Malvern MPT-2 User Manual
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Malvern MPT-2 User Manual

Titrator degasser
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MPT-2 Titrator
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  • Page 1 MPT-2 Titrator & Degasser user manual Malvern...
  • Page 3 MPT-2 & Degasser User Manual MAN0318 Issue 4.0 September 2012...
  • Page 4 United Kingdom. Tel + [44] (0)1684-892456 Fax + [44] (0)1684-892789 Zetasizer, Malvern and the 'hills' logo are registered trademarks in the UK and/or other countries, and are owned by Malvern Instruments Ltd. NIBS and M3-PALS are trademarks of Malvern Instruments.

  • Page 5: Table Of Contents

    Introduction ...1-3 MPT-2 Multi-purpose titrator / Vacuum degasser - Overview Connection and accessory preparation ..........2-1 Introduction .
  • Page 6 Table of Contents MPT-2 & Degasser Page ii MAN 0318...

  • Page 7: Introduction And Hardware Introduction

    Introduction and hardware Introduction This manual details the important features of the Zetasizer Nano accessories; the MPT-2 Multi-purpose titrator and Vacuum degasser. Accessory Part number MPT-2 Multi-purpose titrator ZEN1001 Malvern Vacuum degasser: Auto-degas DEG0003 unit for the MPT-2 This manual is a supplement to the following manuals: Zetasizer Nano User Manual ...
  • Page 8 Chapter 1 Introduction and hardware Software and Control This chapter describes the accessory software controls identified in the Zetasizer Nano user manual and explains how to use the accessories to make measurements on the system. Maintenance This chapter covers all the user maintenance procedures for the accessories. This includes a maintenance schedule and associated maintenance procedures for inspecting and cleaning each dispersion unit and its respective components.

  • Page 9: Mpt-2 Multi-Purpose Titrator / Vacuum Degasser - Overview

    Introduction and hardware Chapter 1 MPT-2 Multi-purpose titrator / Vacuum degasser - Overview What does the Titrator do? The principal function of the Titrator is to allow zeta potential, size or intensity measurements to be made, while adding quantities of additives (titrants) to the sample when performing a particular titration type, i.e.
  • Page 10 This patented design results in zero vacuum "hysteresis". Control of the Titrator The MPT-2 titrator can be controlled by two methods - both via the Zetasizer Nano application software: Automatically, as part of measurement protocol when controlled through a ...
  • Page 11 This dialogue is described later in the manual. Features of the MPT-2 titrator accessory This section identifies the main features of the MPT-2 titrator accessory. ill 8740 ...
  • Page 12 Chapter 1 Introduction and hardware Magnetic Flea ill 8741  Sample container The sample container is the mixing and reaction vessel for the measurement. Attaching the sample container ill 8742 Page 1-6 MAN 0318...
  • Page 13 Be careful not to splash any sample when inserting and removing the sample con- tainer. The sample containers are disposable - replacement containers can be obtained directly from Malvern instruments. Note This manual will assume that a standard sample container will always be used, unless otherwise stated.
  • Page 14 Chapter 1 Introduction and hardware  Sample exit and return tubes The sample is pumped to and from the cell through these tubes. The ends of the sample exit and return tubes must always be below the surface of the sample, for two reasons: If the sample exit tube is above the level of the sample, no sample can be pumped and circulated.
  • Page 15 These valves are either opened or closed depending on the requirements of the prime and titration sequences. The solenoid valves open and close to control the flow of the titrant from the con- tainer, through the manifold assembly, to the sample container. MPT-2 & Degasser Page 1-9...
  • Page 16 Chapter 1 Introduction and hardware If only one titrant is requested to dispense, its respective solenoid valve will open to allow the titrant to be delivered when the syringe ascends. The other two solenoid valves will stay closed so any titrant dispensed will return to the correct titrant con- tainer.
  • Page 17 All tubing enters the sample container through entry holes in the container holder. The tubing includes three titrant tubes, purge tube, sample in and sample out tub- ing. These are described in the following paragraphs. MPT-2 & Degasser Page 1-11...
  • Page 18 Chapter 1 Introduction and hardware Adjusting the tubing length Depending upon the titration sample volume used and the type of titration being performed, the length of the tubes can be altered to be either higher or lower within the sample container. This is done as follows: Loosen the clamping screw, to loosen the tubing clamping ring.
  • Page 19 Power input socket for the titrator. The external power supply is plugged here.  Communications connector Connects to the RS232 port on the Zetasizer Nano series instruments to allow the software to control the titrator. MPT-2 & Degasser Page 1-13...
  • Page 20 Chapter 1 Introduction and hardware  Stirrer connector Connection for the magnetic stirrer. pH probe The pH probe connects to the rear panel of the titrator. Features of the Vacuum degasser accessory This section identifies the main features of the Vacuum degasser accessory. Front Panel Connections Front of Vacuum...
  • Page 21 Vacuum Degasser is powered up and the vacuum level is below 100 mm of Hg absolute. Rear Panel Connections and Controls Rear of VALIDATION Vacuum Power Degasser Switch POWER 15 - 24V 0.85A MAX EXHAUST ill 8734 MPT-2 & Degasser Page 1-15...
  • Page 22 Chapter 1 Introduction and hardware Power Connector Caution! Only use the AC power adaptor as supplied from Malvern Instruments. Connect the output plug from the AC power adaptor to this connector. See Specifications chapter for further power requirement information. Power Switch...

