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Malvern Hydro 2000uP User Manual

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  • Page 1 Hydro 2000 µP user manual...
  • Page 3 Hydro 2000µP User Manual MAN0389 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: Table Of Contents

    T able of Contents Part 1 - Operator’s Guide Introduction to this manual ..........1-1 Introduction .
  • Page 6 Table of Contents Hydro 2000µP Part 2 - Appendices Specification ..........A-1 Specification Chemical compatibility .

  • Page 7: Part 1 - Operator's Guide

    Part 1 - Operator’s Guide...

  • Page 9: Introduction To This Manual Introduction

    Users must read the Health and Safety information in the Essentials Manual before operating the system. We recommend that users who have never operated a Malvern particle analyser read this manual fully before starting the first measurement. Those who are more familiar with particle size analysers may wish to jump straight to Chapter 4 of the main User Manual which gives details on making measure- Hydro 2000µP...

  • Page 10: Access To The Dispersion Unit

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

  • Page 11: Assumed Information

    “the system”. Menu commands Menu commands from the Malvern software are referred to in the form main menu-menu item. As an example, the command Configure-New SOP refers to selecting the New SOP item in the Configure menu. The same rules apply for...
  • Page 12 Chapter 1 Introduction to this manual Page 1-4 MAN 0389...

  • Page 13: Hardware Features

    Hardware features Introduction This chapter gives a simple overview of the dispersion unit. All key aspects of the dispersion unit’s operation are explained in very simple terms. This chapter covers: What the dispersion unit does. How the dispersion unit is controlled. How the dispersion unit works.

  • Page 14: What The Dispersion Unit Does

    Chapter 2 Hardware features What the dispersion unit does The sole purpose of any sample dispersion unit is to prepare the sample then deliver it to the measurement zone of the optical bench so that it can be measured. The Hydro 2000µP allows the Mastersizer to be used for particle-in-liquid particle sizing and has been specifically designed so that only small amounts of sample and suspending liquids (dispersants) are required.

  • Page 15: How The Dispersion Unit Works

    Hardware features Chapter 2 How the dispersion unit works The dispersion unit looks like this: ill 5473 The dispersion unit comprises two main units: The control unit which contains most of the control electronics.  The cell unit which contains the cell, the sample well, pump, ultrasonic probe ...

  • Page 16: Hardware Features

    The lid is  locked in place by rotating the locking lever  All functions of the dispersion unit are controlled using the Malvern software. Hardware features This section describes the hardware in detail. Main system components The diagram below shows a typical installation for the Hydro 2000µP.
  • Page 17 The PSU used on the Hydro 2000µP is not designed for operation in wet conditions. Do not place it in areas that are prone to spillages. Warning! Only use the power supply and cables supplied by Malvern Instruments.  Control unit The control unit contains most of the control electronics for the dispersion unit.
  • Page 18 Chapter 2 Hardware features ill 5643 Warning! If using hazardous dispersants or samples, do not allow the beaker to become over-full. If dispersants or samples are noxious, the instrument should ideally be used in a fume cupboard.  Drain beaker holder The drain beaker may hold hazardous samples and dispersants.
  • Page 19 Non-aqueous valve – suitable for use with a large range of chemically aggres- sive dispersants. The non-aqueous valve is white and has a tap on its side. Replacement valves are available from a Malvern representative. Controller unit This section examines the controller unit in more detail. As stated above, the con- troller unit contains most of the control electronics for the dispersion unit.
  • Page 20 The PSU is not designed for operation in wet conditions. Do not place it in areas prone to spillages. Warning! Only use the PSU and cables supplied by Malvern Instruments.  Accessory comms “in” connector The communications cable from the optical bench or from another dispersion unit connects here.
  • Page 21 Hardware features Chapter 2 Front panel The front panel of the controller unit is shown below and its main features identi- fied. CONTROL UL TRASOU ND H YD RO ill 5410  Status indicator The status indicator illuminates in one of three colours when the dispersion unit is powered up: Green if the dispersion unit is functioning correctly and the cell unit has been loaded into the optical bench (i.e.
  • Page 22 Chapter 2 Hardware features  Ultrasonic control cable (optional) If the ultrasonic option is fitted, this cable will carry power and control signals for the ultrasonic probe between the control unit and the cell unit. Warning! The Ultrasonic control cable carries high voltages. Under normal operat- ing procedures this is perfectly safe.
  • Page 23 The dispersant valve must be used on the dispersant inlet to prevent sample/disper- sant from leaking when the dispersant syringe is removed. Two types of valve are available, as described earlier. Replacement valves are availa- ble from a Malvern representative.  Drain port When the drain valve is operated, the contents of the cell will flow out through this port.
  • Page 24 Chapter 2 Hardware features Additionally, when measurements are performed using solvents, users may occa- sionally find that the background levels are very high. This is due to temperature gradients within the solvent. The normal cure is to wait for several minutes for thermal equilibration, or even to warm the solvent beforehand.

