassembly 9 3 Cleaning 9 4 O ring seals 9 4 Reassembly 9 4 Cleaning the cell windows 9 5 Appendix A...

Page 6: ...is and correction C 1 Appendix D Installing the Qspec MS1 macro Introduction D 1 Appendix E Statement of EMC performance Statement of EMC performance E 1 C O N T E N T S Q S S m a l l V o l u m e S a...

Page 7: ...C H A P T E R 1 Introduction to this manual Introduction to this manual...

Page 8: ......

Page 9: ...utines identified in chapter 9 including changing the fuses Operator An operator is a person trained in the use of the system The operator can perform all user maintenance routines identified in chapt...

Page 10: ...rred to as the Small Volume Sample Dispersion Unit or as the Accessory Throughout this manual the Small Volume Sample Dispersion Unit refers to the Dispersion Unit the Controller Unit Within this manu...

Page 11: ...e the safe installation operation and maintenance of the Accessory You should read this chapter in conjunction with the Health and Safety manual for your Mastersizer system You are provided with infor...

Page 12: ...This chapter will give details on how you can create and maintain your own Standard Operating Procedures Chapter 8 Sample preparation This chapter in conjunction with chapter 9 of the Getting Started...

Page 13: ...and Microplus MAN 0106 The Malvern Software reference manual MAN 0102 The Malvern BASIC reference manual MAN 0103 Health and Safety Mastersizer S and X MAN 0104 Health and Safety Mastersizer Micro an...

Page 14: ...C H A P T E R 1 Q S S m a l l V o l u m e S a m p l e D i s p e r s i o n U n i t P a g e 1 6 M A N 0 1 6 1...

Page 15: ...C H A P T E R 2 Health and safety Health and safety...

Page 16: ......

Page 17: ...on site requirements can be found in section A of the Mastersizer Installation Guide for your system For information on the space required by your Accessory refer to chapter 3 of this manual Warning...

Page 18: ...uitable for the power output and wavelength of the laser in use and avoid even when wearing such goggles direct viewing along the paths of the laser beam Only authorised personnel should be allowed to...

Page 19: ...s suspected that liquid or powder has entered the Controller Unit call your Malvern representative to arrange for a service call Opening the covers of the Controller Unit will render its calibration v...

Page 20: ...including Dispersion Unit to remove any contaminants before making another measurement Always label samples for analysis using industry standard labeling particularly if they are handled by a number...

Page 21: ...the Dispersion Unit is to be moved large distances then it is recom mended that it is repackaged in its original packaging To repackage the Dis persion Unit Repackaging the Accessory Repackaging the A...

Page 22: ...am insert in the carton Close and seal the carton with packing tape Disposing of the Accessory When the need eventually arises to dispose of the Accessory it should be done in a responsible manner The...

Page 23: ...C H A P T E R 3 Installation Installation...

Page 24: ......

Page 25: ...nstallation Guide The space your Accessory requires in relation to the Mastersizer S or X is illustrated below The Controller Unit is designed to be placed on top of the Receiver cover of the Optical...

Page 26: ...exterior of the carton and ensure it is placed upright Cut through the plastic bonding straps Carefully cut the plastic packing tape along the fold lines Open the wings of the carton remove the braid...

Page 27: ...the carton This may include a flow cell and window tool If you have ordered a flow cell and window tool carefully remove the bub ble wrap Retain all packaging in case the Dispersion Unit requires tran...

Page 28: ...Accessory Mastersizer S and X N o t e It is assumed your Dispersion Unit is located as described in the Site Requirements section above and the flow cell is fitted in your Mastersizer If the flow cel...

Page 29: ...r conical flask at least 150 ml capacity below the drain outlet Again ensure the tubing is ar ranged such that the Dispersion Unit can drain under gravity Attach the 37 way D type connector digital I...

Page 30: ...the cell drawer Ensure that the cell has fully drained Remove the cell top by lifting and rotating the locking lever as illus trated below Fit the small volume cell top and lock in position with the l...

Page 31: ...itable length of sample tub ing and connect the sample out bottom connection of the Dispersion Unit to the inlet front connection on the Mastersizer via the associ ated hole in the front of the drawer...

Page 32: ...ntroller Unit is in the off 0 position and that the front panel speed control is fully anti clock wise refer to the illustration below Check that the motor connector to the rear of the Controller Unit...

Page 33: ...he upper tubes back to the Dispersion Unit The rpm reading should change Dispersion Unit Controller I N S T R U M E N T S Dispersion Unit Controller I N S T R U M E N T S RPM StirrerSpeed Malve rn Ins...

Page 34: ...on the cell windows Use the Dispersion Unit to circulate a solution of approximately 2 Decon 90 through the system and switch off When starting up again flush the system at least twice to remove all t...