  • Page 23: Connection And Accessory Preparation

    This chapter describes the actions necessary for preparing the titrator and degasser accessories ready for measurements to be performed. It covers: Connecting the MPT-2 Titrator and Vacuum degasser to the Zetasizer Nano.  Preparing the titrant and sample tubing and containers.
  • Page 24 Chapter 2 Connection and accessory preparation Connections ill 8745   Power cable (direct) RS232 connection to MPT-2 Titrator   Power cable from external PSU Titrant tubing to / from Degasser   Computer connection (USB) Sample tubing to / from Nano cell...
  • Page 25 Connection and accessory preparation Chapter 2 Note Initially the accessory will have been commissioned by a Malvern Instru- ments representative. The below information describes how to fit any new tubing. To Degasser From Degasser ill 8751 Connecting the tubing (titrator to degasser) Position the titrator and degasser suitably for operation, and ensure the tubing ...
  • Page 26 Chapter 2 Connection and accessory preparation Ferrule Connector Tubing Taper ill 8746 Cut the tubing so the end is flat   Move the tubing so its end is flush with base of the ferrule   Screw the connector into one port on the front of the degasser (Channel A, for ...
  • Page 27 If a flowcell is used, insert the sample tubes into the threaded inserts and screw into the top of the flowcell, and then push both tubes down into the pinch valve on the side of the cell area. MPT-2 & Degasser Page 2-5...
  • Page 28 Chapter 2 Connection and accessory preparation ill 8750 Note The pinch valve manufacturer recommends that a vegetable-based oil (e.g. Castor oil) is used to lubricate the section of tube that is inserted into the pinch valve. This is done to help minimise friction, though testing by Mal- vern Instruments has not shown this to be essential.

  • Page 29: Preparation For Measurement

    Preparing the measurement sample. Performed before each titration ses-  sion. Filling of the measurement cell. Performed before each titration session.  To perform these operations the titrator manual control dialogue will be required. Where necessary refer to the Software and control chapter. MPT-2 & Degasser Page 2-7...
  • Page 30 Chapter 2 Connection and accessory preparation Caution! The pH probe will require special care. Never allow the pH probe to dry out. It is important to read the section on the care of the pH probe in Chapter 5. Filling and changing the titrant containers The three titrant containers are typically filled with acid, base, salt, or other addi- tives.
  • Page 31 Each titrant delivery tube can be individually primed, or all tubes can be primed simultaneously. The coloured indicators on the dialogue match the LED indicators next to the titrant container, and also the titrant tubing connectors. MPT-2 & Degasser Page 2-9...
  • Page 32 Chapter 2 Connection and accessory preparation Priming the titrant tubes: Place the filled titrant containers under the container cover, and under the  titrant tubes that are to be primed. Attach a sample container, containing a small amount of clean water, to the dis- ...
  • Page 33 The cell must be filled so that no bubbles are left within the sample path; this is especially important for Zeta potential measurements. Follow the instructions below: Open the Manual control dialogue by selecting Tools-Instrument- MPT-2  Titrator- Manual control within the Zetasizer Nano software, or by select- ing the Manual control icon.
  • Page 34 Chapter 2 Connection and accessory preparation Select the Fill tab.  Select the cycles required and press the Fill button(s) to begin the operation.  Each cycle will pump the volume of the sample tubing and cell. The pump will circulate the sample through the sample tubing and cell until ...

  • Page 35: Software And Control

    Making a measurement using the Zetasizer Nano instrument is fully documented in the Zetasizer Nano User Manuals. Refer to that manual for details. The MPT-2 Multi-purpose titrator can be controlled by two methods - both via the Zetasizer Nano application software: Automatically, as part of measurement protocol when controlled through a ...

