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1. Into the menu Tools Identification you can manage these options using the Delete button It can be used to delete a user name Be careful when removing users Once the username has been deleted you can not restore it You can also change of username using the Select button We have described all the items needed to configuration The Particle Expert software Please configure the software carefully Problems can occur if the user makes bad choices for the settings described in this section 5 7 OPTIONAL ACCESSORIES There are a number of accessories available for your CILAS particle size analyzer These options are designed to better meet all your measurement needs If you have a special need our accessories can solve your problem and improve your measurements The accessories are autosampler improves your productivity when performing routine analysis controls production etc small volume unit a device for reducing the amount of sample and solvent necessary to perform a measurement video camera allows the user to see the shape and the sample dispersion alcohol regenerator reduces the amount of solvent necessary for analysis which results in less waste removal The Particle Expert software controls all of the CILAS accessories If you want to know more about these different devices please refer to the specific User Manual available on your USER CD ROM 63 COMMUNICATION REPRO
2. Users are not authorized to perform corrective maintenance If they do it is under their own responsibility and the warranty will become invalid To reduce the time it takes for maintenance communicate to your dealer as soon as the file Bug report doc is completed The bug report will help him to quickly locate and solve your problem This document is available in your USER CD ROM in the software section of the appendix 6 4 ANSWERS TO FREQUENTLY ASKED MAINTENANCE QUESTIONS If you have additional question or would like advice about the maintenance of your particle size analyzer please see the file available on our website download at www particle size analyzer com or in the USER CD ROM Frequently ask questions pdf You can also contact your local CILAS dealer 72 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 PART 7 SPARE PARTS 73 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 User replaceable items for your CILAS particle size analyzer can be ordered from CILAS A list of these items and their part numbers are provided in the appendix of your USER CD ROM Ori
3. X Z US during dispersion Time 60 s L Mie Report config I Specific surface Erase config I US during measurement T Mono histogram Options SSS Background meas 0 Gample measurement ext Acton Close Help FIGURE 11 Selection of the measurement parameters in wet mode This window allows you to define and to control the measurement First you have to define the parameters of the measurement 34 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 Y Definition of the measurement parameters 9 Before beginning a measurement you will need to define some parameters in the measurement window You will do this at the top of the window In the section called SOP name select from a list of Standard Operating Parameters SOP already defined and saved The list of SOP will appear if you click on the right side of the box SOP contains parameters such as the theory used operating conditions etc You can also create and save a new SOP using the button Save SOP The SOP is designed to provide good reproducibility in your results NOTE A SOP contains all the measurement parameters you have to set on the CILAS particle size analyzer CILAS recommend that you define and save one SOP for each specific product Please name the fi
4. yea X No dispersing Dispersing agent at good High concentration of agent wrong ratio good dispersion dispersing agent wrong dispersion dispersion FIGURE 8 Dispersing agent The amount of dispersing agent introduced in the tank must be not too low and not too high in order to have good dispersion of the product into the carrier liquid The main dispersing agents used are HMP HexaMetaPhosphate Tetra Sodium pyrophosphate Igepal Daxad Dispex Tween 80 Triton The most common are Igepal HMP Tetra Sodium pyrophosphate and Daxad Please always check that the dispersing agent has all the properties listed in the previous section Once the operating conditions are defined the SOP should remain the same for each similar product Before making measurements with a new type of sample please use a microscope or similar device to make sure that you have good dispersion When proper dispersion is obtained you can begin making measurements in wet mode with your CILAS particle size analyzer 5 3 b Making a measurement in wet mode This section describes how to make a measurement in wet mode The measurement is described in several steps Please carefully follow the procedure below 1 Turn on the CILAS particle size analyzer the water or solvent supply and all the accessories if necessary 2 Turn on the PC and launch The Particle Expert software 3 Enter as shown on the figure below your user name your level defined b
5. 15 Fill with water and check to be sure that it does not have a leak S 9 7 FIGURE 30 Sample cell holder 71 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 6 3 MAINTENANCE FOR DEALERS AND AUTHORISED PERSONS This chapter covers corrective maintenance operations Only technicians accredited by your CILAS dealer can perform these actions Corrective maintenance operations need to be made if a problem occurs with the hardware or the software CILAS particle size analyzers will identify a problem when one occurs The system will inform you of the problem via The Particle Expert software During a measurement an error message would appear on the monitor screen If an error message appears there is a problem and the error message is an alarm When an error message occurs the user needs to do the following note the error message provided by the software note the model and the serial number of your particle size analyzer note the version of The Particle Expert software you are using fill in the Bugreport doc document available in the appendix of your USER CD ROM contact your local CILAS dealer They will need all the above information in order to diagnose the problem A technician will proceed with maintenance operations
6. NT 1503192 31 Issue September 2004 PARTICLE SIZE ANALYZER CILAS 920 930e 1064 amp 1180 USER MANUAL 8 avenue Buffon BP 6319 ZI La Source 45063 ORLEANS Cedex France T 33 238645900 amp 33 238 6459 07 E Mail info particle cilas com Web site www particle size analyzer com I COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 USER MANUAL UPDATES This page contains the history of the CILAS particle size analyzer user manual The first version was published in 2001 under version number NT 1503192 31 The table below shows the changes in each version Version number Date Modification First Version 2001 Creation Second version September 2004 Complete update After each update a new version number is give to the user manual and the following information will be noted in this section the new version number the modification date alist of what has been modified This allows users to be informed of all the modifications to this manual made by CILAS II COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 SUMMARY ABOUT THIS MANUAL Page 1 SCHEMATIC SUMMARY Pag
7. automatic display of the results after the measurement with Display measurement automatic printing of the report after each measurement automatic display of the last results with Show last measurement automatic display of the histogram and the cumulative curve for each measurement 56 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 On the right side you can set up the following the acquisition window by choosing whether or not you want to see the value of the signal during the measurement the calibration if you want to use a calibration file from another particle size analyzer active the Different serial number box automatic save to the database This option is highly recommended by CILAS To validate your settings click on Validate You can also cancel the changes quit the window or ask for help Once your settings are validated they are used by default as the standard parameters y Display In this section you can set up all the parameters that affect how the results are displayed To understand the definition of these parameters please refer to section 3 2 in this manual In the display set up window you have the following options Display in choose how the cumulative values amp diameters are displayed in the
8. button you can choose the standard language of the software If you select the Logout box you will choose whether or not to active the security levels You can also set your company name and location which will be set to the default You can add your company s logo so you will see it on each report To load the image click on the button Then set the two parameters Criterion 1 and Criterion 2 These parameters will be requested for each measurement and stored in the results file in the database By default the two parameters are the type of product and the customer s name Y Organization In this section you can set the parameters for the acquisition and display On the left side you have a section dedicated to acquisition You can activate or deactivate by selecting the box from up to down an automatic background for each measurement reloading a background measurement already saved for each measurement force all the measurements in the list of selected measurements in active state you can no longer deactivate them using the button Forced selection require criteria 1 and 2 to be filled in before executing a measurement with Bounded Criteria automatic export of the results after each measurement choice of SOP between the standard SOP and a user defined SOP setting the acquisition time if you select the box you will have a standard time of acquisition for each measurement
9. 140 920L 139 V Quality 2 01 01 20 141 920L 139 V Quality 1 01 01 20 142 920L 139 V Quality 1 01 01 20 143 920L 139 V Quality 2 01 01 20 1447920 V Meas Quality 01 0172 lt 145X920L V Meas Qualty2 01 0172 146 920L V Meas Quality3 atarax lt lt l Nb of measur 17 l Selected Measurements 2 Validate FIGURE 21 Searching the measurement files The window contains four parts In the upper part you will need to enter the parameters used to search for the measurement file You can search for files using the following parameters the name ofthe product measured the date of the measurement the customer which requested the measurement the operator who made the measurement You can also search just the most recent files by selecting the Today box This allows you to search only the files with the selected parameters that were taken on the day selected NOTE The date is in your country s standard format If you do not want to apply any criteria for your search please select All in each box Then all the files stored in the database will appear You can preview the histogram for the selected file in the left corner of the window You can enable this option by selecting the Automatic preview box When you have found the file you want select it by clicking on it If you want to view it you will need to move the file into the right list using the gt button If you wan
10. 2 1 diameter The mathematical formula is Dn xd xd SER Sin xd xd Where ni number of ees of class di diameter of class 1 i bed In The Particle Expert software diameter in surface is calculated from value of diameter in volume DIAMETER WITH LOG NORMAL Log Normal law is a good model for cumulative values of samples such as ceramics It is called L and its mathematical equation is as follows LD L LD j i gt l 20 Where Ci cumulative value for diameter class 1 In D for class i C C H _1_ _ __ histogram value for class i sigma parameter of Log Normal law LD LD l 17 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 L LD must match with Hi The integration of L gives the cumulative values of Log Normal law similar to Cj Y DIAMETER WITH ROSIN RAMMLER Rosin Rammler law is a good model for cumulative values of samples such as cement or sand It is called R and its mathematical equation 1s R Dj 1 ost 2 Where Ci cumulative value for diameter class i 66599 Di diameter for class i in um A and B parameters found using mean square error minimization to match the sample R Dj must match Cj y DISPERSING AGENT The dispersing a
11. 5 b Loading results before the measurement Using the database you can view any results that you want This is a big advantage provided by your CILAS particle size analyzer It allows you to use The Particle Expert software to compare results obtained today with those obtained one year ago Y Searching for a file in the database To open a file already stored in the database you need to click on the button or select the menu File Results A window will appear on the screen Look in the box to see the files that are already loaded If you find all the files you wanted in that list you have already loaded the files If the files are not loaded click on the Modify selection button The following window will appear on the screen 48 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 IV Automatic preview Type produit All x Client Jail 7 Operator ay z M Dates from 01701 2000 To 2070272004 T Today Request issue Selected measurements VY 920LE 01 01 2000 119 1180L Vo 1180L 01 01 2000 41 920D Y 920DE 012017200 194 1180D 119 V 1180D 01 01 2004 42 1064L W 1064LE 01701720C 43 1064D V 1064DE 01 01 20 we 44 940L V S40LE 01 01 2000 45 340D Y 940DE 01 01 200 95 HR850 Y 850LE 01 01 200
12. 7 Save SOP Sample ref ooo P Automatic incrementation Type produit hed Client Comments Poo Operator ha Distribution value 3 I Auto Mie red Tl Specific surface Erase config I Mono histogram Options Background meas d Help FIGURE 17 Selection of the measurement parameters in dry mode 42 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 This window allows you to define and to control the measurement First you have to define the parameters of the measurement Y Definition of the measurement parameters 8 Before starting the measurement you have to define some parameters at the top of the measurement window In the section called SOP name select from Standard Operating Parameters SOP already defined and saved A list of SOP appears when you click on the right side of the box SOP contains parameters such as the theory s used the operating conditions etc You can also save a new SOP using the Save SOP button The SOP is designed to provide you good reproducibility of your results NOTE A SOP contains all the measurement parameters you have to set on the CILAS particle size analyzer CILAS recommends that you define and save one SOP for each specific product Please name the file with an
13. DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 11 In another section you can define the parameters used for the interpretation of results You can select three options The first selection lets you choose Mie s theory instead of the standard Fraunh fer theory Mie s theory is only for thin particles If you select it the window shown in figure 12 will appear In this window you have to enter the refractive index of your product A database is available if you click on the right side of the box Its contains the most commonly used products If you want to introduce a new value into the database enter it in the Index boxes and save it using the Save button Save it with an explicit name and or comment in order to find it rapidly You may also want to measure the specific surface see part 3 2 by selecting the corresponding box A window will appear in to which you need to enter the density of your product and its shape factor NOTE You can measure the shape factor using ExpertShape if you have an 1180 system or a video accessory For density you will need to measure it using standard methods You can also active the MonoHistogram function which allows you to eliminated noise from the signal and will only save one class of sizes This option should only be used for monodispersed samples 12 Finally the last part all
14. SOP used for a measurement with The Particle Expert software Sampling is the major source of errors and so this step of the measurement must follow a defined procedure Users should be very careful because the accuracy of the measurement will depend on the user s ability to prepare a good sample that is representative of the material s properties 5 1 b Choicing the dispersing mode There are two ways to disperse your sample wet or dry mode The choice depends on the product s proprieties fluidity wetability density heterogeneity strength and solubility and on its use the application or environment It is best to analyze a product in the same dispersion mode as the one used for its application The dispersion mode also depends on the initial state of the product On next page you will see how to choose the dispersion mode depending on the initial state of the sample and its properties WARNING For each specific product you will need to define and use one method of dispersion CILAS can use its applications laboratory to help you figure out the best dispersion mode for each product 28 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 v Initial state liquid Wet mode must be used if your sample is a liquid or if you want to measure pa
15. WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 YOU MUST NEVER BE ALONE WHEN OPENING A COMPARTMENT TO CARRY OUT INSPECTION OR REPAIRS ON EQUIPMENT PRESENTING A POTENTIAL HAZARD WARNING Failure to the follow general rules could result in electrocution 2 4 GUARANTEE Like each product the particle size analyzer has its own warranty The start date of the warranty is the date that CILAS headquarters receives your end user list NOTE The end user list must be returned to CILAS CILAS recommends you work with your dealer to sign and send the end user list Once the end user document is received CILAS will inform you of the start of your watranty The warranty applies only if the product is used in standard conditions and does not include consumables like tubes O ring etc Parts are only guaranteed for defects and not for breakage due to non standard conditions of use like improper operating conditions not respecting safety rules etc During system installation use and maintenance the guarantee would be invalid for reasons such as connections at the user s factory are not standard electric water and air connections installation is not done by a trained technician use of parts not accredited by CILAS improper operating conditions to validate your operating method please contact your local CILAS distributor errors made by the users WARNING To ensure proper
16. You must have a signal adsorption of about 15 between the blank measurement and the sample measurement 17 Click on the button Sample measurement The measurement starts and you can visualize the progress with the two indicators During the measurement you can see the amount of time progress the action in progress the signal values 46 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 button allows you to see at the evolution of the histogram during the measurement This option can help you visualize the effects of parameters such as the ultrasound 18 When the measurement is finished the results window appears To see how to view and use the results given by the CILAS particle size analyzer go on section 5 5 NOTE Once the measurement is finished the results are automatically stored in the results database So you can take several measurements before viewing and analyzing the results Now you have seen how to take a measurement in either dry or wet mode The next section describes how to view and use the results After this step we will describe how to configure The Particle Expert software If you have any problems during a measurement please refer to section 5 6 and make sure that the software configuration is correct 5 5 USI
17. can also contact your local CILAS dealer 25 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 PART 5 MEASUREMENT WITH A CILAS PARTICLE SIZE ANALYZER 26 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 5 1 SAMPLE PREPARATION 5 1 a Measurement errors The preparation of the sample is the most important step when making a measurement As you can see on the following graph see figure below preparation for analysis extraction and preparation of the sample is the largest source of errors much larger than errors introduced by the CILAS particle size analyzer Instrument Sample Preparation Error Sample extraction Particle size FIGURE 6 Sources of measurement errors Measurement accuracy depends on sample preparation and extraction You have to carefully define a method for extraction and sample preparation in order to obtain precise and reproducible results WARNING Your measurement results depend primarily on the way you have prepared and extracted your sample Be very careful with this major step of the analysis if you want to obtain
18. explicit name containing for example the product s name or code In section 5 6 the procedure for the creation of a SOP is explained Please refer to that section for more information on how to create a SOP 9 In the section below you will need to enter general information about the measurement such as the sample s reference the operator If you select the box Automatic incrementation you will be able to make several measurements on the same sample A new window will appears where you have to define the number of the first measurement the total number of measurements and the time between two measurements This option is specially designed for companies which make multiple measurements using the same operating procedures This option can also be used with the autosampler accessory 10 The next screen has three small sections In the first section from left to right you can defined the distribution value It can be set automatically manually by entering the number into the corresponding box WARNING The distribution value is a number between 1 and 9 It is the value of the intensity of the distributor which is the vibrating system This system causes the powder to fall in front of the laser beam Like the ultrasound for the wet mode the value has to be tested to make sure it is correct before taking a measurement 43 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE
19. for specific applications and is not selected as the default The results file obtained using the mix is also stored in the database Before mixing files check to make sure that the operating method is the same You can not mixed files with different operating methods or you will introduce errors in your results 52 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 5 5 d Recalculation of the results It is possible to recalculate your results using a different method The standard method gives you results in volume which is the most commonly used method in laser diffraction You can recalculate your results in surface number Log Normal Rossin Ramler or for a monodispersed sample to eliminate noise NOTE For more information about these items please refer to section 3 2 of your user manual First select the list of file s you want to recalculate In the Processing part of the window shown in figure 22 choose the method you want to use for the calculation Click on Parameters to set parameters such as the particle shape Width and Translation You can choose to apply Mie s theory and to have results for the specific surface If you activate the MonoHistogram option you will use only the size that has the largest distribution Other sizes
20. measurements after installation you must carefully read this entire manual at least once The warranty is conditional on only the use of parts certified by CILAS for maintenance 14 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 PART 3 DEFINITIONS 15 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 3 1 THEORY ON LASER DIFFRACTION The operation of your particle size analyzer is based on the principle of light diffraction If you want to know more about this physical phenomenon please see the appendix on your USER CD ROM You will find a directory called THEORY which contains two files in pdf format Laser diffraction in 5 minutes Theory and applications of laser diffraction The first file is a short presentation of the theory and its application to measurement of particle size It is written for people who already have a basic understanding of laser diffraction This document will review the most important points to help you understand the basic measurement principle The second document is more involved It contains theorems hypothesis Fraunhdfer Mie equatio
21. normally enough to enable measurements in any conditions It is highly recommended that you do not specify a lower value that could hide a problem of sizeable deposits and alter the measurements Signals too high The sum of the signals on the 5 last silicon detectors is a good indicator of the cleanliness of the glass cell If this sum is higher than a given limit the background measurement is will be rejected By default this value is set at 2000 58 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 It can be increased if very messy samples are used or lowered if the quality of the measurements requires complete cleanliness of the glass cell we highly recommended the value remain in the range 1000 2500 Back measur OK during is where you define the delay in minutes where the last background measurement is still effective Beyond this delay you will need to take a new background measurement Cancel background is where you can activate an automatic reset of the software after each measurement Error message is where you activate or deactivate a warning message from the instrument ExpertConcentration is where you activate or deactivate the use of ExpertConcentration software The software allows you to have a well defined co
22. or dry mode and a reliable measurement without effecting the integrity of the particles 7 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 v A user friendly interface Making measurements with a CILAS particle size analyzers is made easy by using The Particle Expert a Windows compatible software The Particle Expert software is available in several languages and is available exclusively from CILAS It allows users to measure save and store data easily Its interface is very easy because it uses a mimic screen which shows pictures of each part of the particle size analyzer v A multi level interface The Particle Expert provides three different password protected levels of security The system is compliant with standard CFR 21 part 11 Depending on whether you are registered as an operator an analyst or a controller you can make measurements write procedures or perform maintenance on the particle size analyzer All these characteristics ensure that CILAS particle size analyzers are reliable and precise laboratory instruments They make CILAS particle size analyzers the best choice as your partner in particle analysis 2 3 SYMBOLS AND SECURITY RULES In this chapter the security symbols will be explained to the user and basic recommendations
23. preparation 26 28 39 message 71 Ae levels ey 61 62 Exploitation of results 46 52 See Software 8 F SOP 53 Fraunh fer 18 Spare parts 73 Frequently asked questions 24 64 71 Specifications 6 14 Specific surface 20 G Stock 22 24 Guarantee 14 T H Theory 16 Histogram 18 20 Transport 22 I U Installation 21 24 Unpacking 23 L W Laser safety 8 13 Wetmode 29 39 Launching the sonware 21 Withdrawing from service 75 Log Normal 17 78 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS
24. size analyzer cover 2 Remove fluid lines items 1 and 2 3 Remove the sample cell holder by pulling it up 4 Unscrew the 4 screws item 4 securing the diffuser item 3 5 Remove the diffuser item 3 6 Remove the O ring item 5 from the diffuser item 3 7 Unscrew the 4 screws item 7 securing the flange item 6 8 Remove the flange item 6 9 Remove the O ring item 8 from the flange item 6 10 Slide out and remove the sample cell holder item 9 11 Remove the O ring item 10 70 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 Y Replacement l Clean the sample cell holder item 9 2 Clean seals and mechanical parts rinse and dry 3 Clean the inside of the diffuser without opening it 4 Insert the O ring item 10 in the bottom of the base 5 Insert the sample cell holder item 9 in its support 6 Insert the O ring item 5 in the diffuser item 3 7 Insert the O ring item 8 in the flange item 6 8 Fit the flange item 6 9 Fit the diffuser item 3 10 Tighten the 4 screws items 4 of the diffuser 11 Place the sample cell in the particle size analyzer 12 Tighten the 4 screws items 7 of the flange 13 Connect the fluid lines items 1 and 2 to the sample cell 14 Close the particle size analyzer cover
25. the measurement When all the settings are done you can start the measurement using the last part of the window The following paragraph describes how this is done v Making a measurement 14 Start the background measurement by clicking on the Background meas button The particle size analyzer will start In the window you will see two indicators that show the measurement status The blue one corresponds to the percentage of background time already passed The red one corresponds to the percentage of the total measurement the instrument has completed The blue indicator allows you to see the progress of the background measurement 15 When the background is finished a message Background OK will appear in the window Introduce the sample is also displayed Please make sure that these two messages are displayed before beginning the next step You can pass a step by clicking Next action and you can prevent the background measurement by clicking Cancel background CILAS does not recommend doing that To ensure accurate results you need to do a complete background measurement before each sample measurement 16 Introduce the sample in to the tank see figure below FIGURE 19 Sample introduction in dry mode WARNING The amount of sample necessary to a measure is the amount necessary to fill the dry tank It depends on product s density You can introduce the sample using laboratory tools such as a spatula
26. the parts exactly as described in this section If you do not follow this advice you can deteriorate the parts CILAS is not responsible for problems resulting from errors made by a user cleaning the system The warranty does not apply to parts improperly cleaned by the user The warranty is only valid for standard use in normal conditions 68 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 Sample cell holder Parallel glass faces Glued braces Tissue soaked in alcohol FIGURE 28 Cleaning the sample cell Clean tank as follows Remove the sample cell holder see removal replacement information in section 6 2 e Weta tissue with absolute ethyl alcohol Wipe the tissue back and forth over the plate inner surfaces Repeat several times if necessary changing the tissue each time Rinse assembly with absolute ethyl alcohol Clean outer surfaces of the sample cell holder with a tissue soaked in alcohol Install sample cell holder and sample cell see removal replacement in section 6 2 e v Lens Cleaning the lens is a delicate operation that must be performed only if cleaning the sample cell did not change the high level of the blank signal FIGURE 29 Cleaning the lens 69 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTO
27. to enter the density of your product and its shape factor NOTE You can measure the shape factor using ExpertShape if you have an 1180 system or a video accessory For density you will need to measure it using standard methods You can also activate the MonoHistogram function which allows you to eliminated noise from the signal and will only save one class of sizes This option should only be used for monodispersed samples 13 Finally the last square allows you to load a special report configuration using Report config or to erase the report configuration using the button Erase config The last button is named Option It allows you to set up all the other measurement parameters shown in the window below 36 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 Operating mode Eg Background Measur Cleaning Computation Alarm Processing I Stirring r During M Circulation IM Stirring Alter M Stop pump I Stop stirrer I Rinsing on default FIGURE 13 Operating method in wet mode In the above window you can set all the parameters from background measurement to results interpretation Each step has its own section in the window There are six specific parts The first one is dedicated t
28. will be removed and consideredas noise Finally you can add results that you have obtained by sieving the same sample Once the parameters are defined begin the calculation by clicking on the Execute button An indicator will show you the progress of the calculation A new file will appear in the list This new file corresponds to the results of the recalculation This file is stored like the other files in the database and can be used like any other file 5 6 CONFIGURATION OF THE SOFTWARE The Particle Expert is software specially designed for CILAS particle size analyzers It has many options and is the best tool for particle characterization This software has many functions Those described above are the standard functions This paragraph will explain how to set up other options in order to adapt the software to better meet your needs NOTE This paragraph is meant for technicians and or operators who have a good working knowledge of the CILAS particle size analyzer A person must be trained and must have a thorough understanding of the system in order to understand the different points described in this section The following section describes how to create a standard operating method SOP how to configure the software in order to control the hardware how to use the database how to define security levels how to resolve problems etc Be careful if you modify any of the settings Once they are modified some of the s
