Manual: Surface Zeta Potential Cell (Man0483-1.0)
Contents
1. 78 0 0 50 100 150 200 250 300 350 400 450 500 Displacement um J gw T 25 0 C Pos 4 50mm Attn 7 Page 14 MAM 0483 Surface zeta potential cell ZEN1020 Once all of the specified measurements have been performed at that displacement an instruction is given to set the cell to the next measurement position This process will continue until all measurements have been made at all the positions specified in the SOP and the surface zeta potential measurement is then complete The data is stored as a parent surface zeta potential record with child records relating to the individual zeta potential measurements made at each displacement EE Records View Surface Zeta Potential Record _ Type Sample Name Measurement Date and Time T ZE Me Cond Sa B umcm Vs mS cm E m Surface Zeta 28 June 2011 14 17 10 FORTECY YNA R E T Zeta 1 125 microns 1 28 June 2011 14 17 42 25 0 76 2 5 977 142 Zeta 1 125 microns 2 28 June 2011 14 18 03 25 0 76 2 5 377 143 Zeta 1 125 microns 3 28 June 2011 14 18 09 25 0 76 2 144 Zeta 2 250 microns 4 28 June 2011 14 18 24 25 0 72 5 145 Zeta 2 250 microns 5 28 June 2011 14 18 31 25 0 725 146 Zeta 2 250 microns 6 28 June 2011 14 18 37 25 0 147 Zeta 3 375 microns 7 28 June 2011 14 19 02 25 0 148 Zeta 3 375 microns 8 28 June 2011 14 19 08 25 0 149 Zeta 3 375 microns 9 28 June 2011 14 19 15 25 0 150 Zeta 4 500 microns 10 28 June 2011 14 19 24 25 0 151 Zeta 4 500 microns2. Contacts Beryllium copper Surface Zeta Potential Cell Page 17 Surface zeta potential cell ZEN1020 Page 18 MAM 0483
3. Surface zeta potential I Show cell type to operator when SOP begins File Help Ok O RUA e Measurement type Surface Zeta Potential Instrument configuration a Sample General options Tracer Material Dispersant Temperature Cell Instructions SZP measurement Manual Number of runs 20 SZP measurements Number of measurements per displacement 3 E Delay between measurements seconds o E V Append measurement number to sample name SZP displacement Number of positions A E Size of steps 125 microns 1 4 turn nicrons 1 turn V Append position to sample name MAM 0483 Page 10 Surface zeta potential cell ZEN1020 The SZP measurement SOP window is similar to the standard zeta potential Measurement window Where appropriate please refer to the Measurement description in the Zeta potential SOPs section of the main user manual for more details on each of the measurement options SZP measurement duration The SZP Surface zeta potential measurement duration options are the same as standard measurement duration options available during normal zeta potential measurements SZP measurements The SZP measurements options define the number of repeat measurements made at each displacement away from the surface and the length of any delay between repeat measurements SZP displacement The SZP displacement options define the distances to be used during a surface ze
4. 11 28 June 2011 14 19 30 25 0 152 Zeta 4 500 microns 12 28 June 2011 14 19 37 25 0 153 Zeta 0 Q microns 13 28 June 2011 14 19 49 25 0 154 Zeta 0 0 microns 14 28 June 2011 14 20 08 25 0 155 Zeta 0 Omicrons 15 28 June 2011 14 20 13 25 0 156 Surface Zeta 28 June 2011 15 42 59 25 0 Mean 140 25 0 Std Dev A surface zeta potential report is available to view the results Select View Workspaces Surface Zeta Potential to view the appropriate workspace Editing the results Surface zeta potential results can be edited by right clicking on the record in the records view and selecting Edit result or select Edit Edit result from the main menu With the Edit result window open the Debye length model tracer material and dispersant properties can then all be changed The Surface Zeta Potential edit result option allows points to be removed from the displacement plot by left clicking on them on the displacement graph When OK is clicked a new surface zeta potential record is created containing only the child zeta potential measurements that were included in the analysis Removing the cell from the instrument Follow the procedure for removing the Dip cell from the instrument the operation is the same Surface Zeta Potential Cell Page 15 Page 16 Surface zeta potential cell ZEMN1020 Maintenance Cleaning the Surface zeta potential cell Caution A During cleaning it is vital not to let any fluid enter the top and cap
