Malvern Instruments Mastersizer X Manual

Qs small volume sample dispersion unit

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QS Small Volume Sample
QS Small Volume Sample
Dispersion Unit
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

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Summary of Contents for Malvern Instruments Mastersizer X

  • Page 1 QS Small Volume Sample QS Small Volume Sample Dispersion Unit 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 ©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.
  • Page 3: Table Of Contents

    C O N T E N T S Contents Chapter 1 - Introduction to this manual Access to the Accessory Malvern personnel Supervisor Operator Systems covered by this manual Assumed information Windows terms Menu Commands Where to find information Other reading Chpater 2 - Health &...
  • Page 4 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 C O N T E N T S Unpacking the Accessory Checking the contents Connecting up your Accessory Mastersizer S and X...
  • Page 5 C O N T E N T S Chapter 7 - Creating and changing SOP’s Creating a new SOP Editing and deleting a SOP Chapter 8 - Sample preparation Introduction Trapped air/bubbles Using a slurry The use of ultrasonics Chapter 9 - Maintenance Introduction Replacing the sample tubing Replacing the fuse...
  • Page 6 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 C O N T E N T S Appendix C - Simple fault finding Introduction Fault diagnosis and correction Appendix D - Installing the Qspec MS1 macro...
  • Page 7: Chapter 1 - Introduction To This Manual

    Introduction to this manual Introduction to this manual...
  • Page 9: Access To The Accessory

    C H A P T E R 1 Access to the Accessory Within this manual reference is made to the various people that will have access to the Accessory. Below is a list of these people and their responsibility: Malvern personnel Malvern personnel (service engineers, representatives etc.) have full access to the Accessory and are authorised to perform all service procedures that may be required.
  • Page 10: Assumed Information

    C H A P T E R 1 This manual covers the Accessory in association with the following Mastersizer family members: Instrument. Ref. Number. Mastersizer X standard bench. MAM 5000 Mastersizer X long bench. MAM 5002 Mastersizer S standard bench.
  • Page 11: Where To Find Information

    C H A P T E R 1 Where to find information As stated above, this manual is designed to give a brief overview of what the Accessory can do and how it is used in association with the system. In other words it is a quick guide that allows you to understand how the Accessory operates and runs you through how the Accessory is used when making a measurement, hopefully steering you around the main pitfalls and directing you...
  • Page 12 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 C H A P T E R 1 The first part identifies the features of the Accessory, for example the function controls, connectors and indicators etc.
  • Page 13: Other Reading

    C H A P T E R 1 Other reading More detail on the subjects within this manual can be found in the following manuals: Title Ref. Number Getting Started system manual (Mastersizer S and X). MAN 0101 Getting Started system manual (Mastersizer Micro and Microplus). MAN 0106 The Malvern Software reference manual.
  • Page 14 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 C H A P T E R 1 P a g e 1 . 6 M A N 0 1 6 1...
  • Page 15 Health and safety Health and safety...
  • Page 17: Introduction

    C H A P T E R 2 Introduction This chapter covers health and safety guidelines that should ensure the safe installation, operation and maintenance of the Accessory. You should read this chapter in conjunction with the Health and Safety manual for your system. Warning Failure to follow these guidelines, particularly when making a measurement, could result in the emission of laser radiation.
  • Page 18: Laser Safety

    C H A P T E R 2 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 Laser safety It should be noted that the Accessory does not contain a laser, but is connected to the Mastersizer optical unit that does.
  • Page 19: Electrical Safety Warnings

    C H A P T E R 2 Electrical safety warnings The Accessory is mains powered and input power cables should be treated accordingly. The metal parts of the instrument are earthed via the protective earth connection. Never run the equipment without a protective earth connection. Exert care when measuring samples to avoid liquid or powder spillages over the Controller Unit.
  • Page 20 C H A P T E R 2 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 Wear a protective respiratory mask if noxious samples or dispersants are being handled, particularly in their dry state during sample preparation or measurement.
  • Page 21: Moving The Accessory