29. CD ROM USERCDROM Answers to frequently ask questions Frequently ask questions pdf You can also contact your local CILAS dealer 74 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 PART 8 WITHDRAWING YOUR PARTICLE SIZE ANALYSER FROM SERVICE 75 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 Your CILAS particle size analyzer can be withdrawn from service This would be done if you want to move the system to a new laboratory or move the system to a new building This can happen due to the long lifetime of the CILAS particle size analyzer Technicians who know how to manipulate electromechanical devices must perform the withdrawal If a skilled technician is not available please contact your local CILAS dealer CILAS is not responsible for damage or accidents affecting the users or the particle size analyzer To withdraw the particle size analyzer from service please follow the procedure below l Drain the particle size analyzer 2 Turn off and disconnect the particle size analyzer 3 Close The Particle Expert software and turn off the PC 4 Disconnect the RS232 link bet
30. Create button A specific window will be opened Enter a name for the list of diameters and validate Another window will appear where you can enter the diameters When you have finished click validate and load the list for the SOP s creation You can view the selected list of diameters using Display define the calibration file to use for the measurement add an image to the report using the Image button or erase the loaded image with Erase image define the diameters used for the cumulative curve with the Cumulative curve button A list of diameters will appear on the screen You can change the list in the right column and replace it with the list you want To do that you will need to enter the desired values and click on validate If you want to escape from the window without making any changes please click on Cancel AII If you want to erase just the last action performed click on Cancel Once you have finished save the SOP by validating it using the Save button You will have to enter a file name You have now created a standard operating method SOP which you can use each time you want to make a similar measurement NOTE CILAS can help you to optimize your operating method With our 30 years of experience the application laboratory can help you improve your results by creating a SOP specific to your products If you are interested please contact us at info particle cilas com or visit o
31. DUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 Some optional software packages are provided with the CILAS particle size analyzer and its main software The Particle Expert They are designed to complete the information obtained from the particle size analyzer ExpertShape software allows you to analyze the size and the shape of your samples To use this software you must have a video camera The video camera comes standard on the 1180 and is an optional accessory on all other models ExpertGrab software takes images of your sample if you have a video camera installed on your particle size analyzer A video camera comes is standard on the 1180 and an optional accessory on all other models ExpertReport software allows the user to customize reports from the CILAS particle size analyzer ExpertConcentration software allows you to have better reproducibility of the sample concentration for measurements in wet mode on CILAS particle size analyzers All of these software packages can be launched from The Particle Expert software If you want more information about how to use these different software packages please refer to their specific User Manual and or the Tutorial available on your USER CD ROM in the manuals section 5 8 WASTE FROM A MEA
32. ERTIFICATES The following is a list of all the declaration of conformity certificates of compliance and material data sheets included on the CD ROM Company certification ISO 9001 certificate Particle size analyzer specific norms CFR 21 part 11 compliance CE norms Electromagnetic compatibility certificate Low voltage conformity certificate Certificates of security Laser security certificate Material Safety Data Sheet MSDS If you need more information about any of these items please contact CILAS 5 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 PART 2 SPECIFICATIONS OF THE PARTICLE SIZE ANALYSER COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 2 1 GENERAL FUNCTIONS RANGES AND UTILIZATION Particle size can be measured based on light diffraction To analyze submicronics particles CILAS uses laser diffraction A particle size analyzer is used to determine the size distribution of a powder a suspension or an emulsion Using a particle size analyzer you can very quickly visualize the shape of your particles and have an idea of the sample s di
33. INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 NOTE The restore function will destroy the current database We highly recommend that you save the current database before performing any restore The selection of the backup file is made through the same dialog box described in the previous paragraph Once the file is selected the comment that was saved during the back up will be displayed In you are not sure you want to perform the restore function click on the Cancel button Select database it is possible to select a given database among several databases listed in the software You may want to have several databases for distinct activities for instance a laboratory database and a production control database Managing several databases is a delicate process and should be done only when necessary In any other case we advise that you use just the standard Database By default the standard database is the only database that can be selected The default filename for this database is GRANULOG and it is stored in the folder C Cilas Gwin32 Db To create new databases refer to the following item creating the database To select a different database just click on the filename in the box which lists the file names and click on the Validate button Creating a database First we will ex
34. ION OF CILAS NT 1503192 31 Issue September 2004 C Ca LD LD 19 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 y LIQUID The liquid is the solvent used for a measurement in wet mode Generally the solvent used is water but it can also be an organic solvent The liquid is the solvent which carries the sample through the particle size analyzer MEAN DIAMETER Mean diameter also called mean size is the statistical mean value of particles diameters contained in the sample MEAN SIZE p x MD Where Ci cumulative value for diameter of class i Di diameter value for class i in um D E D 66599 1 MD mean diameter value for class i in um pi Ci Ci probability for MD MEDIAN SIZE Median size is the diameter value for which the cumulative results are 50 This means that half of the particles in the sample are above the median size and half of the particles are below the median size v MIE The Mie s theory is the most complete theory used to measure light diffraction This theory needs to be applied for thin particles If your particles have a diameter smaller than the laser wavelength A 635 nm Az 830 nm you will obtain accurate results using Mie s theory If you want more information o
35. ISSION OF CILAS NT 1503192 31 Issue September 2004 v In dry mode For particle size analyzer in dry mode waste comes only from the sample No solvent or dispersing agent is used The dry mode limits the emission of waste In order to eliminate the emission of waste you will need it to go in to the aspirator connected to the particle size analyzer Refer to the user manual of the aspirator to find out how to remove the waste from the aspirator When throwing the waste away be sure to respect your company s environmental policy and your country s environmental laws WARNING CILAS recommends that all the user of its particle size analyzers set up a circuit compliant with the standard ISO 14000 or similar in order to treat all the waste from measurements Users have to follow their company s policy and their country s laws for handling environmental waste CILAS can not be held responsible for damages caused by waste from particle analysis CILAS particle size analyzers are designed to limit the waste created when making a measurement Special accessories are also available as options Small Volume Unit Alcohol regenerator etc in order to limit the waste and improve productivity If you want more information about this optional equipment please refer to section 1 3 in this manual 5 9 ANSWERS TO FREQUENTLY ASKED MEAUREMENT QUESTIONS If you have additional question or would like advice about measurements made
36. LAS certified technician Other people are not authorized to perform maintenance operations CILAS is not responsible for an accident which happen during maintenance performed by unauthorized persons Authorized users must be aware of laser and electrical risks involved with a maintenance procedure To perform maintenance users have to open the protective cover of the particle size analyzer The laser is not activated when the cover is open because of the safety interlock WARNING Anybody who will work with or on the CILAS particle size analyzer must respect all this safety recommendations The operator in charge of maintenance must have the necessary skills and information to understand the operation of an electromechanical device All users must follow the safety rules and policies of their company Keep in mind that laser radiation is very dangerous even if all the safety tools on the CILAS particle size analyzer are working properly to ensure the operator safety 6 2 PREVENTIVE MAINTENANCE FOR USERS 6 2 a Introduction CILAS particle size analyzer maintenance operations cover regular servicing and cleaning of the optical parts Users and technicians can perform both of these operations Users should only perform preventive maintenance and should never perform any other maintenance operations Servicing needs to be done regularly Cleaning the optical parts needs to be done frequently in order to ensure good reliability of your resu
37. MITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 4 1 TRANSPORT AND STOCK The particle size analyzer is transported in a shipment case that is specifically designed to ensure its safety during transport When you receive the shipping case the first thing you need to do is to check all the items in the case Using the Packing list document included in the shipping case carefully follow all the steps described and make sure all parts are included When you have completed the document please return it to CILAS If a problem occurs when checking the system please note the problem and contact your local CILAS dealer or the CILAS factory If everything is OK you can unpack the particle size analyzer A technician accredited by CILAS must perform installation of the instrument Refer to the Installation manual included with the instrument for more information The Installation manual is also available on your USER CD ROM in pdf format WARNING Remember to keep the shipment box in case the system needs to be moved within your facility or returned to CILAS for maintenance Only this shipping box ensures the integrity of the particle size analyzer during shipment If you want to store the particle size analyzer in its shipment case be sure to choose a safe place The temperature and humidity need to stay within normal operating conditions temperature below 50 C and humidity lt 90 Protect t
38. MITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 This procedure has to be performed each time you want to measure a new product Dispersion is a very important parameter for every measurement Be very careful with this step Once the pressure defined you can start measurements using the CILAS particle size analyzer 5 4 c A measurement in dry mode This section explains how to perform a measurement in dry mode The measurement is described in several steps Please follow the procedure below carefully 1 Turn on the CILAS particle size analyzer the air supply and the accessories if necessary 2 Turn on the PC and start The Particle Expert software 3 Enter see figure 9 your user name and your security level defined by your company as operator analyst or controller NOTE Please do not forget your user name your password and your security level CILAS recommend that all companies store these parameters in a database This database can help someone who has forgot his parameters 4 The main window of the software will appear on the screen For a measurement in dry mode you must have the following figure 1180 D 1 m21 K11180D_DIF 6096 mb FIGURE 16 Dry mode mimic screen LS If this screen comes up you can continue If not please click on the tsa icon to change the configuration of the software 41 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUT
39. NG THE RESULTS The method for viewing and using the results is the same for a measurement made in wet or in dry mode In that section you will learn how to view and how to use the measurement files All the measurements taken by the CILAS particle size analyzer are stored in a database You will also learn how use the database 5 5 a After a measurement When the measurement is finished the results window will automatically appear on the screen The results window for a single measurement is the following 194 1180D 119 1180D 0170172000 x Parameters Results User Data Graphic Maintenance Pressure Distributor 60 mb 0 Concentration 293 Diameter at 10 3 39 um Diameter at 50 26 85 um Diameter at 90 63 17 um Fraunhofer DensityF actor Specific surface _ Meas Rins 0s 0s 4 SOP Standard 1180 L in volume undersize FIGURE 20 Results window 47 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 This window is composed of six different parts The first part that appears on the screen is the part called Results In this part you have a summary of the results and of the operating parameters You can see the concentration the results diameters specific surface and the operating param
40. OM The security levels are very important to ensure an optimized functioning of the instrument If you choose on of the first two security options you will need to enter your user name and a password each time you start the software In case of CFR 21 part 11 security levels the user name will be saved with all the results and will appear in all the documents and reports For each measurement you will know who was the operator You also have three levels of security operator analyst controller You choose the level you want after considering what tasks each user will have to do on the particle size analyzer To create an identity please go to the menu Tools Identification Create The following window will appear 62 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 Create identification User name factias Level REZE hei Password Confirm password 6 characters mini 25 maxi for edition area Validate Cancel FIGURE 27 Creation of identification You will need to set up the user name the level and the password The password must have a minimum of 6 characters and a maximum of 25 characters WARNING Do not forget your user name or your password CILAS recommends creating a table with all the usernames and all the passwords
41. ON ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 4 3 UNPACKING Before beginning installation after you have checked that you have received all the parts please carefully read the entire installation manual part 2 1 and 2 2 This will help you when setting up the instrument Be sure to unpack the particle size analyzer very carefully All components should be stored near the particle size analyzer The shipment case should be kept You will use it if you ever need to move the instrument Using the shipping case is the only way to ensure good protection when transporting the instrument Unpacking is the first step during installation This step is very important please do it carefully If you have scrap from unpacking plastics etc please follow your company s instructions regarding removal of scrap materials For more information please see part 2 2 in your installation manual 4 4 GLOBAL SET UP Before unpacking the particle size analyzer prepare a clean work area The area where you will install the instrument needs to be equipped with sufficient area for the particle size analyzer ventilation system or system to aspirate the effluents regulated temperature 20 C 5 C humidity rate lt 90 clean water supply and or compressed air supply depending on our model When the work area is ready you ca
42. ORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 NOTE If you have an instrument with only dry mode the mimic screen will always be the correct one If you have a 2 in 1 model please check that the mimic screen corresponds to the measurement mode you want dry or wet Change it using the icon if it is not correct 5 On the mimic screen make sure the model of CILAS particle size analyzer and its serial number are correct They appear in the upper right hand corner of the screen If the numbers are correct please continue to the next step If they are wrong you will need to change them Go to the Tools New Serial Number menu to change the serial number If the model is not correct please turn off the PC and the particle size analyzer and restart at step 1 If the problem persists contact local your CILAS dealer 6 Clean the particle size analyzer once by clicking on the icon or by selecting Commands Liquid system Rinsing from the menu NOTE All the commands are available in the Commands menu The most frequently used commands are available more rapidly using the icons situated on the upper bar of The Particle Expert software il 7 Click on the z icon or select the menu item Commands Measuring The following window will appear on the screen 1180 D 7z 0001 SOP name Standard D
43. OSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 FIGURE 4 Side view 11 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 FIGURE 5 Top view 12 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 2 3 b Safety Rules The CILAS 920 930e 1064 and 1180 particle size analyzers comply with safety standard CEI 825 as per ADD1 dated 17 09 1990 v Laser safety When the cover is closed the operator is protected from the laser beam therefore no additional protection is needed This laser product belongs to Class under standard CEI 825 If the cover is open there is no accessible radiation because of safety interlock The general rules for laser safety are Never look at the beam facing the source either with the naked eye or with an optical instrument Never place a reflective surface in the beam s path The use of safety goggles is mandatory when any one of the above rules cannot be followed during maintenance oper
44. RISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 A gt NOTE StoP Do not unscrew the permanent screws on the barrel or you will lose the optical alignment of the system Clean the lens barrel as follows Make sure particle size analyzer is disconnected from the power line Open the particle size analyzer cover Clean the outer surface of the concentrator lens item 1 figure 7 by wiping it once with tissue soaked in alcohol Be careful not to scratch the anti reflection coating Close the particle size analyzer cover The above section describes all the maintenance operations authorized for users The next section will describe what to do if you have a more difficult problem with your instrument Keep in mind that CILAS particle size analyzers are reliable if used in standard operating conditions and if you remember to perform preventive maintenance 6 2 e Removal Replacement of the sample cell This section describes how to remove or replace the sample cell of your CILAS particle size analyzer WARNING Drain the particle size analyzer and disconnect it from the power line before proceeding with removal of any parts NOTE O rings item 5 8 10 are visible only after removing diffuser item 3 NX yy flange item 6 and sample cell holder item 9 Y Removal l Open the particle
45. Result window tab Data select either lines or columns You can also choose between undersize or oversize Undersize mode displays the amount of sample that is smaller than or equal to the related diameter Oversize mode displays the amount of sample that is greater than or equal to the related diameter Undersize or oversize mode will also apply to the cumulative curve if enabled in the display set up window Results display the average diameter statistical average of the results will be displayed in the as Mean diameter results tab Hist bar shows the histogram using bars The line Ref CILAS displays additional information during selected measurements or when carrying out a query This option is disabled by default because it slows down the loading of the measurement results Form parameters allow you to show the shape parameters Particular diameters Q3 displays the cumulative value of a customer defined diameter DQ3 displays the difference between the cumulative values of the customer defined diameter and the previous diameter This allows the user to determine the percentage of a sample that is included between two specific diameters Diameters axis you can choose to have the graph s diameter axis use either increasing values or decreasing values Diameters you can set the diameters that appear in the histogram and the cumulative curve In the Diameter Nb box number of d
46. SUREMENT When dealing with waste from a measurement the user needs to throw the waste away while following the rules of their company and the environmental laws of their country CILAS particle size analyzers do not themselves produce any waste If you have to discard the entire instrument do it in a special location that is dedicated to electronic waste PCs etc WARNING Samples and solvents used in the particle size analyzer can be dangerous chemical products The user must take the necessary precautions after reading the safety data sheet of the products they manipulate v In wet mode Waste can come from the sample the dispersing agent and the solvent You will need to connect the outlet of the particle size analyzer to a path where the solvent will be treated in order to eliminate all the pollutants contained in the carrier liquid If you are using organic solvents there are specific devices available to reduce the pollution and its cost For example if you use alcohol CILAS has designed an alcohol regenerator which limits the amount of solvent used For all the instruments used to prepare the sample dish etc please refer to your company rules and the laws of your country The operator must be knowledgeable about these issues before making a measurement 64 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERM
47. a problem during the procedure If you click on it the measurement in progress will be delete 30 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 5 3 a Preliminary tests This step is only applicable for new products It describes how to define the carrier liquid and the dispersing agent that will be used WARNING If the product has already been tested please refer to the previous results and choose the standard carrier liquid and the standard dispersing agent Note that a dispersing agent is not always necessary CILAS can help you to define these technical points with our applications laboratory After reviewing section 5 1 b you have chosen a wet dispersion This way of dispersion is the most common method used these days for particle characterization You will need to control different parameters such as the sample preparation operating conditions carrier liquid and dispersing agent To see how to prepare the sample refer to the previous paragraph The operating conditions will be described in a following section Y Carrier liquid The carrier liquid must have the following properties nonreactive with the product you are measuring non absorbent at the working wavelength arefractive index different than the product alow viscosi
48. accurate and reproducible results CILAS recommends defining a standard method of sample extraction and preparation for each specific product For thin size particles the most important step is extraction For larger size particles sample preparation is the largest source of errors If you have an idea of your size distribution you can limit the sources of errors playing a major role The previous information shows you the user s importance to a measurement Technicians in charge of making measurements with a CILAS particle size analyzer must be very knowledgeable The company should educate them on the instrument CILAS can not be responsible for measurement errors if a standard operating method is not defined and used from preparation to the treatment of results and if the operator is not well trained in making measurements with the particle size analyzer 27 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 For preparing a sample you have two different steps extraction and preparation Sample extraction is the first of the two steps It consist of the extraction of an amount B from the original sample A You want to know the size distribution of A The extraction must be done correctly in order to have sample B identical to sample A in terms of size distribution To d
49. ance operations PART 8 WITHDRAWING FROM SERVICE Finally the operations for the withdrawing of the instrument are described SUGGESTIONS EEC To submit suggestions on this manual or on a product please contact us at CILAS Particle size analyzers After sales service 8 AVENUE BUFFON B P 6319 Z I LA SOURCE F 45063 ORLEANS CEDEX France TEL 33 2 38 64 59 00 FAX 33 2 38 76 59 07 E Mail info particle cilas com 1 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 SCHEMATIC SUMMARY FIGURES The table below lists all the figures from this user manual DESCRIPTION PART Figure 1 Range of CILAS particle size analyzers 2 1 Figure 2 Back view win w Li Front view Side view Top view Sources of measurement errors Choosing the dispersion mode for a solid sample Dispersing agent Password amp Security levels Figure 10 Wet mode s mimic screen Figure 11 Selection of the measurement parameters in wet mode f Mie s parameters Figure 13 Operating method in wet mode Figure 14 Sample introduction in wet mode Figure 15 Measurement windows Dry mode mimic screen Figure 17 Selection of the measurement parameters in dry mode Figure 18 Operating method in dry mode Figure 19 Sample introduction in dry mode Figure 20 Results w
50. aph sampling and dispersion choices are some of the most important steps when performing analysis with a particle size analyzer CILAS particle size analyzers will provide you exact and reproducible results only if you are careful with these two steps CILAS can help you optimize your operating conditions by using our laboratory of applications Please do not hesitate to contact us if you need help 29 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 5 2 USER SAFETY Any measurement made using a CILAS particle size analyzer is subject to safety recommendations Each operator must respect his or her own company rules All measurements made are the responsibility of the operator and his or her company The particle size analyzer must be in a ventilated area with the temperature regulated to room temperature 20 C 5 C The ventilation system should limit the inhalation of effluents in wet mode The same system must limit the inhalation of small particles in dry mode Users must wear standard protection equipment for operators who work in a laboratory safety goggles smock rubber gloves etc Before making a measurement the operators need to read the safety data sheet of the sample in order to be informed of all possible product dangers The operator must make sure all t
51. ations WARNING Failure to the follow general rules could result in the emission of laser radiation which can be harmful and caused permanent eye and skin damage Safety goggles are required at all times when the cover is opened and the safety interlock is bypassed Y Dangers presented by electricity The equipment described in this manual runs at high voltages that are potentially lethal A voltage of 110 V can result in death At all times personnel must comply with safety provisions Never perform any operations without first cutting off the source of high voltage Be especially cautious with respect to safety systems such as circuit breakers pull out racks or doors First make sure that the safety systems are working correctly When carrying out any operation inside the equipment cut off all the supply sources Remember that safety systems are provided only for parts which are opened as part of routine maintenance and that dangerous circuits can still be encountered when the equipment is disassembled In certain cases dangerous voltages can still exist after the equipment has been shut down because of charged capacitors These must be discharged before carrying out any work on the equipment Wait several minutes in order to be sure the capacitors have fully discharged 13 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED
52. button Create a measurement Machine Type Company Place Sample ref J Report contig Erase Type produit x Liquid Client x l z Comments Poo Dispersing agent Operator x 7 m Particular diameters i Define Modify user Create Display Image Erase image Welibraton Cumulative curve Cancel Cancel All FIGURE 25 Creation of standard operating method SOP To define the SOP you will need to enter the following parameters the model of particle size analyzer in the box Machine Type the company the place the sample reference in the box Sample ref the type of product the name of the customer and the name of the operator 54 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 your comments the carrier liquid and the dispersing agent used You can also define the report configuration you can load one using the Report config button If you want to delete the report configuration already loaded click on Erase The standard configuration will then be used for your reports add measurements using the Particular diameters part You can load a list of measurements already saved in the box You can create a measurement list using the
53. can choose the values you want to measure for the cumulative curve The most commonly selected values of 10 50 and 90 are used as default values You can change these values or add other points on the curve The Alarm section is dedicated to the alarm settings for the CILAS particle size analyzer You can define the limits of concentration recommended default values are 0 300 You can define the number of attempts or you can select only one measurement by choosing the corresponding box A Quality control option is available This option is designed specially for a routine analysis You can define size limits to validate or record your sample Using that the quality control option the instrument can determine if the sample is accepted or not In the last part called Processing you can select the kind of calibration you want from a list of suggestions Be careful when selecting the calibration type because all of the results depend on the calibration being done correctly CILAS recommends you use as a default the latest updated calibration 45 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 To validate all the settings click the Validate button in each specific window If you do not validate the settings the standard settings will be the one for
54. d to perform preventive maintenance 1 3 ACCESSORIES There are a number of accessories available for your CILAS particle size analyzer If you have a specific measurement need an accessory can solve your problem and improve your measurements Accessories available for your system include autosampler improves your productivity when performing routine analysis controls production etc small volume unit a device for reducing the amount of sample and solvent necessary to perform a measurement video camera allows users to see the shape and the sample dispersion alcohol regenerator reduces the amount of solvent necessary for analysis which results in less waste removal The Particle Expert software controls all of the CILAS accessories If you need additional information on any of these accessories or would like a quotation please speak to your local CILAS distributor or directly to CILAS We will be happy to answer any of your questions Information is also available on our website www particle size analyser com 4 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 1 4 DECLARATION OF CONFORMITY TO THE NORMS Certificates of conformity for your CILAS particle size analyzer are provided in the appendix of your USER CD ROM in the directory C
55. e add or delete data To delete an entry it must not be used by any measurements When attempting to delete data that s being used the following error message will appear BDE Master has detail records cannot delete or modify First delete the measurements using the affected data and then delete the data The function Modify can be used even if the data is already used by some measurements But they will all display the new text after the modification Save database this function allows the user to save the entire database in a compressed file Using the displayed dialog box you need to provide a name for the backup file and specify it For example save the file 270498 ZIP in the directory C GWIN EXE SAVE The default file name is C GWIN EXE SAVE The network button can be used to specify a destination on your network To save to a network you need to have already defined a Network drive contact your network administrator to set that up Click on the OK button to confirm the backup or on the Cancel button if you do not want to go on A dialog box will prompt you to input a comment which will be saved in the back up file This can be used to describe the backup An automatic back up of the database will be carried out whenever the software is closed Restore database this function is used to recall a database previously saved using the Save database function 60 COMMUNICATION REPRODUCTION ET UTILISATION
