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Using the CFR Part 11 Functions

NanoPlus Operator’s Manual

F-12

Mar 2014

Viewing File History

Open the file for which you wish to view its details.

Select

Option > 21 CFR Part 11 > File History

on the Main Menu bar (or

History Tracking

at the top of the Results pane); the History Tracking dialog is displayed. This example shows
you the type of history parmeters that are shown.

Click

Print Preview

to review and print a copy of the file history.

Summary of Contents for NanoPlus

Page 1: ...NanoPlus Zeta Potential Nano Particle Analyzer Operator s Manual V5 22 P09 42801 01 March 2014...

Page 2: ...registered trademark of E I Du Pont de Nemours Company Windows is a registered trademark of Microsoft Corporation Particulate Systems 2014 All rights reserved Printed in the U S A The software describ...

Page 3: ...ng Operation 2 4 After Use 2 4 For Storage 2 4 Turning the System On and Off 2 5 Using the Software 2 6 User Operating Modes 2 6 Commands 2 6 Main Menu 2 7 Shortcut Keys 2 8 Pop up Menu 2 8 3 SOFTWARE...

Page 4: ...Settings 3 58 Data Mirroring 3 59 4 OPERATING PROCEDURES Specifying the SOP Designer Display Mode 4 1 Working with SOPs 4 1 Creating SOPs 4 1 Copying SOPs 4 2 Deleting SOPs 4 2 Renaming SOPs 4 2 Editi...

Page 5: ...G AND MAINTENANCE Troubleshooting 5 1 Maintenance 5 6 Cleaning the Analyzer 5 6 Cleaning the Cell Temperature Adjustment Block 5 6 Replacing the Fuses 5 6 Cell Maintenance 5 7 Flow Cell 5 8 Disassembl...

Page 6: ...the Cell A 14 Performing a Measurement A 16 Setting Measurement Conditions A 16 Preparing for pH Titration A 17 Reviewing pH Analysis Results A 18 Calibrating the pH Electrode A 19 Resetting Temperatu...

Page 7: ...tribution D 7 Ln G1 t Plot D 7 Size Distribution Tables D 8 Differential Size Distribution Table D 8 Cumulative Size Distribution Table D 9 AutoCorrelation ACF Function D 9 ACF Listing D 9 Normal Line...

Page 8: ...Weight Analysis E 7 Zeta Potential Determination by Electrophoretic Light Scattering E 8 Electrical Double Layer E 8 Zeta Potential E 8 Electrophoretic Light Scattering E 10 Power Spectrum for Zeta P...

Page 9: ...obat to assist you in locating information Organization This manual is organized as follows Chapter 1 GENERAL INFORMATION Provides a general description of the NanoPlus and its features and specificat...

Page 10: ...tion about the subject matter Appendix B DILUENT PHYSICAL CONSTANTS Provides a listing of diluent constants Appendix C ALPHA BETA VALUES Provides a list of and values for a select number of polymers A...

Page 11: ...les suspended in liquids in the size distribution range of 0 1 nm to 12 m with sample suspension concentrations of 0 00001 to 40 zeta potential of sample suspensions in the 200 mV to 200 mV range with...

Page 12: ...x 11H in Weight NanoPlus 22 kg 49 lbs NanoPlus AT 7 kg 15 lbs Bench Dimensions Width 90W x 60D x 90H cm 36W x 24D x 36H in Add 60 cm 24 in to width when NanoPlus AT is installed Supportable Weight 70...

Page 13: ...mperature Electric Field Open Power Arrow indicators three on each side High Temperature Illuminates when the temperature of the sample cell is elevated above ambient Electric Field Illuminates when v...

Page 14: ...front panel contains a logo which is illuminated when the instrument is turned on Rear Panel N2 Input AC USB connector N2 Used for purging the sample compartment to minimize the potential of condensat...

Page 15: ...Labels The following labels are affixed on the NanoPlus Class 1 Laser Product Label located on the rear panel Class 3B Service Laser Label located inside the sample area Class 1 Laser Label located o...

Page 16: ...nt When using this equipment pay attention to the instructions on the warning labels attached to the equipment Refer to Labels on previous page If the equipment malfunctions immediately stop operation...

Page 17: ...ograms list If your Security settings are set to Security or 21 CFR Part 11 a dialog prompting you to enter your User ID and Password is displayed After a brief initialization the opening screen of th...

Page 18: ...level This setting prevents other users from viewing SOPs and measurement data 21 CFR Part 11 A user ID and password are required upon software startup Authorized users can use electronic records and...

Page 19: ...n The commands displayed on this menu are dependent on the current operation SOP Designer and Data Acquisition commands Primarily for starting and stopping measurements Size Zeta Analysis commands For...

Page 20: ...le to change the display mode Simply press Alt D to access the Display menu then A Advanced or N Normal for the desired mode Pop up Menu Some tasks have a pop up menu when you right click making selec...

Page 21: ...er page 3 2 Data Acquisition page 3 34 Size Analysis page 3 35 Zeta Analysis page 3 46 pH Maintenance Commands page A 5 Maintenance page 3 50 Security page 3 55 Software commands are also available fr...

Page 22: ...a potential analysis An SOP lists the conditions for performing the measurement A measurement cannot proceed without an SOP assigned to it namely the Measuring SOP Zeta tab display Size tab display An...

Page 23: ...ns The SOP and Parameter panels contain options in the upper blue shaded portion of the panel to assist you with the tasks associated with that panel Some are common for all parameters while others ar...

Page 24: ...lete Parameters Add to SOP Adds the selected parameter to the current SOP SOP Listing Add to Measuring SOP Adds the selected SOP to the Measuring SOP Export SOP Displays the Export Particle or Zeta di...

Page 25: ...red text and cannot be removed The SOP will have to be removed from the Measuring SOP before you can edit a parameter Cell Parameters Cell Const Meas For Zeta Potential only Displays the Cell Constan...

Page 26: ...a change in the concentration or sample type See Detecting the Optimal Cell Position page 4 6 for additional information and instructions Conductivity Check Displays the Conductivity Measurement dialo...

