Instruction Manual FRITSCH team/fritsch/Fritsch data/A22... · 2007-03-02 · edition 04/2002 index 001 programme manual "analysette 22“ fritsch zerkleinern partikelmessen teilen

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Instruction Manual

Program „analysette 22“

Laser-Particle-Sizer 32Bit for Windows

Edition 04/2002 Index 001 Programme manual "analysette 22“

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Fritsch GmbH Manufactures of Laboratory Instruments Industriestraße 8 D - 55743 Idar-Oberstein

Phone: 0049 6784 / 70-0 Fax: 0049 6784 / 7011 E-Mail: [email protected] URL: http://www.fritsch.de

Fritsch GmbH, Manufactures of Laboratory Instruments has been certificated by the TÜV-Zertifizierungs-gemeinschaft e. V. on June 24, 1994.

An audit certificated the accordance of the Fritsch GmbH to the DIN EN ISO 9001.

mailto:[email protected]

http://www.fritsch.de/

Table of Contents Page

Programme manual "analysette 22“

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1 General / Introduction..............................................................1 1.1 Information............................................................................................ 1 1.2 Short description of the program.......................................................... 1 1.2.1 The physical basics.......................................................................................... 1 1.2.2 The technical solution ...................................................................................... 2 1.3 Software Copyright Licence Agreement............................................... 4 2 Program Installation ................................................................6 2.1 Hardware and Software Requirements ................................................ 6 2.2 Integration of the data recording card in the Computer

(only COMFORT and ECONOMY models) .......................................... 6 2.2.1 The A/D converter card PCI............................................................................. 6 2.2.2 AD-converter-interface card ISA ...................................................................... 6 2.3 Setup of program.................................................................................. 8 2.4 Problems during Setup......................................................................... 9 3 General operation of windows program ..............................10 3.1 Windows ............................................................................................. 10 3.2 Main Screen ....................................................................................... 10 3.3 Main Pull-Down-Menus ...................................................................... 12 3.4 Dialogue-, Message- and Query-Windows ........................................ 13 4 Measurement ..........................................................................15 4.1 Measurement with Wet Dispersing Unit COMPACT.......................... 15 4.1.1 Execution of a Measurement ......................................................................... 15 4.1.1.1 Background Measurement ............................................................................. 15 4.1.1.2 Sample Dilution.............................................................................................. 15 4.1.1.3 Measurement ................................................................................................. 15 4.1.2 Programming Measuring Cycles .................................................................... 15 4.1.3 Example programming................................................................................... 16 4.2 Measurement with Dry Dispersing Unit COMPACT........................... 18 4.2.1 Execution of a Measurement ......................................................................... 18 4.2.1.1 Background Measurement ............................................................................. 18 4.2.1.2 Measurement ................................................................................................. 18 4.2.2 Programming Measuring Cycles .................................................................... 18 4.2.3 Example programming................................................................................... 19 4.3 Measurement with Wet Dispersing Unit COMFORT.......................... 20 4.3.1 Background Measurement ............................................................................. 20 4.3.1.1 Background Measurement with Multiple Measurements................................ 21 4.3.1.2 Background Measurement with Membrane Keyboard ................................... 21 4.3.2 Sample Dilution.............................................................................................. 22 4.3.3 Measuring the Particle Size Distribution ........................................................ 23 4.3.3.1 Measurement with Mini Cuvette..................................................................... 24 4.3.4 Cleaning Dispersing Units.............................................................................. 25 4.3.4.1 Cleaning Wet Dispersing Unit ........................................................................ 25 4.3.4.2 Flushing the Small Dispersing Unit ................................................................ 25 4.3.5 Monitoring the Flushing Process.................................................................... 26 4.4 Measurement with Dry Dispersing Unit COMFORT .......................... 26 4.4.1 Feeding with the Dry Dispersing Unit ............................................................. 26 4.4.1.1 Technical Specifications of Dust Exhaust ...................................................... 27 4.4.2 Cleaning of Dry Dispersing Unit ..................................................................... 27 4.5 Measuring with the NanoTec and MicroTec

device for wet dispersing or combination devices.............................. 28 4.5.1 Background measurement ............................................................................. 29 4.5.1.1 Background measurement during multiple measurement .............................. 30 4.5.2 Addition of the measurement sample............................................................. 30 4.5.3 Measuring the particle size distribution .......................................................... 31 4.6 Measuring with the NanoTec and MicroTec

device for dry dispersing or combination devices .............................. 32 4.6.1 Sample feed with dry dispersing unit.............................................................. 32 4.6.2 Cleaning the solid matter dispersing unit ....................................................... 33 4.7 Cancel Measurement ......................................................................... 34 4.8 Download Eeprom (only COMPACT)................................................. 34 4.9 Load Settings Last Measurement....................................................... 34



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5 Main Menu File .......................................................................35 5.1 Save Actual Result ............................................................................. 35 5.2 Load comparison curves .................................................................... 36 5.3 Load Old Result.................................................................................. 37 5.4 Export Results .................................................................................... 38 5.5 Database ............................................................................................ 38 5.5.1 Data Control description ................................................................................ 40 5.5.2 Find Dialog..................................................................................................... 41 5.6 Page Layout ....................................................................................... 42 5.7 Setup Printer....................................................................................... 46 5.8 Printout Selected Results ................................................................... 46 5.9 Terminating the Program.................................................................... 46 6 Main Menu Setup COMFORT, COMPACT and ECONOMY..47 6.1 Measurement Parameters.................................................................. 47 6.2 Calculation Parameters ...................................................................... 48 6.2.1 Calculation of the interpolation values ........................................................... 48 6.2.2 Selecting preselected tabular values ............................................................. 48 6.2.3 Calculation model .......................................................................................... 48 6.2.3.1 RRSB distribution........................................................................................... 48 6.2.3.2 Monomodal distribution.................................................................................. 49 6.2.3.3 Polydisperse Form Correction........................................................................ 49 6.2.4 User grain size............................................................................................... 49 6.3 Mie- / Fraunhofer Parameters ............................................................ 50 6.3.1 Reverse Fourier Optics .................................................................................. 50 6.3.2 Fraunhofer Diffraction .................................................................................... 51 6.3.3 Mie Scattering................................................................................................ 53 6.3.3.1 Description..................................................................................................... 53 6.3.3.2 Mie Theory..................................................................................................... 55 6.3.3.3 Complex Refractive Index.............................................................................. 56 6.3.4 Application of Fraunhofer or Mie .................................................................... 57 6.4 Reset to Fraunhofer............................................................................ 57 6.5 Set Measuring Range COMPACT...................................................... 58 6.6 Set Measuring Range COMFORT ..................................................... 58 6.7 Beam Alignment COMPACT .............................................................. 60 6.8 Beam Alignment COMFORT.............................................................. 61 7 Main menu setup NanoTec and MicroTec............................64 7.1 Parameters for measurement............................................................. 64 7.1.1 Parameter 1 ................................................................................................... 64 7.1.2 Enable measurement elongation ratio ........................................................... 64 7.1.3 Parameter 2 ................................................................................................... 64 7.1.4 Other parameters........................................................................................... 65 7.2 Parameters for calculation.................................................................. 65 7.2.1 Calculating interpolation values ..................................................................... 65 7.2.2 Selecting preset table values ......................................................................... 65 7.2.3 Calculation methods for filters........................................................................ 65 7.3 Mie Parameter .................................................................................... 66 7.4 Resetting as per Fraunhofer............................................................... 67 7.5 Setting the measuring range .............................................................. 67 7.5.1 Enable Nano option (only NanoTec wet dispersing) ...................................... 69 7.6 Beam adjustment................................................................................ 70 7.6.1 Manual alignment........................................................................................... 70 7.6.2 Auto alignment ............................................................................................... 72 7.7 NanoTec check................................................................................... 72 7.8 Display elongation ratio (Optional) ..................................................... 72 7.8.1 Principle ......................................................................................................... 72 7.8.2 Measurement ................................................................................................. 74 7.8.3 Presenting the result ...................................................................................... 75



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8 Main Menu Results.................................................................76 8.1 Graphics ............................................................................................. 76 8.1.1 Graphs ........................................................................................................... 76 8.1.2 Edit................................................................................................................. 77 8.1.2.1 Insert Object .................................................................................................. 77 8.1.2.2 Load Object ................................................................................................... 78 8.1.2.3 Insert from Clipboard ..................................................................................... 78 8.1.2.4 Save Object ................................................................................................... 78 8.1.3 Transformation............................................................................................... 78 8.1.3.1 Transformations............................................................................................. 78 8.1.3.2 Undersize / Oversize...................................................................................... 79 8.1.3.3 Changeover to q3 distribution ........................................................................ 79 8.1.4 Style............................................................................................................... 79 8.1.5 Options .......................................................................................................... 80 8.1.5.1 Export ............................................................................................................ 80 8.1.5.1.1 DDE Dialog Excel .......................................................................................... 80 8.1.5.1.2 OLE Dialog Excel........................................................................................... 81 8.2 Statistical Values ................................................................................ 81 8.2.1 Arithmetical Mean .......................................................................................... 81 8.2.2 Geometrical Mean.......................................................................................... 82 8.2.3 Square Mean ................................................................................................. 82 8.2.4 Harmonic Mean.............................................................................................. 82 8.2.5 Cauchy theorem............................................................................................. 82 8.2.6 Median Value................................................................................................. 82 8.2.7 Modal Value................................................................................................... 82 8.2.8 Specific Surface Area .................................................................................... 82 8.2.9 Span .............................................................................................................. 83 8.2.10 Skewness....................................................................................................... 83 8.2.11 Kurtosis.......................................................................................................... 83 8.2.12 Folk & Ward ................................................................................................... 84 8.3 Show d-Values ................................................................................... 84 8.3.1 Diameters ...................................................................................................... 85 8.3.2 D[4,3] and other means ................................................................................. 85 8.3.3 Different techniques give different means. ..................................................... 86 8.3.3.1 Volume equivalent ......................................................................................... 87 8.3.3.2 Weight equivalent .......................................................................................... 87 8.3.3.3 Number and volume distributions................................................................... 88 8.3.3.4 Inter conversion between number, length and volume/mass means............ 88 8.3.3.5 Measured and derived diameters................................................................... 89 8.3.3.6 Which number do wo use?............................................................................. 89 8.4 Average Results ................................................................................. 91 8.5 Control Card d-Values........................................................................ 91 8.6 User Sizes .......................................................................................... 92 8.6.1 Enter Theoretical Values................................................................................ 92 8.6.2 Enter User Sizes............................................................................................ 93 8.6.3 Calculate User Sizes...................................................................................... 93 8.6.4 Combine Oversize ......................................................................................... 94 8.7 Revalidation of Results....................................................................... 94 8.7.1 Revalidation Function .................................................................................... 94 8.7.2 Creating Revalidation Function ...................................................................... 95 8.7.2.1 Revalidation Function File.............................................................................. 96 8.7.3 Revalidation of Measurements....................................................................... 97 8.7.3.1 Selecting result .............................................................................................. 97 8.7.3.2 Selecting revalidation function ....................................................................... 97 8.7.3.3 Revalidation ................................................................................................... 98 8.8 Recalculation ...................................................................................... 99 9 Main Menu Special ...............................................................100 9.1 Winkler Three Phase Diagram ......................................................... 100 9.2 Tromp Calculation ............................................................................ 101 9.3 Mass Balance ................................................................................... 101 9.4 Chart ................................................................................................. 101 10 Main Menu Configuration ....................................................102 10.1 Set Configuration.............................................................................. 102