56. e 2 PART 1 IDENTIFICATION OF THE PARTICLE SIZE ANALYSER Page 3 1 1 Scope of the manual Page 4 1 2 Identification of the equipment and documentation Page 4 1 3 Accessories Page 4 1 4 Declaration of conformity to the norms Page 5 PART 2 SPECIFICATIONS OF THE PARTICLE SIZE ANALYSER Page 6 2 1 General functions ranges and utilization Page 7 2 2 Characteristics of the particle size analyzer Page 7 2 3 Symbols and security rules Page 8 2 4 Guarantee Page 14 PART 3 DEFINITIONS Page 15 3 1 Theory on laser diffraction Page 16 3 2 Vocabulary Page 16 PART 4 INSTALLATION OF THE PARTICLE SIZE ANALYSER Page 21 4 1 Transport and stock Page 22 4 2 Safety requirements for installation Page 22 4 3 Unpacking Page 23 4 4 Global set up Page 23 4 5 Storage and protection during a non use period Page 24 4 6 Answers to frequently asked installation questions Page 24 PART 5 MEASUREMENT WITH A CILAS PARTICLE SIZE ANALYZER Page 25 5 1 Sample preparation Page 26 5 2 User safety Page 29 5 3 Measurement in wet mode Page 29 5 4 Measurement in dry mode Page 39 5 5 Using the results Page 46 5 6 Configuration of the software Page 52 5 7 Optional accessories Page 62 5 8 Waste from a measurement Page 63 5 9 Answers to frequently asked measurement questions Page 64 PART 6 MAINTENANCE Page 65 6 1 Safety requirements Page 66 6 2 Preventive maintenance for users Page 66 6 3 Maintenance for dealers and authorized persons Page 71 6 4 Answers to fr
57. e only will automatically start in dry mode System If the 2 in 1 box is checked the system allows the user to switch between wet mode and dry mode in software This option is only available for wet and dry models of the 920 1064 and 1180 WARNING Switching to dry mode if the particle size analyzer is in wet mode only will cause an overflow and may damage it For 1180 models only you have anther option If the DSP box is checked the particle size analyzer will carry out measurements with the DSP video camera You must restart the software to validate the changes WARNING Do not switch to DSP mode unless your particle size analyzer is an 1180 model If you switch to DSP mode with a different mode you won t be able to perform any analysis 59 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 Remote control there are two options in that section If the box Validate is checked the PC connected to the particle size analyzer becomes a slave PC and can be controlled by the master PC using a RS232 link To validate the remote control module you have to quit The Particle Expert and restart it The communication rate of the master and the slave PC must be the same The remote control serial port configuration file is located in the
58. e saved in the database but you will not lose the old configuration The modifications will be stored in another file which is a copy of the original You can also add specific diameters into the histogram or customize the report using Report config You can also select a different calibration file For the cumulative curve you can add or delete values You can create a new measurement using the Create button This option is described in more detail in section 5 6 of this user manual You can also import a special type of results file that you have already saved in the database Note that measurement files must have the extension mes If it is not the case you will not be able to import the file You can also export the measurement files using the button Export Finally you can set up statistical testing using the Stat button A new window will appear where you can choose the test you will use to compare several results You can choose whether or not to display standard statistics mean min max You can also define your own name for each value With the option Mix you can make a new measurement by mixing several results files For example if you have a sample containing two products you can measure each product separately Then you mix the results using the exact proportion of products in the sample The software will ask for all the necessary information during the calculation This option is designed only
59. e this parameter you need to know the density of your material In Fraunh fer or Mie theories particles are assumed to be spherical When you are working with particles that are non spherical you need to introduce a parameter called shape factor noted S The shape factor will give you a better approximation for non spherical particles The mathematical equation for specific surface is Q3 x O3 Specific surface meaty gt P l xXx X 2 i 5p Where C constant S shape factor 1 for spherical particles p sample density g cm xi diameter value for class i Q3 x cumulative value for diameter of class i You should now have sufficient knowledge to understand how a particle size analyzer works Like all instruments used for control and characterization it is very important to understand how the particle size analyzer works before making measurements Knowing how the system operates allows you to correctly analyze the results provided by the instruments and The Particle Expert software 21 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 PART 4 INSTALLATION OF THE PARTICLE SIZE ANALYSER 22 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANS
60. easure it with a special instrument Y DIAMETER AT 10 and 90 This is the diameter value for which the cumulative result is 10 or 90 These two values give you approximations of the smallest and the largest diameter contained in your sample DIAMETER IN VOLUME The results provided by laser diffraction are in volume This is due to Maxwell s equation By default The Particle Expert software will give you results in volume The standard results are shown in De Brouckere mean diameter also called D 4 3 volume or mass moment mean 16 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 CILAS recommends using this kind of results to improve the reliability of your measurements The mathematical formula used to calculation the diameter in volume is Dx xd Yin xd xd Dy Where ni number of ine of class di diameter of class 1 si 29 DIAMETER IN NUMBER The diameter in number is an arithmetic average of the diameters The mathematical formula is as follows n xd n xd Dy Sn n Where ni number of e of class di diameter of class 1 oy 29 In The Particle Expert software diameter in number is calculated from the value of diameter in volume DIAMETER IN SURFACE The diameter in surface is also called D
61. equently asked maintenance questions Page 71 PART 7 SPARE PARTS Page 72 7 1 List of spare parts Page 73 7 2 Order form Page 73 PART 8 WITHDRAWINGING YOUR PARTICLE SIZE ANALYSER FROM SERVICE Page 74 INDEX Page 76 Ill COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 ABOUT THIS MANUAL PURPOSE This manual covers the utilization of your new particle size analyzer model manufactured by CILAS company ORGANIZATION The following is a guide to the organization of this manual Y PART 1 IDENTIFICATION OF THE PARTICLE SIZE ANALYSER This part gives information on the manual the particle size analyzer and the optional accessories Y PART 2 SPECIFICATION OF THE PARTICLE SIZE ANALYSER In this part we have all the information concerning the technical specifications y PART 3 DEFINITIONS This part describes the theory and the vocabulary of laser diffraction Y PART 4 INSTALLATION OF THE PARTICLE SIZE ANALYSER All advice for the set of the instrument is described y PART 5 MEASURES WITH THE PARTICLE SIZE ANALYSER All the advices for a good measurement with the instrument are given into that part PART 6 MAINTENANCE In this part you will find all the maintenance operations which can be made by users PART 7 SPARE PARTS You will find at spare parts for the mainten
62. es Clean level sensors with cotton tip dipped in alcohol Clean ultrasound tank with lint free cloth dipped in alcohol Clip stirrer back onto the top of the ultrasound tank Check without removing that the optical fibers are properly connected to their respective connectors Check sample cell inlet remove accumulated matter Make sure sample cell fluid connections are properly connected Make sure bellows are properly positioned Close particle size analyzer cover 6 2 d Cleaning the Optical Parts The optical parts need to be cleaned whenever there is an increase in the blank signal this can be seen using the real time signals button when compared to the previous measurements If you use a product that you know will make the sample cell dirty please clean the sample cell regularly A gradual increase in the blank signal over time up to 20 of their original value is considered normal Before cleaning the optical parts rinse the particle size analyzer with detergent and recheck the value of the blank signal If an increase in blank signal persists clean the sample cell holder rinse with detergent recheck blank signal value using the real time signals button clean the optical parts if the increase in blank value persist Next we will explain how to clean the sample cell and the optical parts Be careful when cleaning the sample cell and optical parts are very fragile Please clean
63. eters theory used model of particle size analyzer etc The information need for an accurate report is contained in this part In the Parameters part you find all the information you have entered before the measurement and all the operating parameters This part tells you the operating method used the sample measured etc You can use this part to see if a comparison is possible between two measurements For a comparison the operating methods must be similar In the User part you will find information about the user and in the Data part you will find a table with the results For each measured diameter x the table will show the value of the population density q3 and of the cumulative curve Q3 in percent In the Graphic part you can view the histogram of population density and the cumulative curve Finally in the last part called Maintenance you will find different information reserved for the technicians in charge of the corrective maintenance for the CILAS particle size analyzers After a measurement you have direct access to the results Clicking on the LS button allows you to print the results The results will be print by default in a standard report format NOTE If you want to customize your report use the ExpertReport software designed by CILAS You can design your own custom report using this software To launch ExpertReport from The Particle Expert click on the 5
64. ettings are considered standard and will be used for every measurement If you are not sure of what you are going to do please refer to the user manual CILAS is not responsible for damages caused by an incorrect setting made by the user CILAS has designed the software to avoid problems Our default settings ensure there are no dangerous settings for the instrument or for the operator 53 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 5 6 a Creating a SOP CILAS recommends creating a standard operating method called SOP in The Particle Expert software for each product The SOP contains all the parameters for the measurement When you have defined a SOP you just have to load it before beginning the measurement You will save time and improve your results if you use a SOP to make your measurements NOTE CILAS recommend you to name your standard operating methods SOP with explicit names All new SOPs will be listed in a file that everybody can consult when they are making a measurement with the CILAS particle size analyzer To create a SOP go on the Files Results menu or click on the icon A window will appear where you can click on the Create button in the management part The following window is opened when you clicked on the Create
65. following folder C Program _ files Cilas Gwin exe Tmrs232 ini The particle size analyzer begins measurement when an order comes from either the slave or the master PC If the Top most box is checked the remote control state report window is in Top most mode To validate your settings click on Validate You can also cancel your changes quit the window or ask the help Once your settings have been validated they become the default analyzer settings 5 6 c Database amp security levels The Particle Expert is compliant with the ISO 13320 standard and with CFR 21 part 11 This is why the software has a database to store the results and security levels to identify the user The following section describes how to manage these two options Y Database The database of results from the CILAS particle size analyzers is available on the hard disk of your PC The default directory for data storage is C Cilas Gwin32 The standard file extension is by default Db A PARADOX compatible database is integrated into the software to easily sort and manage the results The database is transparent to the user however a number of operating settings have to be configured Access to the tools of the database is through the Tools menu sub menu Database and contains the following items Secondary database management this function manages the contents of the secondary tables and allows the user to chang
66. gent is used only in wet mode In some cases to get good dispersion of your sample into the solvent you have to introduce another product in a small quantity That other product is called the dispersing agent and necessary for an accurate measurement For the dispersing agent like for the solvent you need to know its refractive index if you want to use Mie s theory FRAUNHOFER The Franuh fer s theory is the most common theory used for light diffraction This theory can be applied for large size particles If your particles have diameter larger than the laser wavelength A 635 nm Az 830 nm you will get accurate results using Fraunhdfer s theory If you want more information on Fraunh6fer theory please see the documents about laser diffraction in the appendix of your USER CD ROM Y HISTOGRAM The histogram gives you the size distribution for different classes of sizes The histogram H is the derivative function of cumulative values If you note Ci cumulative value for diameter of class 1 D diameter value for class i in um Dee MD mean diameter value for class i in um where MD 3 gt LD for class i LD In Dj Let X be the ordinate on X axis and H the ordinate on Y axis We have for the ordinates of the histogram Xj Md 18 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISS
67. ginal spare parts provided by CILAS are manufactured following our specifications and are checked before shipment to prevent any damage to the instrument and to guarantee the high quality measurement results These items must be used for maintenance if you want to maintain your warranty WARNING To ensure accurate measurements after a maintenance operation you must carefully read this entire manual at least once The warranty is conditional on the use of only parts certified by CILAS for maintenance 7 1 LIST OF SPARE PART The list of all the spare parts for your CILAS particle size analyzer is given in the appendix on your USER CD ROM You will find a list of all the spare parts along with their code which is needed for the spare part order form Please make sure that the code corresponds to the spare part you want to order 7 2 ORDER FORM Use the order form available in the appendix of your USER CD ROM for all orders This order form must be returned to your local CILAS dealer If you need to see a list of CILAS dealers please go to our web site www particle size analyzer com Please indicate on your order which model of your particle size analyzer you have its serial number and the version of The Particle Expert software you are using You have additional question or would like advice about a command or an order form please see the file available on our website download at www particle size analyzer com or in the user
68. he new database will be named and click on the O K button In the topic Aliases click on the Path line and type the whole path containing the new database For a network path a network drive has to be defined previously Contact to your network administrator to carry out this operation Exit the application by clicking on Exit in the File menu A confirmation of the changes is required to confirm the new database To confirm the changes click on the Yes button If you are not sure you want to make the changes click on the No button to cancel all changes 61 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 The new database can be selected using the Selection of the database function After the new base is selected you have to import the calibration file for your particle size analyzer To carry out this operation select the database GRANULOG then in the Tools menu sub menu Calibration click on export the calibration This operation must be repeated in wet mode and dry mode if your particle size analyzer has both wet and dry modes Select the new database import the calibration information included in the files KID DIF and KIL DIF Refer to the topic importing the calibration in the results dialog box Enter the serial number of the curren