Page 27: ...add or delete a diluent or mixture When you add a new diluent or new mixture appropri ate fields are shown for you to enter the properties After you have entered the applicable information the Add to...

Page 28: ...ted SOP Lists SOP parameter details Selected SOP Name Displays the file you have selected in the list Details window Common Lists default SOPs These SOPs can be copied to a new SOP added to the Measur...

Page 29: ...urity mode You can display Measurement parameters by category or alphabetically Categorically Alphabetically Select the List icon to display parameters by category and the AZ icon to display them alph...

Page 30: ...tion sec Allows you to enter a delay time for the measurement to begin You can enter up to 100 000 seconds The equilibration time starts when the run begins the measurement starts when the equilibrati...

Page 31: ...for your analyses No uses the temperature currently set in the intensity monitor Use this option when using the same temperature for all analyses Gradient allows you to analyze the same sample at diff...

Page 32: ...o enter the name You can use up to 40 characters Select the QC icon from the Size Analysis panel to access the statistical summary table Wait Time sec Enter the time in seconds to wait between repeate...

Page 33: ...es are 20 50 and 100 selected from the drop down list If the pinhole setting is set at 100 the intensity scattering strength that can be obtained is increased However the state of the coherence deteri...

Page 34: ...order autocorrelation logarithmic display G2 vs Plot Prints a second order autocorrelation function Realtime Size Monitor Prints a plot of the particle size values for each integration cycle being cal...

Page 35: ...The measurement is not started until the set temperature is reached File name The file name for storing measurement data You can enter up to 40 characters File Save Click the name to receive a drop d...

Page 36: ...ll analyses Sample information Provides a description of sample information and measurement parameters You can enter up to 40 characters Statistical Summary Select Yes to save the measurement data in...

Page 37: ...ement Maximum of 10 000 repetitions Wait Time sec Enter the time in seconds to wait between repeated measurements The range is 0 100 000 sec Others Pinhole m Sets the pinhole size The default is 50 m...

Page 38: ...n is printed on the same sheet Distribution Graph Prints a graph of the true zeta potential mobility of the particles corresponding to the speed of movement in the static layer position Peak Value Tab...

Page 39: ...Parameters Panel Categorically Alphabetically Select the List icon to display parameters by category and the AZ icon to display them alphabetically Parameter Panels are unavailable for a User assigne...

Page 40: ...up to 45 channels This is useful when a portion of the distribution is determined to be noise Right Threshold Enter the number of channels you wish to have removed on the right side of the particle s...

Page 41: ...ibution showing both differential and cumulative Refer to Intensity Distribution Graphs page D 3 for examples Ln G2 1 vs Plot Select Yes to display a second order autocorrelation function logarithmic...

Page 42: ...be used for calculating the size distribution The maximum value allowed is 2 the minimum is 1 003 max min Enter the upper max and lower min limits to be used for calculating the size distribution The...

Page 43: ...You can use up to 40 characters Conversion Equation This is used to select the equation for calculating the zeta potential from the mobility You may select Smoluchowski Huckel or Other Generally Smolu...

Page 44: ...of the particles including the electrosmo sis The 3D Graph can be viewed for mobility of the particles For more information and an example of a 3D Graph see 3D Graph page D 17 ACF Select Yes to displa...

Page 45: ...ently depending on the measurement items and types There are four types available for each cell when using the AutoTitrator two available if not Each measurement type includes specific routines and or...

Page 46: ...ell Types 2 and 4 See Detecting the Optimal Cell Position page 4 6 for additional information Cell Name Select the field to display a button to the right Click the button to display a list of register...

Page 47: ...starts the measurement after automatic detection of the optimal cell position at the time of measurement The optimal position for the cell can also be detected in advance For details see Detecting the...

Page 48: ...mber of bins into which the size data are distributed It is the size resolution the more channels the more divisions on the size scale i e X axis Select Auto if you are not sure which channel to use C...

Page 49: ...lue for the pH adjustment It ranges from 0 05 2 Additive Titration Displays when Pipetting is selected Circulation Time min Set the time for the sample to circulate around the flow cell after adding t...

Page 50: ...ore information and an example of an ACF Base graph see ACF Base page D 15 Type 2 performs center detection measures base then zeta potential Type 3 performs pH titration pipetting or circulation with...

Page 51: ...igh concentration and low conductivity cells 1 point 0 Flat surface cell 7 points 0 8 0 6 0 3 0 0 0 3 0 6 0 8 The zeta potential is measured up to five different positions to eliminate the effects of...

Page 52: ...selected pH Table The pH values can be entered from low to high or from high to low Set the pH value to be adjusted The pH range is 1 13 pH Tolerance The pH value is considered to have been completed...

Page 53: ...asurements Refer to Appendix B page B 1 for additional information on diluent constants Group Parameter Description General Comment Enables you to enter a comment about the diluent You can enter up to...

Page 54: ...lected in the Measuring SOP pane allowing you to remove the selected SOP from the Measuring SOP Allows you to re establish communication between the analyzer and computer in the event communication is...

Page 55: ...emperatures Analysis The Analysis window is the default when you select Size Analysis it contains two panels Data Select Panel manage data files Results Panel display results of an open data file Part...

Page 56: ...d in the Results panel Delete File Deletes the selected file a confirmation dialog is displayed Export File Check the file you wish to export and click Export File the Export File dialog is displayed...

Page 57: ...Displays the Import dialog Selected files populate this area each containing a check box Check the file s you wish to import Import Selected Files when dialog is populated Click this button to navigat...

Page 58: ...ipsis button to navigate to the file s After files populate the dialog select Import Selected Files This import function operates like that of the Import function explained above Column Headings Displ...

Page 59: ...rts Results and measurement conditions Recalculate All Displays the Recalculate All dialog allowing you to select the parameters you wish to recalculate Save Recalculated Data Displays the Save Recalc...

Page 60: ...nation of the options on the Print dialog Print Preview Displays the Print Preview dialog allowing you to select and review the data before printing Overlay Use this option to overlay results from mul...

Page 61: ...atistical Summary in the measurement parameters The window for the QC command also contains two panels Data Select Panel displays list of files for which statistical data were requested Results Panel...