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11 Main Menu Help....................................................................102 11.1 Service (only „COMPACT“) .............................................................. 102 11.2 Printing system settings.................................................................... 104 11.3 Install sensor calibration (only COMFORT and ECONOMY)........... 104 11.4 About ................................................................................................ 104 12 Appendix...............................................................................105 12.1 Tromp Calculation ............................................................................ 105 12.1.1 Introduction .................................................................................................. 105 12.1.2 General Calculating Methods....................................................................... 106 12.1.2.1 Definition of a closed grinding circuit............................................................ 106 12.1.2.2 Basic equations (Mass balance) .................................................................. 106 12.1.2.3 Circulating load ............................................................................................ 107 12.1.2.4 Separator efficiency ..................................................................................... 108 12.1.2.5 Tromp value, Tromp curve........................................................................... 109 12.1.2.6 Characteristic data of the tromp curve ......................................................... 110 12.1.2.6.1 Cut point (CTP)............................................................................................ 111 12.1.2.6.2 Sharpness of separation .............................................................................. 111 12.1.2.7 Additional criteria for the slurry classifiers .................................................... 112 12.1.3 Test Procedure ............................................................................................ 113 12.1.3.1 Target of test and conditions........................................................................ 113 12.1.3.2 Sampling and duration of test ...................................................................... 113 12.1.3.3 Sieve analysis .............................................................................................. 114 12.1.3.4 Evaluation of test results.............................................................................. 115 12.1.3.5 Practical Calculation and Example............................................................... 115

Programme manual "analysette 22“ page 1

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1 General / Introduction

1.1 Information • The copyright of these technical documents remains at

Fritsch GmbH, Laborgerätebau. • Reprint and duplication of this instruction manual only by

permission of Fritsch GmbH, Laborgerätebau. • Please read this instruction manual carefully. • The contents of this instruction manual must be wellknown to

the user of this program.

1.2 Short description of the program The "analysette 22" laser particle sizer is a universally applicable device for determining particle size distributions of solids or drops in a liquid or gas (suspensions, emulsions or aerosols). Laser-Light-Scattering-Instruments utilize the physical principle of the scattering of electromagnetic Waves for the determination of particle size distributions. Parallel laser-light is scattered to fixed spatial angles, which depend on the particle size and the optical properties of the particles. Traditionally a lens focus the scattered light concentric to the focal plane, where a detector measures the Fourier spectrum (light energy distribution). The program calculates the particle size distributions according to Fraunhofer- or Mie-theory with the aid of complex mathematical methods. Execution of measurements and control of the measuring unit are part of the program as well as presentation of measurements results with different options. The FRITSCH Laser Particle Sizer “analysette 22” NanoTec is the first laser measuring device worldwide for determining the particle size distribution and for particle shape identification in a process. This new concept is possible with a completely new sensor geometry and revolutionary software.

1.2.1 The physical basics Laser light, which falls on the particles (powder, suspensions etc.), is deviated from its original direction because of scattering of light. The angular distribution of the scattered light mainly depends upon the size of the particles, and also on the wavelength of the laser and the refraction index. For particles, which are smaller than approx. 1 µm, the polarisation of the laser also plays a significant role: Clear differences are seen in the intensity depending upon the way in which the light is observed in the plane - perpendicular or parallel to the direction of polarisation of the laser. This is clearly seen in Figure 1 in the so-called “Polar diagrams”.


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Figure 1: Angular distribution of the scattered light for small particles. The blue (red) curve indicates intensity perpendicular (parallel) to the direction of polarisation of the laser. Laser diffraction devices measure the angular distribution of the scattered light emitted from a test particle. On this basis, the particle size distribution is calculated with special algorithms. The above diagram shows the requirements from the characterisation of particles in the nanometer range. These are: 1. The measurement must cover a maximum possible angular

area. 2. Polarisation of the light is very important. The scattered light

must be measured perpendicular and parallel to the direction of polarisation of the laser.

1.2.2 The technical solution The “analysette 22” NanoTec uses the proven inverse Fourier design patented by Fritsch GmbH. Wherein, a laser beam is focussed on the measuring cell with the test particle. The measurable particle size area can be adjusted by shifting the measuring cell. Measurements on different positions are “compiled” so that a maximum dynamic range is maintained. For the precise range, (particle size from 10 nm – lesser µm) the measuring cell is adjusted only a few millimetres away from the burning point. The new measuring principle is explained in Figure 2.

Figure 2: Forward and backward scattering


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The test particle is first illuminated by laser 1. The light, which is not scattered to the front, is detected by a conventional scattered light sensor. A prism guides light, which is scattered under large angles, to the additional sensor. In the 2nd measurement step, light is thrown on the test particle from behind, so that the light scattered in the backward direction can also be measured. Using a second prism and another additional sensor (not shown in the diagram), you can detect the scattered light parallel and perpendicular to the direction of polarisation of the laser. In this way, all the characteristics of angular distribution of the scattered light can be recorded.

Advantages of the measuring process: • Larger particle size area because of reversed Fourier optics • No expensive graphical optics are required for measuring the

scattered light • Robust; no readjustment/calibration of the additional sensors

is necessary. In the second measuring step shown in the diagram, the ‘analysette 22” NanoTec mixes the particle size distributions in the 100 nm – 1000 µm range. With the second measuring step, the lower measurement limit goes down to 10 nm. The particle size distribution is measured with a specially developed, highly effective algorithm, which is based on the solution of a Fredholm integral equation.


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1.3 Software Copyright Licence Agreement The retail consumer is to use the software of the laser particle sizer "analysette 22" only under the following conditions. By beginning to use the software, the retail consumer accepts these contractual conditions. The following Agreement will therefore exist between the user and FRITSCH GmbH of Idar-Oberstein: The object of the Agreement is the computer program recorded on data media, the related description and instruction manual and any other associated written material. Hereafter this is referred to as "software". For the period of the Agreement FRITSCH GmbH grants the simple (non-exclusive) and personal right - hereafter referred to as "licence" - to use the software on a single computer, i.e. only with one central processing unit (CPU) and only at one location. No utilization beyond this is permitted.

The licensee is prohibited from: • transferring the software or associated written material to

another party, making it accessible to another party or transferring the software to other computers over a network or a transmission channel without the written assent of FRITSCH GmbH,

• modifying, translating, reverse engineering, decompiling or disassembling the software, or producing derivative programs or copying the written material, translating or modifying it for another party or preparing derived programs from the written material.

• Through his purchase of the laser particle sizer "analysette 22" the licensee obtains ownership of the physical data medium but no rights to the software itself. Ownership of the rights is retained exclusively by FRITSCH GmbH. In particular, FRITSCH GmbH reserves all rights to the publishing, processing and use of the software.

• The software is protected for FRITSCH GmbH by copyright. As the licensee you may make one (1) copy of the program solely for backup purposes. You must reproduce and include FRITSCH GmbH's copyright notice on the backup copy. You are not to remove existing copyright notices or registration number in the software.

• You are expressly prohibited from copying or in any other manner reproducing the computer program and the written material fully or in part, in original or modified form or merged with other software or included in other software.

• Any assignment of the software to another party is expressly prohibited. Transferring the program package to another party is permitted only with the written consent of FRITSCH GmbH.


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• The Agreement is not temporally limited. If you act in contraction to the stipulations of the Agreement, you loose the right of use. In this event you are obligated to destroy or return to FRITSCH GmbH upon request the original program, any existing copies, the recorded computer program, including any modified copies, and the written material.

• You are liable to FRITSCH GmbH for any damage which FRITSCH GmbH sustains due to a violation of the provisions of this Agreement.

• FRITSCH GmbH is entitled to act on its own discretion to update or to create new or corrected versions. In this event the exchange or update of the software at your request will be performed only in return for payment of the fee established by FRITSCH GmbH for every updating.

• FRITSCH GmbH warrants to the licensee that on the date of delivery the data medium on which the computer program is recorded is free from defects in material under normal use and service.

• Any other warranty on the part of FRITSCH GmbH for freedom from defects is excluded. In particular, FRITSCH GmbH does not warrant that the software will work together with other programs selected by the purchaser.

• Liability for damage incurred by the licensee is also excluded, unless damage is caused intentionally or due to gross negligence on the part of FRITSCH GmbH. Liability also does not encompass consequential damage which is not covered under the guarantee.


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2 Program Installation

2.1 Hardware and Software Requirements The program runs on all 32Bit Windows system versions. For installation your computer should meet at least the following specifications: • 30 Mbytes of free hard disk memory • 64 Mbytes of main memory (RAM) • one free High-Speed RS 232 interface • screen resolution min. 800 x 600 pixels x 256 colours • for the COMFORT and ECONOMY version, a free PCI or ISA

slot (according to the board supplied) Please note that more main memory is required at high colour density because the program creates and prints out all graphics as a BMP-file. The system resources of Windows are subjected to correspondingly more load when more colours are selected.

2.2 Integration of the data recording card in the Computer (only COMFORT and ECONOMY models)

2.2.1 The A/D converter card PCI The A/D converter card used to capture measured values is a PCI plug-in card. In order to install the card in your computer, a free PCI slot is required. Install the PCI card supplied as described in the instructions for your computer. The corresponding driver software must then be installed.

Proceed as followed: 1. Insert the PCI card CD-ROM supplied in the CD drive. 2. The CD will start automatically if the Autostart option for your

CD-ROM drive is activated. 3. Using the mouse, click on the “Install driver” command. 4. You will then be presented with the “Driver installation” menu;

select “NuDAQ PCI”. 5. A list of various PCI drivers will now be displayed; select PCI-

9113. 6. You must then select your operating system. 7. Once the installation has been successfully completed, restart

your computer to activate the driver.

2.2.2 AD-converter-interface card ISA The AD-converter card needed for data collection is an ISA-type interface card. You need at least one free ISA extension slot in your computer. Fit the interface card into your computer according to the instruction manual of your computer.


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Setting the AD converter address ISA The interface card is switched to default address &H300. That means the programm for analysette 20 expects the card at the address &H300 in the memory of your computer. This address can be occupied by another card (like network- or soundcards). If you want to switch the interface card to a different address, just do this according to the following table. In most cases it is much more easier to change the address of plug-and-play sound- or network cards. Changing the address of an ISA card is NOT plug-and-play! The interface card occupies 16 sequential addresses in the I/O range of the PC. The default address is &H300. Possible is every address between &H000 and &H3F0. The setting must not interfere with other interface cards. If you change the address of the card, you should communicate this change to the programme for analysette 22. For this, you must change the entries on the Windows Registry. Call Fritsch for assistance.