69. he products he will use sample solvent etc can be used with a CILAS particle size analyzer The operator must do this before each analysis Finally after each measurement the operator needs to clean the particle size analyzer as explained in part 6 2 It is especially necessary if you measure a lot of different products These products can have properties that will react with each other WARNING Anybody who will work with the CILAS particle size analyzer must respect all these safety recommendations All users make measurements under their company s rules and responsibility Before starting a measurement operators must read the entire User Manual particularly section 2 3 which describes the symbols and safety rules Now you are ready to learn how to perform a measurement with your particle size analyzer Depending on your model you will refer to part 5 3 and or to part 5 4 5 3 MEASUREMENT IN WET MODE The CILAS particle size analyzer allows you to measure a sample in a wet mode A carrier liquid called Liquid carries the sample Before measuring with the particle size analyzer you need to define a carrier liquid for your product Knowing the sample s physico chemical properties will help you choose a good carrier liquid and a dispersing agent In this section we will explain the step by step process for making a measurement in wet mode A WARNING The w button allows you to stop a measurement if you have
70. he shipment box from all environment risks water gas dust etc 4 2 SAFETY REQUIREMENTS FOR INSTALLATION When installing your new CILAS particle size analyzer please be sure to follow these basic safety rules First never install the instrument alone Make sure two people are present at all times during installation To ensure proper installation we recommend that a CILAS agent or a technician accredited by CILAS be presence during installation This person will be in charge of the installation Other requirements are safety rules for users who manipulate products solvents proper ventilation in the laboratory good aspiration of air near the particle size analyzer by an aspirator or a laboratory hood If you want more details on these items please refer to part 3 4 of the installation manual provided with your particle size analyzer The user is required to read the entire installation manual before beginning system installation They also must follow at all of the safety rules specified in part 2 3 of this manual also available in part 1 5 of the installation manual CILAS is not responsible for damage or accidents that occur during installation Keep in mind that the particle size analyzer has one or two laser and has many electronic parts Be careful with electric and laser risks and completely read all safety advice given in the manuals 23 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATI
71. iameter measurements used to display the bar chart can be defined it must be a number between 10 and 100 You can also set an equivalent distance between each diameter by selecting the Equidistant box Curve you can set the parameters of the cumulative curve such as its thickness the number of points the markers used the color etc Overlay you can set up the parameters for an overlay report in the graphic window You can choose whether or not to view the histograms the cumulative curves and the grid Single you can set the parameters for a single report in the graphic window You can choose whether or not to view the histogram the value of parameters and the grid Another option allows you to normalize all your histograms If you check the Const histo height box all your histograms will have use 80 of the cumulative curve as their maximum value This display option allow the user to provide their customer with precise standardized graphics To validate your settings click on Validate You can also cancel any changes quit the window or ask the help Once your settings have been validated they become the default display settings 57 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 v Printing In this section you can set u
72. in the upper right hand corner of the screen If the numbers are correct please continue to the next step 33 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 If they are wrong you will need to change them To change them go in the menu Tools New Serial Number to change the serial number If the model is not correct please turn off the PC and the particle size analyzer and restart them If the problem persists contact your local CILAS dealer 6 Rinse the particle size analyzer once by clicking on the icon or by selecting from the menu Commands Liquid system Rinsing NOTE All commands are available in the Commands menu The most frequently used commands are available more rapidly using icons situated on the upper bar of The Particle Expert software 7 Fill the tank with the appropriated solvent water alcohol etc It must be the solvent you will use for the measurement To fill the tank use the valve button on the mimic screen i 8 Click on the icon or select from the menu Commands Measuring The following window will appear on screen 1180 L 7 0823 SOP name Standard L v Save SOP Sample ref i T Automatic incrementation Type produit o Liquid Cient o rs Comments i O Dispersing agent Operator ii
73. indow Figure 21 Searching the measurement files Figure 22 Load a measurement file Figure 23 Overlay of results Figure 24 Management of result files Figure 25 Creation of standard operating method SOP Figure 26 Options Figure 27 Creating of identification Figure 28 Cleaning the sample cell Figure 29 Cleaning the lens Figure 30 Sample cell holder MJ Sa eal sw a nf mfr for on fon fofofo bo W W 2 Go Go WW e olele lele 19 2 Iziz F va iQ oa oa oa joe oa jog oa joe 5 S S 8 S S S S S oO oO Q VIa alala lao OO CO NI DI Nn BR WD nN N F AA a ALAA KIRIT MN an an an AJAJAJ s lola DH cr in n N Rlalalo irae cre fava fall D N F 2 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 PART 1 INDENTIFICATION OF THE PARTICLE SIZE ANALYZER COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 1 1 SCOPE OF MANUAL This Particle Size Analyzer User Manual covers installation use and maintenance of CILAS particle size analyzer models CILAS 920 CILAS 930e CILAS 1064 and CILAS 1180 This manual is written for technicians who are thoro
74. ing laboratory tools such as a spatula You must have a signal adsorption of about 15 between the blank measurement and the sample measurement For the dispersing agent you will need about 1 2 ml and you can introduce the dispersing agent using a pipette 17 Click on the Sample measurement button The measurement starts and you can view the progress using the two indicators During the measurement you can view the time delay the action in progress the signal values see the following figure ERP REEEE f 83 Lal an SSuRResagaaae f A D marrer Co The Particle Expert FIGURE 15 Measurement Window 39 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 1 button allows you to see the evolution of the histogram during the measurement This option can help you to see the effects of parameters such as the ultrasound etc 18 When the measurement is finished the results window will appear To see how to view and manage the results from the CILAS particle size analyzer see section 5 5 NOTE When the measurement is finished the results are automatically stored in the database This lets you make several measurements before viewing the results 5 4 MEASUREMENT IN DRY MODE CILAS particle size analyze
75. ings Alarm In this section you define the alarms that warn you about a problem on CILAS particle size analyzer By default this part has been set to ensure proper functioning of the particle size analyzer for a majority of application CILAS recommends modifying the settings only if it is necessary and only after carefully read all the manuals Only technicians with a thorough knowledge of CILAS particle size analyzers should modify the alarm operations You will be able to set Nr of std deviation for background is where you set the deviation that is acceptable for a background measurement By default the value is 3 The standard deviation of the acquisitions that are made during a background measurement must be low enough to ensure a high quality measurement This standard deviation depends mainly on the quality of the bearing liquid A standard deviation of 0 5 would be ideal if it is very pure free from particles and air bubbles and a standard deviation up to 3 is acceptable in other cases If the predefined values are not suitable click on Another value to specify a standard deviation between 0 1 and 9 9 To obtain high quality measurement we recommend that you do not specify a standard deviation above 5 Laser value low limit If the laser signal is too low mainly caused by deposits in the glass cell the background measurement will be rejected The nominal value of the laser is 10 000 A low limit set to 7000 is
76. ix yellow black edged triangles with the electrical danger symbols affixed to elements presenting an electrocution hazard The location of these symbols is as follows transformer module figure 5 ultrasound board figure 4 distributor board figure 4 power line filters figure 4 board rack figure 5 fan figure 5 If one of these symbols is missing it must be replaced with another sticker which you can order from CILAS see part 7 EQUIPMENT COMPLIES CE MATERIEL CONFORME CE 89 936 CEE 73 23 CE NF EN 60825 1 LASER EQUIPMENT CLASS 1 EQUIPEMENT LASER DE CLASSE 1 FIGURE 2 Back view 9 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 M IISIRA MO VIDRE RAGLATION MOOT USD WAEISRE EI 20 9 BO NUI TISIRE VESE U ADAI Eo suw UIR GPE INVISIBLE AND VISIBLE RADIATION RAYONNEHENT LASER INVISIBLE ET WHEN OPEN AND INTERLOCK VISIBLE LORSQUE LA SECURITE DEFEATED EST NEUTRAL ISEE LASER DIODE DIOOE LASER MAX POWER 7 W PUISSANCE HARIAS 1P mi WAVELENGTH 830 635 na LONGUEUR D ONDE 83u LASER PROOUCT CLASS 38 APPAREIL A LASER DE CLASSE 38 FIGURE 3 Front view 10 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCL
77. le with an explicit name containing for example the product s name or code In section 5 6 the procedure for the creation of a SOP is explained Please refer to that section for more information on how to create a SOP 10 Next you will need to enter general information about the measurement such as the sample s reference the operator the liquid and the dispersing agent used If you select the box Automatic incrementation you will be able to make several measurements on the same sample A new window will appear where you have to define the index of the first measurement the total number of measurements and the time between two measurements This option is specially designed for companies which make multiple measurements using the same operating methods This option can also be used with the autosampler accessory 11 The next screen has three little squares In the first one from left to right you can define ultrasound parameters You can choose whether or not to have A dispersion using ultrasound for a defined time before the measurement And or a dispersion during the measurement WARNING Be careful using the ultrasound because it can disintegrate your particles and that would introduce an error in your results The ultrasound is necessary to have single particles and not aggregates You will need to define an appropriated amount of time for ultrasonic dispersion for each product 12 In another par
78. lts 6 2 b Preventive maintenance items Before operating the instrument the user should have the following items 1 set of hexagonal screwdrivers 1 set of flat wrenches 1 flat screwdriver aclean work area 1 cleaning kit wipes absolute ethylic alcohol lint free cloth 67 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 Once the user has gathered these items preventive maintenance can begin 6 2 c Preventitive maintenance These operations need to be carried out before each use of the particle size analyzer If the particle size analyzer is used frequently se preventitive maintenance should be done once a day in the morning before the first measurement is taken Make sure the particle size analyzer is disconnected from the power line Fluid connector module check the condition of hoses and replace any punctured hoses Video and data input connections check the condition of the connections Remove the particle size analyzer cover Check operation of the cover safety with a multimeter Check pump module hose condition replace any punctured polluted or worn hoses Check liquid inlet electrovalve hosing and piping Unclip stirrer from the top of the ultrasound tank Inspect sealing on the level sensors and union flang
79. ming comparisons In the last part called Organization you can choose the parameters you would like to select for comparison You can print an overlay report using the dedicated icon or clicking on the Overlay button in the Print section You will have all the information shown on the screen in a standard report formal To customize your report follow the procedure described above using ExpertReport software 5 5 c Management of the results files In the Management part of the window see figure 24 you can change several items in your results file s You can modify the file itself using the Modify button 51 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 Modify 40 920L 920LE 01 01 2000 Machine Type Company Place Sample ref 920LE Report config Erase Type produit bi Liquid Client 7 x Comments Dispersing agent Operator 7 m Particular diameters oO Define Modify user Create Display Image Erase image Calibration KI920LE DIF 3 36 01 01 1995 10 00 00 x Cumulative curve Cancel Cancel All FIGURE 24 Management of result files In this window you can change any of the parameters you want The modifications will b
80. n Mie s theory please see the documents about laser diffraction provided in the appendix of your USER CD ROM MONODISPERSED SAMPLE A monodispersed sample is a product that has a specific distribution You will only have one kind of population in a monodispersed sample Particles will be similar in size or will have a size distributed compatible with Normal law The particle s size is a well known value plus or minus a percentage You can summarize the particle size by the following mathematical equation X X 20 Where o sigma parameter v Q3 cumulative curve The cumulative curve Q3 x represents the proportion of sample that has a diameter equal or less than x It is obtained with the following equation Q3 x Where nj number of particles with a diameter x nr total number of particles 20 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 v q3 population density The histogram is called q3 in the software The histogram is obtained using the following equation 03 x 03 x loe i Xi q3 xi Where Q3 x value of the cumulative curve q3 x histogram s value 66599 xi diameter of class i y SPECIFIC SURFACE The specific surface is the total surface area of the particles divided by their weight To calculat
81. n install your new CILAS particle size analyzer After installation you will need to connect your instrument to aclean water supply for wet models acompressed air supply for dry models an electrical plug A personal computer PC WARNING The CILAS particle size analyzer is controlled by a personal computer PC The PC must have the proper configuration to run The Particle Expert software correctly The software runs in a Windows environment For more information refer to part 3 1 of your installation manual For more information on set up please refer to parts 2 6 of the installation manual The installation manual is provided in the shipping case of your CILAS particle size analyzer and on the USER CD ROM 24 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 4 5 STORAGE AND PROTECTION DURING A NON USE PERIOD The particle size analyzer is a laboratory instrument It is designed for measuring the size of particles contained in a powder suspension or emulsion If you are not going to use the system for a short or a long time you need to do the following rinse the particle size analyzer for wet model close The Particle Expert software turn off the PC turn off the particle size analyzer using the switch on p
82. ncentration of product for each measurement This will provide better reproducibility for your results To validate your settings click on Validate You can also cancel the changes quit the window or ask the help Once your settings have been validated they become the default alarm settings Y Analyzers In the last section you can configure the particle size analyzer and all your accessories using The Particle Expert software The lower part is inactive It is only accessible to CILAS certified technicians for corrective maintenance Users can only modify the upper part where you will find Options in this part you have to select the corresponding box for the accessory you will have installed on your CILAS particle size analyzer For more details about accessories please see their dedicated manuals available on your USER CD ROM Starting the checked box refers to the mode in which the particle size analyzer will run when the user boots up the software Wet method configures the particle size analyzer for a use in wet mode Microcell configures the particle size analyzer for a use in wet mode with the Microcell option actived Dry method configures the particle size analyzer for a use with dry mode Automatic means that the configuration will be pre set on the Controller board Models with wet mode only and 2 in 1 wet and dry mode are designed to start up using wet mode Models with dry mod