Page 62: ...stical summary The example shown above shows 3 repetitions of the same measurement Use the scroll bar to view all statistics Details Displays details of the selected data file Use these arrows to scro...

Page 63: ...for this command contains two panels and when first opened contains no data New Displays the Gradient New Temperature Mode dialog enabling you to create a new data table Click OK after selecting measu...

Page 64: ...ed automatically Print Preview Allows you to preview before printing Overlay Click this button to overlay plots of multiple analyses An Overlay tab is added with a list of the files overlaid By defaul...

Page 65: ...r the Y axis and or add a second Y axis the Scale dialog is displayed Select Temperature Marker to show a marker on the plot of the temperature at different points of the analysis Simply click on the...

Page 66: ...iew data for analyses performed using gradient temperatures Analysis The Analysis window is the default when you select Zeta Analysis it contains two panes Data Select Pane manage data files Results P...

Page 67: ...s enabled Click Open to choose the file and populate the window The Low Conductivity Cell Analysis graph is displayed in the upper pane and the data table in the lower one Graph If the analysis contai...

Page 68: ...lose buttons function in the same manner as on other windows Temperature Gradient Analysis Select this option to view data generated for an analysis performed at gradient temperatures Refer to Tempera...

Page 69: ...Mar 2014 3 49 pH Maintenance The pH Maintenance button is added to the software commands when you have an AutoTitrator installed Refer to pH Maintenance Commands page A 5 for a description of the com...

Page 70: ...n Administrator or Supervisor to view or edit system configurations The Maintenance panel does not display for other user levels when in Security mode The left pane of the Maintenance panel contains t...

Page 71: ...Constants Cell OffsetX Cell OffsetZ Displays current offset values for the cell block X and Y axes These values are set at the factory and should be edited only with the direction of a service repres...

Page 72: ...is used when adjusting the pH of the sample during autotitration pH Sensor Temp Coefficients These values are set at the factory and are probe dependent They should be changed only if probe is replace...

Page 73: ...ls registered in the software To remove cells Highlight the desired cell and click Remove Cell the cells are removed from the folder view but not from the registered list of cells in the right pane Th...

Page 74: ...Maintenance NanoPlus Operator s Manual 3 54 Mar 2014 System Registration Information Displays the serial number the Mac address and whether or not the 21 CFR Part 11 option is enabled...

Page 75: ...Analyses Edit their SOPs Edit System Maintenance Parameters Change User Information Operator Yes No No Password only Advanced Operator Yes Yes No Password only Supervisor Yes Yes Yes Password only Adm...

Page 76: ...er Profile screen allowing a User with Administrator rights to add a user Name Enter the User s name Password Confirm Password Enter a password containing at least six alphanumeric characters then con...

Page 77: ...file screen for the selected User Administrator or for the logged in User Administrator Change the User s password permission level or the viewing of SOPs and data Logged in User Change password only...

Page 78: ...nistrator or Supervisor rights No Security Allows access for all Users No password is required to start and use the software All functions are available Security Requires a User ID and password The SO...

Page 79: ...or Supervisor rights Enable data mirroring on following location Saves the data only to the specified location Back up setting files on following location before exit Backs up setting files SOPs to th...

Page 80: ......

Page 81: ...rm a measurement Advanced mode displays all parameters Working with SOPs This section describes how to create copy and delete SOPs and how to edit SOP names Creating SOPs 1 Select your user name in th...

Page 82: ...lete the SOP You cannot recover a deleted SOP so be sure it is what you want to do before you click OK Renaming SOPs 1 Select the desired SOP in the SOP Listing 2 Click Rename from the Task options or...

Page 83: ...nel Tasks the Particle or Zeta Export File window is displayed 2 Click the Ellipsis button next to the Export File field the Save As dialog is displayed 3 Select a destination enter a name in the File...

Page 84: ...to import 2 Click the Ellipsis button next to the Import File field a file selection dialog is displayed 3 Navigate to the file location select the desired file and click Open 4 Select the files you w...

Page 85: ...bar select SOP Favorite SOP Add to Favorite SOP the SOP is added to your Favorites list automatically You can view your list or confirm that the SOP was added by selecting SOP Favorite SOP Organize F...

Page 86: ...f the concentration or sample type changes You can repeat the adjustment if the intensity monitor shows the sample concentration is too low 1 In the Cell Parameters panel click Adjust Cell Center from...

Page 87: ...the up down arrows in the Repet Times field to select the number of measurement cycles 3 From the Conductivity group select the conductivity standard you plan to use If you are using a solution other...

Page 88: ...nown 1 In the Cell Parameters panel click Conductivity Check from the Task options the Conductivity Measurement dialog is displayed 2 Click Start to start the measurement When the measurement has been...

Page 89: ...Acquisition page 3 34 for a description of the elements in this pane 2 From the Particle Size or Zeta Potential Listing pane select the SOP you wish to use in the measurement 3 Right click and select...

Page 90: ...pane a Check the Cell Parameters and Diluent Properties If performing temperature gradient analyses be sure you have selected one of the recom mended cells shown below The analysis will not proceed w...

Page 91: ...e Intensity Check screen is displayed Enter the Accum Times select Auto Scale or Manual Scale and click Start to perform the intensity measurement When the measurement is complete the Intensity Plot I...

Page 92: ...Main menu bar Start Stop buttons Use these tabs to display desired graphs tables Displays summary of measurement parameters During the measurement the screens that are selected in the Display section...

Page 93: ...lysis parameters you specified 1 To view the results for other graphs or tables use the tabs located above the Results panel The SOP settings will not be affected Print button 2 Click the Print button...

Page 94: ...nd Zeta Potential analysis Temperature Gradient analysis page 4 23 pH analysis page A 18 Size and Zeta Potential Analysis Simply click the Size Analysis or Zeta Analysis command button to access the D...

Page 95: ...Open File in the Panel Tasks analysis results are displayed in the Results panel Deleting an Analysis Data File 1 In the Data Select panel place a check mark next to the data file s you wish to delete...

Page 96: ...data file s you wish to export 2 Click Export File in the Panel Tasks the Export File window is displayed 3 Click the Ellipsis button next to the Export File the Save As dialog is displayed 4 Select...

