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Manual: MPT-2 Autotitrator (Man0318-3.0)

1. Changing the filter 5 8 Changing the tubing 5 8 Chemical compatibility B 1 Clamping ring 3 8 Clamping screw 3 8 Clean 3 11 Clean tab 3 12 Cleaning 4 1 5 2 5 4 5 9 Cleaning fluid 3 7 3 12 Cleaning the accessory 5 1 Communications connector 3 10 Concentration 4 10 4 12 Conductivity 4 9 Connecting the cell tubing 4 5 Connecting the tubing to the titrator 4 7 Connectors 3 9 3 10 Connectors pack 5 10 Consumables 5 10 Controlling the titrator 2 2 Covers 5 9 Creating an SOP 4 1 MPT 2 Autotitrator D Depth A 1 Dilution titration 4 8 4 9 4 13 Dimensions A 1 Dispenser 4 12 Dispenser unit 2 2 3 1 Dispensing area 3 2 Dispensing area cover 3 2 Dispensing syringe 3 6 5 7 Dispersing area 3 6 Dispersion head 3 2 3 3 Displacement ring 4 14 Disposable sample container 2 2 DOC D 3 E Enable stirrer 3 12 Error condition 3 5 Estimated pH 3 15 European Commission Directives D 1 F FCC D 2 FCC Notice D 2 Federal Communications Commission D 2 File menu 1 3 Fill 3 11 Fill tab 3 13 Filling the cell 3 13 4 7 Filling the titrant containers 4 2 Filter 4 13 5 1 5 8 Flea 3 4 5 10 Flush fluid 2 2 Folded capillary cell 4 5 H Health and safety 1 1 1 4 Height A 1 Help desk 1 4 Help file 1 4 Help About 1 4 Pace i Index How does it do it 2 1 Humidity A 1 Increment value 4 15 Installation C 1 Isoelectric point 4 10 4 21 K Keeping the pH probe wet 5 3 L Large volume conta
2. 20 x tubing cones ferrules and 8m tubing External connections pack to Zetasizer Nano ZEN4039 Inc 15 x Male Luer lock fittings Sample in connection 5 x Female Luer push fittings Sample out connection External tubing to Zetasizer Nano ZEN4040 Inc 1 box 25ft silicone tubing Displacement ring for use with large volume beaker ZEN4041 Internal tubing pack 2 ZEN4043 Includes tubing and fittings for larger bore tubing 1 8 sizes to Dispersion head RS232 cable CAB0020 Page 5 10 MAN 0318 Part 2 Appendices Specification and Site Requirements Specification Parameter Dimensions excluding pH probe Specification Width 170mm Height 260mm Depth 390mm Weight dispenser unit only 5 3Kg Power requirements Power supply 100 240V 50 60Hz 24Vdc via external universal power supply Power rating 30VA Recommended maximum fill capacity of standard sample container When filled with titrant 25ml When filled with sample 20ml Modes of operation Automatic via Malvern software The accessory has been designed to be stored and operated in the following envi ronmental conditions Operating temperature 10 to 35 C 50 to 95 F Storage temperature 20 to 50 C 104 to 122 F Humidity 10 to 90 non condensing Altitude Up to 2000m Pollution degree 2 MPT e Autotitrator Mains supply voltage fluctuatio
3. Disabled 25 L Cell Zeta potential measurement Predicted volume Sample volume Advanced Initial volume ml Data processing 10 0 a Titration gt LLEIS n Sequence Filter Instructions 0 Filter is fitted Reports Export Dispenser O Automatic Pump speed Stir speed Manual 2 E 0 E v Recirculate between repeat measurements MPT 2 Autotitrator Page 4 11 Chapter 4 Page 4 le Making measurements using the Titrator Titrants The Titrants Configuration area is used to set up the features of the titrants used such as their type name and concentration Type of titrant Specifies the type of titrant in each of the containers Use the drop down list to select the type of titrant used i e either acid base salt solvent additive or disabled depending upon the titration type being performed The colour coding to the left of the list corresponds to the colour LED indicators alongside the titrant containers in the dispersion area Titrant name This is a title for the titrant container Either type the titrant name or select from the scroll down list The name entered here will be printed on the titrant report Concentration Specifies the concentration of the titrant in the titrant container For pH titrations the concentration units will always be for Molarity M whilst for other titration types different units can be chosen The concentration chosen will affect the preci sion of titratio
4. It is recom mended the clean procedure is performed three times to ensure adequate cleanliness has been achieved 5 Once started pressing Clean a second time will stop the operation Note The larger the cleaning fluid container the more effective the cleaning operation will be Settings Pump and Stirrer Allows setting of the stirrer and of the pump to circulate the cleaning fluid through the flow cell The slider bar or value box can be used to select the speed and direc tion each control will alter to reflect the other s setting Enable stirrer will turn the stirrer on or off Note Pumping air into the tubing prior to the cleaning fluid will aid the clean ing This will act as a buffer first driving the sample through the tubing before the cleaning fluid cleans the tubes This is simply done by removing the cleaning fluid while leaving the pump running MAN 0318 Identifying the features of the Titrator Chapter 3 Fill tab The Fill tab is used to fill the sample tubing and cell prior to beginning a measure ment This primes the cell in the same way as the titrant tubes below The pump and stirrer controls work in the same way as described above b To fill the cell 1 Insert the full sample container into the dispersion head 2 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 3 The pump will circulate the sampl
5. Titrant indicators Each titrant container has an LED indicator alongside that illuminates whenever that titrant is being dispensed The three LEDs are colour coded red yellow and green to reflect the colour coding in the Titrants SOP dialogue Pump head The pump head is used to pump the sample or cleaning fluid through the cell The speed of the pump is set through the Titrants dialogue MPT 2 Autotitrator Page 3 7 Chapter 3 Page 3 8 Identifying the features of the Titrator Tubing connection bracket All the titrator tubing is routed around the bracket underneath the dispenser lid The illustration below shows details the various connections How to connect or disconnect the tubing is described in the Chapter 5 To access the bracket simply pull the dispersing area cover off Tubing entry and tubing clamping ring 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 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 m Loosen the clamping screw to loosen the tubing clamping ring m Carefully pull the tubing either up or down to the requi
6. 7925 The report is divided into four areas these are described below For different titra tion measurements the details shown will change Sample The Sample section gives details of the sample parameters This includes the sam ple name record number measurement date and time dispersant name the SOP used and the measurement file name The information shown is generally that which was inputted into the SOP measurement dialogues Cell The Cell section gives details on the Cell type used during the measurement Titrants The Titrants section displays the same information specified in the Titrants SOP dialogue The Titrants Configuration area is used to set up the features of the titrants used such as its type name and concentration m Type Displays the type of titrant in each of the containers either acid base or disa bled E Name This is a title for the titrant Page 4 20 MAN 0318 Making measurements using the Titrator Chapter 4 m 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 Results The results are shown in graphical form The graph shows a plot of the titration performed with each titration measurement point indicated on the graph The Total injected Volume ml is indicated at the top of the graph This is the amount of titrant injected into the sample during
7. 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 Cet appareil num rique de la classe A est conforme a la norme NMB 003 du Canada VCCI acceptance Japan only The Voluntary Control Council for Interference VCCI mark on this product signifies compliance to Japanese EMC regulations as specified by VCCI COS FRMERSSE REA ERRE VCCI OBE REICZZZAATREBRMERE TI _DEB RERETCEATICENH He 3lzE_T tHI5UET COBSICMBASPRBICWHHREBST SKABKENSCEPHV ET ill 6793 Translation This is a Class A product based on the standard of the Voluntary Control Council for Interference by Information Technology Equipment VCCI If this equipment is used in a domestic environment radio disturbance may occur in which case the user may be required to take corrective actions MPT 2 Autotitrator Page D 3 Appendix D Regulatory statements Page D 4 MAN 0318 Index A Access to the titrator 1 2 Adding a pH point 3 15 Additive linear titration 4 10 Additive log titration 4 9 Additive titration 4 8 Adjusting the tubing length 3 8 Altitude A 1 Attaching the sample container 3 4 B Back panel 1 1 1 4 3 2 3 10 Bubbles 3 5 Buffers 5 4 5 6 5 10 Cc Calibration points 3 15 Canadian Regulatory Information D 3 CE badge D 1 CE Declaration D 1
8. Once the start value has been obtained a measurement will be performed The sample will recirculate if specified 5 With the first measurement complete more titrants will be added to the sample to bring it to the second measurement point where another measurement will be performed 6 The measurement sequence continues until all points have been measured 7 The measurement sequence will now complete and add a result to the current open file The progress meter indicates the measurement progress during each stage Page 4 18 MAN 0318 Making measurements using the Titrator Chapter 4 Note If Close is pressed while a measurement is in progress the screen will close but only the data for the currently performed titration measurement will be lost The data from all completed titration measurements will be preserved i e if 15 individual measurements are to be performed for one complete titration and the titration is closed on measurement 10 the first nine measurements data will be preserved but the 10th measurement data will be lost For Zeta potential measurements when the titration measurement is closed before all individual measurements are completed no isolelectric point will be generated 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 i
9. any Help button by then pressing the Con tents button Help desk All queries regarding the system should initially be directed to the local Malvern representative Please quote the following information m Model and serial number of the optical unit and accessories MB Version of the Malvern software The serial number of the optical unit and the accessories can be found on the rear panel of each module and on the cuvette holder for the Zetasizer The version number of the Malvern software can be found by starting the software and selecting Help About Contact the United Kingdom help desk if the local Malvern representative is not available The direct line to the United Kingdom Helpdesk is 44 0 1684 891800 It should be noted that this help line is primarily English speaking Remote support Malvern Instruments offers a remote support service delivered by an Internet con nection Benefits include fast and efficient fault diagnosis reducing downtime and costs On line user training is also available plus software updates A direct Internet con nection LAN must be available to make use of this facility Malvern Website www Malvern com The Malvern website offers a comprehensive range of particle characterisation resources for use by customers twenty four hours a day seven days a week Resources include software downloads frequently asked questions a knowledge base and application notes plus information on other part
