Malvern Mastersizer 2000 User Manual
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Malvern Mastersizer 2000 User Manual

Malvern Mastersizer 2000 User Manual

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  • Page 1 Mastersizer 2000 user manual...
  • Page 3 Mastersizer 2000 User Manual MAN0384 Issue 1.0 March 2007...
  • Page 4 © Malvern Instruments Ltd. 2007 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 5 Date 10/03/2010 Manual number MAN0384-1.0 Manual name Mastersizer 2000 User Manual This addendum presents new information on the Mastersizer 2000/2000E from Malvern Instruments. Laser specification The following information adds to the Light Sources information given on page A-1: Red light...
  • Page 6 Page 2 Addendum 0070-2.0...

  • Page 7: Table Of Contents

    ....... 2-1 What the Mastersizer 2000 does ....... 2-2 How the Mastersizer 2000 works .
  • Page 8 Table of Contents Mastersizer 2000 Viewing the results ..........5-1 Introduction .
  • Page 9 Mastersizer 2000 Table of Contents Advanced features ..........9-1 Introduction .
  • Page 10 Table of Contents Mastersizer 2000 Part 2 - Supervisor’s Guide Security ..........10-1 Introduction .
  • Page 11 Mastersizer 2000 Table of Contents Part 3 - Appendices Specification ..........A-1...
  • Page 12 Table of Contents Mastersizer 2000 Page vi MAN 0384...

  • Page 13: Part 1 - Operator's Guide

    Part 1 - Operator’s Guide...

  • Page 15: Introduction To This Manual

    Introduction to this manual About this manual This manual describes the operation of the Malvern Mastersizer 2000 and 2000E particle size analysers. Information is also given on basic use of the Hydro 2000G and Hydro 2000MU sample dispersion units: Instrument...

  • Page 16: Access To The Instrument

    Below is a list of these people and their responsibility: Malvern personnel Malvern personnel (service engineers, representatives, etc.) have full access to the instrument and are authorised to perform all service procedures that may require the removal of the covers.

  • Page 17: Assumed Information

    Assumed information General The Mastersizer 2000/2000E can be used with a variety of sample dispersion units that allow it to measure wet and dry samples. The function of these is identical: to prepare and deliver the sample to the optical bench for measurement. For clarity, this manual assumes that the primary dispersion unit for each system is as follows: For the Mastersizer 2000 the Hydro 2000G.

  • Page 18: Where To Get Help

    Installation – this gives enough information to allow the user, for example, to move the system from one laboratory to another. Instructions are also given on how to install the Malvern software if the user upgrades the computer system. Caution! If the system is covered by a Qspec validation contract, we strongly recom- mend that it is only moved by Malvern representatives.
  • Page 19 Model number of the optical bench and dispersion unit(s). Serial number of the optical bench and dispersion unit(s). Version of the Malvern software – this can be found by starting the software and selecting Help-About. The serial number of the optical bench can be found inside the sample area (remove the cell first).
  • Page 20 Introduction to this manual Malvern website - www.malvern.com The Malvern Instruments website offers a comprehensive range of material charac- terisation resources for use by customers 24 hours a day, seven days a week. Resources include Frequently Asked Questions, a knowledge base and application notes, plus information on other material characterisation solutions that Malvern can provide.

  • Page 21: Overview

    Overview Introduction This chapter gives a complete overview of the system. It explains in very simple terms: What the Mastersizer 2000 does. How the Mastersizer 2000 works. Making measurements. Viewing the results. Saving the results. Most of these points are explained in more detail in later chapters of this manual.

  • Page 22: How The Mastersizer 2000 Works

    Chapter 2 Overview How the Mastersizer 2000 works Scientists have for centuries tried to predict the way particles scatter and absorb light. There are many theories and models that the modern particle size analyst can use. One of the simplest theories used is the Fraunhofer model. This model can pre- dict the scattering pattern that is created when a solid, opaque disc of a known size is passed through a laser beam.
  • Page 23 1ms. Once the measurement is complete, the raw data from it is analysed by the Malvern software using one of the theories mentioned above. Once the data has been analysed the information can be displayed in various ways.

  • Page 24: Making Measurements

    Chapter 2 Overview Making measurements There are two ways to make a measurement; making a manual measurement or using a Standard Operating Procedure (SOP). SOPs SOPs are user-defined procedures that are easily programmed into the software to allow the same type of sample to be measured in a consistent way. Here all the dif- ficult decisions on measurement strategy have already been made.

  • Page 25: Viewing The Results

    Once the measurement information has been gathered and analysed, it can be dis- played in many forms. The Malvern software is supplied with many standard “reports” that each display the information in a specific way. For each report that is displayed on the screen, there is an equivalent “hard copy”...