Page 97: ...n next to the Import File field a file selection dialog is displayed 3 Navigate to the file location select the desired file and click Open A file cannot be imported if it has the same name as one alr...

Page 98: ...asks to display analysis results in the Results pane 3 Click Recalculate Condition at the bottom of the Data Select panel to display the analysis parameters that can be modified Displays details for s...

Page 99: ...saving the data You can choose Manual Input to enter the file name group name and sample information criteria Overwrite to overwrite current data Add Numbering to append a number to the current file...

Page 100: ...k next to the data files you wish to include in the overlay 2 Click Open analysis results are displayed in the Results pane 3 Click Overlay at the top of the Results pane the Overlay dialog is display...

Page 101: ...shown below For an explanation of print options refer to Print Dialog Options for Particle Size Data page 3 14 Print Dialog Options for Zeta Potential Data page 3 18 1 Open the data file s you wish to...

Page 102: ...mark next to the data file s you wish to open 3 Click Open File at the top of the Data Select Panel A list of measurement dates filenames and typical data typical values for the average particle sizes...

Page 103: ...nt Data 1 Select the Temperature Gradient Analysis icon to view data collected when you perform an analysis using gradient temperatures the Temperature Gradient Analysis window is displayed 2 Click Op...

Page 104: ...econd Axis 1 Click the Scale button at the top left of the Temperature Gradient Plot the Scale dialog is displayed 2 Select the Y2 Scale sub option and select the parameter for the axis 3 Click OK to...

Page 105: ...nts in the analysis 1 Click the Scale button at the top left of the Temperature Gradient Plot the Scale dialog is displayed 2 Select the Temperature Marker option 3 Click OK to return to the Temperatu...

Page 106: ...New at the top of the Gradient Temperature Plot window the Select Temperature Gradient Mode dialog is displayed 2 Select the measurement method and click OK a new table and tab are added to the Edit...

Page 107: ...to use in the overlay 2 Click Overlay on the button bar an Overlay tab is added containing the name of the files in the overlay All open files are included by default Plots display in colors with a le...

Page 108: ...bar to discard entries and leave the dialog open to continue or Cancel to discard entries and close the dialog 1 Click Diluent List from the task options in the Diluent Properties panel the Select Di...

Page 109: ...he known temperatures for example 15 C 20 C and 30 C To obtain the Refractive Index of the diluent at a different temperature say 25 C which is not listed in the table enter the temperature as 25 C in...

Page 110: ...ws specified users to perform measurements Requires password 21 CFR Part 11 allows specified users to perform measurements Requires password The procedures in this section are specific to the Security...

Page 111: ...Settings Mar 2014 4 31 Adding Users You must have Administrator rights to add users 1 Click the Security command the User Management window is displayed 2 Click Add User in the button bar at the top o...

Page 112: ...ter password Select the User Level Choose User level refer to User Level page 3 55 Public SOPs Allows other Users to copy and use SOPs Public Data Allows other Users to view measurement data 4 Click O...

Page 113: ...top of the window the Edit User Profile dialog is displayed for the selected User Click to display fields for changing password 2 Complete the fields as described below Password Select Change to the r...

Page 114: ......

Page 115: ...es not move correctly Shutter movement error Contact your Particulate Systems service representative Error reading temperature Improper temperature constant set Verify temperature setting in SOP If th...

Page 116: ...Sample concentration is too low at measurement in cell for low concentration Increase concentration Sample concentration is too high at measurement in cell for high concentration Decrease concentratio...

Page 117: ...malfunction Heater malfunction Malfunction of temperature control on main board Temperature on the display fluctuates Temperature sensor malfunction Contact your Particulate Systems service representa...

Page 118: ...ervice representative Appearance of side peaks Problem with sample Check purity of diluent and sample Instrument is been affected by vibration Remove or turn off the device that is causing vibration L...

Page 119: ...calibration history of pH electrode Exchange the inner KCl solution and recalibrate the electrode If sensitivity does not improve exchange the electrode pH cannot be measured Titration volume cannot...

Page 120: ...ll Temperature Adjustment Block If the cell temperature adjustment block becomes dirty clean by wiping with a soft cloth dampened with water or a neutral solvent Severe buildup of dirt from fluid spil...

Page 121: ...5 23 Flat Surface Cell page 5 16 High Concentration Cell page 5 12 Flow Cell page 5 8 Small Volume Disposable Cell for zeta potential page 5 23 Low Conductivity Cell page 5 26 The size measurement cel...

Page 122: ...ng 8 6 spares 8 Glass Cell 4 Electrode 2 9 Cell Stopper 5 Sealing Rubber 2 6 spares 10 Plug 2 1 2 3 4 5 6 7 8 9 10 Assembled Disassembled Disassembling the Flow Cell Wear protective gloves when disass...

Page 123: ...ove the cell guides Push the cell guides in while lifting the cell guide out of the cell holder Trench Cell guide Cell holder Pin 7 Remove the glass from the cell guide and remove the sealing rubber f...

Page 124: ...the cell guides into the cell holder firmly to the bottom of the cell holder pushing the cell guides against the glass cell and fitting the trenches on the cell guides to the pins on the cell holder...

Page 125: ...ntil it stops Cell holder Cell stopper Cell stopper Washing the Glass Cell Be careful not to scratch or damage the glass cell during handling Do not wash the cell in an ultrasonic cleaner Use the inst...

Page 126: ...e or packing can be washed in an ultrasonic washer using a neutral detergent solution Rinse well with purified water to completely remove the detergent High Concentration Cell This section describes h...

Page 127: ...holder and remove the transparent electrode Surface of electrode Optical surface Transparent electrode holder Electrode rod Transparent electrode 7 Remove the heat conductive adapter upward and remov...

Page 128: ...l to the base then attach the heat conductive adapter Base High concentration cell Heat conductive adapter 3 Attach the transparent electrode to the transparent electrode holder fitting it into the co...

Page 129: ...the concave port in the base Then tighten the clamp by turning knob B clockwise Hook Knob B 6 Attach sealing rubber E to electrode A Attach the small O ring and sealing rubber D to knob A Electrode O...