10. before inserting into the pinch valve channel Zeta potential measurements The tubing is attached to the folded capillary cell DTS1060 using Luer lock con nectors With a half turn these secure to the Luer fittings on the top of the cell do not overtighten The tubing is then inserted into the pinch valve channel MB Insert one tube until held by the pinch valve m Insert the second tube and rest it above the pinch valve MPT 2 Autotitrator Page 4 5 Chapter 4 Page 4 6 Making measurements using the Titrator Push 1st tube into pinch valve Rest the 2nd tube above pinch valve ill 6841 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 Size measurements The tubing is attached to the sizing flowcell ZEN0023 using threaded inserts As with the folded capillary cell above insert one tube into the channel until held by the pinch valve then insert the second tube into the channel to rest above the valve Ensure the join between the PTFE and silicone tubing is within the cell area Sample in ce Tubing join Sample out within cell area Push 1st tube into pinch valve Rest the 2nd tube above pinch valve ill 6842 MAN 0318 Making measurements using
11. end of the titrant tube Immersing the tubes in the sample will break the surface ten sion 2 Bubbles may be generated from the dropping of titrant into the sample The titrant tubes are the same as those used for the sample If required the titrant tubes can be extended to use a larger volume titrant container A cut out is pro vided at the top of the dispersion area cover for the exit of the tubes Note For protein measurements where only a minimum sample volume is desired loosen the tubing clamp and carefully pull both sample and titrant tubing down towards the bottom of the container see the Tub ing connection bracket section later in this chapter Ideally the stirrer is not used It is not required with protein measurements when the mini mum volume is required Status indicator This indicator shows the status of the titrator The indicator will show m Red if the titrator has encountered an error condition Green if the titrator is in operation Amber if the titrator is in standby mode MPT 2 Autotitrator Page 3 5 Chapter 3 Identifying the features of the Titrator Dispersing area The illustration below identifies the main features of the dispersing area ill 6829 Dispensing syringes and syringe drive The syringes are the mechanism for dispensing precise amounts of titrants from the titrant containers to the sample container When a titrant is requested the syringe drive will descend to firs
12. new titrant i e name type concentration A note on titrant concentration Preparing and specifying the concentration of the titrants is critical to achieving accurate results The concentration specified within the Titrants SOP dialogue must be accurate to within 10 A concentration of 0 25M is satisfactory for most measurements In some situations it may be wise to vary this For example if a large number of points is to be used in a titration measurement or if performing pH measurements close to pH 7 a lower concentration may be needed The titrator can accurately dispense small volumes so concentrations of titrant up to 1M can be used It is recommended that pre diluted titrants are purchased Either use titrants that are diluted to the exact concentration required or purchase titrants of a known Molar concentration that can be easily diluted further For titrations that cover a wide pH range it is useful to use two concentrations of titrant e g 0 25M of acid and 0 01M of the same acid This will ensure that the pH values achieved are closer to the requested values Priming Priming is the act of ensuring that the titrant tubes are completely full of the titrant Over time the titrant may evaporate from the end of the titrant tube and therefore it will not deliver the correct volume when first used It is recommended that the dispenser unit is primed every morning or at the beginning of a new session Select one prime cy
13. pH list and press OK to add it to the Calibration points list in the main dialogue MAN 0318 Maintenance Chapter 5 2 Or if using a pH buffer not available in the list select Custom type the value in the Custom buffer entry box then press OK to add it to the Cali bration points list in the main dialogue If the maximum accuracy of calibration is required over a wide pH range then 3 or 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 As buffers are typically low cost items it will be more economical to source from a local supplier If finding a convenient source proves difficult contact the local Mal vern representative who will be able to give advice Common Problems pH electrodes are versatile but their performance is dependent on the sample being tested For example pH measurement of high purity water or liquids containing sulphur ions will require special electrodes m Slow response can often be caused by the build up of deposits on the glass membrane or frit Initially try cleaning the probe by dipping into concentrated Nitric Acid for 10 seconds If this is unsuccessful repeat for one minute If still unsuccessful then regeneration may be possible by dipping the membrane for one minute into a solution of 2 HF and 5 HCI whilst stirring Should the frit be blo
14. reaction vessel for the measurement Attaching the sample container ill 6832 MPT 2 Autotitrator Page 3 3 Chapter 3 Page 3 4 Identifying the features of the Titrator The sample container initially just contains the sample to be measured Titrants are added to the sample through the titrant tubes and the dispersion is stirred Two sizes of containers can be used the standard container as shown above and a large volume container which will generally be used for dilution titrations To Attach and remove the standard sample container simply screw the container into or unscrew the container from the dispersion unit as shown above Instructions on fitting the large volume container are described in the Titrants SOP dialogue section in the next chapter 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 pH probe The pH probe measures the pH of the sample The performance of the pH probe will deteriorate over time though correct maintenance will extend its life and ensure rapid and accurate titrations It is recommended that the probe is replaced at least once a year Caution A The probe must never be allowed to dry out If it does it may need
15. replac ing See Chapter 5 for details on maintaining the probe Magnetic Stirrer The stirrer agitates the sample and aids titrant dispersion The stirrer motor is pulled forward from the front of the titrator to sit directly below the sample container A magnetic stirrer flea placed in the sample con tainer will agitate the sample once the stirrer is turned on during a titration or pH calibration The speed of the stirrer is set through the Titrants SOP dialogue The optimum speed will depend upon the type of sample being titrated Care should be taken when adjusting the stirrer speed as air may be introduced into the sample If in doubt set the stir speed check box to Automatic MAN 0318 Identifying the features of the Titrator Chapter 3 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 1 Ifthe sample exit tube is above the level of the sample no sample can be pumped and circulated 2 Bubbles may be generated from the dropping of sample back into the sample container Titrant tubes The measured dose of titrant from the titrant containers enters the sample con tainer through these tubes The ends of the titrant tubes must always be below the surface of the sample for two reasons 1 Ifsmall amounts of titrant are dispensed these may stay attached to the
16. stirrer attachment pumped through the flow cell and then measured at each of these conditions In this way the effects of adding various amounts of these titrants on the zeta potential size or intensity can be investigated This method is known as a titration measurement A pH probe continually monitors the pH of the sample while a temperature controller in the optical unit maintains the sample at a selected temperature A pinch valve integrated into the Zetasizer Nano basin moulding pinches the tubing and ensures that fluid is stationary during measurements Once the measurement sequence is complete the sample and titrants can be flushed from the system The sample and titrant containers if required are replaced with ones containing flush fluid The fluid is then circulated through the system to a waste container Controlling the Titrator The Zetasizer system will automatically detect that the titrator has been connected to the instrument Once connected titration measurements can be performed either by performing a manual measurement or automatically by running a Stand ard Operating Procedure SOP For checking the operation of the pH probe and for performing maintenance oper ations such as pH calibration a further manual control dialogue is available This dialogue is described in more detail in Chapter 3 when performing pre and post measurement procedures such as priming and cleaning and in Chapter 5 Controlling th
17. the course of the measurement For Zeta potential measurements the Isoelectric point is also indicated at the top of the graph This is the pH point at which the Zeta potential is zero Please see the Size description in the Zetasizer Nano manual for details on altering the graph MPT 2 Autotitrator Page 4 21 Chapter 4 Making measurements using the Titrator Page 4 22 MAN 0318 Maintenance Introduction 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 This section explains the routine maintenance procedures that the supervisor operator can perform These procedures are m Cleaning the titrator 8 Maintaining the pH probe MW Replacing the Dispensing syringes and o ring m Changing the filter and tubing A summary of how often these procedures should be carried out is detailed in the maintenance schedule later in this chapter Additionally this section contains a list of parts and part numbers of consumables and items that can be replaced by the user in the event of failure Cleaning the accessory Caution A The surfaces of the system may be permanently damaged if samples or titrants are spilt onto them If spillages should occur then the system should be disconnected from the power supply before scrupulo
18. those available for making a manual titration measurement so this chapter will also be of benefit to those who require an explanation of the options available for a manual measurement m To create a new SOP select File New SOP This will open up the SOP Edi tor The SOP Editor consists of several dialogues that can be stepped through by using the Next button Mm Once the SOP has been created press Finish and save the new SOP The various SOP dialogues are described below Measurement type Select an Autotitration measurement and then choose whether a pH Dilution or Additive titration is required Lastly select the type of measurement i e Size Zeta potential or Intensity that is to be performed two measurement types can be cho sen Page 4 8 MAN 0318 Making measurements using the Titrator Chapter 4 Measurement type pH Titration Instrument configuration E Sample Material Dispersant General options Temperature Cell E Size measurement Advanced Data processing A Zeta potential measurement Advanced Data processing B Titration Titrants Sequence Instructions Reports Export The pH Titration SOP Editor menu is The menu shown indicates a pH Titration done against Size and Zeta potential The menu list will change dependent upon the Titration and measurement options chosen Titration types Size Zeta Potential Molecular Weight Flow pH La Size and Intensity Trend gt Dilut