  • Page 26: Saving The Results

    Chapter 2 Overview Saving the results After making a measurement the user can save the result in a measurement file by selecting File-Save or Save as (an SOP can be configured to automatically save the results to a measurement file). A measurement file has the extension .mea. Page 2-6 MAN 0384...

  • Page 27: Identifying The Features

    Typical systems – identifies the main modules of typical systems. Optical bench components – examines the features of the optical bench in more detail. Software – identifies the main features of the Malvern software. Detailed information on the dispersion units can be found in their own manuals. Mastersizer 2000...

  • Page 28: Typical Systems

    Chapter 3 Identifying the features Typical systems These diagrams show typical systems with their key modules: Mastersizer 2000 ill 7917 Mastersizer 2000E ill 7918 Page 3-2 MAN 0384...
  • Page 29 The sole purpose of a sample dispersion unit is to prepare the sample then deliver it to the optical bench so that it can be measured. Malvern makes many sample dis- persion units to handle many forms of sample, including dry powders and samples dispersed in a liquid.

  • Page 30: Optical Bench Components

    Chapter 3 Identifying the features Optical bench components The main features of the optical bench are shown below: ill 7919 The features are:  Cell area protection cover The cell area protection cover can be swung into position when the cell is not in place to prevent dust and dirt contaminating the cell area optics.
  • Page 31 (see the Essentials Manual).  Backscatter detectors These are two detectors that collect some of the light scattering information from the sample. Ensure that these are kept clean and undamaged; the Essentials Man- ual has details. Mastersizer 2000 Page 3-5...
  • Page 32 Chapter 3 Identifying the features End panel The features of the end panel are detailed below: ill 7920  Power input socket This is the power input socket to the optical bench from the external PSU.  Optical bench power switch This is the on/off power switch for the optical bench.
  • Page 33 Cell in connector. This allows any trapped air bubbles to rise through the cell. The connectors are colour coded to aid correct connection.  Locking handle The locking handle is rotated anti-clockwise to lock the cell in place. Caution! Never try to lift the optical bench by this handle. Mastersizer 2000 Page 3-7...

  • Page 34: Software

    Identifying the features Software The Malvern software controls the system during a measurement and processes the measurement data to produce a size distribution. There are two software modules: The main application, described below. This main interface allows the user to define an SOP, run a measurement, display the results and print reports.
  • Page 35 Selecting a report tab displays the data for the selected record(s) in that format. Malvern supplies standard reports that allow the user, among other things, to view the list of records within a measurement file, view the measurement data and view the size distribution as a graph and table.
  • Page 36 Chapter 3 Identifying the features Page 3-10 MAN 0384...

  • Page 37: Making Measurements - A Tutorial

    To do this, obtain a suitable sample to measure and a suitable dispersant to disperse it in. Ordinary single dairy cream dispersed in water is readily available and should give good predictable results. Mastersizer 2000 Page 4-1...

  • Page 38: General Measurement Advice

    Chapter 4 Making measurements - a tutorial General measurement advice Before making a measurement, note the important general advice given here. Sample preparation Good sample preparation is critical. A representative sample must be taken. Dry powders, for example, tend to separate out if stored for some time or vibrated. The larger particles tend to rise to the top and the smaller particles collect at the bottom of the container.

  • Page 39: The Basics Of Making A Measurement

    Manual measurements – used either to make one-off measurements or to try out a sample prior to defining an SOP for it. Follow the section below for the instrument used. Mastersizer 2000 Page 4-3...

  • Page 40: Measurements On A Mastersizer 2000

    Chapter 4 Making measurements - a tutorial Measurements on a Mastersizer 2000 Instrument preparation Before starting a measurement, ensure that the correct cell is installed in the cell area then power up the system as outlined below. (If an SOP is run, the software will check that the correct cell is connected, informing the user if it is not).
  • Page 41 Select Dairy cream using Hydro 2000G.SOP (or Dairy cream using Hydro 2000S.SOP if using the Hydro 2000S) from the directory C:\Program files\Malvern Instruments\Mastersizer 2000\SOP. Select OK. The SOP measurement will start by cleaning the tank. The SOP automatically measures an electrical background, aligns the optical system and measures the optical background.
  • Page 42 Chapter 4 Making measurements - a tutorial Making a basic manual measurement To make a manual measurement select Measure-Manual. The Measurement Display dialogue shown below will appear: ill 7754 The software will automatically make an electrical background measurement and an optical background measurement then align the optics. The main features of this display are: The Status area at the bottom left of the dialogue reports what is going on.
  • Page 43 (pump and stirrer speeds, etc.). The system automati- cally detects which dispersion unit and cell are fitted and changes this dia- logue to suit. Help – pressing this button displays help information. Close – pressing this button closes the measurement window. Mastersizer 2000 Page 4-7...
  • Page 44 Chapter 4 Making measurements - a tutorial A manual measurement test Try making a manual measurement using ordinary single dairy cream. Make sure the system is connected and powered up, then: Select Measure-Manual. The software will automatically make an electrical and optical background measurement as well as aligning the optics.
  • Page 45 Display disappears and the software returns to the main window. The measurement is now complete. Click on the Records tab, select the record and then select one of the report tabs to view the results in detail. Mastersizer 2000 Page 4-9...