Page 130: ...ce Cell This section describes how to maintain the Flat Surface Cell for Zeta Potential 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 Assembled 1 Electrode 2 9 Luer fitting 2 Cell holder 10 Fixing nut 12 3 O...

Page 131: ...let Inject air into the cell Silicone tube Luer fitting 2 Using the special tool remove the fixing nuts and then remove the sample fixing block Special tool Cell block Fixing nut Sample fixing block 3...

Page 132: ...not be possible if other surfaces contain fingerprints or smears Do not dry the plane cell 6 Remove the cell block and O rings on both sides O ring Cell block Assembling the Flat Surface Cell All comp...

Page 133: ...tion 3 Mount the cell block on the cell holder fitting the cut off portions together Then fasten the fixing nut with the trenched face upward Cell holder Cell block Fixing nut Cut off portion Special...

Page 134: ...th 6 Rotate the clamping knob of the sample fixing block counterclockwise until it stops mount it on the sample sealing block Fix the sample fixing block with the fixing nut Then rotate the clamping k...

Page 135: ...o use the flat surface cell at normal temperatures to prevent separation of the coating Washing the Flat Surface Cell Be careful not to damage the Flat Surface Cell during handling Do not wash the cel...

Page 136: ...g oven Beakers as necessary To coat the Flat Surface Cell 1 Immerse the Flat Surface Cell in concentrated sulfuric acid for 2 3 hours Wash it well with purified water and rinse with methanol 2 Dry the...

Page 137: ...e solution then immerse it in the solution and allow to soak 2 hours 12 Remove the cell from the solution Wash with water then with 0 1 mol mL hydrochloric acid to remove excess acrylamide 13 Wash the...

Page 138: ...posable Cell 1 Disengage the fastener of the cell holder 2 Using a micropipette transfer a sample into a disposable cell 130 L 250 L and put a dedicated cap on each of the opening of the cell Be sure...

Page 139: ...ntation of the cell and gently insert the cell into the holder with the side of the cell side with protrusion titled downward as shown in the figure below Place a dedicated cap for high concentration...

Page 140: ...n order to use an organic solvent and since the structure of a cell is not a sealing system use the Low conductivity cell at near ambient temperatures Assembling the Low Conductivity Cell 1 Attach an...

Page 141: ...he cell holder turn clockwise to fully tighten Cell holder Electrode block Protrusion 4 Tighten the other electrode block on the other side Both electrode blocks are identical There is no left versus...

Page 142: ...the cell 1 Rinse the glass cell thoroughly with the same solvent that was used for the dispersant of the sample diluent or with alcohol such as ethanol or methanol Dry thoroughly after rinsing with t...

Page 143: ...e cell Other parts of the glass cell such as the electrodes and O rings can be washed in an ultrasonic washer using a mild detergent solution Rinse well with purified water to completely remove the de...

Page 144: ...ipette transfer at least 60 L of sample into the small volume size cell and put a cap on the cell Inlet 2 mm x 2 mm Do not use a tool made of glass to transfer the sample Doing so can damage the optic...

Page 145: ...lectrode low concentration cell set of 2 P09 00001 01003 Packing set flow cell set of 5 P09 00001 01004 Packing set flow cell Perflour set of 2 P09 00001 01005 Luer fitting flow cell set of 5 P09 0000...

Page 146: ...cell P09 00001 07007 Block flat surface cell P09 00001 07008 Seal sample block flat surface cell P09 00001 07009 Fixing nut flat surface cell P09 00001 07010 Seal Teflon flat surface cell P09 00001 07...

Page 147: ...me temperatures and humidity poor ventilation sunlight dust and salty or sulfurous air Surrounding temperature 15 35 C Relative humidity 30 85 without condensation Consider the frequency and voltage o...

Page 148: ...ll the electric cords are connected correctly and securely During use Be aware of proper instrument function at all times Do not touch any operational parts other than those specified in the instructi...

Page 149: ...te the switch to the right clockwise to adjust the speed of the Stirrer from minimum MIN to maximum MAX Minimum power is the Off position Status indicator Illuminated Green Stirrer on Not illuminated...

Page 150: ...pH Electrode 1 2 3 4 5 6 7 8 9 1 Protective cap 6 Connector protective cover 2 Contact portion to solution 7 Lead wire 3 Responding glass membrane 8 Cap 4 Connector for temperature sensor 9 Rubber sto...

Page 151: ...ons are added to the software commands when you have an AutoTitrator installed Configuration Displays the Configuration dialog allowing you to specify titration solutions Vial Position No Select the p...

Page 152: ...ndard solution of pH6 86 phosphate is necessary for the 2 and 3 point calibrations Calibration Points Select 2 or 3 for the number of standards you are using Buffer n Use these fields to select the st...

Page 153: ...ar 2014 A 7 Priming Displays the Priming dialog allowing you to fill or wash the tubing for the selected vial Consumable Check Enables you to check on the remaining life of the tubing and syringe Use...

Page 154: ...le Circulation dialog allowing you to begin circulation of the sample Select the pump speed from the drop down list The larger the value the faster the circulation speed The recommended speed is 50 pH...

Page 155: ...bber stopper from the refill opening for refilling the inner solution pH electrode Electrode holder Inner solution Rubber stopper for opening for refilling of inner solution Vial plastic The outer tub...

Page 156: ...set and select the type of solution Then enter the molar concentration for each solution If a vial is not going to be used deselect the vial position number 3 Select the type of vial to be used 50 mL...

Page 157: ...solution into the glass or plastic vial place a cap on the vial Cap Vial Vial guide Cap Vial Glass Use glass if the titration solution will be used continuously for more than one day Plastic Use plas...

Page 158: ...the Priming option from the pH Maintenance panel the Priming dialog is displayed 4 Select the vial number and click Start the solution will start filling Click Stop after confirmation that no air rema...

Page 159: ...de the electrode holder down until it reaches the bottom Stirrer Electrode holder Vial plastic 2 Select Sample Circulation from the pH Maintenance options the Sample Circulation dialog is displayed 3...

Page 160: ...n the air bubble trap to a horizontal level position When you see no bubbles in the outlet place the trap on the holder Holder Sample solution Be sure that degassing is complete If bubbles remain in t...

