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PN B05577AC

B-7

Sample Handling

Liquid Sample Dispersion

B

Steric Stabilization

•

Best in organic solutions. Can be anionic, cationic, or nonionic dispersants or block copolymers.
Optimal structure has anchor region that adsorbs strongly on the organic solid (example:
alkane chains, aryl groups), and another region that is highly soluble in the liquid (example:
polyethylene oxide chains are soluble in water).

Physical and Chemical Methods of Liquid Dispersion

Usually, the best dispersions are achieved when both methods are employed on a sample. A
combination of wetting the sample with a dispersant followed by spatulation and sonication has
proven to give the best dispersions.

Special cases

•

Emulsions: special care must be taken when dispersing emulsions. Dispersants and sonication
can cause de-emulsification.

•

Liposomes: special care must be taken when dispersing liposomes. Dispersants can disrupt the
liposome wall and sonication can rupture the liposome wall.

A Practical Recipe For Liquid Sample Dispersion

•

Dispersant check

: use watch glass/weigh boats to determine which dispersant has the best

interaction with particles.

•

Wetting:

add just enough dispersant or diluent to the sample to form a thick paste.

•

Spatulate:

use spatula, rubber policeman, etc. to mull the sample and the dispersant into a

paste.

•

Add diluent:

add diluent to form a slurry.

•

Optical check:

use a microscope to visually check the status of the dispersion. If the dispersion

appears incomplete, then either try another dispersant or add more energy to the system
taking care not to disrupt the integrity of the particles.

•

Add energy to system:

use sonication (usually best), stirring, heat, etc., to de-agglomerate

particles.

•

Check for Stability:

Sometimes the sample may re-agglomerate or flocculate over time due to

dilution, change in pH, ionic concentration, or improper dispersant. If this happens, Beckman
Coulter states that the dispersion is not stable. Puffy, loosely held “flocs” may be analyzed with
good results if there is enoug shear from the pump or circulating system to separate the
particles. Tightly held “flocs” or “re-agglomerates” may need more energy added to the system;
to be dispersed with a different dispersant; or put under different conditions such as change in
pH, ionic concentration, etc. Adsorbing polymers onto the surface can help stabilize the
dispersion.

•

Sampling:

While adding sample to the sample vessel, always try to obtain a representative

sample with each addition. A stir bar or pipette aspiration can be utilized while sampling in
order to keep particles suspended.

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Содержание LS 13 320

Страница 1: ...PN B05577AC July 2017 User s Manual LS 13 320 Laser Diffraction Particle Size Analyzer Beckman Coulter Inc 250 S Kraemer Blvd Brea CA 92821 U S A ...

Страница 2: ...arks or registered trademarks of Beckman Coulter Inc in the United States and other countries All other trademarks service marks products or services are trademarks or registered trademarks of their respective holders Contact Us If you have any questions contact our Customer Support Center Worldwide find us via our website at www beckmancoulter com customersupport support Outside of the USA and Ca...

Страница 3: ...rsion of the manual or system help for your instrument Initial Issue B05577AA 2009 Issue AB September 2011 Updates were made to the following sections Updated corporate address Revised Figure 1 2 Certification Label Instrument Back Cover Other minor edits and deletions Revision page added Added the Beckman Coulter Inc Customer End User License Agreement Trademarks page added Issue AC July 2017 Upd...

Страница 4: ...PN B05577AC iv Revision History ...

Страница 5: ...zardous situation which if not avoided could result in death or serious injury May be used to indicate the possibility of erroneous data that could result in an incorrect diagnosis CAUTION CAUTION indicates a potentially hazardous situation which if not avoided may result in minor or moderate injury It may also be used to alert against unsafe practices May be used to indicate the possibility of er...

Страница 6: ...contact your Beckman Coulter Representative RoHS Notice These labels and materials declaration table the Table of Hazardous Substance s Name and Concentration are to meet People s Republic of China Electronic Industry Standard SJ T11364 2006 Marking for Control of Pollution Caused by Electronic Information Products requirements RoHS Caution Label This label indicates that the electronic informatio...

Страница 7: ...h Federal Regulations 21CFR Subchapter J as administered by the Food and Drug Administration s FDA Center for Devices and Radiological Health CDRH defeatable microswitches are located on the right and left of the door panel Because the system contains a laser it should be isolated from non laser instruments Users are advised to keep a copy of ANSI standard 2136 1 SAFE USE OF LASERS near the instru...

Страница 8: ...ty interlock switches LS 13 320 Specific Precautions Never place a mirror or optical surface other than the sample cell assembly into the optical axis of the system WARNING Do not place your hands in the pathway of the door as it closes WARNING Do not place your hands or any object inside the optical bench as the module is docking Safety Labels Radiation Hazards In the design and manufacture of th...

Страница 9: ...hat when removed might expose laser radiation Refer to the figure titled Warning labels Instrument Front Cover And Laser Cover for the warning labels and their locations Warning labels Instrument Front Cover And Laser Cover Certification Label Instrument Back Cover ...

Страница 10: ...ounded correctly Chemical Safety DANGER Normal operation may involve the use of diluents and reagents that are pathogenic or toxic Such materials require that you take all necessary safety precautions Do not use any diluents that are not compatible with the specific wetted surface of the sample module Consult Beckman Coulter or its local representative before using any chemicals not listed in this...

Страница 11: ... Automatic alignment should be performed more often Electrical interference Use of an uninterruptible power supply UPS is recommended Sudden changes in temperature can cause misalignment as well as changes to the measured electrical offsets Scope of Manual This manual is designed to familiarize you with the Optima XE its functions specifications operation and routine operator care and maintenance ...

Страница 12: ...PN B05577AC xii Safety Notice Scope of Manual ...

Страница 13: ... Installation 2 1 Installation Requirements 2 1 Environment 2 1 Power Requirements 2 1 Temperature and Humidity Requirements 2 2 Sample Modules Specific Requirements 2 2 Suspension Fluid for Aqueous and Universal Liquid Modules 2 2 Drain for Aqueous Liquid Module 2 3 Drain for Universal Liquid Module 2 3 Vacuum for Tornado Dry Powder System 2 3 Hardware Connections 2 3 Software Installation 2 4 In...

Страница 14: ...ptions 3 32 Security Setup 3 34 5 5 2 Types of Users 3 35 5 5 2 1 Administrator 3 35 Add a User Account 3 38 Edit a User Account 3 39 View User Account Info 3 39 Supervisor 3 40 Customize Main Menu 3 40 Customize Run Menus 3 41 Customize Sample Info Names 3 41 Recent Files and Directories 3 42 No Security 3 42 Low Security 3 43 Medium Security 3 45 High Security 3 46 Logging Out 3 48 CHAPTER 4 Reg...

Страница 15: ...are to Standard 5 13 Compute Sizes 5 13 CHAPTER 6 Sample Modules 6 1 Aqueous Liquid Module 6 1 ALM Description 6 2 System Description 6 2 Indicators 6 2 Connecting the ALM 6 4 Recirculation Lines 6 4 Inlet and Drain Hoses 6 4 Loading the Sample Cell Into the Optical Bench 6 5 Software 6 6 8 1 3 1 Control Menu 6 7 8 1 3 2 Standard Operating Methods SOM 6 8 8 1 3 3 Loading an SOM 6 12 8 1 3 4 Standa...

Страница 16: ...ell on the Sample Stand 6 44 Filling Micro Liquid Module with Diluent 6 45 Adding Sample 6 46 Setting the Stirring Motor 6 46 Cleaning the MLM 6 47 Clean the cell components 6 47 MLM Troubleshooting 6 49 Tornado Dry Powder System 6 49 Tornado Description 6 50 Indicators 6 50 Docking the Tornado DPS 6 51 Software 6 51 8 4 3 1 Control Menu 6 52 8 4 3 2 Standard Operating Methods SOM 6 53 Creating SO...

Страница 17: ...1 Liquid Sampling B 1 Solid Sampling B 1 Spinning Riffler B 2 Chute splitter B 2 Table sampling B 3 Scoop sampling B 4 Cone and quartering B 4 Liquid Sample Dispersion B 4 Liquid Sample Dispersion B 5 Physical Methods of Liquid Dispersion B 5 Chemical Methods of Liquid Dispersion B 6 Stabilization by surface charge B 6 Steric Stabilization B 7 Physical and Chemical Methods of Liquid Dispersion B 7...

Страница 18: ...ing the Distribution C 6 Variance C 6 Standard Deviation C 7 Coefficient of Variation C 7 Skewness C 7 Kurtosis C 8 APPENDIX D Troubleshooting D 1 Background D 1 Troubleshooting High Backgrounds D 3 Reference Background Set Up D 3 Part 1 Setting Up a Reference Background D 4 Part 2 Using the Reference Background D 8 APPENDIX E Maintenance E 1 Cleaning Procedures E 1 Cleaning Fluids E 1 Cleaning th...

Страница 19: ...sets Screen 2 16 2 14 Measuring Obscuration Loading Screen 2 16 2 15 Sample Info Dialog 2 17 2 16 Run Settings Dialog 2 17 2 17 Optical Model Dialog Screen 2 19 2 18 Run Cycle Options Dialog 2 21 2 19 Reference Background File Selection 2 22 3 1 LS 13 320 Software 3 1 3 2 User Privileges Dialog No Security 3 43 3 3 User Privileges Dialog Low Security 3 45 3 4 User Privileges Dialog Medium Security...

Страница 20: ...evelopment 6 34 6 20 Figure 4 Select Fluid Dialog 6 34 6 21 Figure 5 Edit Fluid List Dialog 6 35 6 22 Step 2 of SOM Development 6 35 6 23 Figure 7 Step 3 of SOM Development 6 36 6 24 Figure 8 Run Cycle Options Dialog 6 36 6 25 Figure 9 Step 4 of SOM Development 6 37 6 26 SOM Summary 6 38 6 27 SOM List Dialog 6 39 6 28 Create an SOP Dialog 6 41 6 29 Figure 13 SOP List Dialog 6 42 6 30 Miscibility G...