  • Page 46: Measurements On A Mastersizer 2000E

    Chapter 4 Making measurements - a tutorial Measurements on a Mastersizer 2000E Instrument preparation Before starting a measurement, ensure that the correct cell is installed in the cell area then power up the system as outlined below. (If an SOP is run, the software will check that the correct cell is connected, informing the user if it is not).
  • Page 47 Make sure that the system is connected and powered up before starting. Select Measure-Start SOP. A browse dialogue appears; select an appropriate SOP file from this directory: C:\Program files\Malvern Instruments\Mastersizer 2000E\SOP Select OK. The SOP measurement asks the user to clean the cell and then pump in fresh dispersant using the dispersion unit controls.
  • Page 48 Chapter 4 Making measurements - a tutorial Making a basic manual measurement To make a manual measurement select Measure-Manual. First fill the beaker with clean dispersant, then use the dispersion unit to pump the dispersant through the cell - this will be prompted by the software. The Measurement Display now appears and the software automatically makes an electrical background measure- ment, followed by an optical background measurement and alignment of the optics.
  • Page 49 Next – pressing Next automatically moves to the next logical stage of the measurement. For example, if the user has just completed a background measurement (and the Pause between stages check box is enabled), pressing Next takes them to the Add Sample tab. Mastersizer 2000 Page 4-13...
  • Page 50 Chapter 4 Making measurements - a tutorial Accessory – pressing this displays a dialogue allowing the user to control the dispersion unit (pump and stirrer speeds, etc.). The system automati- cally detects which dispersion unit and cell are fitted and changes this dia- logue to suit.
  • Page 51 Display disappears and the software returns to the main window. The measurement is now complete. Click on the Records tab, select the record and then select one of the report tabs to view the results in detail. Mastersizer 2000 Page 4-15...

  • Page 52: Measuring New Samples

    Chapter 4 Making measurements - a tutorial Measuring new samples The above procedures are fine if the SOP is set up or all the parameters for a man- ual measurement specified. For a new material, either create or modify an SOP or set up the options for a new manual measurement.
  • Page 53 Anyone can create an SOP but typically it is the responsibility of the supervisor. An SOP can be created in one laboratory and then distributed to all Mastersizer 2000 users within an organisation. (All the sites must have the dispersion units the SOP refers to.)

  • Page 54: Measurement Options

    Chapter 4 Making measurements - a tutorial Measurement options This section shows each of the dialogues that appear when the SOP Wizard is run and explains the basic options available. As stated above, the choices for the options of both manual and SOP measurements are basically the same; most information in this section applies equally to manual measurements.
  • Page 55 Changes to the frequently used lists can be made by clicking on the Materials or Dispersants buttons which open up the material/dispersant databases. This is also the area where additional materials can be defined or existing ones modified. Mastersizer 2000 Page 4-19...
  • Page 56 Fraunhofer particle type. A small Malvern logo – these items can be deleted or modified but a warning is displayed first. Items marked in this way have been added by Malvern Instru- ments and are thought to have universal application.
  • Page 57 This dialogue also allows messages to be displayed for the operator before and/or after a measurement. For example, it may be necessary to give details on how to prepare the sample before a measurement starts, or how to dispose of it after the measurement. Mastersizer 2000 Page 4-21...
  • Page 58 Chapter 4 Making measurements - a tutorial Report/Saving dialogue The Report/Saving dialogue can be set to allow the results to be printed once a measurement has been made. Use the Reports page list box to select the report to use. If distributing the SOP to other users, ensure that they have the requested report installed.
  • Page 59 This dialogue also gives access to some advanced features and alarms. See Chapter 9 for more details. Mastersizer 2000 Page 4-23...
  • Page 60 Chapter 4 Making measurements - a tutorial Sampler Settings dialogue The contents of this dialogue depend on which dispersion unit was selected in the Sampler Selection dialogue: Use the dialogue to set all dispersion unit control settings. See the appropriate dispersion unit manual for more details.
  • Page 61 A series of prompts guides the user through the cleaning cycle.  Dispersant degassing Selecting the Enable check box causes a degassing routine to be performed each time the tank is cleaned. The degassing routine uses ultrasonic action to help remove dissolved gases from the dispersant. Mastersizer 2000 Page 4-25...
  • Page 62 Chapter 4 Making measurements - a tutorial Quantities dialogue Use this dialogue to define the quantities of sample/additives to be added during a measurement. Page 4-26 MAN 0384...