Address A9 A8 A7 A6 A5 A4

160 0 1 0 1 1 0 170 0 1 0 1 1 1 180 0 1 1 0 0 0 190 0 1 1 0 0 1 200 1 0 0 0 0 0 210 1 0 0 0 0 1 220 1 0 0 0 1 0 230 1 0 0 0 1 1 240 1 0 0 1 0 0 250 1 0 0 1 0 1 260 1 0 0 1 1 0 270 1 0 0 1 1 1 280 1 0 1 0 0 0 290 1 0 1 0 0 1 300 1 1 0 0 0 0 310 1 1 0 0 0 1 320 1 1 0 0 1 0 330 1 1 0 0 1 1 340 1 1 0 1 0 0 350 1 1 0 1 0 1 360 1 1 0 1 1 0 370 1 1 0 1 1 1


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1 0

A9A8A7A6A5A4XX

(shown is the default setting) Connect your computer with the measuring unit. Please use the black flat cable. If the setting is wrong your computer will hang up during measurement, as the program is waiting for an ADC-ready signl, which cannot be received. You can stop the program by using the task manager only.

2.3 Setup of program • Insert the CD-ROM into the pertinent drive. • If your option for Autostart is activated for your CD-ROM drive

than a HTLM-Viewer will start up. Please follow the instructions given there.

• Perform the following steps if the HTML Viewer does not function: Call the SETUP.EXE file directly in the prg\a22___32\\DE directory or \EN on the CD-ROM via “Start”, “Execute” and “Search". The corresponding language version (English or German) is installed from there.

• Naturally you can also use the Windows File Manager or Explorer. Refer to the Windows “Help” for instructions on their use. However we recommend the procedure described above.

• Start the program SETUP.EXE on the diskette or CD-ROM by clicking-on it twice using the mouse.

• An installation directory is recommended in the first dialogue box. You can accept it or change it by making a new entry. The directory will be accepted. If the directory you selected does not already exist, Setup will create it.

• Press the ICON Button to adopt the installation directory or after entering a new one.

• Setup will then copy the pertinent files into the designated directories. Warning and error reports are explained in the section “Problems during Installation”.

• At the end of installation the Setup program will create a Program Manager group and Start icons.


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2.4 Problems during Setup If you encounter Message-Dialog-Boxes like „Couldn’t register vsview3.ocx“ or „Access violation while copying mfc42.dll“ normally it is sufficient to press „Ignore“. This will continue with the next step of the setup process. If you press „Cancel“ Setup will be stopped, if you press „Retry“ the same procedure will be executed again. If you did not change anything, the same error message will appear again. If an ocx file is not registered, there can be problems with your access rights e.g. with Windows NT 4.0 perhaps you do not have the rights to register some files (write to registry) and you must be logged in as administrator. The „Access violation...“ message only apperars, if some other programs or tasks are running in the background and the file to be installed is already be used by another program. Running programs also can be background-tasks like TWAIN drivers, anti-virus or email programs. If you press „Ignore“ setup will not overwrite the existing version of the file but continues with the next file. If your existing file is older than the file setup wanted to install the analysette 22 program probably will not run.

Attention:

The programme stores important programme settings in the Windows Registry under the key HKEY_LOCALUSER\SOFTWARE\VB and VBA SETTINGS\A22___32. If you install the programme under NT, XP or Windows 2000 as administrator, but later want to operate it after logging in as USER, you will be unable to find the entries created under administrator. In this case, you will have to export the corresponding key (REGEDIT.EXE) from the Registry under ADMINISTRATOR and import it back under USER with REGEDIT.EXE. This step should be followed even when you want to operate the programme on the same system with a different user profile.


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3 General operation of windows program

3.1 Windows The clear structure of the "analysette 22" Windows program facilitates learning and ensures simple and clear operation. The program is virtually self-explanatory ("intuitive user prompting"). Users of the "analysette 22" laser particle sizer with experience of similarly structured programs operated in accordance with the Window standard (such as Windows 98 or MS Office) will be able to operate the device without reading this chapter.

3.2 Main Screen After you call up the program, the title page appears and then the main screen of the "analysette 22" program. In the illustration, you can see the designations of the various windows and areas of a typical Windows screen:

• The Control-menu-box is in the upper left corner of each window. The control menu (also called the system menu) is most useful if you use the keyboard to resize, move, maximize, minimize and close windows or switch to other applications.

• The title bar shows the name of the application or document. If more than one window is open, the title bar for the active window (the one in which you are working) is a different color or intensitiy than other title bars.

• The window title can be the name of an application and the name of a document, or the name of a group, directory or file.

• The menu bar lists the available menus. A menu contains a list of commands or actions; you can carry out with Windows.

• By using scroll bars, you can move parts of a document into view when the entire document doesn´t fit in the window.


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• Using a mouse, you click the Maximize button to enlarge the active application window so that it fills the entire desktop or click the Minimize button to reduce the window to an icon.

• After you enlarge a window the maximize button is replaced by the Restore button, which contains both an up and down arrow. Click the Restore button or use the Restore command on the Control menu to return the window to it previous size.

• The window border is outside edge of a window. You can lengthen or shorten on each side of a window. The window corner can be used to shorten or lengthen two sides of a border at the same time.

• The insertion point shows where you are in the document. It marks the place where the text and graphics appear when you begin typing. The mouse pointer appears if you have a mouse installed. When you move the mouse, the position of the pointer changes on the screen.

• The Bottom line is a message line or help line which gives a short explanation of the opened window.

• The combo box at the upper right part of the main screen contains a selection of all open windows owned by the a-22 program. If you use the Alt-Tab-Key you can change between these open windows but you can also make your selection via this combo box. Just click on the down arrow and a list will be opened where you select your specific window by clicking on it. Be careful not to open too much windows at the same time because this involves less system resources for your windows system.

You will encounter these designations throughout the entire text of this handbook - and also in the handbooks for other Windows programs. The menu bar is used to operate in total 6 different pull-down menus. These are individually pulled down as sub-menus. Further menus or windows are opened in them. In general, windows are rectangular regions of the screen, the contents of which are represented independently of the remaining screen. They cover at least a part of the preceding window so that several windows, parts of which may be covered, may be visible simultaneously on the screen. Such windows include, for example, the main menu or the opened pulldown menus. The current window is given in the single-line list field; by clicking on the right-hand arrow on this bar, you can open a further window with the designations of all opened windows, including windows which are not the current window.


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3.3 Main Pull-Down-Menus There are three ways to open windows or to communicate with the pull-down menus: • When operating the program with the mouse, place the

mouse cursor on the program section which is to be selected and open the window of your choice with a click of the left-hand button.

• By pressing the Alt key, you activate the letters having a coloured background. By entering them on the keyboard, you can open the corresponding windows.

• Thirdly, after the sub-menu has been called up, you can use the arrow keys to move laterally into other sub-menus or up and down in the menu already selected so as to indicate the program section to be activated. Then press Return to open the corresponding window or enter a command.

A number of windows can be opened on the screen simultaneously but only one of these is active. A window has to be active before you can work in it. It is selected for activation by clicking on any location in the window (or the window is selected via tab key and activated with the space bar). Communication within the windows is also possible in different ways and differs according to window type. Depending on their contents the windows are classified as • dialogue windows • query windows • message windows


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3.4 Dialogue-, Message- and Query-Windows Dialogue windows always open when the mouse is clicked on a menu option which cannot be executed directly because different presettings still have to be made.

Query windows, like a warning, protect against unintentional aborting. Sometimes their purpose is just to acknowledge simple entries. Normally the window contains a question in an appropriate input box which is to be answered with "yes" or "no". Message windows open to announce a message, an error message, for example. These windows contain • Radio buttons • Check Boxes • Command buttons • Input boxes The radio buttons are used to toggle a specific function on or off. When changing from one button to the other, either use the mouse indicator and "click" to activate the toggle status (the activated status is indicated by a dot set in the brackets) or jump forwards with the tab key (or backwards by simultaneously pressing "Shift" and the tab key) from one switch to the next, activate the desired switch with the space bar and then return entry to the main program with Return. The same is valid for Check Boxes except you can select them independent from each other. The command buttons are used to transfer messages and commands to the program, either close windows by clicking with the mouse, or terminate program steps, and likewise click once with the lefthand mouse button when changing from one switch to the next and trigger the command with a double click or jump forwards with the tab key (or backwards by simultaneously pressing Shift and the tab key) until the "command button" is reached and return entry to the main program with Return.


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The input boxes are rectangular frames in a window which are provided to enter alphanumeric characters for commands or data entries. Characters are entered, deleted or existing ones overwritten via keyboard entry. Using the key commands usual in Winword, the input position can be displaced, or lines, words or letters can be deleted.

Winword Function Del Delete 1 character ^Del Delete the following word Arrow key Character to the left or to the right ^Arrow key 1 word to the left or to the right Pos 1 Start of line End End of line ^Pos 1 Start of text ^End End of text

Preset values in certain input windows can be incremented or decremented. This input can either be placed on the arrows with the mouse cursor on the scroll bar, changed step by step by clicking on a number of values or in jumps with the scroll bar. When the cursor keys are used, the value is only incremented or decremented one step at a time. Pressing the Esc key always interrupts a command sequence and displays the main menu. The characters entered in this window or an input box are not adopted; the ones previously used remain visible and active. The mouse indicator performs the same function when it clicks on one of the command buttons marked Cancel. If you exit the window by pressing RETURN, the new entries are effective; the old ones are deleted or ignored. The mouse indicator performs the same function when it clicks on one of the command buttons marked Ok. Which of the proposed options is utilised depends on the user's wishes and preferences. Keying in the commands requires less time. If the mouse is used, more steps may be required: First the correct menu has to be activated, the desired function selected and then several parameters defined. This is a more convenient procedure, however more steps mean more time. The same applies to the operation of the program with cursor keys. In the following descriptions of the program and the notes regarding its use, instructions refer primarily to the operation with a mouse. In so doing, we assume that the mouse included in the scope of the delivery is actually used.


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4 Measurement

4.1 Measurement with Wet Dispersing Unit COMPACT

4.1.1 Execution of a Measurement All the following parameters should be programmed in the analysette 22 Settings Compact Wet frame.

4.1.1.1 Background Measurement In order to eliminate the influence of the measuring liquid in the case of measurement in suspension a background measurement should be performed before every measurement, in particular if the measuring range has been changed. Any contamination from previous measurements is measured and its influence on the current result eliminated. The values of the background measurement are used as the basis for the calculation of all subsequent measurements. They are lost when the machine is switched off. Values can be obtained again only by a new background measurement.

4.1.1.2 Sample Dilution You should aim for a beam absorption of between 7 and 15 %. The measurement is started automatically as soon as the specified value is reached.