5. be made once the cell has been placed into the instrument this is done using the Count rate meter in the Zeta sizer software Surface Zeta Potential Cell Page 7 Surface zeta potential cell ZEMN1020 From the main menu select Tools Count rate meter to open the count rate meter and set the count rate meter as specified M Select the Forward scatter radio button m Under Cell type select ZEN1020 plate cell Surface zeta potential cell from the drop down list M Set the Attenuator to 11 While monitoring the count rate turn the cell cap slightly clockwise if the cell has been correctly zeroed then the count rate should fall to zero immediately as the cap is turned Note a After the fine alignment step whenever the cell height is adjusted during the experiment it is imperative that the physical position of the cell is not moved within the cell holder Any movement of the cell will result in a dif ferent zero height and this must be constant throughout a given measure ment Any alteration of the height during an experiment will reduce the quality of the data Page 8 MAM 0483 Surface zeta potential cell ZEN1020 Creating an SOP and making a measurement Once the cell has been inserted into the Zetasizer and zeroed a measurement can be made This is done using an SOP or a manual measurement in the usual manner Creating the SOP The majority of the SOP options are the same as for a standard zeta potenti
6. sample surface The electro osmotic flow at the sample surface will tend to fall off with increasing distance hence close to the surface the tracer mobility will be dominated by the electro osmotic surface flow while at distances further from the surface it will be dominated by the electrophoretic motion of the tracer itself The graph below shows a typical plot of reported zeta displacement from the sur face 20 Y 0 1087X 18 79 R2 0 997 gt E E 2 o a s o N ko oO 3 E E g 200 400 600 800 1000 1200 Displacement microns ill 8694 The zeta potential at the surface is then calculated by extrapolating the graph to zero displacement and applying the following formula Surface zeta potential intercept tracer zeta potential where the tracer zeta potential is recorded far from the wall where the electro osmotic flow can be taken as zero In the displacement graph above the blue circles represent the reported zeta potential of the tracer particles while the red squares represent the zeta potential Page 2 MAM 0483 Surface zeta potential cell ZEN1020 of the tracer particles measured far from the sample surface and also independent from any electro osmotic effects Measurement preparation Before a measurement can be performed the cell must first be loaded onto the sam ple holder and then attached to the cell The complete cell is then inserted into a standard cuve
7. to turn the cap on the top of the cell by a given amount this will set the distance to the first required displacement position This is a manual operation and the user must open the cell area lid turn the head of the cell the specified amount then close the lid again before continuing Surface Zeta Potential Cell Page 13 Surface zeta potential cell ZEm1020 PO Manual measurement no sample name Settings dl Accessory Start E pe Eject ver Reported Zeta Potential versus Displacement Ee 1 Open cell area 2 Rotate cell top counter clockwise bv 1 4 turn to 125 microns 3 Close cell area lid T 25 0 C Pos 4 50mm Attn 7 Each 1 4 turn of the cap counter clockwise corresponds to a movement or displacement of 125 microns a second 1 4 turn will correspond to a total displacement of 250 microns and so on The amount to move the cap will be indicated in the SOP and in the measurement instructions D Manual measurement no sample name kaka Em ed Settings Bl Accessory p Start Stop Eject Help Reported Zeta Potential versus Displacement Multi view Expert advice Log sheet Reported Zeta Potential versus Displacement i Conductivity 0 279 mS cm 3 Count Rate 100 0 kcps 64 Surface zeta potential 29 9 mv I Fit residual 7 06e 08 66 68 Em 5 72 5 a 2 74 o N dE
8. Surface Zeta Potential Cell ZET 11020 MANO483 Issue 1 0 September 2011 English Copyright Malvern Instruments Ltd 2011 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 www malvern com Zetasizer is a registered trademark in the UK and or other countries and is owned by Malvern Instruments Ltd Malvern and the green hills logo are registered trademarks in the UK and or other countries and is owned by Malvern Instruments Ltd Windows is a registered trademark of the Microsoft Corporation Printed in England Surface zeta potential cell UZEI ULI Introduction This document gives a brief overview of the Zetasizer Nano cell for measuring sur face zeta potential It primarily describes how to use insert and clean the cell to ensure reliable and consistent measurements The surfa