  • Page 63: Viewing The Results

    All the tabs in a Measurement window display the same measurement data but in different formats. Malvern provides several default reports, identified by the “(M)” in their name, that will be sufficient for most users. The user can also create their own custom reports as required.

  • Page 64: Displaying The Information

    Chapter 5 Viewing the results Displaying the information Open a measurement file by selecting File-Open. Once a file has been selected, a Measurement window will appear. A typical Measurement window is shown below. The information displayed for a measurement is controlled by the tabs. The first tab is always Records. This lists all the measurement records (individual measurements) that are held in that measure- ment file.
  • Page 65 This report displays various statistics comparing two or more measurements. Fit report This report shows how well the analysis data was fitted to the optical model. Grade Efficiency report This report shows grade efficiency data. The online help gives more information on this. Mastersizer 2000 Page 5-3...
  • Page 66 Chapter 5 Viewing the results Changing the Records tab By default the Records tab displays seven fields which include Record number, Sample name, Source, Measured on, etc. The record tab can be customised by adding or removing any of the fields that are stored with the measurement record.
  • Page 67 A red arrow will show the insertion point. Be careful to only release the header while a red arrow is displayed, otherwise the field may be removed from the Records tab. Mastersizer 2000 Page 5-5...

  • Page 68: Changing Views - The Report Designer

    Chapter 5 Viewing the results Changing views - the Report Designer Using the Report Designer, custom reports can be designed by the user. These provide a standardised output for the result of a selected measurement record which can be tailored to the user’s needs. Two views must be edited due to the different aspect ratios of the printed page and the computer screen.
  • Page 69 Send to front Send to back Objects can be selected individually by a left click on the mouse button, cumula- tively by holding down the Shift key while clicking the mouse button or in a group Mastersizer 2000 Page 5-7...
  • Page 70 Chapter 5 Viewing the results by “marquee selection”, dragging a box over a group of items. If an item has been overlaid by another item and cannot be selected, use the tab key to step through all the items one-by-one until it appears. Changing an item’s properties Set the properties of any added element by selecting it and double-clicking to open the Properties dialogue(s).
  • Page 71 Grade efficiency – grade efficiency curves created from particle sizing results are used to establish the efficiency of separators such as hydrocyclones, sedi- menting centrifuges or gravitational clarifiers. The table’s colour, font and number of rows and columns can be altered using its Properties box. Mastersizer 2000 Page 5-9...
  • Page 72 Chapter 5 Viewing the results Page 5-10 MAN 0384...

  • Page 73: Understanding The Views

    How the result is expressed in terms of equivalent spheres. How the distribution parameters are derived. Optical models – contrasts the Fraunhofer approximation used in some instru- ments with the Mie theory which underpins Mastersizer 2000 operation Mastersizer 2000 Page 6-1...

  • Page 74: Understanding The Display

    Chapter 6 Understanding the views Understanding the display The result from the analysis is the relative distribution of volume of particles in the range of size classes. From this basic result the statistics of the distribution are cal- culated. The result is also interpolated so that the result at points in between the size class boundaries is available.
  • Page 75 This “at a glance” inspection of the results is difficult if the result is shown as a cumulative plot. Another use for frequency curves is to compare results from different measure- ments. Other graph types can be over-plotted but the results may be confusing. Mastersizer 2000 Page 6-3...

  • Page 76: Report Features

    Chapter 6 Understanding the views Report features A typical report is shown below, followed by a brief description of the key features:. ill 7755 The residual is an indication of how well the calculated data was fitted to the  measurement data.
  • Page 77 (i.e. with no sam- ple). Obscuration is usually expressed as a percentage: 100 x Ob. An ideal range is between 3 and 20%, depending on the sample and dispersion unit used. Mastersizer 2000 Page 6-5...
  • Page 78 Chapter 6 Understanding the views Distribution – shows the type of distribution the analysis has used. Options  include change from volume to surface area, length or number. Remember that the Mastersizer measurement is fundamentally a measurement of the vol- ume distribution - transforming the result into a surface, length or number dis- tribution is a mathematical process that may amplify any error in the original result, especially at the fine end of the size distribution.