4.1.1.3 Measurement When the measurement is finished, the raw data are stored in the EPROM of the measuring unit. The particle size distribution (PSD) must still be calculated from these data. The program will load the raw data from the measuring unit and calculate the PSD.

4.1.2 Programming Measuring Cycles You programme complete measuring cycles on Settings Compact Wet frame of the main screen. Each click on a check-box programs the measuring unit with the appropriate settings. Some check-box are switched to inactive depending on the specific settings. Once programmed, cycles are maintained until further programming. The Start Measurement button initiates a measuring cycle which has been programmed and stored in the measuring unit. However, you can also press the START button on the measuring unit membrane keyboard. If you switch off the COMPACT measuring unit, all programmed steps will be lost. They must be reprogrammed after switching the measuring unit back on. The last settings are in each case saved in the "analysette 22" for Windows program.


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4.1.3 Example programming The points indicated on the „Settings Compact Wet“ frame are self-explanatory and do not normally need to be further explained. We shall therefore give only one example for the programming of a measuring cycle. You wish to carry out a background measurement, then go to Sample Dilution and next carry out the measurement. Sample Dilution is to be ended when 7% beam absorption is achieved. Your sample lies in the 2-200 µm range and you wish to expose it to ultrasound waves for precisely two minutes after adding the sample.

Select the following points (Select means there must be a cross in the associated check boxes. For explanation of check box see chapter 3.4 Dialogue-, Message- and Query-Windows). 1. Select check boxes Background Measurement, Sample

Dilution and Measurement. After Sample Dilution you will see an input field with a spin button. With the arrows up and down, you can set the desired beam absorption at which the COMPACT measuring unit leaves Sample Dilution and starts measurement. Sample Dilution values are saved in the output file and appear on subsequent printouts.

2. Under the Measurement check box you will find a second input field with the spin-button Scans. Here you set the duration of the measurement, i.e. the number of values which will be taken during measurement. Where the sample is not homogeneous, the number of values should be high, with monomodal, easily dispersible samples the standard setting of 5 scans (i.e. around 15 seconds) is sufficient. The duration of the background measurement cannot be changed.


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3. After adding the sample you wish to expose it to ultrasound for 2 minutes; i.e. select Ultrasonics check box first and then the available options After Sample Dilution. If the Ultrasonics check box is not selected, the option radio buttons remain inactive and you cannot select anything. The associated spin-button is used to set the duration of the exposure to ultrasonics. A value of 1 means that you wish to set an ultrasonics exposure of 30 seconds, a value of 2 means 60 seconds etc.

4. If you wish to clean the measuring circuit automatically after measurement, so that it is once more filled with clear liquid, select the check box Clean Fill After Measurement. Cleaning can also be carried out before measurement. In this case select check box Clean Fill before Measurement. If you discover that isolated particles are present in the measurement circuit after rinsing, you can increase the number of rinses using the associated spin buttons. The system is then rinsed not once but several times as required.

5. According to the specific weight of your sample in each case you can vary the stirrer speed using the Stirrer Speed spin button between settings 1 and 3. Stage 0 means stirrer off.

6. You can start the measurement by activating Start Measurement or pressing the green button on the COMPACT measuring unit. The programmed measuring cycle will be performed.

After measurement the "analysette 22 Program for Windows" calculates the particle size distribution automatically and you can display the result.


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4.2 Measurement with Dry Dispersing Unit COMPACT

4.2.1 Execution of a Measurement All the following parameters should be programmed in the analysette 22 Settings COMPACT dry frame.

4.2.1.1 Background Measurement In order to eliminate the influence of the compressed air or the influence of dust in the measuring area a background measurement should be performed before every measurement, in particular if the measuring range has been changed. Any contamination from previous measurements is measured and its influence on the current result eliminated. The values of the background measurement are used as the basis for the calculation of all subsequent measure-ments. They are lost when the machine is switched off. Values can be obtained again only by a new background measurement.

4.2.1.2 Measurement When the measurement is finished, the raw data are stored in the EPROM of the measuring unit. The particle size dis-tribution (PSD) must still be calculated from these data. The program will load the raw data from the measuring unit and calculate the PSD.

4.2.2 Programming Measuring Cycles You programme complete measuring cycles on Settings Compact Dry frame of the main screen. Each click on a check-box programs the measuring unit with the appro-priate settings. Some check-box are switched to inactive depending on the specific settings. Once programmed, cycles are maintained until further pro-gramming. The Start Measurement button initiates a measuring cycle which has been programmed and stored in the measuring unit. However, you can also press the START button on the measuring unit membrane keyboard. If you switch off the COMPACT measuring unit, all pro-grammed steps will be lost. They must be reprogrammed after switching the measuring unit back on. The last settings are in each case saved in the "analysette 22" for Windows program.


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4.2.3 Example programming The points indicated on the Settings Compact Dry frame are self-explanatory and do not normally need to be further explained. We shall therefore give only one example for the programming of a measuring cycle. You wish to carry out a background measurement and next carry out the measurement. The sample concentration limits should always lie between 2 and 5% beam absorption. Your sample lies in the 2-200 µm range. After measurement the system should be ready for the next measurement. Select the following points (Select means there must be a cross in the associated check boxes. For explanation of check box see chapter 3.4 Dialogue-, Message- and Query-Windows).

1. Select check boxes Background Measurement and

Measurement. Set the Minimum Absorption Value spin button to 2% and the Maximum Absorption Value spin button to 5%. (With the arrows up and down, you can set the desired beam absorption.) The mean measured sample dilution value is saved in the output file and appears on subsequent printouts.

2. Under the Measurement check box you will find a second input field with the spin-button Define Measure Duration. Here you set the duration of the measurement, i.e. the number of values which will be taken during measurement. Where the sample is not homogeneous, the number of values should be high, with monomodal, easily dispersible samples the standard setting of 5 scans (i.e. around 15 seconds) is sufficient. The duration of the background measurement cannot be changed.

3. If you wish to clean the measuring circuit automatically after measurement, select the check box Empty system after Measurement. The complete sample will be fed to the dust exhaust after measurement.


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4. You can start the measurement by activating Start Measurement or pressing the green button on the COMPACT measuring unit. The programmed measuring cycle will be performed. The Vibrating feeder is controlled through the measuring unit. The feed rate and the quantity of sample is set to a value which is enough to reach a sample dilation between 2 and 5%.

After measurement the "analysette 22 Program for Win-dows" calculates the particle size distribution automatically and you can display the result.

4.3 Measurement with Wet Dispersing Unit COMFORT Measurements with the wet dispersing unit are running in a similar way as with the COMPACT version. Just define your measuring cycle in the corresponding frame and press Start button for starting the measurement. Choose the number of scans for defining the number of measureming sweeps for the detector. Pump and stirrer speed can be varied from 0 to 100%. If you select a value for ultrasonics thne then ultrasonics will run the whole time during measurment. You can restrict this selection by choosing ultrasonics only during sample dilution or ultrasonics only during measurement. You also can preselect a waiting time after sample dilution for dilution of the sample. It is self-evident that you also can select a cleaning cycle after measurement.

4.3.1 Background Measurement For eliminating the influence of the used liquid with wet dispersing or dust in the measuring chamber with dry dispersing before the measurement there has to be done a background measurement. During the background correction also residues from preceding measurements are registered and the influence on the actual measurement is removed. For backgouend measurement you have prepared • Beam alignment is OK • Measuring range is OK • clear liquid is circulating • pump, stirrer and ultrasonics is trunning with mid power A click on the icon Background Measurement opens the window. You must set Pump, Stirrer and Ultrasonics by hand before. In the window a message appears that the measuring cell is moved to the righ position (if not already done).


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The light intensities for 31 channels of the detector are shown. After some seconds (depending on your setting of number of measuring scans) the measuring values are stored to a file. These values are the basis for all following measurements until a new background is done. Also after switching off the unit these values will survive. You can stop the actual backgound measurement by pressing Cancel. The main screen will be shown and the measuring values will not be stored. The break can be necessary if you selected background measurement wrongly. Pressing Ok stores the measuring values until now and also closes the window.

4.3.1.1 Background Measurement with Multiple Measurements

If you selected multiple measurements in Set Measuring Range then a background measurement will be taken for each cell position. As with normal background measurement you have to set pump, stirrer and ultrasonics before start. The background measurement itself is running automatically.

4.3.1.2 Background Measurement with Membrane Keyboard

Pressing the Zero-button on the membrane keyboard of the dispersing unit (it can look different to the picture show above, but has the same buttons) you also can start background measurement. The course of events is the same as if the procedure was started by the icon Background Measurement. If you want to have defined intensities for pump, stirrer or ultrasonics just press the appropriate „+/-“ buttons until the desired value is reached. Pressing Drain open a valve below the ultrasonic bath and the liquid is flushing out of the system. Releasing the button closes this valve. Pressing Dispersant fills the ultrasonic bath with liquid. Releasing this button closes the valve.


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4.3.2 Sample Dilution For sample dilution you have prepared 1. Beam alignment is OK 2. Measuring range is OK 3. clear liquid is circulating 4. pump, stirrer and ultrasonics are running 5. background measurement is OK One click on the icon opens the corresponding window

In this window even with a very low sample concentration a temporary particle size distribution is shown. This distribution is not very accurate, but it is a hint for the real size distribution and you have the feedback if your choosen measuring range is OK. Filling more sample in you should observe the display of the coloured bar which shows you thesampe concentration. It should be 7 to 15%.

The whole procedure can also be started by pressing the Dilution button of the membrane keyboard. By pressing the Sample button on the membrane keyboard you can open the By-Pass valve if your dispersing unit is connected to a sample line. By pressing Dispersant you can add clear liquid to reduce the sample concentration in the ultrasonic bath. There is an overflow connection to prevent the liquid from run over the ultrasonic bath.


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4.3.3 Measuring the Particle Size Distribution For measurement you have prepared 1. Beam alignment is OK 2. Measuring range is OK 3. clear liquid is circulating 4. pump, stirrer and ultrasonics are running 5. background measurement is OK 6. sample dilution to feed your sample to the laser beam

In the window measurement you see the light intensities of the 31 cahnnels similar to the representation know from background measurement. Intensities are higher now as the sample scatters light to the sensor channels.

Single Measurement The measuring cell is at the same position as with background measurement.Measuring values are directly recorded and processed. The size distribution is calculated directly after finishing measurement and you can test the result immediately.

Multiple Measurement The measuring cell is moved at least to two different cell positions. Measuring values are recorded for all cell positions. During background measurement the cell first is positioned at the left side – coarse range – and then moved to the fine range. Measurement starts with the fine range. Every time the measuring cell is moved a window informs you about the actual cell position.

The measurement can be started by pressing the Meas button on the membrane keybord.