9. al measurement as described in the main user manual Other SOP options are specific to the surface zeta potential cell being used and these are described below Left click on P Measurement type and select Surface zeta potential from the drop down menu Once selected the SOP tree menu will change to match the measurement type b Measurement type Surface Zeta Potential Instrument configuration Sample General options Tracer Material Dispersant Temperature Cell Instructions SZP measurement Advanced Tracer measurement Advanced Data processing Reports Export Tracer Material Please refer to the Sample Material desc section of the main user manual Cell Size Zeta Potential Molecular Weight Flow Titration Trend gt b Surface Zeta Potential ription in the Zeta potential SOPs Please refer to the Sample Cell description in the Size SOPs section of the main user manual As the surface zeta potential cell was selected as the measurement type this cell will be the only cell choice available The Zetasizer software will configure all settings and parameters to match this cell Surface Zeta Potential Cell Page 9 Surface zeta potential cell ZEM1020 File Help Ok O Sa A O gt Measurement type Surface Zeta Potential E The default selection is the Surface zeta potential cell SZP measurement Surface zeta potential measurement Cell type ZEN1020
10. area of the cell assembly Any cross contamination of material from one measurement to the next could affect the result so it is extremely important to ensure the cell is completely clean before use Cuvettes used with the Surface zeta potential cell m Ifa quartz cuvette was used for the measurement it is recommended to clean the cuvette with Hellmanex and then rinse with copious amounts of de ion ised water prior to reusing it m Ifa plastic disposable cell was used for the measurement it is recommended that this is disposed of and a new one used for all subsequent measurements General cleaning As a complete assembly the cell can be cleaned using de ionised water or with a Hellmanex solution If Hellmanex is used the cell must be rinsed with copious amounts of de ionised water prior to reusing it More efficient cleaning can be obtained by immersing the electrode area and sam ple holder in a gentle ultrasound bath 30 Watts for 5 to 15 minutes Over time it is likely that the electrodes will become discoloured or tarnished This is expected and although it cannot be cleaned this will not affect the quality of the data obtained Intensive cleaning Cleaning can be performed as described in the following table The material and chemical compatibility of each component is detailed in the next section Component Cleaning method Cell cap Wipe clean with a mild soap solution Rinse with water once cleaned Outer
11. casing Wipe clean with a mild soap solution Sample barrel Rinse with water once cleaned Sample holder MAM 0483 Surface zeta potential cell ZEN1020 Component Cleaning method Electrodes Scrub gently with a pipecleaner and Hellmanex then scrub with copious amounts of de ionised water Once cleaned leave all parts to be fully dry before re using especially the electrode and sample holder area Chemical compatibility Components of the Zetasizer Nano that may come into contact with the sample are 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 mentioned Warning A It is advisable that the chemical compatibility is checked against the materi als identified below before inserting a sample It is also recommended that a test is performed on the material with the sample before more permanent usage is undertaken Surface zeta potential cell With proper use only the central measurement section see table for components of the surface zeta potential cell will ever come into contact with sample The outer components of the cell will only come into contact if spillage or overfilling occurs Component Materials Casing Natural PEEK Stainless steel 316 Sample barrel Natural PEEK Sample holder Natural PEEK Sample holder screw Nylon Electrodes Palladium
12. ce zeta potential cell is intended for the measurement of the zeta potential at the surface of a flat material in an aqueous environment The cell is a dip cell type device that is incompatible with the MPT 2 titrator Cell cap and adjustment screw White alignment mark Cuvette Electrical contacts Sample barrel Sample holder and screw OOS Electrodes ill 8688 The cell consists of a height adjustable sample barrel in which the sample is glued onto a sample holder and held between two palladium electrodes O A series of Zeta potential measurements are then performed in a conventional cuvette with the measurement position within the cell controlled by adjusting the height of the sample barrel The cell is supplied with a kit of parts Surface zeta potential cell with palladium electrodes a 12 well plate for storing the samples 10 PEEK sample holders a Surface Zeta Potential Cell Page 1 Surface zeta potential cell ZEm1i020 screwdriver for cell tightening a pair of forceps for sample handling a cell height alignment tool and a sample holder for gluing the sample to Measurement technique A surface zeta potential measurement consists of attaching a sample to a mount or holder that is then held in place between two electrodes The sample is then immersed in an appropriate aqueous solution containing tracer particles The apparent tracer mobility is now measured at a number of different distances from the