Page 161: ...3 Remove the cell stopper and confirm that there are no bubbles inside the glass cell and between the cell holder and glass cell If bubbles cannot be removed shake the cell gently or tap the side or...

Page 162: ...irm that the light intensity is within the range of 15000 and 30000 cps If the light intensity is over or under this range check that the Adjustment of ND Filter is set to Automatic Adjust ment If the...

Page 163: ...n SOP that is registered or being used in a measurement you must remove the cell parameter from that SOP in order to edit the cell parameters 2 Under the Titrator section select pH Titration 3 Under t...

Page 164: ...by Zeta Potential Analysis The plot of isoelectric points can be opened by pH Analysis Select pH Analysis from the Main menu Select File Open to display the results of isoelectric points the saved pH...

Page 165: ...n The rubber stopper should always be open during measurement or calibration and closed when not in use 2 Select the pH Calibration icon in the pH Maintenance function panel the pH Calibration dialog...

Page 166: ...asurements with the three standard solutions the results display on the lower part of the pH Calibration dialog Results 8 Click Registration to save calibration results otherwise the results are not s...

Page 167: ...s for electromotive force between pH 7 and pH 4 Specified range more than 90 Wash the electrode exchange the inner solution and perform the pH calibration again Resetting Temperature Constants of pH E...

Page 168: ...e outside of the instrument is coated with a synthetic resin Wipe off any solution spills immediately Applying Grease to Pump Tubing Always apply Grease to the pump tubing Not doing so can cause fluid...

Page 169: ...ar panel Fuses are replaced in the same manner as the NanoPlus refer to Replacing the Fuses page 5 6 Replacing the Syringe O ring Drain the titration solution from the tube and syringe before starting...

Page 170: ...he reference electrode must be 3 33 mol L KCl solution Immerse the electrode in purified water for 12 hours or more if the glass membrane of the electrode has dried out Do not touch the electrode conn...

Page 171: ...with purified water and use the electrode Storage Conditions Store the electrode as follows 1 Wash the sample solution with purified water 2 Put the rubber stopper on tightly 3 Remove the plastic via...

Page 172: ...improve do one of the following as appropriate Remove dirt wipe off with a soft cloth soaked with a neutral detergent Remove oil residue wipe off with a soft cloth soaked with an appropriate organic s...

Page 173: ...the Luer fitting with the Teflon tubing with the small diameter tubing provided with the size flow cell SRA 16 L Do not place the Teflon tubing under the pinch valve The air bubble trap is not necess...

Page 174: ...he size flow cell with Titrator as follows 1 Inset the cell into the cell block 2 Select Size Cell Flow as a cell name in the Cell Parameter of the Size SOP Designer 3 Select Type 3 or Type 4 as the m...

Page 175: ...oximates Exchange Limit or Life Span Tubes 1 and 2 Every exchange of titration solution Tubes 3 5 9 Every exchange of sample solution Tube 4 1 month Syringe packing 6 months Part Number Item and Descr...

Page 176: ...Consumables NanoPlus Operator s Manual A 30 Mar 2014 Tubing...

Page 177: ...NanoPlus Operator s Manual Consumables Mar 2014 A 31 Detail Be careful not to lose the inner Teflon tube in the case of tube 3 decomposition of tube 8 and an assembly 3 8...

Page 178: ...x 2 450 SRA 2 L 4 PharMed 2 4 x 5 5 3 32 x 7 32 in 350 VRF206 VRF206 5 Silicon 1014 21 1 0 x 3 0 200 VRM106 6 Silicon 1014 21 1 0 x 3 0 300 VRM106 7 Silicon 1014 21 1 0 x 3 0 500 VRM106 VRM106 8 Teflo...

Page 179: ...of Solids Ed Palik E D Academic Press New York 1997 Pigment Handbook Ed Lewis P A John Wiley Sons New York 1988 Water Refractive Index Refractive index is the ratio of the wavelength or phase velocit...

Page 180: ...nge from 20 C to 100 C from Swindells J F NBS This viscosity at 20 C is 1 002 cp 2 3 Dielectric Constant Dielectric constant is a measure of the amount of electrical charge a given substance can withs...

Page 181: ...Acetic Anhydride 18 50 90 62 1 3904 20 Acetone 20 25 326 316 1 3589 20 7 Acetonitrile 20 25 360 345 1 3460 37 5 Acetophenone 20 25 1 8 1 62 1 5342 17 4 Allyl Alcohol 20 30 1 363 1 07 1 4135 22 Amyl Ac...

Page 182: ...4175 2 2 Ether Di Ethyl 20 25 233 222 1 3497 4 3 Ethyl Acetate 2 0 25 455 441 1 3722 6 0 Ethyl Alcohol 20 30 1 2 1 003 1 3611 25 Ethyl Benzene 17 25 691 640 1 49 2 5 Ethyl Bromide 20 25 402 374 1 4239...

Page 183: ...3 Glycerin 83wt 2 0 1 4477 Glycerin 82wt 20 1 4461 Glycerin 81wt 20 1 4445 Glycerin 80wt 20 1 4429 Glycerin 79wt 20 1 4414 Glycerin 78wt 20 1 4398 Glycerin 77wt 20 1 4383 Glycerin 76wt 20 1 4368 Glyce...

Page 184: ...n 49wt 20 1 3966 Glycerin 48wt 20 1 3951 Glycerin 47wt 20 1 3937 Glycerin 46wt 20 1 3923 Glycerin 45wt 20 1 3909 Glycerin 44wt 20 1 3895 Glycerin 43wt 20 1 3882 Glycerin 42wt 20 1 3868 Glycerin 41wt 2...

Page 185: ...0 1 3498 Glycerin 13wt 20 1 3485 Glycerin 12wt 20 1 3473 Glycerin 11wt 20 1 3460 Glycerin 10wt 20 25 1 311 1 153 1 3448 Glycerin 9wt 20 1 3436 Glycerin 8wt 20 1 3424 Glycerin 7wt 20 1 3412 Glycerin 6w...