  • Page 25: Software Features

    Making a measurement – the basics of making a measurement using the dis- persion unit. Manually controlling the dispersion unit. Writing a Standard Operating Procedure (SOP) for the dispersion unit. Software features – the features of the Malvern software that are specific to the dispersion unit. Hydro 2000µP Page 3-1...

  • Page 26: Making A Measurement

    Chapter 3 Software features Making a measurement The dispersion unit can either be controlled manually or automatically by running a Standard Operating Procedure (SOP). Making a measurement is fully docu- mented in Chapter 4 of the main User manual. The system automatically detects which dispersion unit and cell is connected. If more than one dispersion unit is connected, the system detects all dispersion units connected, but only the dispersion unit that has its cell installed on the optical bench will be “active”.
  • Page 27 Software features Chapter 3 It features the following:  Pump Speed control The speed of the pump (which controls the speed at which the sample is circu- lated) is altered by moving the slider. Use the up and down arrows under the slider for fine adjustment of the pump speed.
  • Page 28 10°C - 35°C or there is an internal error with the temperature sensor. Contact a Malvern representative if this error condition persists. Drain Valve – illuminates if the drain valve has failed to drive (i.e. it has stuck open or closed).

  • Page 29: Writing An Sop For The Dispersion Unit

    Software features Chapter 3 Writing an SOP for the dispersion unit A Standard Operating Procedure (SOP) can be configured to control all settings for the dispersion unit automatically. When an SOP is run the software (depending on how the SOP is set up) automatically runs a measurement, giving instructions to the operator such as when to add dispersant, sample, etc.
  • Page 30 Chapter 3 Software features the case of this dispersion unit there would be an entry for Hydro 2000µP (A) and Hydro 2000µP (B). If using just one dispersion unit, select the “A” option.  Sample handling unit options This dispersion unit is supplied in two versions, with ultrasonics and without ultra- sonics.
  • Page 31 Software features Chapter 3 measurement can be made without the occurrence of the secondary diffraction pat- tern. When the flake material is suspended in a volatile solvent, such as white spirit, vari- flow is even more useful since it assists the rapid thermal stabilisation of the optics. When the sample well is filled with fresh solvent, very high backgrounds can often be observed.
  • Page 32 Chapter 3 Software features  Pre-Measurement Delay A pre-measurement delay can be added before the measurement to allow thermal equilibration to occur after ultrasound has been applied. If this is not done the anal- ysis may show the presence of large particles which are not in the sample. This is caused by the refractive index differences observed in the sample cell when the dis- persant is not equilibrated.

  • Page 33: Making A Measurement

    Making a measurement Introduction This chapter describes how to make a measurement using the Hydro 2000µP. It covers: Measurement guidelines. Instrument preparation. Anaerobic fill. Measuring new samples. Hydro 2000µP Page 4-1...

  • Page 34: Measurement Guidelines

    Chapter 4 Making a measurement Measurement guidelines The Hydro 2000µP uses very low volumes (approximately 20ml) of dispersant and sample. When using such small quantities, take the following precautions when making a measurement: Minimise the amount of sample lost during sample preparation, or through sample adhering to the sides of the well.
  • Page 35 Making a measurement Chapter 4 Sample loss during sample preparation Choose a sample preparation method that ensures that all particles are transferred to the well. A recommended method is to prepare a slurry in a small container and add this to the well using a pipette. Add as a maximum 2ml of sample volume, but 1ml is preferred.
  • Page 36 Chapter 4 Making a measurement Bubbles and pump speeds Control the pump speed to prevent the introduction of bubbles while ensuring that the sample is kept in suspension. This is true for all wet dispersion units but partic- ularly important with the small dispersant volumes of the Hydro 2000µP. The Mastersizer sees bubbles as particles and measures these.