19. when ready m The Measurement display discussed below will now appear m Follow the instructions on the status line of the measurement display and press the Start di button to start the measurement m The measurement sequence will complete and the results can be viewed see Displaying the results The Titration measurement display The Titration measurement displays are virtually identical to those shown when performing a standard Zeta or Size measurement The only difference being the inclusion of a measurement type versus titration tab i c Zeta Intensity vs pH The standard tabs are explained in the Zetasizer Nano manual Titration measurement type i e pH Zeta This tab details the titration measurement against the measurement type that is simultaneously produced The graph shown will only appear after the measure ment sequence has finished and show a plot of titration v measurement type i e pH v Zeta potential Manual measurement pH Titration Example titration E Stop Q Help ll Zeta Potential Intensity vs pH Multiview Log sheet Expert advice Zeta Potential Intensity vs pH Zeta Potential mV el tal Zeta Potential m Average Zeta potential mY Intensity keps Average Intensity kcps CCCCCCCCCO CECE T 25 0 C Pos 0 00mm Attn 0 pH 6 0 MPT 2 Autotitrator Page 4 17 Chapter 4 Making measurements using the Titrator T
20. 0318 Making measurements using the Titrator Chapter 4 Preparing the sample in the container Before starting the measurement it is necessary to prepare the sample and attach the container to the dispersion head 1 First prepare the sample to be measured and place a known volume into a sam ple container An initial sample volume of 10ml is recommended 5ml mini mum to 25ml maximum The preparation of the sample is of prime importance Read the sections on sample preparation in the Zetasizer Nano manual Note The sample used should be of a suitable concentration that gives an inten sity of scattering within recommended values This is checked at the beginning of each titration If the concentration is too high the titration may proceed slowly due to the sample buffering the pH If a message occurs indicating the sample concentration is higher than recommended dilute the sample and restart the titration 2 Attach the sample container to the dispersion head as described in Chapter 3 Connecting the cell tubing Follow the guidelines on inserting the cell in the Zetasizer Nano manual The tubing has to be attached correctly between the cell used and the titrator unit itself How the tubing is connected to the cell is dependent upon the cell and the measurement being performed Connecting the tubing to the cell Follow the instructions below for connecting the cell For each cell minimise the tubing within the cell area
21. IMPT 2 Autotitrator User Manual MAMNOS16 Issue 3 0 Januar y 2007 Malvern Instruments Ltd 1999 2003 2004 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 No reproduction or transmission of any part of this publication is allowed without the express written permission of Malvern Instruments Ltd Head office Malvern Instruments Ltd Enigma Business Park Grovewood Road Malvern Worcestershire WR14 1XZ United Kingdom Tel 44 0 1684 892456 Fax 44 0 1684 892789 Windows 2000 and XP are registered trademarks of the Microsoft Corporation Printed in England Addendum to manuel Addendum number ADD0075 1 0 Date 04 02 2009 Manual number MAN0318 3 0 Manual name MPT 2 Autotitrator User Manual This addendum presents new information on inserting sample tubes into the pinch valve channel on the Zetasizer Nano instrument when connecting to the MPT 2 accessory This information replaces previous content in the section Connecting the cell tubing on pages 4 5 and 4 6 of the Manual Connecting the cell tubing Follow the guidelines on inserting the cell in the Zetasizer Nano manual The tubing has
22. Polypropylene Magnetic stirrer flea Teflon Manifold PEEK Polyetheretherketone Manifold valves PEEK and FFKM seal Dispensing syringes PTFE Peristaltic pump tubing Silicone rubber Internal Tubing PTFE Tubing to optical unit and cell Silicone rubber Tubing connectors Polypropylene PVDF pH probe Glass Displacement ring MPT e Autotitrator PEEK Polyetheretherketone Page B 1 Appendix B Chemical compatibility Page B 2 MAN 0318 Installation This section gives instructions on how to reconnect the accessory should it be nec essary to move it once it has been commissioned The accessory must be initially commissioned by a Malvern Instruments representative Ensure that the new location of the system has enough space before attempting to move the accessory If the accessory is to be moved short distances then a sample container containing water should be attached to the dispersion head to prevent the pH probe from dry ing out If the accessory is to be moved greater distances then the pH probe should be removed and its protective cover attached to prevent the probe from drying out Follow the installation instructions for the Zetasizer Nano as detailed in the User manual then connect the Titrator as shown below Stirrer On off pH probe 24V PSU Mains Supply USB comms ill 6929 MPT 2 Autotitrator Page C 1 C Appendix C Installatio
23. and press the Prime button to begin the operation Each cycle will pump the volume of the titrant tubes from the container Priming will stop once the number of cycles has been completed Page 3 13 Chapter 3 Page 3 14 Identifying the features of the Titrator 6 Once started pressing Prime a second time will stop the operation 7 When the prime operation has finished titrant should be visible in the bottom of the beaker If none is dispensed the Prime button should be pressed again to repeat the process The titrant tubes can also be cleaned using the same tab Simply insert containers of cleaning fluid in place of the titrant containers pH monitor tab This tab continually reads and displays the current pH of a sample either in the sample container fitted to the titrator or a separate container that the probe is inserted into The reading will update every second If using a separate container place the probe in the sample then wait for the read ing to stabilise before reading the value Note It is good practice to stir a sample during a pH measurement pH calibration dialogue With this dialogue the pH calibration points can be set and the calibration per formed pH Calibration Calibrated 05 December 2006 14 45 26 Calibration Points pH Buffer Points Add eao 0o Xeon Buffer Preparation Clean the pH probe then position the buffer to cover at least 2 cm of the
24. ber of points the range of the titration and the equilibration time Depending upon the titration type selected 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 MAN 0318 Making measurements using the New SOP pH Titration File Help i Gr OIA th 40 gt Measurement type pH Titration Titrator Chapter 4 pH sequence ich configuration Start pH End pH Increment O Points Ee ample Material 3 0 gi 6 0 E 0 5 s Dispersant General options O Start at current pH Temperature Cell E Zeta potential measurement Predicted volume Precision Advanced Target pH tolerance Data processing 0 60 5 Titration Titrants Instructions i Advice Reports more dilute titrant may be required to perform the titrati Export lover the range specified Sequence The sequence arca enables the Start and End pH or concentration values to be set The display will change depending on the type of titration set in the measurement type dialogue MB With a titration selected enter the Start and the End values in the respective boxes At the start of the titration the titrator will change the pH or concentra tion of the sample to match that requested for the start point m Change the Increment value to determine how many titration points
25. cell area Ensure the join between the PTFE and silicone tubing is within the cell area Sample in A I Sample out TM A j V Tubing join eyy Within cell area ill 8419 Addendum 0075 1 0 Table of Contents Part 1 Operator s Guide Introduction to this manual Accessito He Tihao ecese pranane Sob wane Sa ea oe a A aes 1 2 Assumed information LL 1 3 Where to get Helpi i ve i ia nee eae a dee a Glee a 1 3 Overview What does the Titrator d0 LL 2 1 How doesit dolit idrica elica ea 2 1 Controlling the Titrator ee 2 2 Identifying the features of the Titrator Features of the Dispenser sasana nananana aa 3 1 Manual functions of the software 2 0 ccc 3 11 Making Measurements using the Titrator Introduction atanh cee eat ede ea Se hae eg eos eee eas 4 1 SUP ec aaa a alata 4 2 Making a measurement 4 4 Preparing the sample in the container 4 5 Connecting the cell tubing LL 4 5 Filling the Celia e sik ahve a ade edema nd eed wale wae ee 4 7 Creating the Titration SOP 1 1 0 ee 4 8 Starting a Titration SOP measurement 4 16 The Titration measurement display 0 000 eee ee eee 4 17 Displaying the Titration measurement results a u saaana eraann 4 19 MPT 2 Autotitrator Pace i Table of Contents MPT e Autotitrator Maintenance IMTFOQUGHONI 3 ji de eed etd Le ARE AR a ee aed esl dee dee 5 1 Cleaning the accessory LL 5 1 Ma
26. cked by proteins then try soaking the electrode in an appropriate organic solvent or a solution of 10 pepsin in 1M HCL As such actions usu ally dehydrate the glass membrane it will be necessary to soak overnight in 3M KCI solution If these actions are unsuccessful then the electrode will need to be replaced m Always ensure that the level of the electrode s electrolyte is above that of the liquid under test This will prevent electrolyte contamination and ensure a good electrical contact With the blue rubber cover removed the electrode uses a small amount of electrolyte per day When in continuous use weekly top ups are recommended Replacing the dispensing syringes and o ring 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 MPT 2 Autotitrator Page 5 7 Chapter 5 Page 5 8 Maintenance gt To remove a syringe and o ring 1 2 3 Turn off the accessory and remove the side cover Manually push down the syringe mount Pull the base of the syringe out of the syringe mount and then out from the o ring Using a small screwdriver push the o ring out of the manifold assembly The o ring will fall out the back of the manifold onto the base of the dispensing area ill 6835 Replacement i
27. cle when performing a daily prime The dispenser unit should also be primed when a titrant container is changed in order to remove any traces of the original titrant that may be left in the titrant tubes Three prime cycles will be sufficient to remove previous titrant MPT 2 Autotitrator Page 4 3 Chapter 4 Making measurements using the Titrator MPT 2 Manual Control Clean Prime Fill pH Monitor Titrants o a aO O ll v Cancel Help b To prime the titrant tubes 1 Attach a sample container containing clean water to the dispersion head Water in the container is not essential but will eliminate the effect of surface tension at the end of the titrant tube 2 Open the titrator application by selecting the Manual control icon 3 Select the cycles required and press the Prime button 4 Priming will be finished once the number of cycles has completed Making a measurement As explained in the Zetasizer Nano manual a measurement can be made in two ways either as a Manual measurement or by using an SOP The sections that follow will concentrate on making measurements using SOPs It should be noted that when performing either a manual or SOP titration the same dialogue structure that is detailed in the Zetasizer Nano manual will be used though certain dialogues will change slightly to accommodate the Titrator selec tions where necessary these changes will be explained in the text Page 4 4 MAN