Страница 21: ...on Screw Removal 6 82 6 49 ULM Pencil 6 83 B 1 Figure 1 Spinning Riffler B 2 B 2 Figure 3 Table Sampling B 3 B 3 Figure 3 Table Sampling B 3 B 4 Figure 4 Scoop Sampling B 4 B 5 Figure 5 Cone and Quartering B 4 D 1 Normal Background D 1 D 2 Background Showing the Presence of Bubbles D 2 D 3 Background Showing the Presence of Contaminants D 2 E 1 Fourier Lens Location and Cleaning Technique E 2 E 2 ...

Страница 22: ...xxii Tables Tables 2 1 Table 4 1 LS 13 320 Power Requirements 2 2 2 2 Initial Dialog Box After Software Launch 2 6 2 3 Controls Used With Specific Sample Modules 2 13 C 1 Mean Diameters C 6 ...

Страница 23: ... button The symbol points you to where additional information on a subject can be found LS 13 320 Overview The Beckman Coulter LS 13 320 Figure 1 measures the size distribution of particles suspended either in a liquid or in dry powder form by using the principles of light scattering The LS 13 320 particle size analyzer provides reliable and reproducible results for researchers quality control lab...

Страница 24: ... that analyses are the same run after run Every element of the analysis from method set up to the final printout can be locked into a user definable SOP The SOP routine is divided into two distinct components an SOM Standard Operating Method and a Preference prf file The SOM includes all aspects of the analysis relating to the instrument settings The Preference file prf includes choices relating t...

Страница 25: ...superimposed creating a single composite scattering pattern that represents the contributions from all the particles in the sample cell Detectors the Fourier plane record this composite scattering pattern Over the course of a measurement a running average is created from the changing flux patterns When the duration of the measurement is long enough that the flux pattern accurately represents the c...

Страница 26: ...spended in liquid or air scatter the incident light in characteristic patterns according to their size Fourier optics collect the diffracted light and focuses it onto three sets of detectors one for the low angle scattering the second for mid angle scattering and the third for high angle scattering A block diagram of the LS 13 320 optical system is presented in Figure 4 Figure 4 Optical System of ...

Страница 27: ... nm 600 nm and 900 nm through two orthogonally oriented polarizers at each wavelength Light from a laser diode is monochromatic a requirement of the theoretical models that describe a particle s scattering function However as opposed to gas or liquid lasers the light from a laser diode is not focused The monochromatic light from a laser diode must also be treated to produce a clean beam The device...

Страница 28: ...or in dry powder form These modules are Tornado Dry Powder System DPS Universal Liquid Module ULM Aqueous Liquid Module ALM Micro Liquid Module MLM In addition the ALM can be used in conjunction with the AutoPrep Station Computer System The operation of the LS 13 320 requires a personal computer PC and the PC based control and analysis software If you are not using a Beckman Coulter supplied PC yo...

Страница 29: ...fine analysis profiles to automate your most frequently used analysis protocols Use the built in security features supervisor modes automatic 21 CFR Part 11 compliance function use with the compliant version of software only Hard Drive 20 Gb 35 Gb or better Monitor 800X600 1024X768 Keyboard Enhanced 101 102 Enhanced 101 102 Mouse 2 Button 3 Button MS Windows Version Win 98 or better Win Vista Tabl...

Страница 30: ...PN B05577AC xxx LS 13 320 Introduction System Components ...

Страница 31: ...itted through long optical paths through the atmosphere during dawn and dusk Utilizing this wavelength dependence Beckman Coulter uses red as the color for the stoplight and foralltrafficcontrolwarningsignsbecausered light has the least scattering powerinthe visible light spectrum This allows the transmitted light to go through fog rain and dust particles and reach the intended detector in this ca...

Страница 32: ... of arbitrary size as a function of angle given that the wavelength and polarization of the light are known and that the particle is smooth spherical homogeneous and of known refractive index This theory is more complex than the theory set forth by Fraunhofer in that it accounts for all possible interactions between particles and light yet it s only applicable to spheres Spheres produce light scat...

Страница 33: ...ight percentage of each component In addition choosing a correct optical model is often the key step in obtaining the correct results Polarization Intensity Differential Scattering PIDS Many samples have particle sizes that extend into the submicron range creating a wider size distribution range However as a particle size gets smaller the ratio of particle dimension to light wavelength d l is redu...

Страница 34: ...h as soils sands and mineral powders are irregularly shaped and can have either a smooth or a rough surface The analysis strategy that all commercial instruments employ in the measurement of these particles is to use a spherical approximation and treat every particle as a sphere This method produces a size distribution with diameter as the only variable which is easily traceable and comparable to ...

Страница 35: ...cattering at the boundary which often has a similar influence as absorption of light within the particle Thirdly the particles may be optically heterogeneous as is the case for porous particles This may lead to an apparent presence of significant amounts of very small particles which are non existent PIDS Sizing As mentioned above with its patented PIDS assembly the LS 13 320 can provide informati...

Страница 36: ...ially with vertically and horizontally polarized light of the three different wavelengths colors The three wavelengths of light permit three independent measurements of the PIDS effect at different ratios of particle sizes to light wavelength For each of the three wavelengths the differential scattering pattern PIDS pattern is observed at six detectors centered at a scattering angle of about 90 In...

Страница 37: ... LS 13 320 find a site that is Clean and free of dust Well ventilated Smoke free Isolated from external vibration sources Temperature controlled as large or frequent variations in temperature can change the alignment of the laser beam The system requires a flat stable surface at least 0 7 m 2 5 ft wide and 1 8 m 6 ft in length A height clearance of at least 0 7 m 2 5 ft is recommended Power Requir...

Страница 38: ...out condensation Sample Modules Specific Requirements Suspension Fluid for Aqueous and Universal Liquid Modules IMPORTANT Ensure that the material being sized and the suspension fluid do not violate any hazard waste or clean water discharge regulations The Aqueous Liquid Module requires clean bubble free liquid as suspension fluid Regular tap water that is filtered and degassed can be used Beckman...

Страница 39: ...If you choose to supply one you will need a unit capable of sustaining rates up to 420 L minute at 740 to 750 torr 15 cfm at 5 to 10 inches of water below atmospheric pressure A remote power switch and hoses are also needed to connect your vacuum source to the Dry Powder System Your Beckman Coulter Representative can recommend a vacuum source for your system Hardware Connections See Figure 2 2 for...

Страница 40: ... connection parameters for your LS 13 320 and PC 1 From the LS 13 320 software program select Security 2 From the security dialog box select Enter Supervisor Mode 3 Select Connections The dialog box displays Figure 2 3 In the Connections Parameters box Port accept the current setting or select the radio button to select a different communications port Baud Rate verify that the port speed is set to...

Страница 41: ...samples to check the operation of your instrument A qualitycontrol program isalso available which is a convenient way to have the performance of your instrument tracked and any problems identified by qualified Beckman Coulter personnel Getting Started The PC software has been designed to control all the operations of the LS 13 320 Once the instrument and its corresponding module have been set up a...

Страница 42: ...sh to use For more on security levels refer to Security Options Once a security level has been selected the dialog screen shown in Figure 2 4 will not be displayed again Figure 2 5 shows a diagram of the steps and dialog screens to follow after selecting a security level Table 2 2 Initial Dialog Box After Software Launch Non Compliant Software Compliant Software ...

Страница 43: ...on as described in Security Options a dialog box appears requiring you to enter a user name and password If the security option was not selected it can be selected at this time The following procedure must be followed when setting up security the first time the software is installed The administrator must complete the high security set up ...

Страница 44: ... Security The security level option dialog box is displayed 2 21 CFR Part 11 to display the following screen 3 Click on the Add a User to display the Add a User Account dialog box The Full Name Login Name and Password are required fields Select the Administrator as the user ...

Страница 45: ...2 4 After completing the required information and selecting OK another user may be added at this point After all users have been added select Cancel and the following dialog screen will be displayed 5 You will be prompted to choose a new password ...

Страница 46: ...il in CHAPTER 3 Security Options User Privileges Dialog 21 CFR Part 11 Security Selecting a Module The optical module is automatically recognized by the optical bench when the module is docked into the optical bench Run from the menu bar Figure 2 6 Use Optical Module COM 1 If there is no module connected to the LS 13 320 or there is a problemwithcommunication between the computerand the LS 13 320 ...

Страница 47: ... occurs ensure that an optical module is connected to the LS 13 320 bench Make sure that the module is docking properly otherwise contact your Beckman Coulter Service Representative Also check the connections between your computer and the LS 13 320 bench Once a module has been identified the screen shown in Figure 2 8 will be displayed Figure 2 8 Ready Screen ...

Страница 48: ... Here the light intensity levels received by the detectors are measured with no sample in the system and then subtracted out This procedure eliminates the signal due to the outer edges of the Gaussian laser beam in addition to any light leakage or scattering from dust on the lenses or any other particulate present in the optical path The background should always be measured prior to adding sample ...

Страница 49: ...he controls provided by Beckman Coulter to be used will depend on the sample module being used and are listed in Table 2 3 The following section describes the procedure to follow in order to verify the operation of the instrument by running a control sample 1 Run 2 Run Cycle as shown in Figure 2 9 Figure 2 9 Run Menu Table 2 3 Controls Used With Specific Sample Modules Sample Module Control Univer...

Страница 50: ...PN B05577AC 2 14 Installation Making Measurements 3 New Sample and select the Include PIDS check box seeFigure 2 10 ifyoursample contains particles below 0 4 µm ULM and ALM only Figure 2 10 Run Menu ...

Страница 51: ...llation Making Measurements 2 4 Start A sequence of steps will automatically follow after selecting Start as indicated below a Measuring offsets Figure 2 11 Measuring Offsets Screen b Alignment Figure 2 12 Auto Align Screen ...

Страница 52: ...urements c Background measurement Figure 2 13 Measuring Offsets Screen d Measure loading Figure 2 14 Measuring Obscuration Loading Screen Once the correct obscuration is obtained click on the Start Analysis button to continue to the next step ...

Страница 53: ...PN B05577AC 2 17 Installation Making Measurements 2 e Sample information Figure 2 15 Sample Info Dialog f Run information Figure 2 16 Run Settings Dialog ...