    C H A P T E R 2 Moving the Accessory If it is necessary to move the Accessory the following guidelines should be followed: . Empty the Dispersion Unit. . Always disconnect the power supply before attempting to move the Con- troller Unit.
  • Page 22: Disposing Of The Accessory

    C H A P T E R 2 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 . Place the tank cover into a plastic bag, then place the cover into the tank of the Dispersion Unit.
  • Page 23: Chapter 3 - Installation

    Installation Installation...
  • Page 25: Introduction

    C H A P T E R 3 Introduction This chapter provides you with the information required to install the Accessory Unit and includes information on: . Positioning the Dispersion Unit & Controller Unit. . Unpacking the Dispersion Unit & Controller Unit. .
  • Page 26: Unpacking The Accessory

    C H A P T E R 3 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 e e e r S S t i r r 300mm...
  • Page 27: Checking The Contents

    C H A P T E R 3 . Lift the Dispersion Unit out of the carton and place on a suitable work- bench. Always lift the Dispersion Unit supporting the base. Place the Dis- persion Unit upright on its feet. .
  • Page 28: Connecting Up Your Accessory

    Ç Controller Unit. È Software (Qspec MS1 macro) installation disk. É Mains power cable. 37 way cable. (digital I/O connector) - Mastersizer X/S only. Connecting up your Accessory Mastersizer S and X It is assumed your Dispersion Unit is located as described in the Site...
  • Page 29 C H A P T E R 3 nt ro lle r nt ro lle r Stirre r Spee Stirre r Spee n Un it Co n Un it Co Di sp er sio Di sp er sio . Similarly, make a connection between the outlet (top connection) of the flow cell Ã...
  • Page 30: Mastersizer Micro And Microplus

    C H A P T E R 3 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 Mastersizer Micro and Microplus It is assumed your Accessory is located as described in the Site N o t e : Requirements section above.
  • Page 31 C H A P T E R 3 . On the under side of the cell drawer, remove the sample tube À connect- ing the cell inlet to the outlet. . Referring to the next two illustrations, cut a suitable length of sample tub- ing and connect the sample out (bottom connection) of the Dispersion Unit À...
  • Page 32: Power Up The Accessory

    C H A P T E R 3 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 . Similarly, connect the sample return à to the outlet Ä on the Mastersizer with sample tubing, via the associated hole in the front of the drawer Å.
  • Page 33: Installation Check

    C H A P T E R 3 . After a short delay, check the pump speed display on the front panel is illu- minated. Stirr er Spee Installation check To check that the Accessory is installed and works correctly: .
  • Page 34 C H A P T E R 3 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 Stir rer Spe .
  • Page 35 Getting to know your Getting to know your Dispersion Unit Dispersion Unit...
  • Page 37: Introduction

    C H A P T E R 4 Introduction This chapter is designed to enable you to identify the physical features of the Accessory and is divided into two parts. The first part identifies the features of the Dispersion Unit & Controller Unit, for example the function controls, connectors and indicators etc.
  • Page 38 C H A P T E R 4 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 À Controller unit The Controller Unit is used to power and control the Dispersion Unit.
  • Page 39: Controller Unit Rear Panel

    C H A P T E R 4 anti-clockwise the pump speed will be zero, with it turned fully clockwise the pump speed will be at its maximum. É Qspec logo If your company operates within the pharmaceutical industry, you will be pleased to know that the Qspec label means that the instrument is eligible for coverage by a Malvern Qspec Validation contract which can help you to meet the requirements of the Food and Drug Administration (FDA).
  • Page 40: The Malvern Software

    U n i t à Digital I/O connector This connector is only used on the Mastersizer X or S. It is connected to the digital I/O connector on the receiver unit of the Mastersizer S or X. It allows the stirrer speed to be automatically read by the Malvern Software.
  • Page 41 C H A P T E R 4 water to the tank”, “add 7mg of sample” or “set the stirrer speed to 2500rpm”, that will ensure the measurement is made consistently. There are two macros that the operator should be aware of. The first (Qspec MS1 macro) is run when the button is pressed.
  • Page 42 C H A P T E R 4 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: Chapter 5 - How The Accessory Works