  • Page 79: Fundamental Concepts

    From scattering theory the light attenuated by a particle i may be described by: πr Where: is the efficiency of light extinction (by scattering and absorption), calculated from Mie theory for a particle of radius r Mastersizer 2000 Page 6-7...
  • Page 80 Chapter 6 Understanding the views The second term is the cross-sectional area of the particle and the final term n is the number of particles of radius r In terms of the volume of particles , the equation above becomes, for -- - πr an ensemble of particles: ∑...
  • Page 81 The system calculates concentration, however, using the size distribu- tion result and the obscuration. For a polydispersed sample the curve of the above figure can be used if the Surface Weighted Mean (D[3, 2]) of the material is taken as single size. Mastersizer 2000 Page 6-9...
  • Page 82 Chapter 6 Understanding the views Volume-based results The first, and probably most important, point to remember in interpreting results is that the fundamental size distribution derived by this technique is volume-based. This means that when a result indicates, for example, that 11% of the distribution is in the size category 6.97-7.75 microns, this means the total volume of all particles with diameters in this range represents 11% of the total volume of all particles.
  • Page 83 All of these answers are correct but each is measuring a different aspect of the matchbox. We can therefore only seriously compare measurements that have been measured using the same technique. Mastersizer 2000 Page 6-11...
  • Page 84 40mm. If there’s a need to correlate laser diffraction results with values from some other technique, consider applying a shape correction using the Result Modification procedure built into the Malvern software. Page 6-12 MAN 0384...
  • Page 85 --------------------------------- - ∑ skewness ∑ – – 3σ Skew --------------------------------- - ------------------------------------------------------------------------ - ∑ σ σ kurtosis ∑ – – d 4D K 6dσ Kurt --------------------------------- - 3 – ------------------------------------------------------------------------------------------------------------------------- - 3 – ∑ σ σ Mastersizer 2000 Page 6-13...

  • Page 86: Optical Models

    Optical models This section contrasts the Fraunhofer approximation used in some instruments with the Mie theory which underpins Mastersizer 2000 operation. Fraunhofer approximation Older instruments and some existing instruments rely on the Fraunhofer approxi- mation only. This assumes that: The particle is much larger than the wavelength of light employed.
  • Page 87 Mie theory The Mastersizer 2000 uses the full Mie theory which completely solves the equa- tions for interaction of light with matter. This allows completely accurate results over a large size range.
  • Page 88 Chapter 6 Understanding the views Page 6-16 MAN 0384...

  • Page 89: Handling Measurement Files

    Introduction This chapter outlines the storage, sorting and exporting of measurement data. It covers: Records and files. Searching and sorting records. Exporting results – how to export information to other applications. Extracting an SOP. Mastersizer 2000 Page 7-1...

  • Page 90: Records And Files

    Chapter 7 Handling measurement files Records and files The fundamental unit of storage is the “record”. A record contains all the informa- tion for an individual measurement, including the original measurement data and all parameters that have been set to calculate the size distribution. All records are stored in a measurement file which may contain one or more records.

  • Page 91: Searching And Sorting Records

    By default this is set to *.mea, which will search for all measurement files in the selected directory. Wild cards can be used to narrow down the search. For example selecting “Titanium*.mea” will search for all measurement files beginning with “Titanium”. Select the Parameters tab to specify the search criteria. Mastersizer 2000 Page 7-3...
  • Page 92 Chapter 7 Handling measurement files ill 7756 The main list box displays all the search criteria that have been set (when  starting a new search this will be blank). To add search criteria to the list, select the Add button. More than one criterion can be specified. When the search is initiated all records that match all search criteria are displayed.
  • Page 93 Records tab. Selecting any of the field headers will rearrange all records into alpha-numeric order based on that field. For exam- ple, selecting the Measured on header lists all records into numeric Measured on date order. Mastersizer 2000 Page 7-5...

  • Page 94: Exporting Results

    Chapter 7 Handling measurement files Exporting results There are several ways to export information from the Malvern application to other applications. These are: One or more records can be selected in the Results tab and “Dragged and dropped” directly into another application (provided that the application sup- ports tab separated formats e.g.
  • Page 95 Selecting New Template adds a new template name in the Available Templates list and then gives the user the option of changing the template’s name. (The tem- plate name can be changed later by pressing the Rename button.) Mastersizer 2000 Page 7-7...

  • Page 96: Extracting An Sop

    Chapter 7 Handling measurement files Having created it, set the template’s parameters by pressing the Edit.. button to open this dialogue: The Parameters list box displays all parameters available in a measurement record. The Selected list box displays all parameters that are to be included in the tem- plate.

  • Page 97: Sample Preparation

    (using an SOP) so that comparisons can be made between samples. This chapter gives information on: Sample preparation flow chart – summarises the process. Representative sampling. Considerations for dry samples. Considerations for wet samples. Symptoms of poor sample preparation. Mastersizer 2000 Page 8-1...