28. e Titrator from an SOP A Standard Operating Procedure SOP is like a template that pre defines all the measurement settings This ensures that measurements made on the same type of sample are made in a consistent way SOPs are ideal if the same type of sample is Page 2 2 MAN 0318 Overview Chapter 2 regularly measured inputting the same parameters each time a measurement is made is tedious and runs the risk of making errors SOPs can be created or modi fied as required Titration SOP measurements use basically the same dialogues as the standard SOP measurements except for the addition of titrator specific dialogues Typically the extra information required for a titration SOP is m The type of measurement to be made zeta potential size etc m Which titrant is to be added and its concentration m The type of titration measurement to perform Number of titration points etc Manually controlling the Titrator A manual measurement is where all the measurement parameters are set immedi ately before the measurement is performed This is ideal if measuring many differ ent types of sample or experimenting with the measurement parameters and different levels of titrant addition To perform a manual measurement select Measure Manual from the menu bar A manual measurement dialogue will appear where the measurement settings can be chosen and if required saved as an SOP Once chosen the measurement can begin by simply press
29. e through the sample tubing and cell until the number of cycles has been completed or the Fill button is pressed a second time Use the pump and stirrer controls below to adjust the pump and stirrer speeds during the filling Note Filling the cell should be performed at a lower speed i e 40 than during a normal titration This prevents the introduction of bubbles into the tub ing which will affect the measurement result especially when performing a zeta measurement If bubbles appear invert the cell while still pumping and tap it lightly to dislodge them Prime tab Priming is the process of ensuring that all the titrant delivery tubes are free of air and full of liquid Generally this is done after changing titrants or after the system has not been used for a time e g overnight 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 b To prime the titrant tubes 1 MPT 2 Autotitrator Place the filled titrant containers under the container cover and under the titrant tubes that are to be primed Insert an empty waste sample container into the dispersion head to catch the titrants Select the radio button for the titrant tube that is to be primed or All to prime all three titrant delivery tubes at once Select the cycles required
30. eing correctly calibrated If the pH probe has not been calibrated then the pH values will be incorrect It is recommended that the pH probe is calibrated before each titration session To calibrate the pH probe the following is needed Mm At least two pH buffers The default buffers are pH 4 and pH 9 these are sup plied with the probe See Choosing the buffers when calibrating later in this section for advice on selecting buffers A maximum of four buffers can be used for the calibration m A container of clean deionised water to rinse the probe between measurements MAN 0318 Maintenance Chapter 5 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 gt To calibrate the probe Calibration is performed by selecting a calibration point that will match the pH buffer to be used and pressing the Measure button Instructions are present on the calibration dialogue to give guidance through the process 1 Rinse the electrode in deionised water and dab dry with a good quality lens tis sue one that does not shed fibres lint free 2 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 pH Calibration Calibrated 05 December 2006 14 45 26 Calib
31. ent SOP 4 11 Zeta measurements connecting the cell 4 5 Zetasizer Nano manual 1 1 Page iv MAN 0318
32. er Nano manual for details Only the Sample viscosity option will be shown if an Intensity only measurement option is chosen Sample Temperature See the description in the Zetasizer Nano manual Note As the temperature probe is not temperature compensated it is recom mend that titrations are performed with ambient temperature conditions Adjust the temperature in the SOP to the ambient value Sample Cell See description in the Zetasizer Nano manual Size measurement See the description in the Zetasizer Nano manual MAN 0318 Making measurements using the Titrator Chapter 4 Size measurement Advanced See the description in the Zetasizer Nano manual Size measurement Data processing See the description in the Zetasizer Nano manual Zeta measurement See the description in the Zetasizer Nano manual Zeta measurement Advanced See the description in the Zetasizer Nano manual Zeta measurement Data processing See the description in the Zetasizer Nano manual Titration Titrants This dialogue enables the titrants used to be specified and the pump and stirrer speed to be set New SOP pH Titration File Help Get td A e gt Measurement type pH Titration Titrants Instrument configuration Type Name Concentration Conc units A Sample IG A v 0 004 M Material pas HL JL vl Dispersant Acid v 0 001 M General options Temperature
33. f as a mixing bowl The sample to be meas ured is placed in a container that is screwed to the underside of the Dispersion head Titrants are added and the sample stirred The dispersion head also houses the pH probe This area is explained in more detail later in this chapter Dispensing area Warning For safety reasons the dispensing area cover must always be in place during a measurement sequence The dispensing area houses the dispensing syringes titrant bottles valves and the pump head This area is explained in more detail later in this chapter Dispensing area cover The dispensing area has a removable cover that allows access to both the titrant and sample tubing and the sample filter The cover simply pulls up and off the unit Rear panel The rear panel contains all electrical connections to the computer and optical unit This area is explained in more detail later in this chapter pH probe The pH probe connects to the back panel of the titrator Page 3 2 MAN 0318 Identifying the features of the Titrator Chapter 3 Dispersion head The sample to be measured is placed in a sample container that is attached to the dispersion head Titrants are added and the sample stirred The dispersion head also houses the pH probe The illustration below identifies the main features of the dispersion head Magnetic Flea ill 6831 Sample container The sample container is the mixing and
34. g 4 11 Titrants 4 8 4 11 Titration Export 4 16 Titration Instructions 4 16 Titration Reports 4 16 Titration sequence 4 8 4 14 Zeta measurement 4 11 Zeta measurement Advanced 4 11 Zeta measurement Data processing 4 11 Spares 5 10 Specification A 1 Standard Operating Procedure 1 2 2 2 Standard sample container 3 4 Standby mode 3 5 Start button 2 3 Status indicator 3 5 Stirrer 2 2 3 4 3 10 4 7 Stirrer flea 3 4 Stirrer settings 3 12 Stirrer speed 4 12 Storage temperature A 1 Supervisor 1 2 Syringe 2 2 3 2 3 6 5 7 Syringe drive 3 6 T Temperature A 1 Titrant concentration 4 3 Titrant containers 2 2 3 7 4 2 Titrant indicators 3 7 Titrant name 4 12 Titrant tubes 3 5 3 8 3 9 Titrants 4 12 Titrants SOP 3 4 Titration Export SOP 4 16 Titration Instructions SOP 4 16 Titration Reports SOP 4 16 Titration Sequence SOP 4 14 Titration Titrants SOP 4 11 Titration SOPs 4 8 Titration types 4 9 Total injected Volume 4 21 Tubing clamping ring 3 8 Tubing connection bracket 3 5 3 8 MPT 2 Autotitrator Pace iii Index MPT e Autotitrator Tubing length adjustment 3 8 Type of titrant 4 12 U User consumables 5 10 Using the Titrator 4 1 V Valve 3 6 VCCI acceptance D 3 Volume 4 13 Ww Website 1 4 What does the Titrator do 2 1 Width A 1 www Malvern com 1 4 Z Zeta measurement Advanced SOP 4 11 Zeta measurement Data processing SOP 4 11 Zeta measurem
35. has been completed or the Fill button is pressed a second time Use the pump and stirrer controls to adjust the pump and stirrer speeds during the filling see the note below MPT 2 Autotitrator Page 4 7 Chapter 4 Making measurements using the Titrator 5 Before starting the titration check that this procedure has eliminated all bub bles from the cell Note i Filling the cell should be performed at a lower speed than during a normal titration i e 40 of normal speed This to prevent the introduction of bub bles into the tubing which will affect the measurement result especially when performing a Zeta measurement If bubbles are present invert the cell while still pumping and tap it lightly to dislodge them Creating the Titration SOP 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 Also note that some of the other dialogue pages will alter slightly to accommodate extra parameters necessary to perform the titra tion measurement For information on the standard SOP dialogues please refer to the Zetasizer Nano manual where necessary This section focuses on how to create a new SOP and details all the measurement settings that are available Almost all the options for creating a titration SOP are the same as
36. he accessory Below is a list of these people and their responsibilities Malvern personnel Malvern personnel service engineers representatives etc have full access to the accessory and are authorised to perform all service procedures that may require the removal of the covers Supervisor The supervisor is the person responsible for the management safety of the system and of its operation The supervisor is responsible for the training of the operators The supervisor can perform all user maintenance routines identified in Chapter 5 The supervisor must under no circumstances remove the covers of the instrument or accessory Operator An operator is a person trained in the use of the system The operator can perform all user maintenance routines identified in Chapter 5 The operator must under no circumstances remove the covers of the instrument or accessory Page 1 2 MAN 0318 Introduction to this manual Chapter 1 Warning A Removal of the covers by unauthorised personnel will invalidate the war ranty of the accessory Assumed information Naming convention Within this manual the Zetasizer Nano series instruments will be referred to as the Optical Unit or the instrument The MPT 2 Autotitrator will be referred to in full or as the Titrator The combination of the Optical Unit one or more accessories and the computer will be referred to as the System Menu commands Menu command
37. he electrode using a similar action used with a clinical thermometer Keeping the pH probe wet If the pH probe is allowed to dry out even for short periods the performance of the probe can be severely affected It may not be possible to recover a degraded pH probe Typically when the probe is immersed in a buffer solution the pH should be attained to within 0 1 of the pH within 10 seconds If this time exceeds 30 sec onds and the probe cannot be recovered then the probe should be replaced When changing the sample container do not allow the probe to be exposed to air for more than 20 seconds Make sure that the next sample container is ready to attach or alternatively have a spare container of storage solution available What is a soaking solution A soaking solution is a liquid that the probe can be immersed in to prevent it from drying out The following guidelines should be followed when using a pH probe m The probe can be immersed in the sample solution for short periods a few hours m The probe can be immersed in tap water for the up to a day Do not use de ionised water as it will destroy the charge equilibrium of the glass electrode MPT 2 Autotitrator Page 5 3 Chapter 5 Page 5 4 Maintenance m For long periods more than a day the probe should be immersed in either a dilute acid solution pH 2 to pH 4 or an acidic buffer such as pH 4 Mm If the electrode is not being used for a period of say mo