83. ns Maxwell etc You will also find information on the applications of laser diffraction The second description is a bit more complete but is more complex This document is designed for someone who wants to know more about laser diffraction and how we can measure a particle s size using this physical phenomenon Please refer to the document that best fits your needs 3 2 VOCABULARY In this section we will define different terms that are used throughout the manual This section is very important to help the user fully understanding of measurements provided by their CILAS particle size analyzer These definitions are used for the designation and calculation of all measurement parameters If you do not understand any terms used by The Particle Expert software in an analysis report or in a manual please refer to this section for a definition The definitions are given in alphabetical order All the equations and the entire vocabulary section refers to standard ISO 9276 1 v OPTIC CONCENTRATION OBSCURATION Percentage or fraction of incident light attenuated due to the diffusion and the adsorption of light by the particles This parameter is used to adjust the amount of sample necessary for an accurate measurement DENSITY The density is the density of your sample in g cm You will need to enter the density in the software to calculate parameters such as specific surface If you do not know the density of your sample you can m
84. o the background measurement You can set the amount time for the background measurement You can also set parameters such as the speed of the pump the use of ultrasound or the stirrer before during and after the measurement If you select the box Rinsing on default you will rinse the tank of the particle size analyzer after each measurement The second part is designed for the settings during the measurement You can set the measurement time and all the parameters before during and after the measurement Before the measurement you can set the ultrasound the pumping fast and then normal speed time and the stirring During the measurement you can set the pump and or the ultrasound You can choose to dilute the sample for a defined time Finally after the measurement you can set a default stop value for the pump and the stirrer The Cleaning section is dedicated to the rinsing settings You can choose the number of cleanings By default the number is 4 Next you can choose the frequency of cleaning and the configuration after each cleaning to stop or not stop the pump and or the stirrer NOTE CILAS recommends cleaning the tank of the particle size analyzer after each measurement If you do several measurements with the same sample CILAS recommends you rinse the tank only at the end of the measurements The next part is called Computation It is dedicated to the results of calculations done by the CILAS par
85. o this there are many different methods CILAS recommends you choose one specific method for each particular product considering the sample proprieties and the international and or the national standards in place in your country Preparation consist of a division of the sample B obtained by extraction into a smaller amount C in order to be measured with the CILAS particle size analyzer The amount of sample needed for a measurement in dry mode is between mg and 100 mg We have the same problem as before The sample C must be representative of the sample B and therefore an accurate representative of sample A If these conditions are met then when you measure the properties of C you measure the properties of your sample A in terms of size distribution For sample preparation there are many methods CILAS recommend that you to choose one specific method for each particular product considering the sample proprieties and the international and or the national standards in place in your country WARNING For each specific product you will need to define and use one procedure for sampling and extraction CILAS can use its laboratory of applications to help you select the correct procedure CILAS will use its experience in particle analysis to help you in the development of your sampling method With our laboratory of applications we try to improve both the sampling extraction and preparation of the sample and the standard operating procedure
86. osition 0 turn off the clean water supply and or the compressed air supply depending of your model clean the optical parts sample cell and lens barrel protect the particle size analyzer from dust using a plastic cap CILAS recommend you do not move the particle size analyzer during a non use period You can store the particle size analyzer if you are sure you have performed all the steps described above If the non use period is longer than 2 months CILAS recommends that you disconnect the electrical connections the water supply and or the air supply If you want to move to another place plant the particle size analyzer you will need to follow the procedure described in part 8 of this manual Be sure that you have cleaned the entire device and that water is removed from the tubing system If everything is OK you can place the particle size analyzer in its shipment case Be sure to also move all the documentation originally provided with the system manuals CD ROM parts etc CILAS recommends you move the PC with the instrument in order to save all measurements already in the database If you are not moving the PC you can zip the database and burn it on a CD ROM 4 6 ANSWERS TO FREQUENTLY ASKED INSTALLATION QUESTIONS If you have any question or want advice about the maintenance of the particle size analyzer please see the file available on our website download at www particle size analyzer com or on the user CD ROM You
87. ows you to load a special report configuration using Report config or to erase the report configuration using the Erase config button The last button is called Option It allows you to set up all the other measurement parameters in the window shown below Operating mode x Modes Computation Alarm Processing m Background Time jor 00 a E ml Measurement Time joo 15 Fa cal l Sample preparation Supply duration Ho Cleaning after measurement M Venturi Time 60 s FIGURE 18 Operating method in dry mode 44 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 In the above window you can set all the parameters from background measurement to results interpretation Each step has its own section into the window There are four specific parts The first section is dedicated to the measurement In the part called Modes you can select the measurement time for both the background and the sample You can also enter the sample preparation time in the Supply duration box You can also set the cleaning procedure You can choose to clean the venturi system after each measurement and can set the cleaning time NOTE CILAS recommends cleaning the venturi system after each measu
88. p the printing parameters Results obtained with a CILAS particle size analyzer can be printed directly from The Particle Expert software In the software you have Print with where you can choose to view the curves and or the table of data Below Print with you can link an image to the report To do that select both the Scale and Image boxes If you select Scale the image will automatically be the standard size Using Image you can choose the size of your image Enter the coefficient of size into the s box and the values for limits dX and dY This option is not used often because the ExpertReport software allows the same thing with optimized parameters Curve allows you to define the size of the graphical part The graphical part can be printed in a reduced format The size of the graphic to be printed can range from 33 to 100 of the original size Print with ExpertReport allows you to print the report using the optional ExpertReport software Identification if activated will print the users name in the report This option does not affect software compliant with CFR 21 part 11 When using 21 CFR part 11 the user name will automatically be included in each report print To validate your settings click on Validate You can also cancel the changes quit the window or ask the help Once your settings are validated they become the default print sett
89. plain how to create the directory and the files for the new database The default database filename GRANULOG is included in the file C Cilas Gwin32 Db To create a new database 1 On the Workstation or in Windows Explorer open the folder in which the new directory will be created 2 In the Files menu select New then click on File The new file is displayed on the screen with a temporary name 3 Type the desired name of the directory you are creating then press ENTER 4 Copy all of the files included in the folder C GWIN DBO into the new directory Be careful when creating a new database No calibration information will be included in the new database so you should perform an import of the calibration values before the first measurement The second item concerns the naming of the database The database engine requires a configuration file containing the name and the place for each different database You need to name the new database in this file This operation can be done by running the BDECFG program in The Particle Expert group of programs The The Particle Expert group can be accessed from the Start menu in the sub menu Programs from the task bar in Windows 95 or from the group of programs found in the office in Windows 3 11 The program then displays a dialog box containing 6 tabs Click on the Aliases tab and then on the New Alias button An input box will be displayed Input the name alias under which t
90. r allows you to measure a sample in a dry mode The sample is carried by compressed air Before measuring with the particle size analyzer you need to set the pressure of the compressed air to ensure proper dispersion The following section describes step by step how to perform a measurement in dry mode 5 4 a Preliminary tests Before beginning measurements for each product you will need to define the compressed air pressure needed to ensure proper dispersion Follow the procedure below 1 Introduce the sample in to the dry feeder The amount of sample needed is about 150 g 2 Start The Particle Expert software Be sure the mimic screen for the particle size analyzer is set to dry mode 3 Begin a measurement see the procedure in the following section 4 Check for proper dispersion by analyzing the results 5 If the dispersion is not correct select a different air pressure value and take another measurement If the results are good keep this pressure as a standard one for this specific product NOTE Each product has a specific setting for the compressed air pressure You will need to determine the right air pressure setting before making a measurement The same air pressure must be used as part of the standard operating conditions Good results are due to proper dispersion 40 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANS
91. rement If you make several measurements on the same sample CILAS recommends that you clean the particle size analyzer only after all the measurements The next part is called Computation It is dedicated to the results of calculations done by the CILAS particle size analyzer This window is important because the results you are shown depend on how it is set up You can choose the format of your results in the Adjustments box You can choose between several result formats The most commonly used is the default format called Results in volume For more information on these items see section 3 2 of this manual You can select a list of particular diameters you want to measure in the second part If this list is already saved you can load it by selecting it from in the box You can display the selected list of diameters by clicking on Display You can also create a new list using the Create from selection button In the Sieve part you can compare results given by the particle size analyzer with those obtained by sizing You will need to enter the sieve s size and the distribution of particles This allows you to compare the two most common methods of particle characterization using The Particle Expert You can set the shape parameters in the Form section You will need to enter the width and the translation in the corresponding boxes These values will be used for the calculations Finally you
92. rticles contained in an emulsion or in a suspension Dry mode cannot be used with these kinds of materials y Initial state solid The choice of which mode to use for a solid is more complicated than for a liquid The choice is made after considering all the characteristics of the product and the amount of sample needed for analysis Many parameters enters in to the final decision To find the best dispersion mode the best way is to try making some measurements with your particle size analyzer CILAS can use our experience with particle analysis to help you determine which method should be used The procedure for choosing wet or dry mode is shown in the following table Sample s proprieties 1 Quantity of sample l necessary for one analysis WET DRY ow low WET DRY 2 Heterogeneity WET DRY with high sample divider ow ow I WET DRY 3 D high DRY with Free Fall DRY with low pressure idi 6 Reactivity to organic and inorganic solvents ow pii l WET DRY 1 Toxicit its high FIGURE 7 Choosing the dispersion mode for a solid sample After revieing all these parameters you will be able to determine the dispersion mode for your solid sample Once the dispersion mode is chosen please use the same dispersion mode each time you make a measurement on the same type of product Keep in mind that a dry dispersion requires a bigger amount of sample than a wet dispersion The two steps described in this paragr
93. spersion CILAS provides a complete solution with three products corresponding to three different measurement ranges CILAS offers a series of particle size analyzers with measurement ranges between 0 04 um to 2500 um The figure below shows the CILAS model numbers and their corresponding measurement range CILAS 920 CILAS 930e CILAS 1180 0 04 0 3 400 500 2500 um FIGURE 1 Range of CILAS particle size analyzers Laser diffraction is now a very common and widely used method for particle characterization With over 30 years of experience and knowledge CILAS is the best choice to be your partner in particle analysis 2 2 CHARACTERISTICS OF THE PARTICLE SIZE ANALYSER Compared to others systems or methods CILAS particle size analyzers have many advantages Our instruments are compact with a high level of performance The most important characteristics of CILAS system are v A precise and reliable system CILAS uses a short bench concept which means users do not have to worry about optical alignment The optical short bench is only available from CILAS and provides more reliable measurements Its robust design ensures reliable operation even in a hazardous industrial environment v A fast and easy to use system The user simply has to introduce a sample into the particle size analyzer A few seconds later results will appears on the computer screen CILAS particle size analyzers are designed to ensure proper dispersion liquid
94. t you will define the parameters used for the interpretation of results You can select from three choices The first selection allows you to choose Mie s theory instead of the standard Fraunh6fer theory Mie s theory is used for thin below 1 um and or transparent particles Fraunhofer is the most common used theory corresponding to an approximation of Mie s theory If you select Mie s theory the following window appears 35 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 Sample Save Delete Index 0 000 0 000 i Liquid o Index 10 000 Save Delete FIGURE 12 Mie s parameters In the window you will need to enter the refractive index of your product and of your carrier liquid The refractive index is a complex number with a real and an imaginary part A database is available for both if you click on the right side of the box Its contains the most commonly used products If you want to introduce a new value into the database enter it in the Index boxes and save it using the Save button Save it with an explicit name and or comment in order to find it rapidly You may also want to measure the specific surface see part 3 2 by selecting the corresponding box A window will appear in to which you need