  • Page 98: Sample Preparation Flow Chart

    Chapter 8 Sample preparation Sample preparation flow chart This flow diagram shows the route taken to prepare an unknown sample: SAMPLE Take Representative Sample (mix well or riffle if dry powder) Does it disperse in water? Ultrasound if necessary Does it float? Analyse Try Surfactant...

  • Page 99: Representative Sampling

    Sample splitters/rifflers are also available for liquid samples. Beware of using a magnetic stirrer to mix a liquid sample. Large particles tend to move to the outside of the container due to centrifugal separation, and this can lead to sample biasing. Mastersizer 2000 Page 8-3...

  • Page 100: Considerations For Dry Samples

    Note Application Notes describing how to develop a method for dry sample analysis are available at www.Malvern.com. Page 8-4 MAN 0384...

  • Page 101: Considerations For Wet Samples

    Another solution is to warm the dispersant (for water typically to 60-80 °C) and then allow it to cool before use. Warning! Do not warm a dispersant to allow re-gassing if the dispersant is volatile. Never allow dispersants to reach their boiling points. Mastersizer 2000 Page 8-5...
  • Page 102 Most local regulations forbid hazardous samples and dispersants to be tipped down the drain, allowing them to enter the water system. Note Application Notes describing how to develop a method for wet sample analysis are available at www.Malvern.com. Page 8-6 MAN 0384...
  • Page 103 Admixtures aid dispersion by modifying the properties of the dispersant that are responsible for the problem. Admixtures are added in larger quantities, typically 1g/ l. A list of commonly used admixtures is given below: Sodium Hexametaphosphate (e.g. Calgon) Sodium Pyrophosphate Trisodium Phosphate Ammonia Mastersizer 2000 Page 8-7...
  • Page 104 Chapter 8 Sample preparation Sodium Oxalate Calcium Chloride As many of these are solid materials that are dissolved into the dispersant, the solu- tion should be filtered after preparation to remove impurities. Slurries The act of mixing up a small quantity of concentrated sample, dispersant and addi- tives before it is added to the dispersion unit tank is known as preparing a slurry.
  • Page 105 De-Gas button in the Configure-Accessory dialogue or select the Dispersant degassing check box in the SOP Wizard’s Cycles tab. Note Software degassing is a last resort in removing bubbles and dissolved gases. Ensure that all dispersants are degassed before being added to the system. Mastersizer 2000 Page 8-9...

  • Page 106: Symptoms Of Poor Sample Preparation

    Chapter 8 Sample preparation Symptoms of poor sample preparation Use this table to identify sample dispersion problems: Problem Symptom Action Sample dissolving Obscuration decreases. Try another dispersant. Dispersant contains Poor background readings. Filter the dispersant impurities before use. Bubbles within the Bubbles typically show as a Degas the system.

  • Page 107: Advanced Features

    Averaging records – creates an average record from several records (usually repeats of the same sample). Importing results from older instruments. Result emulation – a technique that allows a Mastersizer result to be modified to emulate a result from an alternative particle sizing technique. Mastersizer 2000 Page 9-1...

  • Page 108: Obscuration Settings

    Chapter 9 Advanced features Obscuration settings The obscuration is a measure of how much sample is in the beam at any one time. If this is too high multiple scattering may occur, if it’s too low insufficient signal will be detected and precision lost. Setting limits enables the system to detect poor conditions and take action either to ignore data, raise alarms or trigger the meas- urement process once a limit has been exceeded.
  • Page 109 Obscuration limits can be set up manually or using default values for the chosen sampler. Once the sample obscuration has stabilised within these limits for the specified time, the measurement is started. Mastersizer 2000 Page 9-3...
  • Page 110 Chapter 9 Advanced features Obscuration filtering Obscuration filtering rejects data that does not fall within the set limits. To enable it click on the Only include measurements…. check box and enter a Time-out period. Measurement will stop if the required number of snaps has not been made in this time-out period.

  • Page 111: Advanced Result Processing

    Reducing the result range The standard result range is: For the Mastersizer 2000 – 0.02 to 2000 microns. For the Mastersizer 2000E – 0.1 to 1000 microns. By reducing the result range it may be possible to remove the effects of contami- nants and bubbles.
  • Page 112 Chapter 9 Advanced features Transforming results The basic result produced by the analysis is a volume distribution which is the vol- ume proportion within each size class of the total volume of the particles. It is pos- sible to convert this volume distribution to a number, volume or length distribution.
  • Page 113 Select Edit-Result and then click OK in the displayed dialogue. Select the Material tab. Select the Advanced button in the Specify new result calculation section. Select the Enable transformation check box and select the relevant Trans- form Volume to radio button. Click OK twice. Mastersizer 2000 Page 9-7...