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4.3.3.1 Measurement with Mini Cuvette For a measurement with the mini-cuvette please put the cuvette into the laser beam and take it out again. The laser emitter switches off automatically by the protective switch when you open the internal protection hood. It restarts automatically when you have inserted the cuvette into the holder and the hood is closed again. A small measuring range is usually set for the measurement with the mini-cell: Cell distance is < 40 mm what corresponds to a particle size of < 100 µm. The shift of the cell holder with the mini-cell is automated if you selected the use of the mini-cell when setting the parameters for the measurement. Each set measuring range with cell position < 100 mm activates a special program when the "Mini-Cell Switch" is activated: When running the background measurement, the measurement is conducted in the customary manner because the special program assumes that you set the measuring range correctly and that the cuvette filled with clear liquid is in the holder for the mini-cell. After the background measurement, a window opens with the message that the cell is to be placed at position 100; the automatic version handles this automatically. In this position it is very easy to take out the mini cell for feeding in your suspension. Afterwards a second window opens with the request that the sample is to be entered and - after you have done this - to inform the program by clicking at <OK> that the auto-ranger is permitted to move the cell into the measuring position. If you do not utilise an automatic version, you will be requested prior to adding the sample and thereafter to push the cell to the position you selected. In the measuring position the program first measures the absorption of your sample, i.e. it determines whether you have placed enough sample material in the mini-cell. You are familiar with the pertinent image from the program section "Feeding the Sample". By pressing RETURN you can terminate the check image and - in the next window - accept the offer to replenish the sample by clicking OK or start the measurement by click MEASUREMENT.


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4.3.4 Cleaning Dispersing Units 4.3.4.1 Cleaning Wet Dispersing Unit As soon as the actual measurement (and any repetitive measurements) have been completed, you have to flush the measurement circuit. Avoid unnecessarily leaving the measurement sample in dispersing unit and thus in the entire measurement circuit for a protracted period of time. Under no circumstances are you to leave the feed pump for the suspension dispersing unit switched off for a long time while there is a sample in the measurement circuit. When the feed pump is switched off, the liquid stops circulating. The particles settling out as a result could produce deposit of particles in the measuring and tubing system which would be difficult to remove.

By pressing the key "Clean Fill" on the membrane keyboard of the dispersing unit you can start the flushing.

4.3.4.2 Flushing the Small Dispersing Unit Conduct the flushing of the small dispersing unit directly at the dispersing unit. Turn the valve handle which is during the measurement set to "Measurement" to "Drain/Fill". When supply via the connected hosing "Liquid Supply" is unobstructed, clear liquid then flows into the glass tank. When the pump is switched off, the level of the liquid rises and permits thorough flushing of the glass tank, measuring cell, valve and tubing system. Alternately turning the

valve handle off and on intensifies the flushing process. In addition, you can intensify and accelerate the flushing action by varying the pumping speed.

Drehzahlregulierung Pumpe und Rührer speed control pump and stirrer

Ventilhebel valve

zur Messzelle to cell

Zulauf liquid supply

von der Messzelle from cell

Abfluss drain


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4.3.5 Monitoring the Flushing Process To monitor the effect of the flushing, click once in the tool bar of the main menu to call up the program "Adjusting the laser beam":

Following a good flushing when the glasses of the measuring cell are clean, you may have opened such a pleasing window. A similar test method is to call up the program "Addition of sample". If the display indicates a value which is between 0 and 1 for the absorption, the flushing process was good.

4.4 Measurement with Dry Dispersing Unit COMFORT Select the number of the scans, backround measurement and measurement exactly the same as for measuring with the liquid dispering unit. You can chose whether the whole sample inside the funnel of the vibratory feeder will be measured or whether the system will be emptied automatcally after the measurement. As minimum beam absorption you should be set at least to 1%, maximum to 8%. Standard values are minimum 2% and maximum 4%. You can preset the values for the promotion rate and the delivery when the window Sample dilution is displayed. During the measurement the amount of the sample will be automatically regulated to keep the range of beam absorption.

4.4.1 Feeding with the Dry Dispersing Unit Using the solids dispersing unit in connection with the measuring units of the COMFORT version. It is possible to measure particle size distributions from about 0.6 to about 1250 µm. For this purpose, the post-dispersion nozzle and exhauster for the dispersion of solids are installed in the measuring unit. During the measurement the sample poured into the funnel tube of the dispersing unit is fed in metered doses by the vibratory feeder. A stream of air carries it to the post-dispersion nozzle in the measuring unit. In the post-dispersion nozzle it is again disagglomerated, accelerated and blown into the laser beam. Mounted across from the nozzle is an exhauster with a hose through which the measure sample is sucked out of the measuring unit. The exhauster is always activated automatically during measurement. This ensures that the samples transported into the measuring unit are also sucked out.


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Before the feeder channel is activated it is imperative to insert the suction hose of the exhauster into the side wall of the measuring unit, to insert the connection line of the exhauster into the control box and to switch on the exhauster (see instruction manual COMFORT version). If the pressure in the intake air line (min. 5 bar) does not change significantly during operation, it is only necessary to check the values for the air pressure before the measurement (3 to 4 bar). For the measurement, the sample is poured into the funnel. The feeder is switched on during sample dilution and the feeder amplitude and sample quantity can be controlled by pressing the appropriate keys in the settings frame of the main screen. The more uniformly the sample is distributed on the channel, i.e. the more evenly it can also flow out of the funnel beforehand, the quieter the measurement. During Background measurement the nozzle is positioned automatically. The sample concentration during Sample Dilution should be set to 2 to 4 %. Under no circumstances it should be higher than 15%. After the "Feeding the sample" sequence is concluded and the necessary sample quantity transported, the Measurement" is started.

4.4.1.1 Technical Specifications of Dust Exhaust The following values are only an index for the used dust exhaust

Power: max. 1100 Watt

Air capacity: 40 l/s

Vacuum: 23 kPa

Sucktion Power: 270 Watt

Filter Area: 2400 cm²

Container Capacity: 9,0l

4.4.2 Cleaning of Dry Dispersing Unit After the measurement is done the program stops feeding. Feeder, Dust exhaust and air are switched off. A cleaning of the dispersing unit is not necessary. Every time before background measurement a short cleaning cycle is done internally.


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4.5 Measuring with the NanoTec and MicroTec device for wet dispersing or combination devices The window for measurement, background measurement and addition of the sample is always the same; only different index cards are enabled depending upon the measuring step. You cannot manually close this window, it closes automatically after the measurement. In this window, you can also obtain information about the system status by selecting different index cards or display the measured values as numerical values instead of graphics.

Attention:

Do NOT select the menu item “Beam adjustment” during the measurement. This will result in an error. Besides, minimum possible action must be started in the programme during a measuring process. A measuring process can always be cancelled with “Stop measurement”.

Measurements with the NanoTec and MicroTec wet dispersing unit take place on the basis of the same pattern as for the COMPACT, Comfort and Economy versions. Define your measurement process with the corresponding scope and press Start for starting the process of measurement. Select the number of scans to determine the number of measured values. The pump speed can be varied between 0 and 100%. If you select ultrasound, this features will be enabled for all points during the measurement. You can restrict this selection by selecting ultrasound before, during and after the addition of the sample. In this case, you can also specify a stop time for the ultrasonic treatment. You can also select that the system should be automatically cleaned after or before the measuring process. The minimum beam absorption indicates the value at which the item “Addition of sample” is left and which starts the measurement automatically. Select the number of scans to determine the number of single measurements you want to combine to form one complete measurement. 100 scans correspond to approximately 10 seconds of measurement time.

Attention:

Select the appropriate measurement option in the upper area (e.g. “Select wet dispersing” for making wet measurements).

After you press “Start measurement”, the wet measuring cell is turned in the beam path of the laser. The corresponding filter discs for releasing the forward and backward laser are released. If the measuring cell distance is different than before during the current measuring process, the measuring cell is shifted to the correct position and the measuring process started with the set parameters.


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4.5.1 Background measurement To avoid the influence of the measuring fluid during the process of measurement in suspension or the influence of dust in the measuring room while measuring solid materials, a background measurement is essential before every measuring process, particularly if the measuring range has changed. Possible impurities in previous measurements are also recorded and their influence on the current result eliminated. The following preparations must be made for the background measurement: 1. The adjustment of the laser beam is regulated, 2. the measuring range is set, 3. the measuring circle is filled with clean measuring fluid and

the pump, stirrer and ultrasound are set to medium power.

Click on the symbol for background measurement or press Start measurement to open the window.

The window then opens with a symbolic presentation of the intensities of the 80 channels. The bars shown in brown correspond to the horizontal channels of the detector, the red the vertical. The 5 detector channels for wide angle scattering are displayed immediately after this. To the right of these channels are the 16 channels for determining the elongation ratio and 5 position channels required for automatic beam adjustment. If the picture fades out after a few seconds, the measured values of every measuring channel are saved in the computer. The values for background measurement are taken as a basis while calculating all subsequent measurements and are also retained when the device is switched off – the values of the “previous” measurement process are overwritten only after a new background measurement.

Attention: If you change the measuring range or replace the measuring cell or carry out any other activities on the measuring cell, you must execute a new background measurement process.

The measurement process can be cancelled with “Stop measurement” at any point of time. The programme then goes back to the main menu and the saved values of the previous background measurement process are retained. This interruption is essential e.g. if you select the background measurement accidentally, i.e. you do not wish to overwrite the measured values.


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4.5.1.1 Background measurement during multiple measurement

If you have selected multiple measurement, a background measurement too is carried out on each item of the measuring cell. To this effect, switch on the pump and ultrasonic bath as well. The background measurement process runs automatically.

4.5.2 Addition of the measurement sample The following preparations must be made for the test: 1. the adjustment of the laser beam is regulated, 2. the measuring range is set, filled with clean measuring fluid, 3. the pump and ultrasound are set to medium power, 4. a background measurement has been carried out

Click on the symbol for addition of the measurement sample or press Start measurement to open the window. In the Addition of sample window you will see a size distribution of your sample after a slight addition of the sample. This is not yet accurate, but it gives you an idea of the actual size distribution. Most important of all: You can check whether you measuring range has been set correctly, i.e. the required width is covered. To the right in the Addition of sample window near the window that displays the temporary particle size distribution, you will see three remark fields. In the topmost field is the value of the central beam of the forward laser during background measurement and in the next field is the current value for the addition of the sample. This value reduces as you add more of the sample. The beam absorption is calculated on the basis of these two values. Below this is the remark window, which shows whether all values of the detectors lie in the permissible range. If any detector channel reaches the saturation limit, this field will give you a new tip “Saturation”. Do not add any more sample, otherwise the measurement will be incorrect. If you make further addition, observe the display in the colour bars in the lower window: It will show you when to stop the addition: You must strive for a value between 7 and 20 %.


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Attention: avoid a saturation of the detector channels by adding too much sample.

The “Addition of sample” window includes a dynamic check of the dispersing action. The window will close automatically if the defined value is reached and the sample does not differ by more than +/- 1% from the achieved value. You can also leave the window by pressing “Cancel beam adjustment”. This might be necessary if a stable beam adjustment status is not set (e.g. non-homogenous samples or samples with high rough portion etc.).