Страница 54: ...PPENDIX B Sample Handling for more information on sample dispersion and preparation The steps to follow to analyze a sample are similar to those used to analyze a control sample SOPs can also be created to set up the analysis of a particular sample 1 Run Run Cycle Figure 2 9 2 Under Run Cycle select New Sample If PIDS is to be used select the Include PIDS data check box to activate this option Sel...

Страница 55: ...reated for each particular sample module The reference background can be subsequently used to compare how the module is operating The reference background must be created with the best background obtained during a run that indicates that the module windows are clean and if using the ULM MLM or ALM the diluent is particle free When comparing backgrounds from different analysis runs with the referen...

Страница 56: ...enu select Run Cycle Options Figure 2 18 3 Select New Reference Background 4 From the dialog box select the file you want to use as the reference background file Click Open The background from the file you select will then be saved in the calibration files folder using the following filename format ZXBYYYY ls where X L for the ALM U for the ULM M for the MLM P for the Tornado DPS Y the last four d...

Страница 57: ...PN B05577AC 2 21 Installation Making Measurements 2 Figure 2 18 Run Cycle Options Dialog ...

Страница 58: ...PN B05577AC 2 22 Installation Making Measurements Figure 2 19 Reference Background File Selection ...

Страница 59: ...PN B05577AC 3 1 CHAPTER 3 LS 13 320 Software Figure 3 1 LS 13 320 Software ...

Страница 60: ...en command displays a dialog containing a list of stored files Select the file you wish to open either by highlighting the file and using the Open button or by double clicking on the filename in the list NOTE n order for a file to be displayed by default in the dialog box whether new imported or acquired directly from the LS 13 320 it must have an extension that matches what is shown in the Files ...

Страница 61: ...PN B05577AC 3 3 LS 13 320 Software File Menu Options 3 To open a file 1 File Open or click on the Open icon 2 Select the file you want to open and click Open ...

Страница 62: ...20 Software File Menu Options The results screen is displayed along with a box that displays the statistics as shown below If the statistics box is not displayed you may access it by selecting Analyze Show Statistics on Graph ...

Страница 63: ... Open but allows you to open a total of 30 files and display them as an overlay in one graph Saving an overlay as a ovr file only saves a list of the names of the files in the overlay In order to open an ovr file all the files named in the list must be present in their original locations ...

Страница 64: ... files is not included in the composite file but the individual runfiles themselves are not altered by the Average function Averaged files may be printed edited and saved with a av extension using the Save As command under the RunFile menu You may also save the file by selecting Save List of Averaged Files from the RunFile menu The saved file will be assigned the extension avg This file can later ...

Страница 65: ...he mean particle diameter for each run on the same graph The display of the Trend Graph and or Listings will depend on the settings selected under the Preferences menu Using Size Trend 1 File Create Size Trend The Create Size Trend dialog box see figure is displayed 2 Select the files to include in the Size Trend Analysis 3 OK 4 To select the variables to be plotted Graph on the RunFile menu bar T...

Страница 66: ... located in the Edit menu Import Size Data Select Import Size Data to import data generated by the software that is in file format of types txt or xls To convert these types of data files click on the File menu and then click on Import Size Data Next type the file name in the space provided or select the file of interest in the Open for Import dialog box Using file names with a 3 character extensi...

Страница 67: ...PN B05577AC 3 9 LS 13 320 Software File Menu Options 3 In the dialog box see next figure select the first and last lines that include the data of interest followed by the channel sizes and data ...

Страница 68: ... folder directory for the storage of new or renamed data files Print Reports The Print Reports command allows a separate report to be generated for each file that is selected from a list offilesthat appears in the Print Reportsdialog box The form and content of these reports is defined by selections made in the Reports section of the Preferences pull down menu Print Window Print Screen Print Windo...

Страница 69: ...ible Open result windows are displayed one behind the other Tile Horizontal Using the Tile Horizontal display function up to 16 open result windowscontaining different sample data runs can be displayed on the screen simultaneously with the major axis running horizontally Tile Vertical Using the Tile Vertical display function up to 16 open result windows containing different sample data can be disp...

Страница 70: ...n Cycle The Run Cycle menu allows you to set all the parameters necessary to perform an analysis on a sample This menu allows the selection of the PIDS data option is found as well as Measure Offsets Align Measure Background and Measure Loading These options are customized for each sample module and are explained in more detail in CHAPTER 2 Installation Making Measurements ...

Страница 71: ...ng a Control for more information on the options under the Run Cycle menu Run Cycle Options This option allows the user to set up parameters for various parts the offset alignment and background measurements that will be used under the Run Cycle menu described above ...

Страница 72: ...ModuleSection to learn more about how to create load and use an SOM and to the Preferences section to set up particular preferences Create SOM SOMs allow you to set all the analysis parameters that will be needed to perform the analyses on your samples The SOMs can be used in conjunction with SOP s or by themselves Create an SOM consists of a sequence of six screens which provide a range of option...

Страница 73: ...Refer to your specific Sample Module section in this manual for further instructions Make Optical Model Makingopticalmodelsis necessarytoobtain the correctsize distribution onyourparticularsample For more on optical models refer to APPENDIX C Optical Models ...

Страница 74: ...File ID 60 Will use up to the first 60 characters of the name selected under File ID in the Enter Sample Info dialog box O Operator 60 Will use up to the first 60 characters of the name selected under Operator in the Enter Sample Info dialog box D Date 16 Will use date format of your computer R Run Number 5 Will use the run number from the Enter Sample Info under Run Number Run Number is also foun...

Страница 75: ...he Printed Report tab displays a dialog box that specifies the content of printed reports This function allows you to choose any combination of the following report elements to be included in your printout Sample Info Comments sample collection parameters and other file specific data Short Sample info content provided in a shortened format Size Graphs Provides a graphical display output selected f...

Страница 76: ...tabular or graphical using sieve format by mesh size or mesh number Size Graphs This option displays the Size Graphs tab box Your first selection determines the default format for the graph display format Additional selections determine the other types of graphical presentations to be included in your report Up to 12 distribution types may be selected in the desired printing order Both the x axis ...

Страница 77: ...s you to customize tabular data presentations by selecting specific listing information and designating column sequence for quick output to the printer Make your selections by clicking the desired option boxes click again to deselect Up to seven categories of information may be included in tabular data output ...

Страница 78: ...rpolation dialog box to enter up to 150 interpolation points In the group box labeled Interpolation Type select the distribution type to size that you want printed Selecting the Size to distribution type will activate the Volume Surface Area and Number check boxes This section also determines whether data are displayed as a cumulative percentage of values either above or below user defined percent...

Страница 79: ...tribution and statistic type used It is also useful in defining which percentiles and statistics appear on the size statistics report and when selecting Analyze Statistics option from the individual run file menu See APPENDIX D Troubleshooting for more information on the statistics used in particle characterization ...

Страница 80: ...PN B05577AC 3 22 LS 13 320 Software Preference Options ...

Страница 81: ... The sieve option allows you to show a Sieve Graph Sieve Listing as well as Define Mesh Sizes The Sieve Graph option allows you to select up to 12 different graphs by distribution type Use this function to define which sieve graphs are printed and their printing order The first graph type appearing in the Graph Printed Order list box defines the order of the sieve data when it is printed ...

Страница 82: ...uantity such as the mean can be plotted versus time of analysis date of analysis or several otherchoices Two options in the Preferences menu determine what information isincluded in the trend reports and listings The Graph option allows you to select the variables to be displayed on the X and Y axes Custom Points lets you select three additional interpolation points The Listing option allows you t...

Страница 83: ...ons 3 Result Options Result Options will allow you to select the units of measure in which the data will be reported i e mm3 for volume The Default View option under this menu lets you choose the display format that will appear at the end of an analysis ...

Страница 84: ...ype and trend limits type It allows file names printed with their full path and an option to add data from other averaged or trend files Data Export Choices in the Data Export dialog allow the user to specify which subsections of the runfile e g the sample info statistics etc will be exported An extension such as xls may be entered so that another application will recognize the exported data ...

Страница 85: ...e Page Setup tab provides all the options necessary to set up how the report will be printed By checking the radio button for Custom Bitmap under the Logo section you can use your company logo on all the reports Just input the folder name followed by the logo file name must be a bitmap file in the dialog box next to the Custom Bitmap option ...

Страница 86: ...PN B05577AC 3 28 LS 13 320 Software Preference Options ...

Страница 87: ...PN B05577AC 3 29 LS 13 320 Software Preference Options 3 Graph Options Under this tab you will find all the option to set up the way graphs will be printed in a report ...

Страница 88: ...th the names of stored preference files Selecting one of these files will alter the appearance and function of the software as defined by all of the choices made in previous parts of this section The default prf file loads automatically each time the program is launched Edit Preferences Info allows the user to change the name and associated comment of a stored preference file Save Preferences writ...

Страница 89: ...name for the preference file under the File Name field Make sure the file is saved under the correct folder If you want this preference to be your default preference use the Save Preference As Default option Loading a saved preference file 1 Select Preferences Preference Files 2 Select Load Preference 3 Choose the preference file from the corresponding folder ...

Страница 90: ... version of software only compliance This option also permits the operation of the software with some degree of security to be able to keep the integrity of the data being acquired by the instrument and stored in electronic form This is done by selecting different levels of security from No Security to High Security from the Security Set up dialog box shown below ...

Страница 91: ...PN B05577AC 3 33 LS 13 320 Software Security Options 3 This diagram summarizes the steps when setting up a security level ...

Страница 92: ...hanged different settings are accessible through the User Privileges options which is accessible only by the administrator These security options can also be selected at a later time If you want to set up the security levels at a later time refer to Regulatory Compliance for more information 1 Select a level of security 2 Add a User 3 The Add a User Account dialog box is displayed The Full Name Lo...

Страница 93: ...quired to sign in by use of a Login ID and a password NOTE The Log in dialog box will automatically close after 60 seconds of inactivity 5 5 2 Types of Users Under the security options there are different types of users with different levels of privileges Depending on the user type menu screens will change providing each user with a range of menu options that can be used to set the operation and s...