  • Page 114: Editing Results

    Chapter 9 Advanced features Editing results What happens if the user makes a measurement then at a later date wants to change one of the parameters of the result? For example, suppose that days after a measure- ment the Refractive Index specified as an optical property is found to be incorrect. A user can change the properties of the record by selecting it then using Edit- Result editor.

  • Page 115: Defining User Size Bands

    Type the particle size that will form a new size band boundary in the Size (µm) box. Select ADD. The new size boundary will be added to the List of User Sizes list box, creating a new size band. Mastersizer 2000 Page 9-9...
  • Page 116 Chapter 9 Advanced features A size band can be removed using this dialogue by selecting a size from the List of User Sizes list box and pressing the Remove button. Pressing the Clear button removes all entries in the List of User Sizes list box. Note The default size bands can be loaded by pressing the Clear button then OK.

  • Page 117: Alarms

    Select this and use the Cleanliness level slider to set the threshold for the alarm trigger. Display background (exited by key press) – a display appears, showing the background signal. This display disappears when any key is pressed. Mastersizer 2000 Page 9-11...
  • Page 118 Chapter 9 Advanced features Display background (exited by time-out) – a display appears, showing the background signal. This display disappears when the time-out set in the Time-out box is exceeded. Alignment alarms In normal operation the alignment of the system is monitored by the software and an auto-alignment procedure is automatically performed if the system is out of alignment.

  • Page 119: Averaging Records

    A dialogue will appear that will give the user the opportunity to enter a sample name and the record numbers that were used to create the average. The average will be created as a separate new measurement record capable of being saved and recalled. Mastersizer 2000 Page 9-13...

  • Page 120: Importing Results From Older Instruments

    Chapter 9 Advanced features Importing results from older instruments Records created on Mastersizer S, Mastersizer X and Mastersizer Micro/Microplus instruments running v2.15 or later software can be viewed using the current soft- ware. This provides an ongoing means of viewing records without the need to retain the original instrument.

  • Page 121: Result Emulation

    When results to be emulated are variable as is frequently the case with sieve analy- sis, it is good practice to use an average result as the basis of result emulation. Consult the online help for details on how to use result emulation. Mastersizer 2000 Page 9-15...
  • Page 122 Chapter 9 Advanced features Page 9-16 MAN 0384...
  • Page 123 Part 2 - Supervisor’s Guide...

  • Page 125: Introduction

    Security Introduction This chapter describes: Security principles. Setting up the Administrator. Security guidelines. Setting up user groups. Setting up individual users. Mastersizer 2000 Page 10-1...

  • Page 126: Security Principles

    Chapter 10 Security Security principles As instrument users may have varying skill levels, user access can be limited so that certain functions such as editing SOPs, deleting records and editing results are reserved for specific users only. Administrators, users and permissions One or more persons are set up as administrator.

  • Page 127: Setting Up The Administrator

    Confirm the blank password for the Administrator account (that is, do not type anything in) and click OK. Click Options-Security settings... and in the Security Settings dialogue shown below select the Enable security check box and click OK. Mastersizer 2000 Page 10-3...

  • Page 128: Security Guidelines

    Chapter 10 Security Security is now enabled on the system. This forces subsequent users to log in to access the software. Note If the 21 CFR part 11 feature key is installed a different dialogue is dis- played. Once 21 CFR part 11 security is enabled, it cannot be disabled. Security guidelines Once security is enabled each user must log in when the software starts.

  • Page 129: Setting Up User Groups

    Supervisors – skilled users who can perform configuration and create SOPs. The Members list shows all the users currently assigned to the group. To add a user click Add; a list of all users not currently allocated to that group is Mastersizer 2000 Page 10-5...

  • Page 130: Setting Up Individual Users

    Chapter 10 Security shown. Select one or more users (hold down the Ctrl key to select multiple users) and press OK to add those users to the group. If no users have been added yet, add these as described below, then add them to the group.
  • Page 131 Press the Groups button to display this Group Memberships dialogue: Use the Add button to allocate the user to appropriate group(s) by moving each group to the Member of: list. After adding the user to all required groups, click OK. Mastersizer 2000 Page 10-7...
  • Page 132 Chapter 10 Security To edit a user: To edit an existing user double-click their name in the Security Configura- tion dialogue to display the User Properties dialogue. Proceed as described above for adding a user. When a user logs on If security is configured users are prompted for a password when they try to log in: If the administrator selected the User Must Change Password at Next Logon check box (see above), the user sees this dialogue when they log in:...

  • Page 133: Part 3 - Appendices

    Part 3 - Appendices...