Page 186: ...n Amyl Alcohol 20 50 2 948 1 42 1 4099 13 9 n Butyl Acetate 20 73 1 3951 5 0 n Butyl Alcohol 20 50 2 948 1 42 1 3993 17 8 n Decane 20 50 92 615 1 4120 2 0 Nitrobenzene 20 50 2 0 1 24 1 5529 35 Nitrom...

Page 187: ...aton 1999 Liquid T C CP R I Dielectric Constant Pyridine 20 95 1 5102 12 5 Sec Butyl Alcohol 25 50 3 096 1 332 1 3954 15 8 Styrene Vinyl Benzene 20 50 749 502 1 55 2 4 Sulphuric Acid 20 254 1 8430 84...

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Page 189: ...5 Poly butadiene linear Dioxane 25 6 34 10 5 0 496 Poly butyl methacrylate 2 propyl alcohol 21 5 6 3 10 5 0 5 Poly cetyl methacrylate Heptane 21 1 74 10 3 0 64 Poly cholesteryl acrylate Benzene 21 3...

Page 190: ...ysical Chemistry Handbook The values are only valid for the specific molecules or particles in the specific solvent or dispersing medium and temperature although the temperature variation may be minim...

Page 191: ...nts of the standard samples and use the Cumulants analysis to obtain the molecular weight The obtained values are called the apparent molecular weight Mw app 5 Plot Log Mw versus Log Mw app for all st...

Page 192: ......

Page 193: ...olume Distribution Graph page D 5 Distribution Graph with Mobility of the Sample page D 14 Distribution Graph with Zeta Potential of the Sample page D 13 Differential Intensity Distribution Graph page...

Page 194: ...splays NanoPlus Operator s Manual D 2 Mar 2014 Real time Size Displays Real time Size Monitor Shows the stability of the sample during measurement Real time Size Table Shows the realtime size data raw...

Page 195: ...the NanoPlus In these histograms the magnitude of each peak is proportional to the percent amount of the total scattered intensity due to particles For example in the Differential Intensity Distributi...

Page 196: ...ough the conversion is accurate only for spherical particles a good approximation is obtained for non spherical particles with an axial ratio 3 1 and for particles 500 nm with an axial ratio of 5 1 Th...

Page 197: ...NanoPlus Operator s Manual Volume Distribution Graphs Mar 2014 D 5 Differential Volume Distribution Cumulative Volume Distribution...

Page 198: ...Number Distribution graph represents the number distribution for the same sample shown in the Differential Intensity Distribution graph shown earlier page D 3 For example in the graph below the number...

Page 199: ...7 Cumulative Number Distribution Ln G1 Plot Shows the natural logarithmic graph of G1 vs decay time This indicates if there is any noise in the signal The curve should be smooth where the ACF exists a...

Page 200: ...our selected size range The listings give the size corresponding to each bin and the relative amount of scattered intensity in each bin The total intensity adds up to 100 The absolute percentages appe...

Page 201: ...unction Mar 2014 D 9 Cumulative Size Distribution Table AutoCorrelation ACF Function ACF Listing This presents the Autocorrelation Function ACF raw data in tabular form Normal and abnormal correlation...

Page 202: ...AutoCorrelation ACF Function NanoPlus Operator s Manual D 10 Mar 2014 Normal Linear ACF ACF with Short Sampling Time In the ACF with short sampling time the sampling time has to be increased...

Page 203: ...NanoPlus Operator s Manual AutoCorrelation ACF Function Mar 2014 D 11 Normal Log ACF ACF Noisy Low Sample Concentration...

Page 204: ...Condition Summary NanoPlus Operator s Manual D 12 Mar 2014 ACF for Small Particles Less than 10 nm Condition Summary This presents the summary of the measurement analysis cell and diluent conditions...

Page 205: ...ppler Shift 24 16 Hz Lorentzian Peak Sample Zeta Potential Blue line Raw data Red curve Fitted data To change the position select the desired position from the Select Relative Position drop down menu...

Page 206: ...Distribution Graph NanoPlus Operator s Manual D 14 Mar 2014 Distribution Graph with Mobility of the Sample The values displayed in this graph represent the mobility of the sample...

Page 207: ...d the Doppler Shift modulator signal is calculated The Base frequency is dependent on the type of cell used and the concentration of the sample Typically for the flow cell and Flat Surface cell the Ba...

Page 208: ...e displayed For example Positive Test Results 12 5 Negative Test Results 15 8 Polarity Negative This decision is based on the Doppler Shift in the frequency To interpret the results assume the sign of...

Page 209: ...be viewed at all positions at which the zeta potential mobility is measured The positions can be set in the Cell parameters of the Zeta SOP Designer see Cell Parameters Panel page 3 25 To switch from...

Page 210: ...3D Graph NanoPlus Operator s Manual D 18 Mar 2014 With Mobility and 3D View The Lorentzian Peak represents the Brownian motion of the particles Lorentzian Peak 3D View...

Page 211: ...ue Table Provides the mobility zeta potential of the sample and the electric field applied Also provides apparent mobility and zeta potential peak values at the locations specified in the cell conditi...

Page 212: ...Gradient Plot NanoPlus Operator s Manual D 20 Mar 2014 Temperature Gradient Plot The Temperature Gradient analysis enables you to perform measurements on the same sample at different temperatures With...

Page 213: ...NanoPlus Operator s Manual Temperature Gradient Plot Mar 2014 D 21 With Temperature Marker...

Page 214: ...menu and a data grid is displayed at the bottom of the graph A scroll bar is also provided for you to scroll through all points Pop up menus with an arrow to the right indicate a fly out menu contain...

Page 215: ...Mar 2014 D 23 Editing Graph Axes Place your cursor on the X or Y axis to edit axes properties Place your cursor specifically on the title to edit only title properties These options also display on t...

Page 216: ...dit graph properties If you select Toolbar on this menu graph options are displayed as icons at the top of the graph Hover your cursor over the icon to display its function Place your cursor directly...

Page 217: ...of particles in liquid media it is possible to determine their size Light Scattering From Particles in Brownian Motion In dynamic light scattering the fluctuations in time of scattered light from par...

Page 218: ...s and more slowly for larger slower moving particles The fluctuations of the scattered light are analyzed using the autocorrelation function The Autocorrelation Function The calculation of the autocor...