  • Page 36: Control Of The Accessory Via An Sop

    Chapter 3 Software and Control Control of the accessory via an SOP An SOP can be configured to control all settings for the accessories automatically. A titration measurement follows the same SOP format as performed when doing a normal Size or Zeta measurement, with a few exceptions. When a titration meas- urement is chosen two extra dialogues - Titrants and Titration sequence - will be included in the SOP selections.
  • Page 37 Adjust the temperature in the SOP to the ambient value. Titration - Titrants This dialogue enables the titrants used to be specified, and the pump and stirrer speed to be set. MPT-2 & Degasser Page 3-3...
  • Page 38 Chapter 3 Software and Control Settings Description Titrants The Titrants Configuration area is used to set up the fea- tures of the titrants used, such as their type, name and con- centration. Type of titrant - Specifies the type of titrant in each of the containers.
  • Page 39 The display indicates by colour the volume and risk level of any overflow. Unless a dilution titration is being performed (see below) the display will always show the 'standard' sample container. MPT-2 & Degasser Page 3-5...
  • Page 40 Software and Control Settings Description Predicted The maximum volume of the 'standard' sample containers volume supplied by Malvern is 25ml. (continued)  No risk: The display will show green if the predicted vol- ume is within the range 5 to 15ml. ...
  • Page 41 - pH, dilution or additive - the dialogue will alter accordingly. The same format will be used, with generally just the text and titration units altered to reflect the titration chosen. The dialogue shown is for a pH titra- tion. MPT-2 & Degasser Page 3-7...
  • Page 42 During a pH titration the pH probe measures the cur- rent pH value of the sample; but, as there is no facility to read the current concentration of the sample on the MPT-2, a value must be specified here stating the concentration of the sample before any titrants are added.

  • Page 43: Starting A Titration Sop Measurement

    The status bar will prompt for certain actions during the course of the measurement. A titration measurement performs exactly the same processes that are done when performing a standard measurement, plus the inclusion of titration specific steps. MPT-2 & Degasser Page 3-9...
  • Page 44 Chapter 3 Software and Control For details of the standard measurement sequence refer to the Zetasizer Nano manual for details. The actual measurement sequence will depend upon the measurement being per- formed, though in general an autotitration measurement sequence will be as fol- lows: With the sample container and the cell inserted, Start is pressed.

  • Page 45: The 'Titration' Measurement Display

    The graph above shows a plot of the titration performed, with each titration meas- urement point indicated on the graph. A weighted average line joins the mean measurement result obtained from each group of measurement points. MPT-2 & Degasser Page 3-11...

  • Page 46: Displaying The 'Titration' Measurement Results

    Chapter 3 Software and Control Displaying the 'Titration' measurement results To display a titration report, select a 'Titration' type measurement record and then select the appropriate report tab. The report will show all appropriate measure- ment information for that record. When a Titration result is selected in the Records view, all individual associated measurements will be selected too.
  • Page 47 The Titrants Configuration area is used to set up the features of the titrants used, such as its type, name and concentration. Type.  Displays the type of titrant in each of the containers; either acid, base, or disa- bled. MPT-2 & Degasser Page 3-13...
  • Page 48 Chapter 3 Software and Control Name.  This is a title for the titrant. Concentration.  Specifies the concentration of the titrant, this is usually between 1.0M and 0.01M. The concentration chosen will affect the precision of titration measure- ment. ...

  • Page 49: Manual Control

    Software and Control Chapter 3 Manual control There are two ways to control the MPT-2 Titrator accessory manually, these are: The Manual accessory control dialogue.  The pH calibration dialogue.  The Manual control dialogue The Manual control dialogue is used to clean and prepare the unit prior to a measurement.
  • Page 50 Chapter 3 Software and Control It should be noted that all prime, fill and clean quantities are determined by the number of cycles performed, each cycle performs either one complete fill, prime or clean operation. Option Description Clean tab The Clean tab enables the sample tubing and cell to be flushed and cleaned.
  • Page 51 It is recommended that the calibration should be performed at the beginning of each titration session. The pH calibration dialogue is displayed by selecting Tools-Instrument- MPT-2 Titrator- pH calibration within the Zetasizer Nano software, or by selecting the pH calibration icon. Brief instructions on performing the cali- bration appear on the dialogue.
  • Page 52 Chapter 3 Software and Control Also displayed in the dialogue is the pH probe output from calibration (mV) value. This is a direct voltage reading generated by the pH calibration circuitry and corresponds directly to the pH point from calibration value alongside. During the calibration routine this value should constantly change.