Page 35: ...C H A P T E R 4 Getting to know your Dispersion Unit Getting to know your Dispersion Unit...

Page 36: ......

Page 37: ...eas of the Malvern software which are pertinent to the Accessory Features of the Accessory The illustration below identifies the main features of the Accessory Dispersion Unit Controller I N S T R U M...

Page 38: ...rain control The drain control is a lever that opens and closes the drain The drain is closed when the lever is fully clockwise when viewed from the right hand side and the drain is opened by moving t...

Page 39: ...ains on off switch controls the mains power supply to the Accessory Dispersion Unit connector The Dispersion Unit connector carries the power supply and control signals to the Dispersion Unit from the...

Page 40: ...ed software packages there is usually more than one way to perform a task Making a measurement using the Accessory is no exception It is possible to use the standard measurement interface described in...

Page 41: ...n when the button is pressed This macro allows you to make a measurement using an existing SOP or to create a new SOP The second macro can be run by selecting Edit Qspec MS1 macro from the Control men...

Page 42: ...C H A P T E R 4 Q S S m a l l V o l u m e S a m p l e D i s p e r s i o n U n i t P a g e 4 6 M A N 0 1 6 1...

Page 43: ...C H A P T E R 5 How the Accessory works How the Accessory works...

Page 44: ......

Page 45: ...available limits the amount of dispersant that can be used to dilute it or where a small volume of dispersant is desirable the sample or dispersant may be toxic or expensive for example The Accessory...

Page 46: ...culating through the cell Note that the sample is always pumped to the cell in an upwardly direction This is to allow any trapped air to percolate up through the system On completion of a measurement...

Page 47: ...he sample The perpose of these stages are fully described in chapters 3 and 4 of the Getting Started manual All these stages are automatically controlled by the Qspec MS1 macro The next chapter will r...

Page 48: ...C H A P T E R 5 Q S S m a l l V o l u m e S a m p l e D i s p e r s i o n U n i t P a g e 5 4 M A N 0 1 6 1...

Page 49: ...C H A P T E R 6 Making a measurement using the Accessory Making a measurement using the Accessory...

Page 50: ......

Page 51: ...aminants To flush the Accessory If the tank in the Dispersion Unit is full use the drain control to empty the tank sample tubes and cell Close the drain control and fill the tank with clean dispersant...

Page 52: ...now perform the measurement It will ask you to perform specific tasks throughout the measurement for example it may ask you to add a certain amount of water sample or surfactants to the tank or it ma...

Page 53: ...C H A P T E R 7 Creating changing SOP s Creating changing SOP s...

Page 54: ......

Page 55: ...name that will be obvious to other system users Accessory name The accessory name is provided automatically by the program as MS1 This is used by the macro to ensure that the accessory defined in the...

Page 56: ...or the measurement The optimal operating range is 2000 to 3500 rpm Background Sweeps Each time the Qspec MS1 macro is run an alignment and background measurement is performed in accordance with the re...

Page 57: ...which must be added to the sample unit prior to aligning the instrument and measuring the background Bearing in mind that the maximum capacity of the Dispersion Unit is 130ml this figure will be 130 m...

Page 58: ...he sample is placed in the dispersion unit The user is expected to define a value in seconds less than 999 seconds Pause Time The pause time defines the delay between the inspect and the measurement s...

Page 59: ...cro Editing and deleting a SOP What happens if you make a mistake when defining your SOP Malvern provides a separate macro that allows you to edit or delete an existing SOP To run this macro select Co...

Page 60: ...C H A P T E R 7 Q S S m a l l V o l u m e S a m p l e D i s p e r s i o n U n i t P a g e 7 6 M A N 0 1 6 1...

Page 61: ...C H A P T E R 8 Sample preparation Sample preparation...

Page 62: ......

Page 63: ...h off the Dispersion Unit for a period to allow trapped air to rise out of the system During installation you should ensure there are no twists or loops in the connected sample tubing When you are adj...

Page 64: ...sample in the suspension medium When mixing the sample in the suspension medium a visual inspection will often indicate whether ultrasonics are necessary If there are large agglomerates of particles...

Page 65: ...C H A P T E R 9 Maintenance Maintenance...

Page 66: ......

Page 67: ...ubing originally supplied by Malvern is Tygon R 3603 available from Cole Palmer Instrument Company Tygon is chemically compatible with a wide range of materials Contact the manufacturers for specific...

Page 68: ...cleaning The illustration below shows the Dispersion Unit in its disassembled state The main body of the Dispersion Unit must only be dismantled after draining any dispersant in the system and disconn...

Page 69: ...3mm A F hex key Do not disturb the fourth largest screw The drain section can now be separated from the tank and motor section The pump impeller is now visible on the underside of the tank section Re...

Page 70: ...rings can be obtained from Malvern Instruments Reassembly Reassembly is the reverse order to disassembly Ensure that the impeller above is secure on the motor shaft and that the three bolts above in t...