Страница 94: ...all the options needed to set up the different privileges for each user The options on the left hand column deal with the creation and saving of methods SOMs SOPs as well as changing and saving preferences The right hand column deals with file operations Under the User Privileges dialog box you may also select the User Settings button to access the User Names and Passwords dialog box The entire lo...

Страница 95: ...ths Select the options in the dialog box and click OK NOTE The dialog has a button marked 21 CFR 11 for the compliant version of software only When activated this ensures all options are set so that the settings meet with the rules as applicable to 21 CFR part 11 Refer to Regulatory Compliance 21 CFR Part 11 for more information ...

Страница 96: ...ail settings allows you to select the events to monitor These events relate to SOMs SOPs as well as analysis runs electronic signatures and preference files For more information on audit trailing see Audit Trail Add a User Account This option enables the Administrator to add additional users 1 Add a User Account 2 Follow the steps under Setting Up For Compliance ...

Страница 97: ...can be edited Note that only the Type of user Log in Name Full Name and ID can be edited View User Account Info This option keeps track of any changes done to a user s account as well as the number of log ins done by the user For all other options under the Administrator menus see Regulatory Compliance 21 CFR Part 11 ...

Страница 98: ...g in steps as long as there is an account set up for a supervisor Both the administrator and supervisor have access to the menu items shown in the figure above Customize Main Menu Choices made in this dialog determine the menus that will NOT be available in the main window when setting up Files Runs and Preferences Clicking on any one of these options will deactivate it ...

Страница 99: ...e when settingupRunFile Edit and View and Analyze Clicking on any one of these options will deactivate it Customize Sample Info Names These options will change the default field name in the Sample Info dialog box For example File ID is the default name for this particular field Using Sample 1 see figure below will change File ID to Sample 1 ...

Страница 100: ...rity there is no need for log in ID s or passwords Any user can make changes to data files without the need for signatures The operator may also create Standard Operating Methods SOMs and Standard Operating Procedures SOPs Access to all the administrator options are also available where changes can be made to any of the options provided i e Audit Trail Settings The editing of files will still be t...

Страница 101: ... Privileges Dialog No Security Low Security Low security requires an administrator to set up accounts for other users A full name log in name and password are required as well as the type of user 1 Select Security 2 From the Security Set Up screen select Low Security ...

Страница 102: ... list box After filling in the dialog boxes with the proper information and selecting OK you will be prompted to add a user account If OK is selected the Add a User Account screen is displayed again EnteringAdministrator Mode and selectingUser Privileges willshowthe default optionsforthislevel of security Refer to Regulatory Compliance for more information on High Security level and 21 CFR Part 11...

Страница 103: ...ith low security Medium Security requires the Administrator to set up accounts for other users The User Privileges dialog screen default in the medium security setting is set so that all users are required to log in but only the administrator and supervisor need a password These options can be changed by selecting the option boxes for each user under the User Privileges dialog screen shown below ...

Страница 104: ... add an electronic signature is left open only for the Administrator and Supervisor High Security High Security requires the Administrator to set up accounts for other users The User Privileges dialog screen default in the high security setting is set so that all users are required to log in and to provide a password These options can be changed by selecting the option boxes for each user under th...

Страница 105: ...PN B05577AC 3 47 LS 13 320 Software High Security 3 Figure 3 5 User Privileges Dialog High Security ...

Страница 106: ...user is logged out after a certain period of time set by the Administrator The user can also log out by selecting Log Out from user dialog box When a user logs out the software will go into a stand by mode showing the log in dialog box as shown in the next figure Selecting Exit from this dialog box will exit the program ...

Страница 107: ...performs data input and operational checks to ensure that valid data is entered into the system and all required steps have been completed to perform the task at hand The purpose of all such data checking and validation allows for strict procedural enforcement within the LS 13 320 software system recording all changes that are made to data generated from within LS 13 320 software File History is e...

Страница 108: ...d Control 21 CFR Part 11 be ensured that audit trail documentation is retained for a period at least as long as that required to maintain records To access the File History information 1 On the RunFile menu click Get File History The History Tracking dialog box displays ...

Страница 109: ... associated with the electronic file itself the LS 13 320 software offers two additional levels of auditing as follows 1 A general system trails all records and stores information at a system level for example who logged in when when users were added to the system and so on 2 Error audit trail stores and records errors associated with the system for example missing files communication errors and s...

Страница 110: ... representation of a user s identity developed to insure the distinct and unique identity of that user The use of electronic signatures as the legally binding equivalent of traditional handwritten signatures then must be certified to the agency in writing Biometric and non biometric forms of electronic signature are methods of verifying an individual s identity based on an individual s physical fe...

Страница 111: ...t be unique No two users on the same LS 13 320 system can have the same user name It is also required that users supply a password to access the LS 13 320 software thus satisfying the requirement of employing at least two distinct identification components identification code and password Passwords can be controlled to prohibit the use of duplicates and to force the selection of new passwords afte...

Страница 112: ...lectronic signature from the pull down options or type a new meaning The Electronic Signature Meanings can be created from the User Privileges dialog box To create the Electronic Signature Meanings 1 From the dialog User Privileges box select Edit Electronic Signature Meanings 2 Type the meaning in the space provided 3 Add 4 Selecting Remove will remove any meaning you highlight ...

Страница 113: ...onfigured to ensure that inappropriate use of these identifiers can be performed only by the intentional divulgence of security information The LS 13 320 software uses the application of the user name and password to authenticate the user making and saving the changes in conjunction with file history and audit trailing to independently record the date and time of operator entries and actions that ...

Страница 114: ...at specified by a user This is done by enabling the data mirroring option which can only be accessed under administrator mode 1 From the Administrator mode select User Privileges 2 Select Data Mirroring 3 Check Enable Data Mirroring 4 Select the drives in which you wish the data to be saved IMPORTANT It is important that drives you are mirroring to are part of your network The computer must be map...

Страница 115: ... You can also choose to mark it as a normal file or as only a hidden file Starting Security Enabled Software After all settings for 21 CFR Part 11 security have been configured every time the LS 13 320 software is started the user is prompted to enter a user name and password The software will automatically configure according to the privileges granted to the user by the administrator ...

Страница 116: ...PN B05577AC 4 10 Regulatory Compliance 21 CFR Part 11 Starting Security Enabled Software ...

Страница 117: ...nFile menu contains options for saving and printing files You can also obtain file information and history Open for Overlay The LS 13 320 software enables you to view more than one data file on the same graph This is useful when you want to compare data from different files To open new data files for overlay 1 RunFile 2 Open for Overlay ...

Страница 118: ...PN B05577AC 5 2 Data File Menus RunFile Menu 3 Select the file you wish to overlay with the current opened file 4 Open ...

Страница 119: ... These changes will be recorded in the File History NOTE When working under a high security level you must provide a reason for any changes After selecting Save the following dialog box is displayed Make an entry in the Reason dialog field and click OK Export The Export option enables you to send selected information about a file to for example a spreadsheet using the file name with a csv comma se...

Страница 120: ...re 5 1 Export Data Dialog Box 2 Click the appropriate export option check boxes 3 By default files export to Microsoft Excel You can select a different location in the Export To section 4 When finished click Export The Preferences dialog box displays ...

Страница 121: ... B05577AC 5 5 Data File Menus RunFile Menu 5 Figure 5 2 Preferences Data Dialog Box Exporting Data 5 Select additional settings as necessary After selecting Settings the following dialog box is displayed ...

Страница 122: ...us RunFile Menu Get Info Information about the run parameters and sample info are contained in this dialog Get File History The file history is linked to the Audit Trail This screen records any changes that have been made to a file ...

Страница 123: ...ple can be edited through this option Under all levels of security except No Security any changes made during the editing process will be recorded in the File History NOTE Expect that all edit options change depending on the level of security Under No Security any user can edit the data file For Low Security the operator and reviewer may edit data only if the administrator selects the options unde...

Страница 124: ... Results option allows you to add or delete data points from the distribution The Auto Step option allows you to create size classes by either adding or multiplying a value entered in the Auto Step dialog field Add an Electronic Signature For compliant version of software only The addition of an electronic signature is controlled by the security level being used Under No Security electronic signat...

Страница 125: ...een This format can be printed as it appears on the screen using the RunFile Print command The data can be displayed in graphical form by listings or by showing a set of interpolation points Graphs Graphs of data can be displayed in different formats The figures below are examples of one type of graph format a listing and an interpolation ...

Страница 126: ... channel and press the left button of the mouse to display a cursor and the channel s value Display Multiple Channel Values Left click on one channel and drag to a second channel to display the cumulative values for the area they delimit The channel values for the lower cursor LC and upper cursor UC also appear Expand Part of a Graph 1 Add two cursors to the graph 2 Point the arrow between two cur...

Страница 127: ...77AC 5 11 Data File Menus View Menu 5 Listing The listing options are shown in the following figure The options selected will be displayed in tabular form with the first column being the first option selected ...

Страница 128: ... view the statistics for the active run file 1 On the Analyze menu click Statistics Statistics information displays Figure 5 4 Statistics information 2 The Statistics page is displayed 3 If working in No Security or Low Security modes select Save or Close NOTE Medium and High Security modes will not allow you to save the Statistics because these are displayed as read only ...

Страница 129: ...h an optical model or to reanalyze size data with a different optical model than the one used when the sample was run See also APPENDIX C Creating an Optical Model To select an optical model 1 On the Analyze menu click Compute Sizes The Select Optical Model dialog box displays Figure 5 5 Select Optical Model Dialog Box 2 Select the appropriate optical model If the optical model is not in the list ...

Страница 130: ...her optical model or to change the results back to the original Only the results from the last optical model used for analysis are stored with the run file e factor This factor also known as the shape factor helps correlate results obtained from the LS 13 320 to those obtained by other methods such as the Coulter Principle SEM etc ...

Страница 131: ...pable of suspending samples in the size range of 0 017 µm to 2000 µm Figure 6 1 Aqueous Liquid Module ALM with Sample Cell The ALM presents the entire sample to the instrument by re circulating the sample The amount of sample needed depends on its size and concentration Prior sample preparation is often needed to achieve proper dispersion see APPENDIX B Sample Handling for more information on how ...