  • Page 135: Specification

    Blue light: Wide angle forward and back scattering (Mas- tersizer 2000 only) Light sources Red light: Helium neon laser. Blue light: Solid state light source (Mastersizer 2000 only) Optical alignment Automatic rapid align system with dark field optical reticle system and multi-element alignment detector.
  • Page 136 Appendix A Specification Page A-2 MAN 0384...

  • Page 137: Chemical Compatibility

    Aluminium (hard anodised) Drain assembly Stainless steel, Tygon™ tubing Cell shroud Polyurethane Caution! The paint finish of the external covers may be permanently damaged if samples or dispersants are spilt on them. Clean up any spillage immedi- ately. Mastersizer 2000 Page B-1...
  • Page 138 Appendix B Chemical compatibility Remember to check the chemical compatibility of the sample dispersion units before using a new sample and dispersant. Page B-2 MAN 0384...

  • Page 139: Unpacking Instructions

    Bei irgendwelchen Zeichen von Transportschäden den Spediteur sofort benachrichtigen. Si se advierte algún signo de deterioro, contactar inmediatamente con el transportista. Contacte imediatamente a empresa transportadora se houver qualquer sinal de embalagem danificada. ill 1708 Mastersizer 2000 Page C-1...
  • Page 140 Appendix C Unpacking instructions Cut through the plastic bonding straps. Découpez les courroies d’attache en plastique. Die Kunststoffbänder durchschneiden. Cortar las tiras de sujeción de plástico del embalaje. Corte as tiras plásticas que prendem o conjunto. ill 1721 Carefully cut the plastic packing tape along the fold lines.
  • Page 141 Never lift the instrument by its covers. Pour soulever l'instrument, ne le tenez jamais par ses couvercles. Niemals das Gerät an den Abdeckungen anheben. No levantar nunca el aparato por sus cubiertas. Nunca levante o instrumento pegando pelas suas tampas. ill 4927 Mastersizer 2000 Page C-3...
  • Page 142 Appendix C Unpacking instructions Always place the instrument on its feet. Placing it on its side will damage the covers. Posez toujours l'instrument sur ses pieds. Si vous le posez sur le côté, vous endommagerez les couvercles. Das Gerät stets auf seinen Füßen aufstellen. Ein seitliches Aufliegen beschädigt die Abdeckungen.

  • Page 143: Regulatory Statements

    Regulatory statements This appendix shows the regulatory information for each product. Mastersizer 2000 Page D-1...

  • Page 144: Ce Declaration Of Conformity (Apa2000

    Appendix D Regulatory statements CE Declaration of Conformity (APA2000) The CE badge on this product signifies conformance to European Commission Directives. ill 7964 Page D-2 MAN 0384...

  • Page 145: Ce Declaration Of Conformity (Epa2000

    Regulatory statements Appendix D CE Declaration of Conformity (EPA2000) The CE badge on this product signifies conformance to European Commission Directives. ill 7965 Mastersizer 2000 Page D-3...

  • Page 146: Fcc Notice (Us Only

    Note Changes or modifications not expressly approved by Malvern Instruments Limited could void the user’s authority to operate the equipment. Page D-4 MAN 0384...

  • Page 147: Canadian Regulatory Information (Canada Only

    Canadian Department of Communications. Note that Canadian Department of Communications (DOC) regulations provide, that changes or modifications not expressly approved by Malvern Instruments Limited could void your authority to operate this equipment. This Class A digital apparatus complies with Canadian ICES-003.
  • Page 148 Appendix D Regulatory statements Page D-6 MAN 0384...

  • Page 149: Index

    8-10 Distribution Drain Dry cell Cell Dry samples Cell holder Cell in connector Cell out connector Edit Sizes tab 9-11 Cleaning Editing an SOP 4-17 automatic Editing results cycles 4-25 Edit-User sizes Cleanliness Mastersizer 2000 Page i...
  • Page 150 Health and safety extension Help - obtaining records Help desk searching Help-About Measurement files Help-Help topics Measurement Options dialogue How Mastersizer 2000 works Measurement snaps 4-23 Hygroscopic samples Measurement tab Measurement window 3-9, 5-2 Measuring new samples 4-16 Importing old results...
  • Page 151 Mastersizer 2000 Index re-analysing searching Obscuration transforming result changing settings Records and files defined 4-2, 9-2 Records tab filtering adding field graph colour changing guidelines for levels changing record order limits removing a record mathematical expression Reducing result range what to use...
  • Page 152 Website transforming result Wet cell Sorting records defined Span features Specification Wet samples Spinning rifflers What Mastersizer 2000 does SSA (Specific Surface Area) Window Standard deviation 6-13 features Standard Operating Procedure (SOP) 2-4, 4-3 Window tool Statistics graph Page iv...

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