  • Page 53: Vacuum Degasser - Operational Guide

    LED will illuminate. As well as checking the front panel LEDs, the running of the vacuum pump can be checked by placing a hand onto the instrument and checking for vibration Start the titrant flow through the system and check for leaks around the connectors. MPT-2 & Degasser Page 4-1...
  • Page 54 Note The MPT-2 Titrator should be primed after the degasser has reached equi- libration. This will ensure that the titrant in the tubes from the degasser to the sample tube is fully degassed. The Vacuum degasser uses Teflon AF®...
  • Page 55 PTFE extruded tubing. In addition, unlike the process used in extruding PTFE, no extrusion agents are MPT-2 & Degasser Page 4-3...
  • Page 56 Chapter 4 Vacuum Degasser - Operational guide needed (like kerosene, etc.) which contaminate titrants until they are extracted by the titrant over time. Likewise, this molecular structure, combined with the very small surface areas required to degas the titrant, reduces the possibility of carryover from one titrant to another to virtually zero.

  • Page 57: Maintenance

    MPT-2 Titrator maintenance Caution! Only a qualified Malvern representative, is allowed access to the inside of the titrator. There are no user serviceable parts inside the titrator. The titrator has been designed so that supervisor/operator maintenance is kept to a minimum.
  • Page 58 Chapter 5 Maintenance Cleaning the Titrator surfaces Periodically, the covers should be thoroughly cleaned using a mild soap solution on a damp cloth. Always ensure that the accessory is disconnected from the power supply before cleaning. Never use excess liquid to clean the accessory and always avoid the electrical com- ponents on the rear panel.
  • Page 59 In this respect a pH probe can be thought of as a "Consumable" item. Malvern recommends that the probe is replaced every year, but this frequency may vary.
  • Page 60 Chapter 5 Maintenance Preparation before first use Remove the screw end-cap and connect to the cable supplied. Remove the membrane protection teat. This teat contains a small amount of saturated KCl solution (3.8M). To allow air pressure equalization in the reference junction part of the probe, remove the rubber cover, or sleeve that covers the reference junction vent.
  • Page 61  Ideally, the pH probe should be calibrated while fitted to the system and using the standard sample containers. Note The pH probe should be recalibrated if the room temperature changes by more than 5°C. MPT-2 & Degasser Page 5-5...
  • Page 62 Rinse the electrode in deionised water and dab dry with a good quality lens tis- sue (one that does not shed fibres/lint free). Open the pH calibration dialogue by selecting Tools-Instrument- MPT-2 Titrator- pH calibration within the Zetasizer Nano software, or by selecting the pH calibration icon.
  • Page 63 4 buffers should be used The pH probe for the Titrator is supplied with sachets of pH4 and pH9 buffers. Follow the instructions supplied with the sachets for the best methods of making the buffer solutions. MPT-2 & Degasser Page 5-7...
  • Page 64 It is recommended that all three dispensing syringes and o-rings are replaced at least every 12 months or sooner if leaks develop. Replacement syringes and o-rings are available through the Malvern representative (see User consumable and spares at the end of this section).
  • Page 65 To replace the tubing on the Sizing flowcell, simply pull the used silicone tubing off the harder PTFE tube and replace with new tubing. Connect the tubing at the tubing connection bracket as shown below. MPT-2 & Degasser Page 5-9...
  • Page 66 Chapter 5 Maintenance Screw-fit connection “Luer” connection ill 8744 Maintenance schedule The following maintenance schedule should be followed to ensure the accessory continues to correctly function. Procedure Period Every morning or at the beginning of a new Priming the system. measurement session.

  • Page 67: Vacuum Degasser Maintenance

    Plug all of the ports on the degasser. Store the degasser in a clean, dry location.  Before using the degasser, completely purge it with the correct titrant before  reconnecting the titrator and restarting the system. MPT-2 & Degasser Page 5-11...
  • Page 68 Chapter 5 Maintenance Preventative Maintenance Perform preventive maintenance to ensure that your Vacuum Degasser will per- form consistently at an optimal level. To maintain the Vacuum Degasser in the best condition, the following measures are recommended: Adhere to standard laboratory cleanliness practices. ...
  • Page 69 Draw ments. the titrant through the channel to dissolve the buffer. Do not push the titrant through the chan- nel. If this flushing action does not work, contact your Service Represent- ative. MPT-2 & Degasser Page 5-13...