  • Page 37: Instrument Preparation

    Making a measurement Chapter 4 Instrument preparation Before starting a measurement, ensure that the correct cell unit is installed in the cell area and then power up the system. The stages are outlined below. Powering up Power up the system by: Switching on the dispersion unit(s).
  • Page 38 Chapter 4 Making a measurement Vessel Heater Ultrasonic bath ill 5638 Once the water has been degassed, a number of bubbles may have formed on the inside surface of the vessel. To remove these, fit the lid to the vessel and very carefully turn the vessel on its side (see the diagram below).
  • Page 39 Making a measurement Chapter 4 To fill the syringe: Insert the syringe into the vessel of dispersant. Draw back the syringe very slowly. Pulling back too quickly will cause “boil- ing” on the surface of the syringe plunger (see the diagram below) or air may be dragged back through the syringe seal.
  • Page 40 Chapter 4 Making a measurement Filling the cell Finally, fill the cell with the clean dispersant. To fill the cell: Connect the syringe to the valve attached to the front of the cell unit. Hold the syringe with the plunger facing upwards (as shown below) so that any bubbles in the syringe rise to the top and are not injected into the cell.

  • Page 41: Anaerobic Fill

    Making a measurement Chapter 4 Anaerobic fill Due to the small volume of the Hydro 2000µP and associated problems of remov- ing bubbles from the system, a special fill sequence called Anaerobic fill can be used. During an anaerobic fill the pump speed is increased in steps to a target speed. A short pause is added between steps to allow bubbles to disperse.

  • Page 42: Measuring New Samples

    Chapter 4 Making a measurement Measuring new samples The above procedures are ideal if the SOP is set up or all the parameters for a man- ual measurement have been specified. Users measuring a new material must either create or modify an SOP or set up the options for a new manual measurement. This section outlines the setup for measuring a new sample.
  • Page 43 Remember that no instrument needs to be connected to the software to write an SOP. The Malvern software can be installed on a remote computer and SOPs cre- ated and edited before they are tried out on an instrument. (The Essentials Man- ual has details on installing the software on another computer.)
  • Page 44 Chapter 4 Making a measurement Page 4-12 MAN 0389...

  • Page 45: Changing Cell Holder Position

    Changing cell holder position Introduction The Essentials Manual covers most maintenance procedures. This chapter describes one non-essential procedure, how to move the cell holder from its posi- tion on the right of the optical bench, should this be necessary. The Hydro 2000µP is typically configured to be positioned on the right of the opti- cal bench .
  • Page 46 Chapter 5 Changing cell holder position To swap over the cell holder: Disconnect all connectors from the control unit. Carefully tip the control unit and the cell holder onto its back to expose the feet and connection plate (as shown on the illustration below). ...
  • Page 47 Part 2 - Appendices...

  • Page 49: Specification

    Particle size range 0.05-120µm, depending on particle shape and density. Power requirement 100-120V / 200-240V AC, 48W Only use the PSU and cables provided by Malvern. Using any other PSU may compromise safety and will void any warranty. Hydro 2000µP...
  • Page 50 Appendix A Specification Pump Speed 0 and 500-5000 rpm Accuracy 500-5000 rpm, +/-5% of F.S. Max dispersant viscosity 0.54 Poise (0.054 Pa.s) Safety: Over current and over temperature protected. Ultrasound Frequency 48 kHz (nominal) Power 0 - 20W (dependent upon dispersant) Safety Over current protected.

  • Page 51: Chemical Compatibility

    Chemical compatibility Introduction The Hydro 2000µP is manufactured from materials that give the widest protection from chemical attack. However, it is important to check that any sample or disper- sant used is chemically compatible with the materials it will come into contact with in the dispersion unit.
  • Page 52 Appendix B Chemical compatibility Page B-2 MAN 0389...

  • Page 53: Regulatory Statements

    Regulatory statements This appendix presents regulatory information. Hydro 2000µP Page C-1...

  • Page 54: Ce Declaration Of Conformity

    Appendix C Regulatory statements CE Declaration of Conformity The CE badge on this product, shown below, signifies conformance to European Commission Directives. ill 8005 Page C-2 MAN 0389...
  • Page 55 Index Dispersant inlet port 2-11 Dispersant input/syringe Accessory comms in connector Dispersant temperature Accessory comms out connector Dispersant valve Accessory control dialogue function 2-11 Anaerobic fill 3-4, 4-9 two types Anaerobic fill dialogue types Anaerobic fill sequence Dispersion unit operation Aqueous valve 2-7, 4-8 Drain...
  • Page 56 Index Hydro 2000 µP Making a measurement Sample well Manual control Sampler Selection dialogue Manual drain Sampler Settings dialogue Measurements Scattered laser light guidelines Slurry Menu commands SOP control Model number Specification Stabilising temperature Status indicator Status indicators Non-aqueous valve 2-7, 4-8 Supervisor functions Swapping cell holder position...

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