38. he 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 Measurement sequence Note 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 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 1 With the sample container and the cell inserted Start is pressed The cell is first checked to identify the cell type fitted and that it agrees with that selected in the SOP Once identified the measurement sequence continues automati cally The pump and stirrer will be set to the values requested in the SOP and the pH value will be read 2 The titration will now start at the value specified with in the SOP This will either be the Start value or at current value 3 If Start at current value was selected the system will immediately go into performing a measurement If this was not selected the unit will add titrants to the sample to bring it to the start value specified 4
39. he titrant tubes 3 13 Problems 5 7 Progress bar 3 15 Pump 2 2 3 2 3 7 4 7 Pump head 3 7 5 10 Pump settings 3 12 Pump speed 4 12 Purge connector 3 9 Purge tube 3 8 MAN 0318 MPT e Autotitrator Index R Rear panel 1 4 3 2 3 10 Recirculate between repeat measurements 4 12 Record view 4 19 Remote support 1 4 Reports 4 19 S Sample Cell SOP 4 10 Sample Dispersant SOP 4 10 Sample General options SOP 4 10 Sample Material SOP 4 10 Sample Temperature SOP 4 10 Sample SOP 4 10 Sample buffering 4 5 Sample concentration 4 15 Sample container 2 2 3 3 Sample exit tubes 3 5 Sample in connector 3 9 Sample out connector 3 9 Sample preparation 4 5 Sample return tubes 3 5 Sample to pump 3 9 Sample tubing 3 8 Sample tubing cleaning 3 12 Sample volume 4 13 Sequence 4 15 Serial number 1 4 Service engineer 1 2 Settings Pump and Stirrer 3 12 Setup 4 1 4 2 Site requirements 1 2 A 2 Size flow cell 2 2 Size measurement Advanced SOP 4 11 Size measurement Data processing SOP 4 11 Size measurement SOP 4 10 Size measurements connecting the cell 4 6 Sizing flowcell 4 6 Soaking solution 5 3 Solenoid valves 3 6 SOP 1 2 2 2 SOP dialogues Measurement type 4 8 Sample 4 10 Sample Cell 4 10 Sample Dispersant 4 10 Sample General options 4 10 Sample Material 4 10 Sample Temperature 4 10 Size measurement 4 10 Size measurement Advanced 4 11 Size measurement Data processin
40. icle characterisation solu tions that Malvern can provide MAN 0318 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 pH Dilution or Additive This allows the effect of adding these titrants on the measurement to be investi gated How does it do it A schematic of the Titrator system is shown below ill 6826 MPT 2 Autotitrator Page 2 1 Chapter 2 Overview The heart of the Titrator is the dispenser unit The sample to be measured is placed in a disposable sample container The dispenser unit has an internal pump that circulates the sample through the cell in the optical unit A size flow cell will be required if size measurements are to be made The dispenser unit has three titrant containers that can be filled with either an acid base or some other additive The titrants used can be different concentrations of the same acid or base This will improve the accuracy of obtaining a target pH or concentration and limit the quantity of titrant used The syringe system can deliver a precise quantity of titrant from one of the titrant containers into the sample container The software can be set up so that measurements are made under a number of sam ple conditions The sample is stirred using the
41. ill make the measurement save the results print a report and display the results on the computer Cleaning This is the process whereby the sample and titrants if necessary within the system are flushed out leaving the tubing clean and ready for the next measurement As can be seen if a routine measurement is being made then the setup stage can be omitted In this case making a measurement is a very quick and easy procedure Note This chapter will assume that a standard sample container will always be used unless otherwise stated MPT e Autotitrator Page 4 1 Chapter 4 Making measurements using the Titrator Setup Some setup procedures will have to be performed daily while others will only have to be performed at much longer intervals Typically setup involves one or more of the following m Filling the titrant containers Only required when the containers are nearly empty m Priming the titrant syringe pumps and tubes Usually done at the begin ning of the day or at the start of a new session m Calibrating the pH probe Usually performed before each titration session Caution A 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 For most applications al
42. iner 3 4 LED indicators 3 7 Magnetic stirrer 3 4 Mains supply voltage A 1 Maintaining the pH probe 5 1 Maintenance 5 1 Maintenance schedule 5 9 Making a measurement 4 4 Making measurements 4 1 Malvern personnel 1 2 Malvern Website 1 4 Manifold assembly 3 6 Manual control dialogue 2 2 3 11 4 3 4 7 Manual functions of the software 3 11 Manual measurement 2 3 Materials list B 1 Materials Safety Data Sheets 4 2 Measure Manual 2 3 Measurement 4 1 Measurement display 2 3 4 17 Measurement sequence 4 18 Measurement type SOP 4 8 Menu commands 1 3 Model number 1 4 Modifying an SOP 4 1 N Naming convention 1 3 Nitrogen purge 3 9 A 2 Note on titrant concentration 4 3 Pace ii MPT e Autotitrator O On off switch 3 10 On line help 1 4 Operating temperature A 1 Operator 1 2 O ring 5 7 Oxygen absorption 3 9 P Part number 1 1 pH buffers 5 4 5 6 5 10 pH calibration 3 4 3 11 3 14 5 2 5 4 5 5 5 9 pH concentration 4 15 pH monitor 3 11 pH monitor tab 3 14 pH point from calibration 3 15 pH probe 2 2 3 2 3 4 3 10 5 2 5 4 5 9 pH probe maintenance 5 2 pH probe output from calibration mV 3 15 pH titration 4 8 4 10 Pinch valve 2 2 4 5 Pollution degree A 1 Power input 3 10 Power rating A 1 Power supply A 1 Precision 4 16 Predicted 4 13 Predicted volume 4 13 4 16 Preparation before first use 5 3 Preparing the sample 4 5 Prime 3 11 Prime tab 3 13 Priming 4 2 4 3 5 9 Priming t
43. ing the Start button on the Measurement display Manual measurement pH Titration Example titration Oe p p Pi Stop 2 Help 5 ll Zeta Potential Intensity vs pH Multi view C Log sheet Expert advice Zeta Potential Intensity vs pH Zeta Potential mV Zeta Potential m Average Zeta potential mY Intensity keps Average Intensity keps COCCCOCCCO T 25 0 C Pos 0 00mm Attn 0 pH 6 0 The features of the measurement display are described in Chapter 4 MPT 2 Autotitrator Page 2 3 Chapter 2 Overview Page 2 4 MAN 0318 Identifying the features of the Titrator This chapter s aim is to help identify both the physical and software features of the Titrator Use it as a reference guide where an explanation of all the features will be found whether it is an LED indicator or a check box within the software This chapter is divided into two sections The first section will examine the features of the dispenser unit in more detail while the second section will look at the fea tures of the software in detail Features of the Dispenser The illustration below identifies the main features of the dispenser note that some of the tubing and cables are not shown in their final positions for clarity ill 6830 MPT 2 Autotitrator Page 3 1 Chapter 3 Identifying the features of the Titrator Dispersion head The Dispersion head can be thought o
44. inimum and 25ml maxi mum When the magnetic stirrer is used a minimum of 8ml is necessary for pH titrations and 5ml for all others Filter This option should be enabled when running the Titrator with a filter fitted This is to ensure correct operation of the pump With the Filter is fitted checkbox ena bled the pump reverse action is disabled to avoid dislodging particles from the fil ter Extra pressure from reverse pumping when the filter is attached may create leaks within the system Predicted volume On the left of the Titrants dialogue a display is shown indicating how full the sam ple container will get This display estimates the predicted total volume that will eventually end up in the sample container initial sample volume plus all the titrant additions to ensure that the container does not overflow and is full enough to cover the dispense tubes 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 The maximum volume of the standard sample containers supplied by Malvern is 25ml No risk The display will show green if the predicted volume is within the range 5 to 15ml Low risk The display will show amber if the predicted volume is greater than 15ml High risk The display will show red if the predicted volume is greater than 20ml Note The predicted volume is onl
45. intaining the pH probe LL 5 2 Replacing the dispensing syringes and O riN ee 5 7 Changing the filter and tubing iL 5 8 Maintenance schedule naasa sananen aaa 5 9 User consumables and spares 0 cece es 5 10 Part 2 Appendices Specification and Site Requirements Specifications risi an a oie Meats ala wie ee at ae GN Sle A 1 Site requirements LL A 2 Chemical compatibility Materials list aaau uaaa ee ee eee eee eee eens B 1 Installation Installation eek evens Lee ices Ba eee a neh see a ak hed OS alg eee C 1 Regulatory statements CE Declaration of Conformity 0 es D 1 FCC Notice US Only octets ce there ea ee ware aoe aan eee D 2 Canadian Regulatory Information Canada Only 2 000 eee eee D 3 VCCI acceptance Japan only LL D 3 Pace ii MAN 0318 Part 1 Operators Guide Introduction to this manual Note This manual must be read in conjunction with the main Zetasizer Nano manual This manual covers the operation and maintenance of the MPT 2 multi purpose titrator Instrument Part number MPT 2 multi purpose titrator ZEN1001 This manual can be thought of as a stand alone manual that covers the operation and maintenance of the MPT 2 The aim of this manual is to m Identify what the accessory is m Explain in simple terms how it works m Identify the physical features of the accessory m Explain how the accessory should be used to make a meas
46. ion Zeta Potential and Intensity Additive gt Size and Zeta Potential Additive Log Conductivity gt Intensity Only There are four types of titration available For each type Size Zeta potential or Intensity measurements can be performed The types of titration available are Dilution The Dilution titration is used to monitor either sample Size or Zeta potential parameters as a function of sample concentration Additive log titration Conductivity This titration is used to monitor the conductivity of a sample by adding salts Results are shown as a function of conductivity MPT 2 Autotitrator Page 4 9 Chapter 4 Page 4 10 Making measurements using the Titrator Additive linear titration Concentration This titration is used monitor the effects of formulation additives on the Size and Zeta potential of the sample Results are shown as a function of concentration pH This is a standard pH titration used to monitor solution properties or sample size as a function of sample pH During a Zeta potential pH titration the Isoelectric point can be determined Sample See the description in the Zetasizer Nano manual Sample Material See the description in the Zetasizer Nano manual Sample Dispersant See the description in the Zetasizer Nano manual Sample General options This dialogue includes information from both the Size or Zeta Sample General options dialogues See description in the Zetasiz