Page 219: ...will be a single exponential 4 where B a constant dependent on instrumental parameters such as the aperture pinhole size the decay constant which is proportional to the diffusion coefficient as shown...

Page 220: ...r has high resolution within the limited range of decay time and is suitable for very small particles of narrow distribution The Correlation Method During a sample run the scattered light intensity is...

Page 221: ...les usually scatter weakly and the situation is such that the photon counts per sampling time become very low In this case the Time Domain method is an inefficient means of data collection With the Ti...

Page 222: ...larized nonnegative least squares technique combined with the Eigenfunction analysis It has been implemented as the main data retrieval algorithm CONTIN uses a non linear statistical technique to smoo...

Page 223: ...this happens Distributions obtained by this method tend to have narrow and separated peaks Molecular Weight Analysis The Molecular Weight MW analysis is performed for all types of particle size distri...

Page 224: ...tive ions exist in the area far from the particle s surface so that electric neutrality is maintained This ion distribution is called a diffuse electrical double layer and can be divided into two laye...

Page 225: ...articles are stable due to high electrostatic repulsion between particles On the contrary a low zeta potential value approaching zero increases the probability of particles colliding and thus forming...

Page 226: ...ince the frequency of the scattered light is shifted from the incident light in proportion to the speed of the particles movement the electrophoretic mobility of the particles can be measured from the...

Page 227: ...n vacuo and of the solvent respectively Power Spectrum for Zeta Potential Measurements Power Spectrum analysis provides an easy and direct way to obtain electrophoretic mobility information The instru...

Page 228: ...zian fit Zeta Potential Determination by Electrophoretic Light Scattering NanoPlus Operator s Manual E 12 Mar 2014 Figure 8 ACF and Power Spectrum of Test Measurement Figure 9 ACF and Power Spectrum o...

Page 229: ...particle true mobility Figure 10 Schematic Diagram of the Electroosmotic Flow Occurring in a Close Cell Electroosmotic flow has a symmetric parabolic profile when the particle concentration in the ce...

Page 230: ...and lower surfaces of the cell 0 W1 W0 2 0 the difference of electroosmotic flow between upper and lower surfaces of the cell 0 W1 W0 Hence apparent particle mobility obs 0 z transforms into 15 Equati...

Page 231: ...nt Particle Mobility in the Cell Electroosmotic flow becomes asymmetric in this cell due to the difference in the surface charges of upper and lower surfaces of the cell However the Mori and Okamoto e...

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Page 233: ...mprove an organization s quality control while preserving the FDA s charter to protect the public Activating 21 CFR Part 11 Obtaining an Authentication Code 1 Click the Maintenance option on the side...

Page 234: ...rer navigate to the directory into which the NanoPlus software is installed The default directory is C Program Files Micromeritics Instrument Corporation Paste the passdata dat file into the directory...

Page 235: ...ake effect 7 Click File Exit to close the program 8 Restart the NanoPlus software Enabling CFR Part 11 The Security Settings must now be changed to complete activation A user with Administrator rights...

Page 236: ...R Part 11 is enabled in the NanoPlus software An Option menu containing CFR Part 11 functions Two additional audit trails Signature Enables you to view the electronic signature s of selected file File...

Page 237: ...ou must have Administrator rights to add users If you have worked in the Security environment before activating CFR Part 11 the Users should carry over 1 Click the Security command the User Management...

Page 238: ...es in Range 45 to 300 days Automatically log out after Range 4 to 120 minutes Close Signature Dialog after Range 20 to 180 minutes 4 Click OK when finished to add the User Disabling and Enabling Users...

Page 239: ...play fields for changing password User01 2 Edit the fields as described below Password Select Change to the right of the Password field two fields are inserted allowing you to enter a new password and...

Page 240: ...Click Save Recalculated Data the Save Recalculated Data dialog is displayed 4 Select the method you wish to use for saving the data You can choose Manual Input to enter the file name group name and sa...

Page 241: ...ample user and when logged in when users were added to the system all operational steps and so on Parameter Audit Trail stores and records parameter change history for example date time user name para...

Page 242: ...maximum number of lines that have been set for each audit trail 3 Edit the values as desired you can use up to 9 999 lines shown at bottom of viewer 4 Click Save to save the new values or Cancel to di...

Page 243: ...cted user Use the down arrow to the right of the fields to make your selections User Exports all details for a specific user Use the down arrow at the Select User field to select the user 4 Click Expo...

Page 244: ...ou wish to view its details 2 Select Option 21 CFR Part 11 File History on the Main Menu bar or History Tracking at the top of the Results pane the History Tracking dialog is displayed This example sh...

Page 245: ...ectory The file is given the same name as the SOP appended with Par particle size or Zeta zeta potential 1 Select Option 21 CFR Part 11 Playback on the Main menu bar the Playback file selection dialog...

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Page 247: ...ers panel particle size 3 19 zeta potential 3 23 Analyzer cleaning 5 6 turning on and off 2 5 weight and dimensions 1 4 Audit trails F 9 editing options F 10 exporting details F 10 Autocorrelation fun...

Page 248: ...3 14 Doppler effect E 10 shift D 16 Dynamic light scattering E 1 E Electrical conductivity measuring 4 8 double layer E 8 specifications 1 4 Electronic recordss F 1 Electronic signature F 8 Electroos...

Page 249: ...G1 t vs t Plot 3 14 Lorentzian fit specifying peaks 3 24 Lorerntzian peak E 11 Low conductivity cell 5 26 assembling disassembling 5 26 base frequency 3 30 cleaning 5 28 consumables 6 2 temperature f...

Page 250: ...og particle size data 3 10 3 14 zeta potential datat 3 16 3 18 Q QC Data Select panel 3 41 Results panel 3 42 R Realtime size monitor 3 14 Real time size monitor graph D 2 Real time size table D 2 Rea...

Page 251: ...and power spectrum D 16 Theory of operation E 1 Time Domain method E 5 Time Interval method E 5 Titration modes 3 28 Titrator solutions configuring A 10 filling A 11 loading and circulating A 13 Troub...

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