Страница 132: ...mL The ALM has the capability of auto filling and auto rinsing using a self contained internal pump that is operated through software commands The pump fills the vessel to a set level controlled by liquid level sensors refer to Figure 6 2 If the vessel is manually filled an alarm will sound to indicate when the liquid level has reached the overflow sensor this is intended to avoid fluid overflow F...

Страница 133: ...el is being filled Pump indicates that the pump is ON Sonicate turns the sonicator ON the LED is a visual indicator for this state Rinse activates the rinse ring This feature washes the walls of the vessel Figure 6 4 shows the Open Close knob This knob can be used to manually open or close the drain valve The software can also be used to control this valve Figure 6 4 Drain Valve Knob ...

Страница 134: ...ple cell line 2 returns the fluid to the module making it a closed loop system Figure 6 5 Figure 4 Line Locations and Connections Inlet and Drain Hoses Two hoses are used to fill and drain the system These hoses connect to the back of the instrument Figure 6 6 The inlet hose is also connected to a pressure regulator and gauge used to maintain the appropriate water pressure see specifications for t...

Страница 135: ...ch Figure 6 7 Sample Cell 1 Open the LS 13 320 door to load the sample cell by undocking the auto docking tray Press the OPEN button on the instrument and the sliding door moves to the left When it is open press the EJECT MODULE button to extend the tray toward the user 1 Drain Hose 2 Inlet Hose 3 Pressure Regulator 4 Pressure Guage ...

Страница 136: ...gle into the auto dock tray This is done to clear the forward pins and engage the back pins first 4 When these pins have engaged into the slots on the back of the Sample Cell tip the Sample Cell up to its vertical position The Sample Cell should now be resting on the auto dock tray 5 Press the EJECT MODULE button and the Sample Cell will be drawn into the LS 13 320 CAUTION Do not place fingers ins...

Страница 137: ...t the entire module system During this process the drain valve knob will automatically open and close Do not attempt to stop this action manually To stop the system from rinsing select Cancel The Aqueous Liquid Module system can be operated through a series of manual controls accessed through software commands These controls offer flexibility when there is a need to operate the system manually To ...

Страница 138: ...l Close Inlet Closes the inlet valve regardless of how much fluid is currently in the vessel Open Drain Opens the drain valve Once the fluid drops below the bottom level sensor if the pump is ON the pump will be turned OFF Sonicate Applies sonication to aid in the dispersion of the sample Maximum allowable time is 999 seconds The maximum output power by the probe is 73 W 8 1 3 2 Standard Operating...

Страница 139: ...ut a description of both the sample and the SOM being created for this particular sample You can also select the PIDS option if your analysis will include particles in the sub micron region smaller that 0 4 µm If you are using the robot arm select the Robot check box 4 Step 2 allows you to enter specific information about your sample as well as the file name format entered ...

Страница 140: ...ws you to set Run Cycle options such as offsets alignment and background The Run Cycle Options button will take you to the Run Cycle Options dialog box where the measurement times of the offsets background and alignment are set Sonication is also set within this screen ...

Страница 141: ...of surfactant that pump speeds be kept low i e 30 to prevent the formation of air bubbles Should bubbles be present alternating high pump speed with low pump speed is useful when trying to de bubble the suspending fluid If the pump speed is increased to its maximum 100 and then reduced to an approximate 50 air bubbles can be eliminated This procedure may need to be repeated two to three times to e...

Страница 142: ... version ofsoftware only SOMs can onlybe saved by the Administrator Under Operator mode the Save button in step 5 of the SOM creation is not displayed 8 1 3 3 Loading an SOM To load an SOM 1 Run 2 Select Load an SOM 3 Select an SOM file from the list When an SOM is loaded the status panel will display information about the loaded SOM The Start Cycle button will change to Start SOM Clicking on this...

Страница 143: ...s SOPs are the last step in setting all the parameters necessary to fully define restricted operation of the instrument To create an SOP 1 Run 2 Select Create an SOP 3 From the Create an SOP dialog box select an SOM and Preference file 4 Select Save By default the SOP file will be saved under the SOP folder Loading an SOP To load an SOP 1 Run ...

Страница 144: ...ts greater than 43 3 C 110 F and meet the requirements listed below Examples of fluids that can be used in the ALM are water weak aqueous based acids or bases mineral oils ethylene glycol etc The suspension fluid used depends on the type of sample to be analyzed Suspension fluid requirements Chemical Compatibility does not adversely react with the ALM components mentioned above Transparency transp...

Страница 145: ...leaning solution supplied with the module for cleaning the inner surfaces of the ALM sample system Beckman Coulter recommends lens cleaning paper for cleaning the lenses and sample cell windows Cleaning the Cell Clean the inner surfaces of the sample system pump hoses and within the sample cells whenever they become coated To clean the sample system 1 Select Control 2 Select Rinse Rinse for approx...

Страница 146: ...d with your accessory kit to clean the inside of the cell windows 12 Use the same solution prepared in step 6 to swab the windows clean Figure 6 8 PIDS Windows Thumbscrews Make sure you clean both the PIDS and diffraction windows Refer to Figure 6 9 Figure 6 9 Diffraction and PIDS Windows 1 PIDS Windows Thumbscrew 2 Swab with Exstension 3 Cleaning Solution 1 Diffraction Window 2 PIDS Window ...

Страница 147: ...window that is scratched or damaged To replace a diffraction sample cell window 1 Drain liquid from module CAUTION Wear appropriate safety equipment for the suspension fluids being handled 2 Open the Optical Bench door and remove the sample cell 3 Drain remaining liquid in the cell by disconnectingthe two hoses from the line 1 and line 2 ports on the sample cell front 4 Loosen the two nylon screws...

Страница 148: ...tand so the window to be replaced is facing up 6 Stick a piece of masking tape on the window and lift the tape up to remove the O ring and window This may take several tries 7 Discard the old O ring window and nylon screws 8 Hold the new window by its edge to determine the coated side Refer to the figure below to determine which side is the correct one 1 Difraction Cell Window 2 O ring 3 Retaining...

Страница 149: ...ny lens or sample cell window Do not touch optical surfaces with your fingers or skin Body oils are difficult to remove without harming the anti reflective coating 9 Lay the window coated side down on a piece of lens tissue 10 Clean the window using lens tissue wetted with lens cleaner 11 Gently place the window coated side to the outside of the sample cell into the diffraction window opening It m...

Страница 150: ...tion window as described in step 10 19 Replace the window on the other side if needed using steps 4 through 18 20 Insert both hoses into the bottom of the sample cell stand Make sure they are tight 21 Load the ALM sample cell into the optical bench and dock it 22 Perform a leak test a Select Control Fill b After the sample vessel is filled select Control Pump On c If any leaks are noticed after 2 ...

Страница 151: ...dule won t fill Check to see if it is already full Check that connections are air tight Make sure there is enough inlet pressure Module won t drain Check that drain hose is clear of obstructions Pump will not work Module is not completely filled with fluid Check power to the system Sample cell not fully docked Module leaking Check fittings If leakage is inside contact Beckman Coulter service Item ...

Страница 152: ...es a sonicator to aid in the dispersion of samples a tray to dispose of used sample tubes tubing and hoses necessary for the transfer of liquids i e water and dispersants Each sample tube will hold a maximum of 13 mL of liquid The system is fully automatic and controlled via software commands Connecting the APS Hoses The Auto Prep Station is connected to the Aqueous Liquid Module through a set of ...

Страница 153: ... are made through two separate cables that connect from the APS to the right side of the LS bench as shown in the figure above and from the APS to the computer Refer to Figure 6 14 Figure 6 14 Electrical and Communications Connections 1 Inlet 2 Drain from ALM 3 To APS 4 To ALM 1 Cable Connection to the Computor 2 Interface Connection Between APS and LS Bench ...

Страница 154: ...Prep Station Selection of this option will display the Run the Auto Prep Station dialog screen This set up screen allows you to select the sample tube slots that will be used during the analysis as well as providing options for selection of SOMs Auto Prep settings and operation of the carrousel Each slot can be selected individually by clicking on the square next to the slot number This activates ...

Страница 155: ...allows you to load slots that have been previously saved in a file in the same order in which they were saved Load Slot 1 and Up loads slots that have been saved in a file but starting from slot 1 and increasing sequentially Save Slot Settings saves selected slots into a file of type aps File Name Generation see File Name Generation for more information ...

Страница 156: ...nto all other slots Copy Comments copies the comments from one completed slot into all other slots Copy Run Settings copies the SOM from one completed slot into all other slots Copy preferences copies the preference from one completed slot into all other slots Color Options sets the colors to be used with the icons on the Select Auto Prep Slots dialog screen 8 2 3 1 APS Run Menu The Run Menu is us...

Страница 157: ...each option has a different set up All tubes the same selecting this radial button sets all slots to use the same SOM which is selected by clicking on the Load an SOM button Once an SOM is selected it can be removed from all slots by clicking the Remove SOM button as shown in the figure above By slot number Only the slots that have been selected and defined will be used during an analysis when thi...

Страница 158: ...o help optimize your analysis Clicking on the Edit List button displays the following dialog box This dialog is employed to create a list of bar codes that will be used to read the sample tube Bar codes are machine readable symbols made of patterns of black and white bars that encode bits of information The list associates a specific tube to an SOM The bar code is the digital number on the bar cod...

Страница 159: ...ensity alpha numeric coding scheme that uses all 128 ASCII characters It also allows for the inclusion of special characters not present on a keyboard Codabar NW 7 is a numeric only symbol used mostly by libraries and blood banks Code 3 of 9 or code 39 is the most popular for ID inventory and tracking purposes that supports alpha numeric strings Code 93 encodes numbers and upper case letters Inter...

Страница 160: ...ion 2 2 for more information on electrical and communication connections Time out error no communication with module Power cable to ASP not plugged in Does not perform according to selected SOM Wrong SOM type Make sure the SOM selected is for the ALM APS Time out error Auto Prep Station tube pusher motor timed out Tube may be stuck in disposal slot Check the disposal slot Bar code label causes tub...