  • Page 70: User Consumables And Spares

    Chapter 5 Maintenance User consumables and spares This section lists all available user consumables and spares. Contact the Malvern Instruments representative, quoting the part number listed below. Part Part number 500 'Standard' sample and titrant containers plus caps. BEK0008 Maximum fill : 25ml 10 'Large-volume' sample and titrant containers plus lids.

  • Page 71: Appendices

    Appendices Specification MPT-2 Multi-purpose titrator Dimensions Width: 170mm (excluding pH probe). Height: 260mm Depth: 390mm Weight (dispenser unit only). 5.3Kg. Power requirements. ~ 100-240V, 50-60Hz Power supply: 24Vdc via external power supply Power rating. 30VA Recommended maximum fill capacity of standard sample container.
  • Page 72 Appendix A Appendices Vacuum degasser General Dimensions: Height: 5.0 in. Width: 2.87 in. Depth: 9.81 in. Weight 6 lb Channels 3 independent Degassing Process Gas permeation through a fluoropolymer mem- brane Maximum Flow Rate 10 mL/min. Degassing Capacity ~2 ppm at 1 mL/min. Dead Volume ~480 microliters per channel for standard channel Materials contacting...
  • Page 73 Connector and Tubing sizes Connectors Material PEEK Size / description 1/4-28 flangeless fittings for 1/16" 'Outside Diam- eter' tubing Connecting tubes from MPT-2 PTFE Material 1.6mm x 0.8mm (Outside Diameter x Inside Diam- Size eter) MPT-2 & Degasser Page A-3...

  • Page 74: Site Requirements

    Space Requirements The Vacuum Degasser is designed to sit on a standard laboratory bench top, and is plumbed into the MPT-2 Titrator system between the titrant supply and titrator pump. Enough space should be given to allow easy access to all components of the system.
  • Page 75 A set of four interchangeable adaptor plugs are is included to allow the AC adapter to be plugged into the standard electrical wall sockets in North America, Japan, the U.K., most countries in continental Europe, and Australia. If it is necessary to replace the AC Adapter - Contact Malvern instruments about replacement. Note Refer to the Health and Safety section on the main Zetasizer Nano User manual for more information.

  • Page 76: Chemical Compatibility

    The sections below detail all materials that come into contact with the sample and titrants in the normal operation of the accessory. MPT-2 Multi-purpose titrator Component Materials Sample/titrant containers (25ml)
  • Page 77 Ensure that hazardous exhaust gases are properly vented. Corrosion All parts that contact the titrant (solvents) are made of PEEK, Kel-F®, Tefzel® or Teflon AF®, PTFE or Glass-filled PTFE PEEK is sensitive to Sulphuric acid and certain solvents. MPT-2 & Degasser Page A-7...

  • Page 78: Regulatory Information

    For more detailed information about recycling of this product, please contact your local city office, your waste disposal service, or your Malvern representative. Page A-8 MAN 0318...
  • Page 79 Note Changes or modifications not expressly approved by Malvern Instruments Limited could void the user’s authority to operate the equipment. MPT-2 & Degasser Page A-9...
  • Page 80 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 81 5-14 Increment value Consumables 5-14 Installation Controlling the titrator Isoelectric point Covers 3-3, 3-14 5-10 Keeping the pH probe wet Depth Dilution titration 3-2, 3-3, 3-6 Dimensions Large volume container Dispenser LED indicators Dispenser unit 1-10 MPT-2 Autotitrator Page i...
  • Page 82 Index MPT-2 Autotitrator Preparation before first use Preparing the sample 2-11 Magnetic stirrer Prime 3-15 Mains supply voltage Prime tab 3-16 Maintaining the pH probe Priming 2-7, 2-9, 5-10 Maintenance Priming the titrant tubes 2-10, 2-12 Maintenance schedule 5-10 Problems...
  • Page 83 MPT-2 Autotitrator Index Titration - Instructions Titrants SOP Titration sequence Titration - Instructions (SOP) 3-2, 3-7 Spares Titration - Sequence (SOP) 5-14 Specification Titration - Titrants (SOP) Standard sample container Titration SOPs Standby mode Total injected Volume 3-14 Start button...
  • Page 85 Printed in England ill 8808 Malvern Instruments Limited Enigma Business Park Grovewood Road, Malvern Worcs, WR14 1XZ, U.K. Tel: +44 (0) 1684 892456 Fax: +44 (0) 1684 892789...

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