47. l that is required is to check that there is enough titrant in the containers and re fill if necessary Alternatively if different titrants are continually being used one of the titrant con tainers may need to be changed prior to the measurement Always consult the Materials Safety Data Sheets for any titrant being used for infor mation on safe handling Changing and Re filling the containers The titrant containers will hold up to 25ml of titrant When the level reaches approximately 5ml it is recommended to re fill the container To refill m Remove the titrant container by lifting the container cover up and sliding out the container MB Dispose of the remainder of the titrant and rinse the container Mm Prepare 25ml of titrant to the correct concentration see A note on titrant concentration later in this section m Add the titrant to the container Page 4 e MAN 0318 Making measurements using the Titrator Chapter 4 MW Re fit the container Lift the container cover up and slide the container in to the empty holder position Close the cover ensuring all containers are fitted correctly into the cover MW Prime the titrant tubing using the Manual control dialogue Note If changing the titrant type used it is important to clean the tubing and containers if re using Refer to Chapter 3 the Manual control dia logue and its operation for details Also change the titrant settings in the SOP as appropriate for the
48. lass A digital device The device complies with part 15 of the FCC Rules Operation is subject to the following two conditions 1 This device may not cause harmful interference and 2 this device must accept any interference received including interference that may cause undesired operation Note Q This equipment has been tested and found to comply with the limits for a Class A digital device pursuant to part 15 of the FCC rules These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment This equipment generates uses and can radiate radio frequency energy and if not installed and used in accordance with the instruction manual may cause harmful interference to radio communications Operation of this equipment in a residential area is likely to cause harmful interference in which case the user will be required to correct the interference at his own expense Note Changes or modifications not expressly approved by Malvern Instruments Limited could void the user s authority to operate the equipment Page D 2 MAN 0318 Regulatory statements Appendix D Canadian Regulatory Information Canada Only This digital apparatus does not exceed the Class A limits for radio noise emissions from digital apparatus set out in the Radio Interference Regulations of the Canadian Department of Communications Note that Canadian Department of
49. n Page C 2 MAN 0318 Regulatory statements CE Declaration of Conformity The CE badge on this product signifies conformance to European Commission Directives CE Declaration of Conformity Supplier details Name NAME OF MANUFACTURER English company number REGISTERED Malvern Instruments Limited 1020602 Address ADDRESS OF MANUFACTURER Enigma Business Park Grovewood Road Malvern Worcestershire WR14 1XZ UK Product details Product description name and model Name MPT 2 Model ZEN1001 Description Multi Purpose Titrator Directive s and Standard s to which conformity is declared EMC directive 89 336 EEC as amended by 92 31 EEC and 93 68 EEC Low Voltage Directive 73 23 EEC as amended by 93 68 EEC EN 61326 1997 BS EN 61010 2001 Declaration hereby declare that the product specified conforms Signature of managing director Date with the provisions of Council Directive s and standard s listed above o Alan Bragginton PRINT NAME ill 6939 MPT 2 Autotitrator Page D 1 Appendix D Regulatory statements FCC Notice US only The Federal Communications Commission FCC mark on this product signifies conformance to FCC regulations relating to Radio Frequency Devices These have been satisfied by testing the product against and being found to be compliant with FCC CFR 47 Part 15 March 2003 C
50. n measurement Note When titrating over certain pH ranges the program may prompt for a sec ond more dilute titrant to be used Dispenser Automatic Manual Select Automatic to let the software control the pump and stirrer speeds or spec ify an appropriate speed for the sample using Manual Pump speed Sets the speed of the pump that recirculates the sample through the flow cell For normal operation this will generally be between 30 and 80 Stirrer speed Sets the stirrer speed Care should be taken not to introduce bubbles into the meas urements by setting the stirrer speed too high Recirculate between repeat measurements If more than one measurement is being made at one titration point then this check box gives the option of either making all measurements on the sample within the cell or recirculating the sample between measurements This option is selectable for Size measurements but is always on when performing pH vs Zeta potential measurements This is to prevent the pH reading from being affected when the Zeta voltage field is applied MAN 0318 Making measurements using the Titrator Chapter 4 Sample volume This is used to inform the software how much sample is initially added to the sam ple container The more accurately this volume is specified the more precise the titration will be The initial start volume will vary according to the titration type being performed generally this will be between 3ml m
51. n of the first pH point is complete the pH point will show a alongside 7 Remove the probe from the first pH buffer rinse with deionised water and dab dry 8 Continue the calibration until all required pH points have been calibrated During the calibration a progress bar at the bottom of the dialogue indicates how far the calibration routine has proceeded The ticks or crosses alongside the pH probe indicate the following x A pH point has been chosen but not yet calibrated A A pH point has been chosen and been calibrated Calibration points selected during a previous calibration which have not been calibrated during the current session If required select these points wv and perform the calibration process as described A tick will appear once it is complete Points can be deleted by selecting the point and pressing Remove Choosing the buffers when calibrating The default buffers for calibrating are pH 4 and pH 9 Other values may be used but ensure that the lowest and highest values are at least 3 pH values apart Also if all titration measurements tend to be in the lower end of the pH table it is advisable to use pH 2 and pH 5 buffers to calibrate the probe Adding a pH buffer point To use a different pH value a new pH buffer point must be added to the selection list Press Add to display the Calibration point dialogue then perform either of the below actions 1 Selecta defined pH point from the Calibration
52. nformation for that record Records iew Record Type Sample Name Coffeemate When a Titration result is selected in the Records view all individual associated measurements will be selected too These correspond to the number of titration points measured during the complete titration For example if a Zeta titration measurement used 16 titration points then 16 Zeta measurements records will be shown directly underneath the prime titration record The standard report for titration measurements is shown below The particular graph displayed is a pH v Zeta potential plot MPT 2 Autotitrator Page 4 19 Chapter 4 Making measurements using the Titrator D Titration Type Sample Name SOP Name File Name Record Number pH Titration Autotitration M Coffeemate Manual measurement settings Example results 2 dts 6 Measurement Date and Time Measurement Type s Zeta 24 June 2004 17 03 34 2 Cell Description Green disposable zeta cell Type Name Concentration M o Bottle 1 Acid 0 0250 Bottle 2 Acid 0 250 Bottle 3 Not used 0 00 IEP s in pH Total Injected Volume mL 0 208 Isoelectric Titration Graph 4 22 30 pH 4 22 20 ho 10 Sag Bo dundee SA 5 10 Th 5 5 20 ha k 30 ae r 40 i 3 4 5 6 7 pH Zeta Potential Coffeemate 4 Weighted Mean Zeta Potential Coffeemate s Isoelectric Point Cofteemate ill
53. ns 10 of nominal voltage Page A 1 A Appendix A Specification and Site Requirements Site requirements Note These requirements should be read in conjunction with the system requirements as stated in the Zetasizer Nano user manual Nitrogen purge specification Warning A A Nitrogen supply must be used in a well ventilated environment Turn off the supply when not in use Ifa nitrogen supply is required then it must conform to the following specifications and flow rate conditions MW It is important that the nitrogen supply is dry free from oil and filtered to remove any contaminants that could affect the sample being measured m The flow rate should be adjustable between 2 and 20ml min Page A 2 MAN 0318 Chemical compatibility The sample flow path in the titrator 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 titrant used is chemically compatible with the materials that they will come into contact with within the accessory This appendix lists all materials that comes into contact with the sample and titrants in the normal operation of the accessory Materials list Component Materials Sample titrant containers 25ml Polypropylene Sample titrant containers 125ml Polypropylene Sample container mount i e dispersion head Polypropylene Titrant container mount
54. oxygen that may change the pH char acteristics of the sample i e cause a pH drift Though the amount of pH drift is dependent upon the alkalinity of the sample even for a sample with a low alkalinity this drift will be noticeable The need to eliminate this drift is therefore of particu lar importance when performing protein charge titrations pH drift during this operation will lead to extended titration times The amount of Nitrogen needed to prevent oxygen absorption should be just enough to cover the immediate space above the sample The Nitrogen can be intro duced into the container by blanketing the area directly above the sample or by bubbling the nitrogen through the sample If too much nitrogen is introduced or the flow rate is too high there is a risk of bubbles being generated in the sample MPT 2 Autotitrator Page 3 9 Chapter 3 Identifying the features of the Titrator Rear panel The illustration below identifies the main features of the rear panel ill 6828 pH probe connection The pH probe is connected to the pH probe connection on the rear of the titrator The pH probe connectors must be clean and dry at all times Contaminated con nectors may affect the performance of the probe On off switch The power on off switch for the titrator Power input Power input socket for the titrator The external power supply is plugged here Communications connector Connects to the RS232 port on the Ze
55. probe 1 The performance of the pH probe will be severely affected if it is allowed to dry out even for short periods 2 The pH probe should be calibrated at regular intervals 3 The probe should be cleaned regularly If the probe responds slowly a message to clean the electrode will be given This electrode operates over a range of pH 1 to pH 14 and temperature range of 0 to 70 C though it is recommended that the titrations are performed at ambient temperature conditions i e by setting the measurement temperature to equal the ambient temperature Page 5 2 MAN 0318 Maintenance Chapter 5 This is for two reasons 1 The pH Probe is not temperature compensated so the sample in the container must be the same temperature as the cell 2 At higher temperatures the operating life of the pH probe will be greatly reduced Preparation before first use 1 Remove the screw end cap and connect to the cable supplied 2 Remove the membrane protection teat This teat contains a small amount of saturated KCI solution 3 8M 3 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 4 Check that the reference electrolyte is about 1cm below the level of the open ing Top up with the electrolyte supplied if necessary 5 Check that there are no air bubbles within the inner glass membrane Bubbles may be removed by shaking t