Страница 161: ... see APPENDIX B Sample Handling for more information on how to disperse samples in order to obtain accurate and valid results MLM Description The Micro Liquid Module is a chemically resistant integrated system consisting of A sample vessel Micro Liquid Cell with stirrer to introduce the sample to the system Main housing consisting of stirrer control and magnetic stirrer motor The system is designe...

Страница 162: ...bottom with the other hand Place it in the auto dock tray by tipping the Sample Cell to the rear at an approximately 30 degree angle into the auto dock tray This is done to clear the forward pins and engage the back pins first 4 When these pins have engaged into the slots on the back of the MLM tip the Sample Cell up to its vertical position The MLM should now be resting on the auto dock tray 5 Pr...

Страница 163: ... The stirrer keeps the sample suspended without creating bubbles Stirrer On Off Will turn the stirrer ON and OFF when manual control is needed Standard Operating Methods SOM The Standard Operating Methods are used in part to assure consistency in the way analyses are performed The options available when creating SOMs are similar to those available when using the Run Cycle Creating SOMs To create a...

Страница 164: ... for this particular sample Figure 6 19 Figure 3 Step 1 of SOM development a Select Fluid to select or edit the suspension fluid to be used figure 4 This screen is a database of common fluids plus any other fluids added by the operator b Edit List to edit or add fluids see figure 5 for Edit Fluid List dialog screen Figure 6 20 Figure 4 Select Fluid Dialog ...

Страница 165: ...he sample as well as the file name format under file name are entered Figure 6 22 Step 2 of SOM Development 5 In Step 3 figure 7 offsets alignment and background are selected The Run Cycle Options button will take you to the MLM Run Cycle Options dialog box figure 8 in which the measurement times for offsets background and alignment are set ...

Страница 166: ...PN B05577AC 6 36 Sample Modules Micro Liquid Module Figure 6 23 Figure 7 Step 3 of SOM Development Figure 6 24 Figure 8 Run Cycle Options Dialog ...

Страница 167: ...It is recommended for samples that require some type of surfactant that the stirrer speed be kept at low speeds i e 30 to prevent the formation of air bubbles Figure 6 25 Figure 9 Step 4 of SOM Development Optical models are also selected from this dialog box For more on optical models refer to APPENDIX C Optical Models 7 Step 5 Figure 6 26 provides the user with a summary of the options selected ...

Страница 168: ...er of your choice as well Figure 6 26 SOM Summary Under high security 21 CFR Part 11 for compliant version of software only SOMs can only be saved by the Administrator UnderOperatormode the Save buttoninstep 5oftheSOM creation is not displayed Loading an SOM To load an SOM 1 Run 2 Select Load an SOM 3 Select the SOM file from the list Figure 6 27 ...

Страница 169: ...PN B05577AC 6 39 Sample Modules Micro Liquid Module 6 Figure 6 27 SOM List Dialog ...

Страница 170: ...ating an SOP To create an SOP 1 Run 2 Select Create an SOP 3 From the Create an SOP dialog box Figure 6 28 select an SOM and a preference file When an SOM is loaded the status panel will show information about the loaded SOM and the Start Cycle button will change to Start SOM Clicking on this button will start an analysis using all the settings unique to that SOM Clicking on the Remove SOM button ...

Страница 171: ... be saved in the SOP folder Figure 6 28 Create an SOP Dialog Loading an SOP To load an SOP 1 Run 2 Select Load an SOP SOPs can also be loaded from the status panel by clicking on the Load SOP button 3 Select the desired SOP file from the SOP subfolder or the subfolder where the file was last saved ...

Страница 172: ...cetone weak aqueous based acids or bases mineral oils ethylene glycol hexane etc The suspension fluid used depends on the type of sample to be analyzed Suspension fluid requirements Chemical Compatibility does not adversely react with the MLM components mentioned above Transparency transparent in the 450nm to 900 nm range Clarity no contamination or extraneous particles Consistency no bubbles Dens...

Страница 173: ...ble and then change to the new suspension fluid Mixing of immiscible fluids will form an emulsion that may be very difficult to remove from the system Figure 6 30 provides a miscibility guide for some common solvents Butanol Butanone Carbon Tetrachloride Chloroform Ethanol Ethylene Glycola Glycerola a These fluids are highly viscous and result in a slower flow rate Use only when diluted so that vi...

Страница 174: ... Guide MLM System Preparation Placing the Cell on the Sample Stand Open the door to the optical bench If the module has been docked undock it Place the sample cell on the sample stand with the locator pin fitting into the locator notch on the sample stand as shown in figure 14 ...

Страница 175: ...Open the door to the optical bench If the sample cell is placed on the stand remove it 2 Remove the cap 3 Tilt the cell toward the back away from the locator pin in order to trap less air inside the cup Pour fluid slowly into sample entry Figure 6 32 Figure 6 32 Cell Diluent Sample Entry 1 Cell 2 Locator Pin 3 Locator Notch ...

Страница 176: ...ple is added to the sample cell until the correct obscuration is obtained To add sample 1 Open the Optical Bench door 2 Remove the cell cap and add a small amount of sample to the sample cell 3 Close the door and note the obscuration 4 Repeat the previous two steps until the correct obscuration is obtained IMPORTANT Do not allow liquid to spill inside the optical bench while loading sample into th...

Страница 177: ...p of the cell 4 Unscrew the cell body from the cup and remove the stirrer bar 5 Remove the O rings from the stirring bar Clean the cell components 1 Wash everything except the cell body in a 2 solution of MICRO Critical lab cleaner Rinse and dry 2 Clean the inside of the cell body by rinsing with acetone or isopropyl alcohol IMPORTANT Do not use any abrasive cleaners in the cell 3 If any particles...

Страница 178: ... is not necessary to take the cell apart every time there is a need for cleaning Adding a small amount of cleaning solution and scrubbing with the swab supplied can also clean the inside of the cell 1 Sample Entry Funnel 2 Cell Body 3 Locator Pin 4 O Ring 5 Stirring Bar 6 Cap 7 Window 8 Cup ...

Страница 179: ...eck fittings The Tornado Dry Powder System is intended for use with the LS 13 320 Optical Bench It is capable of feeding and measuring dry powder samples in the size range 0 4 µm to 2000 µm The Tornado DPS measures the entire sample presented to the instrument with a sample volume that allows an analysis that will provide statistically accurate results The range of sample volumes the instrument ca...

Страница 180: ...the samples are run wet with proper manual pre dispersion The sample to be measured is contained in the system to prevent airborne contamination of the work area throughout This is accomplished by maintaining a negative pressure vacuum system for the sample path and trapping the sample via a filtration system in the vacuum Indicators A set of LEDs mounted in the front panel of the module provide v...

Страница 181: ... have engaged into the slots on the back of the DPS tip the Sample Cell up to its vertical position The Tornado module should now be resting on the auto dock tray 5 Press the EJECT MODULE button and the Tornado will be drawn into the LS 13 320 CAUTION Do not place fingers inside bench as automatic sliding door closes Do not place fingers inside bench as module docks into bench It is sometimes nece...

Страница 182: ...rnado DPS Feed Sample Raises the sample lift This cycles with either the vacuum on vacuum off options selected allowing for feeding the sample to the system and maintaining the obscuration that has been pre set in the preference file Selecting Sample Lift Home stops this command Sample Lift Up Sample Lift Home moves the lift to its maximum height and back to its home stage Useful when cleaning the...

Страница 183: ...ating Methods SOM The Standard Operating Methods SOMs are used in part to assure consistency in the way analyses are performed The options available when creating an SOM are similar to those in the Run Cycle dialog Creating SOMs To create an SOM 1 Run 2 Select Create an SOM A sequence of screens will guide you through the creation of an SOM 3 Step 1 prompts you to input descriptions of the sample ...

Страница 184: ...l as the file name format under the file name is entered 5 Step 3 Run Cycle options such as offsets alignment and background are set during this step The Run Cycle Options button will take you to the Run Cycle Options dialog box in which the measurement times for offsets background and alignment are set ...

Страница 185: ...Tornado DPS this value should be between 4 and 8 The ISO 13320 standard suggests an obscuration value of 5 ISO 13320 1 Particle size analysis Laser diffraction methods Part 1 General Principles Section 6 2 4 page 8 The Directory option allows the user to select a specific folder to save the data in or to simply utilize the current folder for saving data ...

Страница 186: ...Administrator UnderOperatormode the Save buttoninstep 5oftheSOM creation is not displayed 8 4 3 3 Loading an SOM To load an SOM 1 Run 2 Select Load an SOM 3 Select the desired SOM file from the SOP subfolder or the subfolder where the file was last saved When an SOM is loaded the status panel will show information about the loaded SOM and the Start Cycle button will change to Start SOM Clicking on...

Страница 187: ... the SOMs and the preference files thus setting all the parameters necessary to fully control the operation of the instrument as well as data presentation Creating SOPs To create an SOP 1 Run 2 Select Create an SOP 3 From the Create an SOP dialog box select an SOM and preference file 4 Select Save By default the SOP file will be saved under the SOP folder ...

Страница 188: ... can cause erroneous results Some samples may coat the inside of the sample cell windows If the instrument is in a dusty or smoky environment or if vapors are present the lenses and outer surfaces of the windows may become coated Check the optical surfaces forcleanliness at least every three months and clean if needed Depending on the environment cleaning may be required more frequently Using the ...

Страница 189: ...odule housing 1 Loosen the screws that hold the bracket in place Lift the bracket to disengage the pins from the pin slots See Figure 6 36 Figure 6 36 Bracket Screws 2 Undo the four top and bottom latches found in the back of the module that attach the sample cell to the module housing Figure 6 37 1 Pin 2 Bracket 3 Slot 4 Screw Securing the Bracket ...

Страница 190: ...Cell Latches 3 Remove the sample cell Clean the inner and outer surfaces of the sample cell windows refer to Figure 6 38 whenever they become coated To clean the cell windows 1 Remove the set of screws holding the window you wish to clean Remove the window 1 Sample Cell Latches ...