4.5.3 Measuring the particle size distribution Make sure that the following preparations have been made for a particle size distribution: 1. the adjustment of the laser beam is regulated, 2. the parameters for measurement are fixed, 3. your comments for the measurement have been entered, 4. the measuring range is set, filled with clean measuring fluid, 5. the pump and ultrasound are set to medium power, 6. a background measurement has been carried out and 7. your sample has been added

In the Measurement window, you will see the intensities of individual measurement channels - as you already know from the background measurement, the intensities are higher since the particles generate scattered light in their sample.

Single measurement: The measuring cell remains in the same position where you have executed the background measurement. The measured values are immediately accepted, processed and a particle size distribution calculated. You can get the result immediately.

Multiple measurement: During multiple measurement, the measuring cell is taken to at least two different positions and the measurement of its sample executed there – as for background measurement. During background measurement, the multiple measurement begins on the right side of the measuring unit – i.e. in the “precise” range; also while measuring the sample, the multiple measurement begins on the right side of the measuring unit – i.e. in the “precise” range. Before the actual process of measurement begins, a short pause may be taken, during which the measuring cell is moved to the corresponding position.


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4.6 Measuring with the NanoTec and MicroTec device for dry dispersing or combination devices Select the number of scans, background measurement and measurement as for the process of measurement with the wet dispersing unit.

Select “Select dry dispersing". The measuring cell for dry measurement is then automatically turned in in the beam path. If the wet measuring cell was previously turned in, it is turned out. This can last for 10 seconds.

Enter a minimum of 1% and maximum of 8% for minimum beam absorption. Standard values are minimum 2% and maximum 4%. The device automatically sets the values for the flow rate and flow quantity such that the standard values of beam absorption are maintained.

4.6.1 Sample feed with dry dispersing unit Particle size distributions from ca. 0.1 to ca. 1000 µm (600 µm) can be measured with the solid matter dispersing unit along with the measuring units of the NanoTec and MicroTec version. For this, the dispersing nozzle and suction device for dispersing of solid matter is installed in the measuring unit. During the measurement, the sample is filled in the funnel tube of the metering channel and transported through the vibration channel of the dispersing unit. An air current catches the sample and transports it to the dispersing nozzle (two-component nozzle) in the measuring unit, where it disperses once again with the help of adjustable supplementary air (nozzle air) and is blown in the laser beam with increased speed. A suction device is installed opposite the dispersing nozzle the measured sample is sucked out from the measuring unit with the suction pipe. The vacuum cleaner is switched on and off during the measuring process. Thus, it is ensured that the samples transported to the measuring unit are also sucked out.

Before switching on/opening the conveying channel, the suction tube of the vacuum cleaner must be inserted in the side wall of the measuring unit, the connecting pipe of the vacuum cleaner in the socket of the control box (s. Operating instructions for NanoTec and MicroTec) and the vacuum cleaner must be switched on.

If you forget this, the measuring cell glasses will become dirty and your sample will be blown around in the room.

As a preparation for the measurement process, the compressed air (and/or gas) is set to a value of 3 to maximum 4 bar with the reducing valve on the rear side of the dispersing unit (manometer).

For sensitive samples, the pressure must be reduced to 1 bar.


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It suffices to inspect the values for air pressure before the measurement (3-4 bar), provided that the pressure in the air pipe (min. 5 bar, 125 l/min) does not change significantly during the operation. A pressure reduction device is integrated for stabilisation, which keeps the secondary pressure constant when the primary pressure is changing. For the measurement, the sample is filled in a funnel. When the sample is added, the metering channel is on and is automatically regulated. The measurement process becomes smoother as the sample is distributed more uniformly on the channel, i.e. the more uniformly it flows out of the funnel. During the background measurement, the dispersing nozzle is automatically taken to the selected position. The programme sequence Addition of sample starts automatically. The beam absorption displayed on the screen should not exceed 15 % in any case. Experience shows that good results are obtained during beam absorption between 2 and 5%. Attention: A very high beam absorption causes faster dirtying of the measuring cell glasses. The process of measurement is started after the Addition of sample concludes and the required sample quantity is transported.

You cannot interfere during the process of measurement. The metering channel is automatically controlled in the conveying rate so that the pre-defined minimum and maximum beam absorption values are maintained. You can cancel the current measurement process by pressing “Stop measurement”.

Technical data of the vacuum cleaner for the dry dispersing unit The following specifications are approximate values and may differ as per the vacuum cleaner used. Power consumption: max. 1100 Watt Air supply: 40 l/s Vacuum: 23kPa Cleaning power: 270 W Filtering surface: 2400 cm² Capacity of dust bag: 9.0l

4.6.2 Cleaning the solid matter dispersing unit After the actual process of measurement is concluded, the programme automatically stops transporting the new solid matter: Metering channel, vacuum cleaner and pressure gas are switched off. An extra cleaning of the solid matter dispersing unit is not necessary. A cleaning sequence is carried out automatically every time before a background measurement.


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4.7 Cancel Measurement You can cancel the programmed measuring cycle at all times using the Stop Measurement button. This button also interrupts Auto-Alignment.

4.8 Download Eeprom (only COMPACT) If measurements are executed without having a computer connected up to 10 consecutive measurement data are stored to an eraseable Eprom memory inside the measuring unit. After reconnecting the measuring unit to a computer you can download these stored measurements by clicking Download EEprom. The last measurement data will be downloaded and the particle size distribution will be calculated from these data. The last measurement will be removed from memory inside the measuring unit Eeprom (This option is not available for all units, please ask for information).

4.9 Load Settings Last Measurement The actual measurement settings for the measuring- and dispersing unit are stored to the result file. After loading a stored result file you can set the system to this measurement settings by clicking thwe command button Load Settings Last Measurement. Settings like „Measuring Range“, „Stirrer Speed“ or „Feed Rate“ will be actualized.


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5 Main Menu File

5.1 Save Actual Result In the Save Actual Result dialog box you can save your actual measurement result files. Select a drive and a directory and assign a name with up to 256 characters. Ok copies the file \FRITSCH\OUTPUT.DAT to the desired designation and desired name, Cancel closes the dialog box without saving the result file. Unless you specify otherwise, a-22 program automatically adds the default filename extension .DAT. If you type the name of an existing result file, a-22 displays a message warning you that you'll be overwriting an existing file. Choose Ok to replace the existing file, Cancel to close the dialog box without saving the file. For more help see the Windows help system. This is a Windows dialog box. You can activate automatic saving of results directly after measurement if you select the check box Save Result after Measurement in the windows Setup, Measurement Parameters. The 256 characters provided by your standard Windows 32Bit operating system are often not enough to unambiguously characterize files. The program can help you to manage your result files by means of a database. Please select the option Write Values to Database in the window Measurement Parameters. A database file will be initialized and after closing the Save Actual Result dialog box a new window opens where you can enter comments and supplementary information which will be stored in a database. Enter several pieces of supplementary information here - for your own benefit. With the option File, Database you can use the information entered here for selections and searches. For each stored result the values d1, d2, d3, ...d10....d50...d90... also are stored to the database. Store to Database writes the values to the database, Save Database saves the complete database. To physically store your entries you MUST choose Save Database before closing this window.


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5.2 Load comparison curves

In the Load comparison curves window, Analysette 22 can load up to 100 different result curves in the memory. You can compare your current measurement result with the loaded curves (e.g. min and max limits for a fresh measurement result). The comparison curves will be shown additionally to your result curves whenever you select Results and Graphics. In this window, you can also determine the behaviour of the menu items “Control card D values”, “Printing of selected results” and “Determination of average value of the results”. These procedures also access the list defined here. A filter is inserted below the file window, where you can select certain files. E.g. on entering *glass405*, only those measurements will be displayed, which contain this chain of symbols.


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Options in the dialogue field “Load comparison curves”

Option Description

Drive Select a drive from the list. You can filter out removables, ram drives, network drives, etc.

Directory Select a directory from the list. Select the drive or directory where the result file is stored if different from your current path. (The current path is displayed above this box.)

Selected Files Double Click holds the selected files in the Listbox.

OK Loads all selected files and holds them in memory.

Cancel Closes the dialog box without saving the result file.

Hold List Holds the selected files in the Listbox.

Select All Selects all files in the actual directory

Deselect All Deselects all files in the actual directory

Delete Item Deletes one entry in the hold listbox

Delete List Deletes all entries in the hold listbox

5.3 Load Old Result In the dialogue field File, Load previous result, you can load the saved results. You select the drive and the directory. A click in the file-list-box sends your desired file to the input field. Your next click on Ok brings the selected file to the current result memory, where you can treat it as if it had just been measured. If the path changed during this process, it is stored to memory and will be the actual result path for further actions. Ok opens the selected file, Cancel closes the dialog box without opening a file. For more help see the Windows help system. This is a Windows dialog box.


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5.4 Export Results

In the File, Export Results window you can transform and export your results into Lotus, MS Chart or MS Excel format by selecting the appropriate option button. First choose the command button Select Files. The opening window is the Load Comparisons window. Define the files you want to transform. Afterwards you select the output path and then, after one click on Start Transformation, the program recalculates the selected files so that their format is understood by the program Lotus or MS Chart. Your files are listed in the selected directory under the same name - during the transformation the suffix has been changed to "WKS" in case of Lotus, "CHA" in case of MS Chart or "XLS“ for MS Excel.

5.5 Database In the Database window you will find assistance while searching and selecting your stored result files. Following your click a database is opened. The data is read from the database via a so called DataGrid custom control. This is a bound editable grid that can be used in an application to display and edit data. You have a fully functional program that allows the user to view, edit, add and delete rows in a database.

Select one row in the database, which contains information about the stored result file you want to load. Ok opens the selected file, Cancel closes the window without opening a file.


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Since the DataGrid uses virtual data management techniques, meaning it can handle any amount of data without using up all of Windows memory, you can use it to handle large lists of data. The DataGrid does not manage or store the data internally. When the DataGrid is ready to display a particular row, it simply triggers an event in which you return the data to be displayed. Conversely, when the user modifies data in a particular row and then moves off the row to commit the update, the DataGrid triggers a CellUpdated event which the program can process to update the underlying data source.

Selecting Rows To select a row, click on the row label at the left of the row. To select a range of rows, click on the first row in the range, then hold down the shift key and click on the last row in the range.If the record set is non editable, you can select rows by clicking on the row.

Selecting Columns To select a column, click on the column heading. To select a range of columns, click on the first column heading in the range, then hold down the shift key and click on the last column heading in the range.

To Add A Row: To add a row, position the cursor on the last row of the grid. (The icon will appear at the left of the last row.) Enter the new data directly into this row. When you leave the row, a new row containing the data just entered will automatically be added to the table.

To Delete Rows Rows can be deleted by selecting the entire row or range of rows, then pressing the delete key. The DataGrid will prompt you with a warning which can be overridden in the DeleteBegin event procedure.