13. elp Gack gt KK 0 gt Measurement type Surface Zeta Potential Tracer measurement duration Instrument configuration Sample General options Tracer Material Dispersant Manual Number of runs Temperature 20 Cell Instructions E SZP measurement Advanced Number of measurements Delay between measurements seconds EWEN a measurement 3 2 0 Advanced E Data processing Reports Export Automatic Minimum runs Maximum runs 10 t 100 Tracer measurements SZP displacement Tracer measurement displacement microns 1000 SZP displacement The final stage in a surface zeta potential measurement is a fast field reversal FFR only measurement The purpose of this is to make a measurement only of the tracer mobility which will not include any electro osmotic component and this will be used in the surface zeta potential equation The Tracer measurement displacement defines the distance from the sample at which this FFR only measurement takes place The displacement is altered in 125micron increments Tracer measurement Advanced Please refer to the Measurement Material description in the Zeta potential SOPs section of the main user manual Data Processing This window allows the advanced analysis parameters to be set It is generally best to leave these set to default Size ranges and measurement thresholds can be applied to the analysis to filter spurious peaks prior to the ana
14. f the tool indicated by the white spot and tilting forward Adjust the cell cap to alter the sample barrel position until the surface of the sample is aligned with the zeroing target on the tool window ill 8691 The sample barrel position should be adjusted so that the sample surface and the centres of the two zeroing targets all line up exactly With the sample height set the cell cap also needs to be zeroed Loosen the cap screw then rotate the cell cap until the white mark on the cap is in line with the white mark on the cell body Secure the screw afterwards Surface Zeta Potential Cell Page 5 Page 6 Surface zeta potential cell ZEMN1020 Filling the cuvette and inserting the cell into the instrument Both disposable plastic and glass or quartz 10mm square cuvettes can be used with the cell Prepare an appropriate aqueous suspension containing the tracer particles Fill the cuvette with 1 2mL of the prepared aqueous suspension then insert the cell this must be done at an angle to avoid any bubbles being caught between the sample electrodes and to ensure that the sample plate is entirely submerged The level of the dispersant must be significantly above the top of the electrodes and the nylon screw that holds the sample in place Note With the procedure complete the measurement face of the cuvette some have a small triangle at the top of the cell and the white mark on the cell body must face in the same d
15. irection This is to ensure the orientation is correct when inserted into the cell holder m The cuvette must not be filled more than the recommended maximum depth of 20mm before insertion of the cell m Tilt the cuvette to a maximum angle of 45 This is to avoid spilling the dis persant m Slowly insert the cell into the cuvette until the sample holder barrel and elec trodes are covered As the cell is inserted it displaces the sample so any bub bles will be pushed out from the top of the electrode gap m Once the electrodes are covered bring the cuvette up to the vertical m Inspect the combined cell and cuvette and check for any bubbles If bubbles are present around the electrode or nylon screw gently tap the bottom of the cuvette to dislodge these If not dislodged repeat the above sequence MAM 0483 Surface zeta potential cell ZEN1020 Coloured band Triangle ill 8693 m Hold the base of the dip cell cap and the top of the cuvette simultaneously Ensure the white mark on the cell body and cuvette triangle is facing the front of the instrument and push the cell into the cell holder until it stops a stop on the surface potential cell must rest on the top of the cell holder Check that the cell is sitting flat and that the cuvette is also fully inserted and rests on the base of the cell holder Fine alignment using the Count rate meter A final fine adjustment of the zero position can
16. lysis being performed These can be setup using the Configure button Please refer to the Help file for more information MAM 0483 Surface zeta potential cell ZEN1020 ME E New SOP Surface Zeta Potential File Help Gz OA HAO Measurement type Surface Zet Plate Instrument configuration Sample General options Tracer Material Dispersant Temperature Cell mm lt a Plate Analysis Parameters Instructions SZP measurement Advanced Tracer measurement Advanced 4 Display range Lower limit Upper limit 4 Thresholds Lower threshold 150 150 0 05 5 ek Data processing Reports Export rrai Lower limit Lower display limit V Default is 150V Configure button Pressing the Configure button will display the Plate analysis parameters window which enables various attributes of the analysis model to be altered These include the measured Zeta Display range and the measurement thresholds If it is known that all particles within the sample will fall within a certain zeta potential range then the Zeta Display range can be set to improve the repeatability of the measurement result similarly a lower threshold sets the noise rejection baseline in the zeta potential distribution Performing the measurement With the cell loaded into the instrument and the SOP configured a measurement can be performed When the measurement is started a user instruction is given