Страница 191: ...s tissue 4 Place the lens tissues on the window surface holding the tissue in place with two fingers 5 Slowly wipe the window 6 Discard the used lens tissue 7 Re assemble the windows and sample cell Cleaning the Sample Tubing The lines that carry the sample into the sample cell may need to be cleaned separately when the sample cleaner cannot clean them completely 1 Screws 2 Sample Cell Windows ...

Страница 192: ...ove the module cover by undoing the two latches found in the back of the module Figure 6 39 Figure 6 39 Cover Latches 2 Remove the wall impact plate by removing the four screws Refer to Figure 6 40 Figure 6 40 Wall Impact Plate 1 Cover Latches 1 Wall Impact 2 Screw ...

Страница 193: ... direction shown by the arrows in Figure 6 41 Use the same brush to clean the tube that runs perpendicular to the suction tube and runs towards the sheath flow tube Figure 6 41 Suction and Sheath Flow Tubes Cleaning the Sheath Flow Filter 1 Remove the module cover by undoing the two latches found in the back of the module Figure 6 39 1 Sheath Flow Tube 2 Suction Tube ...

Страница 194: ...on Module not responding Module docked incorrectly LEDs will not light Eject module and re dock Apply slight pressure on the front of module while docking If LEDs turn on check cable from optical bench to the computer Vacuum will not start Check that vacuum is plugged in Check that vacuum remote power switch is in the ON position Check that remote power switch cable is connected to the optical ben...

Страница 195: ...ter missing Install filter Leaks Tighten windows screws Sheath flow tube plugged Clean tube Vacuum bag full or filter clogged Replace vacuum bag and or filter High vacuum pressure Suction nozzle plugged Clean nozzle Sheath flow filter dirty Clean or replace filter Problem Possible Cause Solution ...

Страница 196: ... F Humidity 0 to 90 without condensation Dimensions Height 46 4 cm 18 25 in Width 20 3 cm 8 0 in Depth 21 6 cm 8 5 in Weight 8 2 kg 18 lb Vacuum System Flow rate 420 L min Pressure 740 to 750 torr 15 cfm at 5 to 10 inches of H2O below atmospheric pressure The ULM measures the entire sample introduced to the instrument by re circulating the sample The amount of sample needed depends on its size and...

Страница 197: ...mp is controlled by an automated level sensor that signals when the container is full or empty The pump fills and rinses the unit automatically expelling all waste into a waste container provided with the module Loading the ULM 1 Open the LS 13 320 door to load the ULM by undocking the auto docking tray Press the OPEN button on the instrument and the sliding door moves to the left When it is open ...

Страница 198: ...on The ULM should now be resting on the auto dock tray 5 Press the EJECT MODULE button and the MLM will be drawn into the LS 13 320 CAUTION Do not place fingers inside bench as automatic sliding door closes CAUTION Do not place fingers inside bench as module docks into bench ULM Software This section covers the controls found in the software program to operate the ULM It also covers the parts of t...

Страница 199: ...opens the inlet valve to fill the vessel with the diluent The drain valve if open will be closed Make sure the fill hose is completely submerged in the diluent Rinse Selecting this option will start an automatic rinse cycle The order of operations is Open Drain Close Drain Fill and Pump On This cycle is repeated for a set number of times set in the Run Cycle Options dialog box De bubble This routi...

Страница 200: ...en Inlet Open Drain Close Drain Opening the drain will stop the pump automatically when the fluid level falls below the bottom sensor If Fill orRinse is selected thedrainis automatically closed You can have thedrainopen while adding fluid to the vessel by selecting both the Open Drain and Open Inlet options at the same time Only in this set up will the pump stay on 8 5 3 2 Standard Operating Metho...

Страница 201: ...sal Liquid Module 6 3 Step 1 prompts you to input a description of both your sample and the SOM you are creating for this particular sample 4 Step 2 information about the sample as well as the file name format under the file name is entered ...

Страница 202: ...ons such as offsets alignment and background are set during this step The Run Cycle Options button will take you to the Run Cycle Options dialog box in which the measurement times for offsets background and alignment are set Run Cycle Options are selected from this screen as well ...

Страница 203: ...ted in this dialog It is recommended for samples that require surfactant that the pump speed be kept low i e 30 in order to prevent the formation of air bubbles Should bubbles be present alternating high pump speed with low pump speed is useful when trying to de bubble the suspending fluid If the pump speed is increased to its maximum 100 and then reduced to about 50 air bubbles can be eliminated ...

Страница 204: ...iant version of software only SOMs can only be saved by the Administrator UnderOperatormode the Save buttoninstep 5oftheSOM creation is not displayed 8 5 3 3 Loading an SOM To load an SOM 1 Run 2 Select Load an SOM 3 Select the desired SOM file When an SOM is loaded the status panel will show information about the loaded SOM and the Start Cycle button will change to Start SOM Clicking on this butt...

Страница 205: ...d Operating Procedures SOPs is the last step in setting all the parameters necessary to fully control the operation of the instrument To create an SOP 1 Run 2 Select Create an SOP 3 From the Create an SOP dialog box select an SOM and preference file 4 Select Save By default the SOP file will be saved under the SOP folder ...

Страница 206: ...eater than or equal to 0 6 and that meet the requirements listed below Examples of fluids that can be used in the ULM are water acetone weak aqueous based acids or bases mineral oils ethylene glycol hexane etc The suspension fluid used depends on the type of sample to be analyzed Suspension fluid requirements Chemical Compatibility does not adversely react with the ULM components mentioned above T...

Страница 207: ...cible and then change to the new suspension fluid Mixing of immiscible fluids will form an emulsion that may be very difficult to remove from the system Figure 6 43 provides a miscibility guide for some common solvents Butanol Butanone Carbon Tetrachloride Chloroform Ethanol Ethylene Glycola Glycerola a These fluids are highly viscous and result in a slower flow rate Use only when diluted so that ...

Страница 208: ...dusty or smoky environment or if vapors are present the lenses and outer surfaces of the windows may become coated Check the optical surfaces for cleanliness at least every three months and clean if needed Depending on the environment cleaning may be required more frequently Cleaning Fluids Beckman Coulter recommends using the cleaning solution supplied with the module for cleaning the inner surfa...

Страница 209: ...ver they become coated To clean the sample system 1 Select Control 2 Select Rinse 3 Select Open Drain after the Rinse routine has finished 4 Prepare the cleaning solution 5 Place the inlet hose into the container of cleaning solution 6 Select Fill 7 Let the cleaning solution circulate for 15 minutes to 1 hour depending on how dirty the cell is 8 Select Control Rinse ...

Страница 210: ... cover you will have access to the inside of the cell This will allow you to insert a swab with an extension provided with your accessory kit to clean the inside of the cell windows Figure 6 45 Cleaning Inside the Cell Windows 11 Use the same solution prepared in step 1 to clean the windows with the swab 1 ULM Cell Window Cover 2 Cell Cover Thumbscrews 1 ULM Module 2 Cell Window 3 Exstension Swab ...

Страница 211: ... Use this procedure to replace a diffraction sample cell window that is scratched or damaged To replace a diffraction sample cell window 1 Drain liquid from module CAUTION Wear safety equipment appropriate for the suspension fluids being handled 2 Eject module 3 If there is liquid remaining in the cell drain it by applying pressure on the two levers at the same time Refer to Figure 6 47 1 Diffract...

Страница 212: ...Cell Window Levers 4 Loosen the two nylon screws to remove each window Refer to Figure 6 48 Figure 6 48 ULM Cell Window Nylon Screw Removal 1 Difraction Cell Window Levers 1 Difraction Cell Window coated side out 2 O ring 3 Retaining Ring 4 Nylon Screws 5 Sample Cell 6 Supply Hose ...

Страница 213: ...end of a pencil and hold it close to the window near its edge Note the two reflections of the pencil dark and light colored b Turn the window over and repeat step a c The side that reflected a dark reflection is the coated side CAUTION Use lens tissues only once then discard Never use silicone coated eyeglass lens tissues to clean lenses or sample cell windows as this type of tissue may leave a fi...

Страница 214: ...wn and around the window 16 Clean the retaining ring then gently place it on top of the window 17 Replace the two new nylon screws that hold the retaining ring 18 Clean the outer surface of the diffraction window as described in step 10 19 Replace the window on the other side if needed using steps 4 through 18 20 Insert both hoses into the bottom of the sample cell stand Make sure they are tight 2...

Страница 215: ...kman Coulter service Module will not drain Check that the waste container is not full Check that the drain hose is clear of obstructions Pump will not work Module is not completely full of fluid Check power to the system Check belt drive Module leaking Check fittings If leakage is inside contact Beckman Coulter service Item Specification Power The ULM derives its power directly from the optical be...

Страница 216: ...PN B05577AC 6 86 Sample Modules Universal Liquid Module ...

Страница 217: ... Humidity 0 to 90 without condensation Dimensions Unit Height Width Depth Optical Module 44 5 cm 17 5 in 101 cm 40 in 25 4 cm 10 in Computer Processor with Disk Drive 13 cm 5 in 36 cm 14 in 41 cm 16 in Monitor 32 cm 12 5 in 32 cm 12 5 in 41 cm 16 in Printer 23 cm 9 in 39 cm 15 5 in 41 cm 16 in Weight 71 5 lbs 32 5 kg Altitude Sea level to 3 000 m 10 000 ft Laser Classification I for operator no ac...

Страница 218: ...on Aqueous Liquid Module approx 10 mg to 100 g Universal Liquid Module approx 1 mg to 10 g Micro Liquid Module approx 1 mg to 50 mg Tornado Dry Powder System approx 5 cc to 30 cc Data Presentation Video display and hard copy printouts Data Formats Listing Intensity Detector group intensity flux picoamps and millivolts Background flux and picoamps Offset millivolts Gains for the diffraction and PID...

Страница 219: ...tc These are generally used to keep particles in suspension while attempting to draw a measurement sample Even though these techniques are effective in obtaining a representative sample from liquid the overall sampling for powder samples will be representative only when the initial solid sampling is performed correctly Solid Sampling The sampling of powders involves a reduction process from bulk s...