Changing Row Data To change data in a row, position the cursor on the cell you want to change. Start typing in the new value for the cell. The icon on the left will change to to indicate a change is being made. When you leave the row, the change will be made to the table.

Using the Arrow Keys To Edit a Cell Value If you need change a value in the cell without retyping the entire value, position the cursor in the cell and press F2. You will then be able to move around the cell with the arrow keys.

Canceling a Change in a Cell To cancel a change to a cell, press the Escape key and the original value will be placed in the cell.

Canceling a Change in an Entire Row To cancel a change of an entire, press the Escape key twice and the original values will be placed in the cells of the row.


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5.5.1 Data Control description

First Record Jumps to the first record in the database. This button is displayed/hidden by the ShowFirstLastButtons property.

Previous Page Jumps to the previous page in the database. A page is determined by the setting of PageValue. This button is displayed/hidden by the ShowPageButtons property.

Previous Record Jumps to the previous record in the database. This button is displayed/hidden by the ShowPrevNextButtons property.

Add Record Adds a new record to the end of the database. This button is displayed/hidden by the ShowAddButton property.

Cancel Add Cancels the adding of a new record to the database. This button is displayed/hidden by the ShowCancelButton property.

Delete Record Deletes a record from the database. This button is displayed/hidden by the ShowDeleteButton property.

Update Record Updates the selected record in the database. This button is displayed/hidden by the ShowUpdateButton property.

Add Bookmark Adds a bookmark for the current record. This button is displayed/hidden by the ShowBookmarksButton property.

Clear All Bookmarks Clears all stored bookmarks. This button is displayed/hidden by the ShowBookmarksButton property.

Current Record When the DataField property is set, the active record is displayed. When DataField is left blank, the Caption is displayed.

Goto Bookmark Presents a list of all stored bookmarks (up to a user-definable limit of 100). This button is displayed/hidden by the ShowBookmarksButton property.

Find Record Invokes the Find dialog, allowing the user to search the database.

Find Previous RecordSearches backwards in the database for the next occurrence of data


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specified in the Find dialog.

Find Next Record Searches forwards in the database for the next occurrence of data specified in the Find dialog.

Next Record Jumps to the next record in the database. This button is displayed/hidden by the ShowPrevNextButtons property.

Next Page Jumps to the next page in the database. A page is determined by the setting of PageValue. This button is displayed/hidden by the ShowPageButtons property.

Last Record Jumps to the last record in the database. This button is displayed/hidden by the ShowFirstLastButtons property.

Finding information in a database field is a snap with the Enhanced Data Control.

5.5.2 Find Dialog

To activate the Find dialog, click the Find Record button. You can use the Find Previous Record and Find Next Record buttons to continue searching once you’ve found a match. The search window is always available in English. Find Specify the data to search for. A list of recent

searches is available by clicking the button. Direction Specifies the direction in which to search.

Selecting Down will search from the current point to the end of the database. Selecting Up will search from the current point to the start of the database.


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Less Than Match only if the text entered in the Find dialog is less than the value in the database. Examples of this are 1 < 2 and APPLE < BEAR

Less than or equal Match only if the text entered in the Find dialog is less than or equal the value in the database. Examples of this are 2 <= 2 and APPLE <= BEAR

Equal Match only if the text entered in the Find dialog equals the value in the database. Examples of this are 5 = 5 and DOG = DOG

Greater than or equal Match only if the text entered in the Find dialog equals or exceeds the value in the database. Examples of this are 7 >= 2 and DOT >= DOS

Greater than Match only if the text entered in the Find dialog exceeds the value in the database. Examples of this are 10 > 9 and TREE > BARK.

Partial Match Match only if a portion of the string specified in the Find dialog matches a portion in the database. An example of this is specifying "Eng" in the Find dialog and returning "Engine" and "England". This works for strings only.

Soundex Match only if the string sounds like one in the database. An example of this is specifying "Skool" and returning "School". This works for strings only.

Note: The user can press the ESC key during an extensive search to exit.

5.6 Page Layout In the Page Layout window you can choose the style for printout of your results. Here you define positions, graphics sizes and font styles for the selected options. There are three printout pages available where you can select different options with different layouts. If you watch the window, handling is very simple. Everything you activate on the left-hand side with a small cross (click on the symbol) is inserted into the middle field. After the elements appear in the middle field, you can move them within the field with the left-hand mouse key depressed and let it "drop" wherever you wish. The size of the graphics is also easy to change: place the top left-hand corner of the graphics at its correct location and click on Set Graph Size to open an input field on the right-hand side - change the size by clicking with the mouse. You can also include several pages for your layout in planning. You jump back and forth between the pages with one click on Page Up and Page Down. If you need a number of different layouts, you can store them and access them again as needed.


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• Left: all of the output options that you can print out • Middle: printout sheet which is the symbolic representation of

the paper format currently set on your system printer. • Right: Select the fonts you want the individual output options

to be printed in with. • Bottom right: Specify whether you also want to print the date

line and a statistics line while printing the measurement parameters. The date line contains information on the device and user. The statistics line mainly contains the specific surface.

• Bottom left: Here, you can specify whether you also want to print out the name of recently loaded result file. If you do not load any file, but print the current measurement, this will be called “OUTPUT.DAT”.If you have loaded comparison curves, you can also select whether you want to print the comments for measuring the comparison curves.


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Please follow the steps for first using this option. 1. Deselect all of the crosses in the check boxes in the left-hand

frame by clicking on them with the mouse. The boxes must be empty. After this your printout sheet also should be empty.

2. Please activate the check box “User Message” (you have to see a cross in the check box) and then press the right-hand mouse. A pop-up menu will open: select the option “Remove graphics” in it. Any inserted user graphics will be removed.

3. In the right-hand frame, select the option Main Title (always preselected when the window is opened) and then Fonts. You will see a Windows font dialogue box in which a font (font name) and options (e.g. underlined, italics, etc.) are specified. Please choose, for example, how you would like the main title be printed.

It is imperative that you take this step for all of the options (user title, analysis report, etc.) because the program finds an error during printout if no font available on the system is selected for a single output option. The situation may arise on a few systems that no font name at all is prespecified in this dialogue box after the installation. Please enter one.

4. Select the option Main Title in the left-hand frame. The main title will appear in the printer window. By clicking and dragging with the mouse, place the title anywhere on the printer sheet.

5. Select Tabular Data (cross in check box). Pressing the right-hand mouse button reopens a pop-up menu in which you select complete or abbreviated printout. This output option can also be placed anywhere by clicking and dragging with the mouse.

6. To display graphics, select Combination for example. Graphics will appear in the print window. What matters here is not so much the appearance of the graphics as their size and position when printed out.

7. Click on the graphics with the mouse and a command key Graphics Size will appear in the left-hand frame. If you select this command button, you can set the X- and Y-dimension of the graphics. It is imperative that you press the End key when you have set the size of the graphics. Naturally your graphics can also be placed anywhere by clicking and dragging with the mouse.

8. If you are satisfied with the layout in the print window, select the file card Preview next. This card shows you a more exact preview of the printout. You can store the layout for subsequent reuse. Select Store or Load to load a layout which has already been stored.


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The print window provides you with a rough overview of the position and appearance of the selected options when they are printed out. Depending on the resolution of your screen and printer, the correspondence between the preview and the printout may be good or not so good. It may be necessary to print out and correct repeatedly to achieve the desired result. While the second card file card Preview is better than the print window, it cannot work wonders! Before you select the check box for Fixed values you have to make certain that the appropriate fixed value files have been selected in Setup, Calculation Parameters. You can create these files anywhere and store them to calculate the interpolation values into fixed grain sizes and/or fixed percentages.

Example: You are particularly interested in printing out the d10, d37, d50, d63 and d90 value. In the window Calculation Parameters select the option Fixed percentages (undersize). The first time it is selected, the program opens a dialogue window to load a file. Load a file with the extension FPV (Fixed Percentage Volumes). When you load the file VIRGIN.FPV, you obtain an empty table. In the right-hand column enter the following values: 10, 37, 50, 63 and 90. Store the new file and end the program part with OK. You will then see that the file just stored is standing in the frame above Information. The program now searches for the corresponding grain sizes in the undersize cumulative curves while printing out the specified percentages. This also functions for default grain sizes. You load and store FPS (Fixed Particle Sizes). As above, during the printout the percentages associated with the default grain sizes are output from the passed cumulative curve. When you use fixed-value files, you always have to enter more than 3 values, otherwise the program will not print out correctly.


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When you select the option Tabular data, you generally do not receive a preview in the print window. The table is always output on a separate page at the end of printout. Consequently, you should always select the tabular printout on the first page. After you click on it with the right-hand mouse, select an abbreviated or complete printout. To enter a user title or insert user graphics (e.g. company logo) to your layout, select User Title and press the right-hand mouse. In the pop-up menu select the text for the Title or user graphics.

5.7 Setup Printer This is a Windows dialog Box, see Windows help.

5.8 Printout Selected Results After selecting this menu item, all the results selected in “Load comparison curves” are sent to the printer.

5.9 Terminating the Program You can close the program at any time by simultaneously pressing the "Ctrl" key and the function key "F4". The next possibility - also customary in Windows - is to click the mouse twice on the top left corner. Finally, you can click once on the bottom line in the open pulldown menu. You will not be asked whether you really want to exit the program but the program closes directly. This is perhaps the safest procedure to end the program.


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6 Main Menu Setup COMFORT, COMPACT and ECONOMY

6.1 Measurement Parameters In the Setup, Measurement Parameters window you can set parameters needed for measurement and result storage. The comments and measurement number entered here are linked to the following measurement. If you do not change the entries they will remain for all following measurements. If you select File, Page Layout and activate the check-box Measurement comment the entries will be printed out, provided that the printout-font is defined (see File, Page Layout). If you select Write fixed values to ASCII File, Date, Time and the measurement comment is written to a sequential ASCII file called ASCII.DAT located in the FRITSCH directory. Following this up to 100 percentage volume figures and the corresponding particle sizes are stored separated by a quotation marks. You can load this with a database like Superbase or with Excel if you make use of the appropriate import fuctions. Selecting Write Values to Database opens a database window each time you store an actual measuring result. In the database window you can enter additional information to manage your result handling seen from the aspect of ISO 9000. The percentage volume figures together with the belonging particle sizes also are stored in this database in one percent steps. Selecting Printout after Measurement prints out the actual result with a layout defined in Page Layout. Selecting Save Result after Measurement stores your actual measurement directly after executing a measurement. After selecting the card User Parameters you can enter user specific parameters like user name or unit serial number. This information will be printed out if you select printout of Measurement comment in the File, Page Layout window. More parameters like First Name or Keyword are parameters, which will be stored to the Database for administration of your result files. If you set the Keyword 1 to e.g. Batch Test XR40-E then every file stored with activated Write Values to Database can be searched in the database very easy by searching keyword 1 equal to „Batch Test XR40-E“.