95. t particle size analyzer in the menu Tools gt Change serial number This operation must be repeated in wet mode and dry mode if your particle size analyzer has both modes WARNING Be careful Save your database regularly CILAS can not held be responsible for the lost of data due to a problem with the database Before performing any operations save the database CILAS recommends that you frequently burn a CD ROM with the saved database You may want to move change or zip the current database Before zipping or moving your database please be sure that you have saved all the results Be careful because you can lose your data if you do not follow this advice If you only want to change your database go on the menu Tools Update database Secondary database management You can add a new folder which will be your new database If you want to zip and or move your database open the menu Tools Update database Save database To move your database you should zip it Select the directory you want and enter the name Click on Ok to validate You have zipped your database Y Security levels The security levels are defined the first time you run The Particle Expert software after installation The software will ask you if you want security levels compliant to CFR 21 part 11 multi level security free access without security levels Please refer to the installation manual available on your USER CD R
96. t to select all the files click on gt gt To unselect file s use the same procedure in the opposite direction using the lt and lt lt buttons When you have chosen the file s you want click on Validate 49 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 3 1 Issue September 2004 y Several measurements Once you have clicked on validate the following window will appear on the screen List of selected measurements Ea Modify selection m Visualization gt gt Management Single Modify 119 1180L Y 1180L Overlay Create di y 194 1180D 119 1180D 017C Import m Printing Export Stat Single ble ik Overlay Processing Result in volume Execute 2 useful 2 Selected Delete il None Close Help FIGURE 22 Loading a measurement file I In this window you can view modify compare and print the results obtained with your CILAS particle size analyzer To do something with a file you have to select it You can select all the files available in the list by clicking on All You can unselect all the files by clicking on None You can select the files one by one using your mouse or the space bar on your keyboard To view or print a single file select a file
97. the cumulative curves The most commonly selected values of 10 50 and 90 are used as default values You can change these values or add other points on the curve The Alarm section is dedicated to the alarm settings for the CILAS particle size analyzer You can define the limits of concentration recommended default values are 0 300 You can define the number of attempts or you can select only one measurement by choosing the corresponding box A Quality control option is available This option is designed specially for a routine analysis You can define size limits to validate or record your sample Using the quality control option the instrument can determine if the sample is accepted or not In the last part called Processing you can select the kind of calibration you want from a list of suggestions Be careful when selecting the calibration type because all of the results depend on the calibration being done correctly CILAS recommends you use as a default the latest updated calibration To validate all the settings click the Validate button in each specific window If you do not validate the settings the standard settings will be used for the measurement When all the settings are done you can start the measurement using the last part of the window The following paragraph describes how this is done v Making a measurement 14 Start the background measurement by clicking on the Background meas but
98. ticle size analyzer This window is important because the results you are shown depend on how it is set up 37 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 You can choose the format of your results in the Adjustments box You can choose between several result formats The most commonly used is the default format called Results in volume For more information on these items see section 3 2 of this manual You can select a list of particular diameters you want to measure in the second part If this list is already saved you can load it by selecting it from the box You can display the selected list of diameters by clicking on Display You can also create a new list using the Create from selection button In the Sieve part you can compare results given by the particle size analyzer with those obtained by sizing You will need to enter the sieve s size and the distribution of particles This allows you to compare the two most common methods of particle characterization using The Particle Expert You can set the shape parameters in the Form section You will need to enter the width and the translation in the corresponding boxes These values will be used for the calculations Finally you can choose the values you want to measure for
99. to send with the instrument the safety data sheets of all the products samples measured using CILAS particle size analyzer The withdrawal of an instrument is a very complex and difficult thing There can be problems with your particle size analyzer if a highly skilled technician does not perform the withdrawal 76 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 INDEX TI COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 A M Accessories 62 Maintenance 65 71 Alarms 37 44 57 58 Measurement mode wet or dry 29 46 Mie 19 B Mimic screen 32 40 41 Background measurement 37 44 C O 9c Options 36 Carrier liquid 19 30 Order form 73 Cell 69 70 Certificates of conformity 5 P Cleaning 67 70 Printing 48 53 Configuration 54 59 Protection 24 Create a SOP 34 42 53 55 D R Ranges 7 angers oe Real time signals 38 Database 59 61 Rejects 63 64 Diameters 10 50 90 16 19 Koi 47 Dunas oe n Research of results 47 49 Dispersing agent 18 30 31 Results 46 48 Distribution results 17 20 Rosin Ramier 18 Dry mode 39 46 E S Electrical safety 8 14 Safety 8 14 Errors measure 26 27 Sample
100. ton The particle size analyzer will start In the window you will see two gauges that show the measurement status The blue one corresponds to the percentage of background time already passed The red one corresponds to the percentage of the total measurement the instrument has completed The blue gauge allows you to see the progress of the background measurement 15 When the background is finished a message Background OK will appear in the window Introduce the sample is also displayed Please make sure that these two messages are displayed before beginning the next step You can pass a step by clicking Next action and you can prevent the background measurement by clicking Cancel background CILAS does not recommend doing that To ensure accurate results you need to do a complete background measurement before each sample measurement 38 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 16 Introduce the sample in the ultrasound tank see figure below If your sample is an emulsion or a suspension go on to the next step If your sample is a powder you have to also introduce the dispersing agent FIGURE 14 Sample introduction in wet mode WARNING The amount of sample necessary to perform a measurement is about 100 500 mg You can introduce it us
101. ty to avoid bubbles and a low evaporation point homogeneous compatible with the different parts of CILAS particle size analyzer see tables given in the appendix of your USER CD ROM If the liquid does not comply with one of the above points you can not use it as a carrier liquid for your analysis Once you have determined the carrier liquid for a specific product do not change it The main carrier liquids used are water alcohol methanol ethanol isopropanol isobutanol benzyl alcohol cyclohexane ethylene glycol acetone oil palm oil parafin oil hexane ammonium citrate an ammonia solution glycerol xylene diethyl ester toluene benzene etc The most commonly used solvents are water and alcohol For all solvents please check their compatibility with the tubing and the joints of CILAS particle size analyzer Y Dispersing agent The use of a dispersing agent is recommended by CILAS in order to improve your results Like the carrier liquid the dispersing agent must have some basic properties nonreactive with the product and the carrier liquid non absorbent at the working wavelength must improve product s wetability see figure below homogenous and stable 31 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 3 Be
102. ughly familiar with instruments used in laboratories for physicochemical characterization of materials This user manual is available on the USER CD ROM provided with your particle size analyzer in the directory MANUALS The manual is available into pdf format and can be print if necessary Keep in mind that this document can not copied disclosed or transmitted without written permission of CILAS 1 2 IDENTIFICATION OF THE EQUIPMENT AND DOCUMENTATION CILAS particle size analyzers are designed to measure the particle size of powder matter ranging from 0 04 um to 2500 um depending of the model Our systems allow the user to measure particles of many different sizes without changing the optics or the calibration of the equipment The particle analysis is based on diffraction of a light source by the samples under analysis The system requires the use of a monitor connected to an IBM PC or compatible for processing the results Optional pieces of equipment sample feed CCD camera can extend the particle size analyzer s capabilities This particle size analyzer user manual explains how to use the particle size analyzer it does not cover optional equipment It is a part of a group of manuals which describe all the specific functions of the particle size analyzer Installation or maintenance are covered in this manual and are also described in more detail in other manuals available on your USER CD ROM Keep in mind that users are only authorize
103. ur website www particle size analyzer com 5 6 b Configuration You may have to reconfigure the system software and or hardware during the life of CILAS particle size analyzer These operations are very delicate and can be the sources of errors in the instrument if not done properly Be careful with all setting that you modify There are some specific cases where you will have to reconfigure the system such as when setting up a new accessory alarms etc To configure the system go on the Tools Options menu or click on the ued icon A new window will appear see figure on the next page The window is composed of different parts Each part is dedicated to a special configuration interface measurement treatment of results printer and hardware alarm and configuration of the analyzer The next section describes what you can change in each part 55 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 Interface Organization Display Printing Alarm Analysers Language V Logout Company v Place bd Logo 5 Criterion 1 T ype produit Criterion 2 Client Cancel Help FIGURE 26 Options y Interface In the interface part you can set global parameters of The Particle Expert software Using the Language
104. ween the particle size analyzer and the PC 5 Turn off the water supply and or the compressed air supply depending on the model of particle size analyzer 6 Disconnect the links between the particle size analyzer and the two supplies air and or water 7 Remember to keep all the accessories with the instrument including all the tubing system and other items originally provided with the particle size analyzer 8 Clean the sample cell and the optical parts of the particle size analyzer 9 Retrieve the shipping case and place it near the particle size analyzer 10 Set the particle size analyzer in to the shipment case 11 Place all the accessories and devices originally provided with the instrument in the shipping case 12 Put the PC or the database already zipped and burned on a CD ROM with the particle size analyzer if you want to save the results of previous measurements The procedure above is also applicable if you have to ship the particle size analyzer to your dealer or to CILAS headquarters in France for maintenance If you are sending your system for maintenance you will need to determine which parts of the system you need to send In order to do that you have to provide a good description of your problem using the Bug report document The technician will tell you which parts of the system you will need to ship WARNING If you ship the particle size analyzer to the CILAS plant for the maintenance please remember
105. will be made in order to ensure the safety of users and maintenance technicians WARNING Anybody who will work with or on the CILAS particle size analyzer must respect all these safety recommendations The operator in charge of maintenance must have the necessary skills and information to understand the operation of an electromechanical device All users must follow the safety rules and policies of their company 2 3 a Symbols Laser and electrical safety symbols are affixed on the outside and on the inside of the instrument If one of the symbols is missing it must be replaced with a new safety sticker v Laser symbols On the back of the instrument figure 2 there are two labels in French and in English specifying the laser source class 1 and its certification of compliance with standard CEI 825 ADD 1 dated 17 09 1990 Two yellow black edged labels figure 3 located on the front of the optical block specify the laser radiation hazard maximum laser diode power 3 mW wavelength 830 nm and device class 3B when the cover s safety interlock is de activated A yellow black edged triangle figure 3 with the laser danger symbol is affixed to the optical block tube 8 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 y Electrical symbols There are s
106. with the mouse and click on the Single button in the Visualization or Printing section If you select visualization the results window will appear on the screen If you select print the report will be printed By default the standard report format is printed It is possible to change the report format Please refer to the following section to learn more about the management of the result files You can also view several files at the same time Select all the files and click on the Overlay button A window appears on the screen like the figure below 50 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS N T 1503 192 31 Issue September 2004 Overlay curves OP x Graphic Results Organization 400 in volume 119 1180L 194 1180D 118 Qy Cumulative values q3 Histogram 410 fone 100 0 il iameter um 4 0 o a B x l FIGURE 23 Overlay of results In the Graphic part of the window you can view the cumulative curves and the histograms In the Results part you can view a table containing the results and the differences between them For each result you will see the minimal value the maximal one and the standard deviation It is possible to save this information as an Excel file This option is specially designed for perfor
107. with your particle size analyzer please see the file available on our website download at www particle size analyzer com or on the user CD ROM USERCDROM Answers to frequently ask questions Frequently ask questions pdf You can also contact your local CILAS dealer 65 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 PART 6 MAINTENANCE 66 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 Maintenance is an important part of taking measurements with any instrument CILAS particle size analyzers do not require much maintenance The short bench concept means your CILAS particle size analyzers is very reliable There is no need for optical alignment if the instrument if it is used in normal operating conditions In this section we will describe the maintenance operations If you have any problems with your particle size analyzer please carefully read this section 6 1 SAFETY REQUIREMENTS Before performing any maintenance operations please carefully read the safety rules described in section 2 3 of this manual The person in charge of the maintenance must be trained during installation by a CI
108. y your company as operator analyst or controller and your password Click on the Validate button GWIN Identification User name durand Level Operator Password xxxxxxxxx crea FIGURE 9 Password amp Security levels 32 COMMUNICATION REPRODUCTION ET UTILISATION INTERDITES SANS AUTORISATION ECRITE DE CILAS THIS DOCUMENT MUST NOT COPIED DISCLOSED OR TRANSMITTED WITHOUT WRITTEN PERMISSION OF CILAS NT 1503192 31 Issue September 2004 NOTE Please do not forget your user name your password or your security level CILAS recommend that all companies keep these parameters in a database This database can help when someone has forgot his parameters 4 The main window of the software will appear on screen For a measurement in wet mode you must have the following screen 1180 L 823 830nm m20 KIL DIF gt Import auto OK FIGURE 10 Wet mode s mimic screen Lso If this screen is shown you can continue If not please click on the icon eso to change the configuration of the software NOTE If you have an instrument with only wet mode the mimic screen will always be the correct one If you have a 2 in 1 model please check that the mimic screen corresponds to the measurement mode you want dry or wet Change it using the icon if it is not correct 5 On the mimic screen check to make sure the model of CILAS particle size analyzer and its serial number are correct They will appear

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