Page 71: ...the window tool The cell windows are sealed by O rings To remove a cell window from the Mastersizer S or X Make sure that the cell has been drained of dispersant and remove the cell assembly from the...

Page 72: ...he O ring did not come out with the ring then carefully remove it with a pair of tweezers The window assembly is shown in the diagram below Inspect both sides of the cell window If there are any signs...

Page 73: ...he windows by first placing the window into the retaining ring place a piece of tissue over the window to prevent finger marks getting onto the surface then pushing the O ring into position The window...

Page 74: ...C H A P T E R 9 Q S S m a l l V o l u m e S a m p l e D i s p e r s i o n U n i t P a g e 9 8 M A N 0 1 6 1...

Page 75: ...A P P E N D I X A Specification Specification...

Page 76: ......

Page 77: ...nsions Controller Unit Height 80mm Width 225mm Depth 180mm Weight 1 5kg Physical dimensions Dispersion Unit Height 390mm Width 140mm Depth 175mm Weight 6 75kg Power requirements Voltage 240V 50Hz 250m...

Page 78: ...A P P E N D I X A Q S S m a l l V o l u m e S a m p l e D i s p e r s i o n U n i t P a g e A 2 M A N 0 1 6 1...

Page 79: ...A P P E N D I X B Chemical compatibility Chemical compatibility...

Page 80: ......

Page 81: ...Unit body Stainless steel Cell windows Glass Window and cell seals Viton Kalrez available as an option Sample tubing Tygon Drain seal PTFE and Kalrez optional Highly flammable and volatile solvents su...

Page 82: ...A P P E N D I X B Q S S m a l l V o l u m e S a m p l e D i s p e r s i o n U n i t P a g e B 2 M A N 0 1 6 1...

Page 83: ...A P P E N D I X C Simple fault finding Simple fault finding...

Page 84: ......

Page 85: ...s insufficiently advanced Check fuse Motor plug is disconnected Controller box is switched on before motor is connected No increase in obscuration as sample is added Check for leaks Speed control is i...

Page 86: ...A P P E N D I X C Q S S m a l l V o l u m e S a m p l e D i s p e r s i o n U n i t P a g e C 2 M A N 0 1 6 1...

Page 87: ...A P P E N D I X D Installing the Qspec MS1 macro Installing the Qspec MS1 macro...

Page 88: ......

Page 89: ...PECMS1 BSC SET_LENS BSC MS1 BMP SOP INF SAM_DETS INF The default location for the Mastersizer Programs directory is C SIZER PROGRAMS From the Mastersizer program assign the macro program Open the Cont...

Page 90: ...button location for example the spare button next to the Print Report Graph Table button Select the MS1 bitmap from the Available Buttons list From the Menu Label list select Control QSPEC MS1 Macro y...

Page 91: ...e Change Button button to update the button list Your screen should look similar to this Press the OK button The QSPEC MS1 Macro program is now set up and ready for use ILL 3665 A P P E N D I X D Q S...

Page 92: ...A P P E N D I X D Q S S m a l l V o l u m e S a m p l e D i s p e r s i o n U n i t P a g e D 4 M A N 0 1 6 1...

Page 93: ...A P P E N D I X E EMC performance EMC performance...

Page 94: ......

Page 95: ...e Dispersion Unit DIF 2021 Test conditions The Small Volume Sample Dispersion Unit is an accessory for the Mastersizer X S Micro and Microplus It stirs and pumps small volumes of a sample through the...

Page 96: ...erformance Complies with DDENV50140 1994 Radiated electromagnetic field to 10V m with performance criteria A ie no loss of function or performance Complies with DDENV50204 1995 Radiated electromagneti...

Page 97: ...Index Index...

Page 98: ......

Page 99: ...tion unit 4 2 Drain control 4 2 Pump speed display 4 2 Qspec logo 4 3 Sample out 4 2 Sample return 4 2 Speed control 4 2 Flushing the Accessory 6 1 Fuse 4 4 Replacing the fuse 9 2 I Installation 3 1 C...

Page 100: ...2 Sample s units 7 3 Site requirements 2 1 3 1 Software 4 4 Qspec MS1 macro 4 4 Solvent name 7 3 SOP see Standard Operating Procedure Specifications A 1 Replacing the fuse A 1 Speed control 4 2 Stand...

Page 101: ...8 1 Troubleshooting C 1 Fault diagnosis and correction C 1 U Ultrasonics 8 2 Ultrasound duration 7 4 Unpacking the Accessory 3 2 W Windows terms 1 2 I N D E X Q S S M A L L V O L U M E S A M P L E D...

Page 102: ...I N D E X Q S S m a l l V o l u m e S a m p l e D i s p e r s i o n U n i t P a g e 4 M A N 0 1 6 1...

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