56. probe tip It is advisable to allow the probe to soak in the bl E 4 seconds before measuring Calibration Point Ensure a stirrer flea is placed in the buffer and ti pulled out Calibration pH TE v When ready press the measure button to begin d Custom Buffer 7 J PH Probe Output from calibration mY pH point from calibration MAN 0318 Identifying the features of the Titrator Chapter 3 It is important that the pH probe is correctly calibrated on a regular basis If the probe is not calibrated then the points of the measurement may be incorrect 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 Calibration points can added or removed using the respective buttons Adding a pH point will display the Calibration point dialogue input a pH point and press Ok to add it to the calibration points list Calibration is then simply selecting the pH buffer points to use and pressing the Measure button Guidance instructions on performing the calibration will appear on the dialogue A progress bar shows how far the calibration routine has proceeded A tick w is displayed once a pH point has calibra
57. ration Points PH Buffer Points Buffer Preparation Clean the pH probe then position the buffer to cover at least 2 cm of the probe tip It is advisable to allow the probe to soak in the bi Cali seconds before measuring Ensure a stirrer flea is placed in the buffer and tl pulled out Calibration pH When ready press the measure button to begin bration Point Custom Buffer 7 pH Probe Output from calibration mY PH point from calibration 3 Select the first calibration point press the Add button and enter the calibration pH required Press OK This point will now be added to the calibration point list MPT 2 Autotitrator Page 5 5 Chapter 5 Page 5 6 Maintenance 4 Repeat the above for all the required calibration points i e pH 4 7 and 9 The chosen pH points will show an X alongside Default pH points will be pH 4 and pH 9 as these are the buffers originally supplied with the pH probe See Choosing the buffers when calibrating later in this section for advice on adding and selecting buffers 5 Select the first pH point and place the pH probe into the matching pH buffer wait for the pH probe output mV value to stabilise and press the Measure button The software will then check that the pH reading is stable before con tinuing After a pH calibration has finished pH probe output mV will change to pH probe output from calibration mV 6 When the calibratio
58. re than a week then it is advisable to protect the glass membrane by replacing the protective rubber teat containing a small quantity of the electrolyte solution It is best to squeeze the end of the teat first to make it easier to slide on and also to prevent electro lyte being forced back into the probe If the probe has become dry then it may be possible to recover the performance by soaking the probe overnight in a solution of 0 1M hydrochloric acid However the performance may never fully recover and there may be no alternative except to replace the pH probe Cleaning the pH probe The probe should be periodically cleaned The calibration procedure detailed below will indicate whether the probe requires cleaning Chemical cleaning is usually sufficient To chemically clean soak the probe over night in a solution of 0 1M hydrochloric acid then use a soft tissue soaked in iso propanol and wipe over the end of the probe Once cleaned re calibrate the probe to see if its performance has recovered Some probes have a PTFE wick which is fibrous This is more easily wetted than the ceramic junction but can become clogged by very fine particles in the disper sion When this happens the pH probe will not respond to pH changes in the sample Carefully brushing this wick can recover performance This effect is reduced by using more dilute samples Calibrating the pH probe The performance of the titrator relies on the pH probe b
59. red height m Tighten the clamping screw to secure the tubing to be clamped in position MAN 0318 Identifying the features of the Titrator Chapter 3 Note The clamping ring can be used for securing both thin and thick tubing diameters in place Thick tubing 1 8 is supplied as standard for connect ing the sample flow in and out of the sample container Titrant tubes The titrant tubes are fed directly from the manifold to the sample container Sample in connector from Zetasizer The sample that has been measured is re circulated to the sample container via this connector Sample out connector to Zetasizer The sample to be measured is recirculated through this connector to the cell in the optical unit For biological samples a syringe filter of minimum size 0 22um can be placed on the exit of this connection to filter oversized particles This filter should be replaced regularly to maintain optimum filtration Sample to pump This connection feeds the sample from the sample container to the pump before passing to the sample out connector Purge connector Warning Ifa Nitrogen supply is used the system must be located in a well ventilated environment Turn off the supply when not in use See Appendix B for a requirement specification for the Nitrogen supply The purge connection is provided to enable connection of a Nitrogen purge sup ply This is used to prevent any absorption of
60. ring meas urement The sample must therefore be allowed to equilibrate to a stable value before measurement This is achieved by selecting a Precision tolerance value This value will allow a balance to be made between performing a slow titration and obtaining points close to the requested value low tolerance values or a faster titration where the points are slightly different to those selected higher tolerance values Predicted volume Please see description under Titrants SOP dialogue Titration Instructions See the description in the Zetasizer Nano manual Titration Reports See the description in the Zetasizer Nano manual Titration Export See the description in the Zetasizer Nano manual Starting a Titration SOP measurement The system is now ready to start the actual measurement To start an SOP measurement select Measure Start SOP The Open SOP dia logue will appear Select the SOP that will be used and select Open If an SOP has not been specified for the sample create one as described in the previous section The titration measurement will then follow the measurement sequence as detailed in the Zetasizer Nano manual m Any necessary pre measurement instructions will appear MAN 0318 Making measurements using the Titrator Chapter 4 m This may be followed by a Labels dialogue allowing the measurement to be named and any other information about the measurement to be entered Select the OK button
61. rrer 50 Calibrated pH 6 59 M Enable stirrer MPT 2 Manual Control 2 Cycles 1 Clean Prime Fill pH Monitor Settings MPT 2 Manual Control x Reverse Forwards Clean Prime Fill pH Monitor Pump Y 80 Titrants a pi Stirrer V 50 Enable stirrer e a0 OK Cancel Help Ok Cancel Help MPT 2 Autotitrator Page 3 11 Chapter 3 Page 3 le Identifying the features of the Titrator 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 Clean tab This tab enables the sample tubing and cell to be flushed and cleaned Note Choose an appropriate cleaning fluid for the sample or titrants being used e g deionised water Ensure that it will reliably clean the sample or titrants used from the tubing gt To clean the sample tubing 1 Remove the sample container and replace with one full of cleaning fluid 2 Press the Clean button to begin the operation 3 The pump will circulate the cleaning fluid through the sample tubing until the Clean button is pressed a second time Use the pump and stirrer controls below to adjust the pump and stirrer speeds during the cleaning 4 Perform the clean a few times to ensure the sample tubing is properly cleaned i e stop the clean operation refresh the cleaning fluid and repeat
62. s in the software are referred to in the form main menu menu item As an example the command File New SOP refers to selecting the New SOP item in the File menu Menu commands are always shown in bold text Where to get help Other manuals Several manuals may be supplied with the system with each one giving informa tion on a different aspect of the system Below is a list of the typical manuals sup plied with the system detailing the information that each manual will contain MPT 2 Autotitrator user manual this manual This manual can be thought of as a basic tutorial It will act as a guide for all opera tions of the titrator Zetasizer Nano series user manual Covers all aspects of the main optical unit i e health and safety issues unpacking instructions system checkouts identification of features and maintenance and Zetasizer Nano application software This manual also covers all aspects of making Size Zeta and Molecular weight measurements from sample preparation to inter preting the results MPT 2 Autotitrator Page 1 3 Chapter 1 Page 1 4 Introduction to this manual The health and safety section in this manual also applies to the Autotitrator On line help The primary function of the on line help is used to give detailed information on the software Each dialogue of the titrator software has Help buttons that when pressed will give help specific to that dialogue All information can be accessed from
63. s the reverse of the above procedure 1 2 Push the o ring into the recess on the manifold Slide the syringe mount up checking that the syringes smoothly enter the manifold assembly ensure the syringe does not bend severely Prime the system once all the syringes have been replaced Changing the filter and tubing The filter removes all particles above the grading size of the filter fitted To main tain optimum filtration it is recommended it should be replaced regularly Replace ment of the filter and any tubing on the titrator is performed using very similar techniques Generally all internal tubing is connected with the screw fit connections and all external tubing and filters use a Luer style The diagram below shows how the MAN 0318 Maintenance connections are made Some conne same Chapter 5 ctions differ slightly but the principle is the To replace the tubing on the Sizing flowcell simply pull the used silicone tubing off the harder PTFE tube and repla ce with new tubing Connect the tubing at the tubing connection bracket as shown below Aa lt lt gt ee Screw fit connection bo Bam d E lt lt Luer connection ill 6836 Maintenance schedule The following maintenance schedule should be followed to ensure the accessory continues to correctly function Procedure Priming the system Period Every morning or at the beginning of a ne