Страница 220: ...eeder supplies a constant flow rate to the collection boxes which move in a circular motion This method according to statistics yields the most accurate results It is recommended that samples be subdivided to the amount of a gram and the sample must be free flowing Figure B 1 Figure 1 Spinning Riffler Chute splitter The sample is placed in a V shaped hopper and migrates down a series of chutes tha...

Страница 221: ... plane The sample stream flows downward and is broken up into fractions as it encounters prisms and holes The draw back of this device is that it depends on the initial feed being uniformly distributed and complete mixing after each separation Thus accuracy is low since errors are compounded at each separation Figure B 3 Figure 3 Table Sampling ...

Страница 222: ...hoping that all four parts are symmetrical If symmetry does not exist in the cutting and flattening of the heap size error will occur This method is greatly dependent on the skill of the operator and consequently should not be used Figure B 5 Figure 5 Cone and Quartering Liquid Sample Dispersion Dispersion can make or break the analysis regardless of the particle analyzer being used in the experim...

Страница 223: ...wders in both aqueous and non aqueous media are quite similar Dispersants aid wetting and stabilization of a suspension and can be ionic anionic or cationic or non ionic However concentrations of dispersants must be low Otherwise their properties are reduced or even inverted i e cause aggregation or flocculation In dispersing a powder in a nonaqueous medium it is critical to select an organic solv...

Страница 224: ...a potential is at least 30 mV Common Ions A solution containing a dissolved ion which is the same as one found in the sample s molecular lattice may help disperse that sample by adsorbing and charging the surface of the particles However be careful for solvation effects Multiple charged Ions For ionic particles or particles with polar bonds in water multiply charged ions that are not part of the c...

Страница 225: ...he sample to form a thick paste Spatulate use spatula rubber policeman etc to mull the sample and the dispersant into a paste Add diluent add diluent to form a slurry Optical check use a microscope to visually check the status of the dispersion If the dispersion appears incomplete then either try another dispersant or add more energy to the system taking care not to disrupt the integrity of the pa...

Страница 226: ...black are available Fumed silica when added to particulate systems 0 5 1 wt can help the flow of the dry powder because of its ball bearing effect The same mixing ratio 0 5 1 can be used for tricalcium phosphate Also its overall effect on particle size measurement can be negligible Sometimes anti static aids such as sprays and a static bar are needed to eliminate static charges Diluent Selection C...

Страница 227: ...nstrument s polyethylene fill and waste tanks over time 2 Will the diluent degrade the instrument s stainless steel fill and waste tanks over time 3 Will the diluent degrade any wetted materials in the instrument Purity 1 Is the diluent chemically pure 2 Is the diluent free of interfering particles If not filtering may be appropriate Refractive Index Is the R I of the diluent the same or very clos...

Страница 228: ...PN B05577AC B 10 Sample Handling Diluent Selection ...

Страница 229: ...needles or rods or birefringent materials the resulting size distribution may not be accurate Refractive Index The complex refractive index consists of a real part and an imaginary part The real part is what is generally thought of as the refractive index the imaginary part represents the absorption coefficient of the material The real part of the refractive index of most samples and suspension fl...

Страница 230: ...when the wavelength dependence of the refractive index is large such as with colored pigments and toners Creating an Optical Model To make an optical model 1 Run and select Make Optical Model IMPORTANT Clicking the R I Table button will open the Refractive Index table Clicking on the Dry Powder Module check box will disable the Extended Optical Model PIDS and will switch to the rff file name exten...

Страница 231: ...for the fluid suspension fluid See Table 1 If the Tornado DPS is being used enter 1 in this field 6 Enter the real and imaginary parts of the refractive index for the sample to be analyzed An optical model can also be created from the RunFile menus or during the creation of a Standard Operating Method SOM Creating an Optical Model from the RunFile Menu From the RunFile menus 1 Analyze ...

Страница 232: ...Make Optical Model is displayed Follow steps 2 through 6 above under Creating an Optical Model Optical models are files that are saved in the opmodels folder under the LS 13 320 main folder These files use extensions that indicate the type of analysis that the model is to be used for All optical model files used with LS 13 320 benches that are equipped with the 750 nm laser use a file extension th...

Страница 233: ... appropriate for particle size distributions that are closer to log normal A log normal distribution is symmetrical when plotted on a logarithmic size scale The statistical formulas used by the LS 13 320 software and a brief description of each are presented in the next sections User Defined Mean There are two general formulas for the user defined mean diameter D p q one for arithmetic means and o...

Страница 234: ...eviation coefficient of variation confidence limits skewness and kurtosis characterize the shape of the particle size distribution A normal distribution is symmetric in shape in a linear horizontal axis and a log normal distribution is symmetric in shape in a logarithmic horizontal axis Many statistical measurements use the normal curve or log normal curve as a reference Variance Table C 1 Mean Di...

Страница 235: ...bout which it is measured The CV s utility is in measuring relative variation as opposed to absolute variation Skewness Skewness g1 is the degree of distortion from symmetry of a distribution Both the degree and direction of skewness may be determined from the following equations Geometric The standard deviation SD is the square root of the variance Arithmetic Geometric Va fi xi x 2 fi Vg 2 fi xi ...

Страница 236: ...ess coefficient is negative g1 0 Kurtosis Kurtosis g2 is a measure of the peakedness of a distribution It is calculated by determining moments about the mean from the following equation The normal or Gaussian distribution is the standard against which the peakedness of other curves is measured A normal distribution is referred to as mesokurtic g2 0 If the distribution has a higher sharper peak tha...

Страница 237: ... Models Statistics C If the distribution has a lower broader peak than a normal curve then it has a smaller degree of kurtosis and is termed platykurtic g2 0 In this type of distribution the particle sizes are more widespread ...

Страница 238: ...PN B05577AC C 10 Optical Models Statistics ...

Страница 239: ...is flux pattern Figure D 1 is an example of a good background pattern Figure D 1 Normal Background If the current background flux pattern is higher in any channel by a factor of two the cause should be determined and remedied before running further samples Figure D 2 and Figure D 3 are examples of bad backgrounds and their causes To check the background flux pattern on a sample run 1 View 2 Intens...

Страница 240: ...PN B05577AC D 2 Troubleshooting Background 3 Graph Background Flux Figure D 2 Background Showing the Presence of Bubbles Figure D 3 Background Showing the Presence of Contaminants ...

Страница 241: ...ction you will need to check the background again to verify if the problem is solved Use the following diagram as a guide in checking the background Reference Background Set Up Backgrounds are an integral part of a particle size analysis to obtain correct and accurate results This document will guide you through the necessary steps to set up a reference background that can be used to compare the b...

Страница 242: ...nd obtained from one optical bench cannot be used on a different optical bench Likewise a reference background obtained on an MLM cannot be used on an ULM etc Part 1 Setting Up a Reference Background An acceptable reference background will be one that is within the recommended flux intensity These values are 2 5x106 for either channel 1 or 2 2 0x106 for the sum of channels 10 to 40 up to 20 for th...

Страница 243: ...PN B05577AC D 5 Troubleshooting Reference Background Set Up D 3 Select all options as shown in the figure above 4 From the Run dialog select Options to display the Run Cycle Options dialog screen ...

Страница 244: ...ns page ensure that the box for Show Reference Background is not checked if there is a loaded background file If no background file is loaded the screen will appear as shown in the figure below a Select 60 sec for Measure Offsets b Select 60 sec for Measure Backgrounds c Then click OK ...

Страница 245: ...e the run 7 After the run is complete select Run Cycle Options from the Run menu 8 Select New Reference Background Select the file you saved in step 6 This file will be assigned a new name under the following format Filename changes as follows Z BKxxxx ls Where is substituted by the module code U for the ULM A for the ALM P for the Tornado DPS and M for the MLM The last 4 digits of the optical ben...

Страница 246: ...tions 3 In the Run Cycle Options page select Show Reference Background Select the file created under step 8 above Click OK 4 When the software gets to the Background graphics page during measurement there should now be 2 curves showing One is the reference curve and the other is the current measurement labeled untitled ...

Страница 247: ...s for cleanliness at least every three months and clean if needed Depending on the environment cleaning may be required more frequently Cleaning Fluids Beckman Coulter recommends the cleaning solution provided with your instrument to clean the inner surfaces of the sample modules Beckman Coulter also recommends LENS CLENS NO 1 lens cleaner for cleaning the lenses and sample cell windows Cleaning t...

Страница 248: ...ample cell window Do not touch optical surfaces with your fingers or skin Body oils are difficult to remove from lenses without harming the anti reflective coating 2 Fold three to four tissues in half 3 Squirt lens cleaner onto the creased area of the folded lens tissue 4 Place the lens tissues across the upper Fourier lens holding the tissue in place with two fingers Refer to Figure E 1 Figure E ...

Страница 249: ...n Lens Use this procedure to clean the projection lens To clean the projection lens 1 If a sample module is docked undock it if not open the Optical Module s door CAUTION Use lens tissues only once then discard Never use siliconecoated eyeglass lens tissues to clean lenses They can leave a film Wash your hands thoroughly before cleaning any lens or sample cell window Do not touch optical surfaces ...

Страница 250: ...lens must be replaced Call your local Beckman Coulter Representative 7 Carefully inspect the lens surface for cleanliness by shining a bright light on it and looking at the surface from all angles 8 Dock the sample module back into the instrument 9 Select the Measure Offsets Auto align and Measure Background functions in the Run Cycle dialog box before running your next sample 1 Projection Lens 2 ...

Страница 251: ...ided that it is used on the computer hardware and in the operating system environment for which it was designed Should the media on which your software arrives prove defective Beckman Coulter will replace said media free of charge within 90 days of delivery of the Product This is your sole remedy for any breech of warranty for this software Except as specifically noted above Beckman Coulter makes ...

Страница 252: ...PN B05577AC Warranty 2 Beckman Coulter Inc Customer End User License Agreement ...

Страница 253: ......

Страница 254: ...mancoulter com Related Documents LS 13 320 Laser Diffraction Particle Size Analyzer Instructions for Use PN B05577 Introduction Theory Installation LS 13 320 Software Regulatory Compliance 21 CFR Part 11 Data File Menus Sample Modules Appendices References ...

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