    How the Accessory works How the Accessory works...
  • Page 45: Introduction

    C H A P T E R 5 Introduction After reading this chapter you will have a basic understanding of the operating procedures of the Accessory and in particular: . Know the basic operating principle. . Know the simple steps involved in using the Accessory when making a measurement.
  • Page 46: How To Make A Measurement Using The Accessory

    C H A P T E R 5 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 Stirr er Spe The Dispersion Unit comprises an electric motor À...
  • Page 47 C H A P T E R 5 . Setup for the measurement. . Align the optics. . Document the measurement. . Measure the background. . Add the sample and check the concentration. . Measure the sample. The perpose of these stages are fully described in chapters 3 and 4 of the Getting Started manual.
  • Page 48 C H A P T E R 5 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 Making a measurement Making a measurement using the Accessory using the Accessory...
  • Page 51: Introduction

    C H A P T E R 6 Introduction This chapter will guide you through the practical steps involved when making a measurement using the Accessory. For convenience it will be assumed you will be using the Qspec MS1 macro (see page 4.4). A Standard Operating Procedure (SOP) is shipped with the macro called “Dairy Milk”...
  • Page 52 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 C H A P T E R 6 given the option of either creating a new SOP or running a measurement that does not conform to a SOP.
  • Page 53 Creating & changing SOP's Creating & changing SOP's...
  • Page 55: Creating A New Sop

    C H A P T E R 7 Creating a new SOP Creating a new SOP is very simple. To create a new SOP start the Qspec MS1 Macro by selecting the button below. The macro will ask if the measurement is to conform to an existing SOP. Select “No”.
  • Page 56 U n i t C H A P T E R 7 The default Malvern Instruments data file extension (.SAM) will be appended to the filename entered by the user. There is a limit of eight characters for the sample filename.
  • Page 57 C H A P T E R 7 Solvent name The Solvent name field defines the name of any solvent used to pre-disperse the sample into a slurry before it is added to the dispersant. The length of the solvent name is limited to twenty five characters. Sample’s units This parameter defines the measurement quantity for the current sample.
  • Page 58 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 C H A P T E R 7 The maximum number of characters in the surfactant name is 25. Surfactant Quantity The surfactant quantity defines the number of drops of surfactant to be added to the sample dispersion.
  • Page 59: Editing And Deleting A Sop

    C H A P T E R 7 Max Obscuration The maximum obscuration defines the upper limit for the obscuration value during the inspect stage. If the maximum value is exceeded, the user has the option of either accepting the obscuration or rejecting it, in which case there is a prompt to clean out the sample tank and start the measurement sequence again.
  • Page 60 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 C H A P T E R 7 P a g e 7 . 6 M A N 0 1 6 1...
  • Page 61: Chapter 8 - Sample Preparation

    Sample preparation Sample preparation...
  • Page 63: Introduction

    C H A P T E R 8 Introduction This chapter, in conjunction with chapter 9 of the Getting Started manual, provides you with information on one of the most important stages in making a measurement. Read very carefully chapter 9 of the Getting Started manual, particularly the advice given on wet measurements.
  • Page 64: Using A Slurry

    C H A P T E R 8 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 Using a slurry The act of mixing up a small quantity of concentrated sample, dispersant and additives before it is added to the Dispersion Unit tank is known as preparing a slurry.
  • Page 65: Chapter 9 - Maintenance

    Maintenance Maintenance...
  • Page 67: Introduction

    C H A P T E R 9 Introduction This chapter provides information on certain maintenance routines that can be carried out by the user. Read the “Access to the Accessory” section in chapter 1, for guidance on what the Supervisor and the Operator are allowed to do.
  • Page 68: Replacing The Fuse

    C H A P T E R 9 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 Replacing the fuse Warning Fuses must not be replaced by the operator.
  • Page 69: Disassembly

    C H A P T E R 9 Disassembly To disassemble the Dispersion Unit, disconnect the Dispersion Unit from the mains supply and unplug the motor connector À from the back of the Control Unit. Remove the sample tubing from the sample out Á and sample return  pipes.
  • Page 70: Cleaning