64. t obtain the titrant from the container and then ascend to deliver the titrant to the sample container this is done in conjunction with the manifold assembly and solenoid valves described below Manifold assembly and solenoid valves The manifold assembly and solenoid valves control the flow of sample through the cell 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 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 3 6 MAN 0318 Identifying the features of the Titrator Chapter 3 To sample container From titrant containers l t Syringes ill 6833 Titrant containers The titrant containers contain the solutions that will be added to the sample during a titration measurement sequence Each container can hold either acid base salt or an additive The tubing connectors from the top of the titrant containers are colour coded at the manifold to match LED indicators below and the colours in the Titrants SOP dialogue How to fill change and insert the titrant containers is described in Chapter 4
65. tasizer Nano series instruments to allow the software to control the titrator Stirrer connector Connection for the magnetic stirrer Page 3 10 MAN 0318 Identifying the features of the Titrator Chapter 3 Manual functions of the software The software can be separated into two distinct areas m Sample measurement controls used when performing Manual and SOP meas urements m Pre or post measurement functions using the Manual control and pH cali bration dialogues The remaining sections in this chapter explain the features of the Manual control dialogue and how they relate to the operation of the titrator The next chapter Making measurements using the titrator details how to make an SOP meas urement including identification of the SOP selections The Manual control dialogue and its operation The Manual control dialogue is used to clean and prepare the unit prior to a measurement This includes setup instructions such as priming cleaning and cali brating the pH probe The Manual control dialogue is displayed by selecting Tools Instrument MPT 2 Titrator Manual control within the Zetasizer Nano software or by selecting the Manual control icon The different tabs Clean Fill Prime and pH monitor and their functions are described below MPT 2 Manual Control Clean Prime Fill pH Monitor MPT 2 Manual Control Settings Clean Prime Fill pH Monitor Reverse Forwards Pump 40 Sti
66. ted 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 If it does not then the probe is either not immersed sufficiently in the pH solution or the probe is broken or disconnected While a pH calibration is being performed pH probe output from calibration mV will change to pH probe output mV and pH point from calibration will change to Estimated pH The complete calibration routine is described in Chapter 5 MPT 2 Autotitrator Page 3 15 Chapter 3 Identifying the features of the Titrator Page 3 16 MAN 0318 Making measurements using the Titrator Introduction This chapter covers the basic operations of the titrator that enable measurements to be made There are three basic steps involved Setup This includes system setup procedures such as filling the titrant con tainers Additionally setup may include priming the system or specifying a new SOP see Creating modifying an SOP in the Zetasizer Nano user man ual and calibrating the pH probe Measurement This involves connecting the cell preparing the sample con tainer selecting the SOP to be used entering sample details and then starting the measurement Typically dependent on how the SOP is set up the system w
67. the Titrator Chapter 4 Connecting the tubing to the Titrator The connections used on the Autotitrator are of the Luer lock variety The dia gram below shows how to connect the tubing from the cells mentioned above to the tubing connection bracket Similar connections are used throughout the unit the connections may differ slightly but the connection principle is the same Sample out to Zetasizer 2 a Sample in from Zetasizer ill 6869 Ifa filter is used attach this to the sample out To Zetasizer connection in the same manner as the direct tubing is done then connect the tubing to it Filling the cell gt With the cell tubing connected and the sample container prepared and mounted onto the dispersion head all that is left to do before configuring the SOP and start ing the measurement is to fill the cell The cell must be filled so that no bubbles are left within the sample path this is especially important for Zeta potential measurements To fill the cell 1 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 2 Select the Fill tab 3 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 4 The pump will circulate the sample through the sample tubing and cell until the number of cycles
68. to be attached correctly between the cell used and the titrator unit itself How the tubing is connected to the cell is dependent upon the cell and the measurement being performed Connecting the tubing to the cell Follow the instructions below for connecting the cell For each cell minimise the tubing within the cell area before inserting into the pinch valve channel Zeta potential measurements The tubing is attached to the folded capillary cell DTS1060 using Luer lock con nectors With a half turn these secure to the Luer fittings on the top of the cell do not overtighten The tubing is then inserted into the pinch valve channel push both tubes down into the pinch valve on the side of the cell area 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 Addendum 0075 10 Page 1 ill 8420 Note Oo 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 Size measurements The tubing is attached to the sizing flowcell ZEN0023 using threaded inserts As with the folded capillary cell above push both tubes down into the pinch valve on the side of the
69. urement m Identify the user maintenance procedures It is important that the main Zetasizer Nano manual is read before starting the first measurement Topics covered in this manual include m Health and safety information Information is given on laser safety electrical temperature and sample handling warnings The information detailed here is also applicable for the MPT 2 Autotitrator Note Further health and safety information is given on the Titrator back panel and underneath the accessory MPT 2 Autotitrator Page 1 1 Chapter 1 Introduction to this manual Mm Site requirements This details what services are necessary for connection of the Zetasizer Nano system Again the information detailed here also applies to the MPT 2 Autotitrator m What are the Zetasizer Nano instruments what are the components of the Zetasizer Nano and what do they do instructions on using the instrument and the software basic measurement and maintenance procedures m Sample preparation for each measurement type m Use of Standard Operating Procedures SOPs organising the measurement files and discussion on each of the analysis theories used m Customising reports and exporting results Warning A Use of the system in a manner not specified by Malvern Instruments Ltd may impair the protection provided by the system Access to the Titrator Within this manual reference is made to the various people who will have access to t
70. usly clean ing any spillage MPT 2 Autotitrator Page 5 1 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 Always ensure that the accessory is completely dry before applying power Never use a solvent based solution to clean the accessory as damage to the painted surface may result Cleaning the sample path To avoid cross contamination of samples the sample flow path should always be kept scrupulously clean Always flush the sample after each measurement session refer to The Manual control dialogue and it s operations section in Chapter 3 Maintaining the pH probe The pH probe is essential to ensure good performance of the Titrator and its maintenance is of paramount importance As with any pH probe its performance will degrade over time and will eventually have to be replaced The frequency of replacement will be determined by the maintenance of the probe how frequently it is used and the types of sample being measured 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 Note three important points when using a pH
71. w measurement session pH probe calibration Preferably before each titration session pH probe cleaning Once a week or according to in house QC procedures Cleaning the covers Once a month Dispensing syringe and o ring replacement The three dispensing syringes should be replaced every 12 months pH probe replacement MPT 2 Autotitrator The pH probe should be replaced at least every 12 months Page 5 9 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 BEK0009 Maximum fill 125ml pH probe SENO0106 Inc pH4 and 9 buffer sachets Dispensing syringe pack ZEN4030 Inc 3 syringes and 3 o rings Magnetic Stirrer bar Flea ZEN4034 Peristaltic pump head ZEN4036 Inc Pump head and tubing Connectors pack ZEN4037 for all internal and external connections on the Autotitrator except pump mostly1 16 fittings Inc 4 x manifold red 2 x push on barb connections 4 x manifold green 4 x black tubing grips 4 x manifold cream 1 x Luer filter fittings 4 x plastic nuts 1x Luer caps Internal tubing pack 1 ZEN4038 for all internal connections on the Autotitrator Inc
72. will be measured The number of points to be measured will be shown alongside Increment points is used for defining the number of different sample condi tions A maximum of 30 points can be measured in a single titration Increment is not available for Additive log or Dilution titrations E Start at current pH or sample concentration Selecting this check box will override the Start value The titrator will then use the current value and equally space the titration points between this value and the end setting The Start value box now will be greyed out but will indicate the current pH or concentration value m Initial concentration For additive and dilution titrations only During a pH titration the pH probe measures the current 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 MPT 2 Autotitrator Page 4 15 Chapter 4 Page 4 16 Making measurements using the Titrator With the dilution titration the concentration specified will be that of the sample container The End concentration will be the desired concentration level required after dilution has finished the dilution being performed in the number of points steps specified Precision This area is only displayed for pH titrations The sample may have a buffering effect that will cause the pH to drift du
73. y an estimate It is least accurate for pH titra tions as buffering is difficult to estimate gt Performing dilution titrations For dilution titration ratios greater than 4 1 the Predicted volume container graphic in the dialogue will change to show that the large volume containers MPT 2 Autotitrator Page 4 13 Chapter 4 Page 4 14 Making measurements using the Titrator should be used This is due to the larger amounts of titrant that will be required to perform the dilution When using the large volume containers the displacement ring should be placed at the bottom The displacement ring will displace the small initial sample upwards within the centre of the container and towards the titrant and sample tubes This minimises the amount of sample necessary to start the dilution and ensures the magnetic stirrer is positioned correctly The sloping top of the ring guides the tubes into the centre of the container whilst also preventing any sample from resting on the top of the ring Predicted volume Io Larger container e Displacement ring ill 6940 The displacement ring will also as act as a weight to keep the container in place when resting on the magnetic stirrer A message will appear to indicate that both the sample and titrant containers used must be the large volume type Titration Sequence This dialogue enables the titration measurement details to be selected such as the num

Manual: MPT-2 Autotitrator (Man0318-3.0)

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