17. n It should be capable of attaching to both the sample and the holder and it should not be soluble in the selected medium so that the sample is securely held in place for the duration of the experiment Inserting the Surface zeta potential cell The insertion of the Surface zeta potential cell into the Zetasizer Nano is done in three stages m First a coarse alignment is performed where the cell has to be aligned to a zero position with respect to the instrument laser this is initially done using a height alignment tool supplied with the cell m Secondly the cell is inserted into the cuvette which is then added into the instrument m Thirdly a fine alignment is performed using the count rate meter in the appli cation software Once these stages are complete a measurement can be performed Zeroing the cell height position Coarse alignment Once the sample holder is in place the surface of the sample must be aligned to a zero height position with respect to the instrument laser using the height alignment tool The surface is aligned to a zeroing target etched on the windows of the tool There are two zeroing targets one on the front plate and one on the back Hold the alignment tool so that the centre of the two targets coincide to avoid a parallax error MAM 0483 Surface zeta potential cell ZEN1020 ill 8690 Insert the cell assembly into the tool so that the white mark on the cell is facing the front o
18. ta potential measurement The Number of positions defines the number of points away from the surface where tracer mobility is to be measured The Size of steps defines the additional distance away from the surface that each measurement is made Note that 500 microns can only be chosen if the tracer measurement displacement in the tracer measurement SOP window is set to 1500 microns or greater This is to ensure that a minimum of three displacement points will be measured SZP measurement Advanced Please refer to the Measurement Material description in the Zeta potential SOPs section of the main user manual Tracer measurement The Tracer measurement SOP window is similar to the standard zeta potential Measurement window Where appropriate please refer to the Measurement description in the Zeta potential SOPs section of the main user manual for more details on each of the measurement options Tracer measurement duration The Tracer measurement duration options are the same as standard measurement duration options available during normal zeta potential measurements Tracer measurements The tracer measurements options define the number of repeat measurements that can be made at each measurement distance from the sample surface and the length of any delay between these repeat measurements Surface Zeta Potential Cell Page 11 Page 12 Surface zeta potential cell ZEMN1020 E New SOP Surface Zeta Potential Em File H
19. tte and placed into the instrument These following operations are described in the next sections once these are com plete the measurement can be performed m Loading the Surface zeta potential cell with sample M Inserting the Surface zeta potential cell into the instrument Loading the Surface zeta potential cell The surface zeta potential cell is loaded with a sample as described below Note Take care not to damage the sample surface during attachment to the sam ple holder The sample to be measured should be cut into rectangular pieces no larger than 7mm x 4mm LxW and no more than 1 5mm thick H UP FU ill 8689 Surface Zeta Potential Cell Page 3 Page 4 Surface zeta potential cell ZEMN1020 The sample is then attached to the sample holder using an appropriate adhesive such as AralditeTM refer to note overleaf for guidelines on glue selection m A sample gluing tool is provided to hold the sample holder during the gluing process Ensure the sample is placed squarely onto the sample holder and not at an angle The sample should be perpendicular to the electrodes once inserted into the bar rel There should be no large gaps between the electrodes and sample lt 200um Wait until the sample has set in place then load onto the cell using the supplied forceps and screw the holder into place Note The glue used should be selected beforehand and be compatible with the experimental desig
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