    ‘O’ rings (Ç and È). The ‘O’ rings can be removed by levering them out using a pair of tweezers. Fitting the ‘O’ rings is the reverse of the above procedure. Replacement ‘O’ rings can be obtained from Malvern Instruments. Reassembly Reassembly is the reverse order to disassembly.
  • Page 71: Cleaning The Cell Windows 9.5

    C H A P T E R 9 Once the electrical connectors and sample tubes have been attached, check the unit for leaks. Remember not to run the motor for more then a few seconds without liquid in the tank. Cleaning the cell windows Cleaning the system by rinsing through with fresh dispersant a couple of times is usually sufficient to prepare for a new measurement.
  • Page 72 C H A P T E R 9 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 To remove a cell window from the Mastersizer Micro or Microplus: .
  • Page 73 C H A P T E R 9 Caution Do not wipe the windows with an ordinary dry cloth as this will cause scratches. Always use the procedure below to clean the surfaces. Inspect the window by reflected light and see if there are any smears or prints on it.
  • Page 74 C H A P T E R 9 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: Appendix A - Specification

    Specification Specification...
  • Page 77: Introduction

    A P P E N D I X A Introduction This specification covers the Small Volume Sample Dispersion Unit only. For specific information that covers the Mastersizer optical unit, refer to appendix A of the Getting Started manual. Physical dimensions - Controller Unit Height: 80mm.
  • Page 78 A P P E N D I X A 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 .
  • Page 79 Chemical compatibility Chemical compatibility...
  • Page 81: Introduction

    A P P E N D I X B Introduction The Accessory has been manufactured from materials that are considered to give the widest protection from chemical attack. However, it is important to check that any sample or dispersant you may use is chemically compatible with the materials that they will come into contact within the Accessory.
  • Page 82 A P P E N D I X B 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 .
  • Page 83 Simple fault finding Simple fault finding...
  • Page 85 This appendix covers the diagnosis of minor faults which may occur from time to time in the Accessory. It is not intended that the user should undertake major repairs and any faults not covered should be referred to Malvern Instruments or their representatives. Further more the user must refrain from carrying out any procedures not described in this manual and any remedial action requiring such procedures should only be carried out by qualified personnel.
  • Page 86 A P P E N D I X C 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 .
  • Page 87 Installing the Qspec Installing the Qspec MS1 macro MS1 macro...
  • Page 89 This section describes the steps that should be followed to install and set up the Qspec MS1 macro into the current configuration of the Mastersizer software. If your computer system was supplied by Malvern Instruments, then this software will already be installed on your system.
  • Page 90 A P P E N D I X D 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 From the Mastersizer program set up the button bar: .
  • Page 91 A P P E N D I X D . In the Status Line Message box add the text “Run QSPEC MS1 Macro”. . Press the Change Button button to update the button list. . Your screen should look similar to this: .
  • Page 92 A P P E N D I X D 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 .
  • Page 93 EMC performance EMC performance...
  • Page 95 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 test cell. It is activated by a control box which displays and adjusts the speed.
  • Page 96 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 A P P E N D I X E EMC performance The equipment under test, when subjected to the following tests was found to be compliant.
  • Page 97 Index Index...
  • Page 99 I N D E X Qspec logo Access to the Accessory Sample out Malvern personnel Sample return Operator Speed control Supervisor Flushing the Accessory Accessory name Fuse Assumed information Replacing the fuse Background Sweeps Installation Bubbles Checking the contents Installation check Unpacking the Accessory Chemical compatibility Cleaning the Accessory...
  • Page 100 I N D E X 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 Disposing of the Accessory Sample’s units Repackaging the Accessory Site requirements...
  • Page 101 I N D E X Tank cover Trapped air/bubbles Troubleshooting Fault diagnosis and correction Ultrasonics Ultrasound duration Unpacking the Accessory Windows terms P a g e 3 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...
  • Page 102 I N D E X 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...

Table of Contents