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6.2 Calculation Parameters In the Calculation Parameters windows you can set parameters for the calculation of the results.

6.2.1 Calculation of the interpolation values You can select fixed particle sizes or fixed volume percentages from undersize or oversize cumulative distribution curves to calculate the interpolation values from your results.

6.2.2 Selecting preselected tabular values The individual interpolation values themselves can be viewed by pressing the Information button. Afterwards a window opens, where you can arrange your fixed values in rows of up to 100 values or you can select a suitable one for the current calculation. The program automatically presents you rows of only fixed particle sizes or fixed percentages, depending on your selection of interpolation values. Please enter values from fine to coarse. Self-evidently you can also store newly created fixed values to datafiles.

6.2.3 Calculation model It is possible for a calculation model to define, i.e. determine, whether the particle size distribution is calculated on the basis of the Model (Standard) or whether an RRSB distribution is to serve as a basis of calculation for monomodal distribution or polydisperse distribution with particles strongly deviating from the shape of the ball. The decisions made here are applied to the measurements that follow, even if the programme has been ended in the meanwhile and the computer shut down.

6.2.3.1 RRSB distribution If you don’t want the standard Modell independent calculation, you can choose another kind of calculation. The representation of a particle size distribution in the RRSB grid is preferred in certain applications. Additional data can be ascertained from the representation. The mass distribution cumulative curve ("undersize" D as a function of particle equivalent diameter) is plotted in the RRSB grid (DIN 66 145; named after the authors Rosin, Ramler, Sperling and Bennett). If the particle size distribution function follows the RRSB function, the distribution cumulative curve appears as a straight line in this grid. With the program of the laser particle sizer "analysette 22", calculation of the particle size distribution to RRSB can be selected in the main program "Init window during the calculation of the particle size distribution. Thereafter, it is assumed that the distribution to be measured follows the line function in the RRSB grid.


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Using the result curve which is then calculated and presented it is then possible, for example, to determine the fineness parameter "d" from the abscissa section at D=0.632 and the gradient of the RRSB line. After a parallel move of the line to the pole the second fineness parameter "n" is found at the inner boundary scale. Further, the numeric value for the nondimensional surface parameter is found on the outer boundary scale. The volume-related surface "Sv" can be determined by dividing the two. If "d'" is inserted in cm, the result is "Sv" in cm2/cm³ or in cm²/g. The mass-related surface is determined, wherein the volume-related surface is divided by the specific density. Parameter D and n are displayed in the graphic.

6.2.3.2 Monomodal distribution Monomodal distribution can also be selected in case of a monomodal sample. The iteration goes to a smaller residuum with a large number of iterations. The disadvantage here is that this type of calculation cannot be used for normal, broad samples, as the iteration process can become unstable.

6.2.3.3 Polydisperse Form Correction If you want to measure particles that strongly deviate from the shape of the ball, you can select "Polydisperse Form Correction“. This calculation considers the fact that e.g. acicular particles scatter more effectively in the desired direction than spherical particles and try to balance the latter. Use this model very carefully, as it affects the results considerably, in some cases.

6.2.4 User grain size Use this procedure, if you want to automatically convert your result to a particular grain size category after the measurement. "Select User grain size“ takes you to a dialog field, in which you can select a file with automatically set User grain sizes. After the measurement, the grain categories given by analysette 22 are automatically converted to the automatically set grain categories and are saved in the measurement file. Attention: Your result is now submitted as a file with new grain categories. You can deactivate this function by selecting the "Deactivate“ command button.


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6.3 Mie- / Fraunhofer Parameters The a-22 program utilizes the full Lorenz-Mie theory for the calculation of particle size distributions. Depending on the optical constants the matrices are calculated in real time. Once calculated, these matrices are stored to memory and can be reused later on.

6.3.1 Reverse Fourier Optics Laser-Light-Scattering Instruments utilize the principle of scattering of electromagnetic waves for the determination of particle size distributions. The construction of such kind of instruments is basically very simple.

Particles in a parallel laser beam deflect the light to fixed spatial angles, which depend on the particle diameter. A so called Fourier-Lens „focus“ the scattered light to a detector built up of annular elements, which is placed in the focal plane of the lens. Not scattered light is focused onto the optical axes. Each individual particle size is assigned to a different ring-radius r. The measured light energy distribution of the detector rings is measured and from this the particle size distribution can be calculated. The word „focal plane“ is equivalent to the word „transformation plane“. The intensity distribution in the transformation plane is equivalent to the two dimensional Fourier transformation of the intensity distributon in front of the lens. Therefore the lens is called „Fourier-Transformation Lens“.


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Fritsch uses his patented optical design, which is known as "reverse fourier optics". The Intensity pattern in the focal plane of the lens can be also achieved by placing the measuring cell in a convergent laser beam. The resulting field is the Fourier-transformation of the screening function and is identical to the field achieved with a conventional setup. The distance measuring cell to detector replaces the focal distance of the conventional setups. The field in the transformation plane is the picture of the spatial frequencies of the field before the lens. Small particles produce big spatial frequencies and large particles small ones. The connection between coordinates in the Fourier plane and spatial frequencies is

f pd

f qdx y=

⋅=

⋅λ λ

The Fourier Transformation now is under control of the user. Enlarging d increases the spatial size of the transformation and small frequencies (large particles) can be examined. This works until the measuring cell is placed right in front of the lens. Reducing d diminshes the spatial size of the transformation and large frequencies (small particles) can be found. Again this works until the measuring cell is placed right in front of the detector.

6.3.2 Fraunhofer Diffraction

When light of the same wavelength (monochromatic light) strikes the boundary edge of two media with a different refractive index, it is deflected (diffracted). Due to interferences which arise in this process, diffraction patterns are produced.

For example, if a spherical particle is illuminated by parallel, monochromatic light, a diffraction pattern referred to as the "Fraunhofer diffraction pattern" after the person who discovered it is produced in the focal plane of a lens in the beam of light behind the particle due to interference of the light waves diffracted at the edge. The diffraction pattern of a round disc or a spherical particle which is visible in the focal plane consists of alternately light and dark concentric rings.


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The equation describing this process is

( )I P U P IJ k a uk a u

( ) ( )= =⋅ ⋅ ⋅

⋅ ⋅

20

12 2

with u = arc tan (r / f) and k = 2π / λ. The diameter of the particle can be calculated from the radius Ro of the rings, the wavelength of the light and the focal length f of the imaging lens. The diameter is inversely proportional to the radius of the first circle of light produced due to diffraction.

0

84.1Rfd λ⋅⋅

=

This simple equation can be applied only if particles of equal size are moved into the beam and their size is calculated with the aid of the diffraction pattern. Even when two particles of different size are involved, the diffraction images create mutual interference and complicate the analysis. In this case two equations would be necessary to ascertain the particle sizes. If you also wished to determine the mutual volume ratio of both size classes, you would have to ascertain the angledependent intensity of the diffracted light as well. If this were inserted into the two equations, each would receive a second element.

Manual evaluation becomes impossible when mixtures of many different particle size classes are involved. The 2 equations grow into a system of equations. The number of equations and the number of elements contained in each equation is equal to the number of size classes. If they are written one below the other, an arrangement in columns and rows results. For determination of the particle sizes and their mutual volumetric ratios, it is necessary to compute the elements in this arrangement (matrix).


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6.3.3 Mie Scattering 6.3.3.1 Description The relationship which has been simplified here and is still clear becomes somewhat more complicated as a result of the fact that, strictly speaking, the above theory named after Fraunhofer is valid only in a range in which the wavelength of the monochromatic light is shorter than the particles to be measured. If the ratio of particle diameter to wavelength approaches the value 1 or actually drops lower, the structure of the diffraction pattern is influenced by material constants (absorption coefficients and refractive indices) of the sample and the surrounding medium. In the case of the heliumneon laser with a wavelength of 0.6328 µm, for evaluation of a measurement in absolute values, these parameters must be taken into account for particles in the 1 µm range. In this case, a size distribution should no longer be computed in accordance with Fraunhofer theory; the socalled Mie theory should be used.

The exact Mie theory is used in the "analysette 22" program if, after selection of an input window, the refractive index and absorption coefficient are entered, that is to say when the values are other than "0". Absorption coefficient and refractive index of sample and suspension liquid affect the elements of the matrix used to compute a particle size distribution. A separate matrix must be computed for every conceivable combination of these 3 material-determined quantities and the cell distance. The program computes this matrix during computation of the particle size distribution without noticeably increasing the measurement time. The short computing time makes it possible to compute a particle size distribution whenever this is appropriate from a physical pint of view, without the computing time having to be taken into consideration.


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Enter the material constants for the Mie Matrix calculation which are also displayed for use as a check. In addition, you are reminded of the current measuring range and the position of the measuring cell. Input of the optical values causes the program to turn to the Mie theory. The matrix covers all combinations of refractive index and absorption coefficient occurring in practice. The program does not require significantly longer than 1 minute even for this. The matrix computed in this manner is stored, for subsequent computations, in the memory on the hard disc so that future measurements and computations with these materials take place with the previously computed matrix in the customary short time. In the event of a subsequent measurement, the program "recognises", on the basis of these constants, an appropriate matrix stored on the computer's hard disc. These material-dependent parameters should be known to an accuracy of 2 decimal places. They can be entered after the pertinent routine is called up. Following the aforementioned scan of the memory, the matrix is either computed or read in. The command switch solid database or for liquid database opens the databases and permits the automatic entry of your optical constants. These databases permit the automatic entry of index of refraction and coefficient of absorption of your sample and refraction coefficient of liquid. The solids are stored in alphabetical order and you can read in their index of refraction and coefficient of absorption. After one click on the pushbutton New you can enter a new solid or liquid. Enter all relevant data in the corresponding input fields. Thereafter, a click on the pushbutton Update transfers your input into the database and alphabetizes it. If you wish to delete data from the database, click on the pushbutton Delete after selecting a solid or liquid.


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6.3.3.2 Mie Theory Lorenz - Mie theory describes the radiation in and outside of a homgeneous particle in a homogeneous, nonabsorbing medium for all spatial directions. The particles may be transparent or fully absorbing. The calculation takes into consideration the optical characteristics of the particles by means of the refractive index. It is defined as complex number

N = n - ik

with n as refractive index and k as absorption coefficient.

If a particle is illuminated by a plane wave expanding in z-direction the scattered wave for the far field can be described as two electromagnetic field components, which are polarized perpendicular to each other.

EE

SS

ei k R

EE

ll S

S

i k R i k zll i

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⊥

=

⋅

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1

2

00( )

( )θ

θ

The scattered electromagnetic field therefore has the same asymptotic form as the Fraunhofer theory. The components of the electromagnetic field perpendicular and parallel to the scattering plane are Ell and E⊥. The distance to the particle is R and θ is the scattering angle. The amplitude funktions are

{ }S nn n

g a bn

n n n n n11

2 11

( )( )

( (cos ) (cos )θ π θ τ θ=++

⋅ +=

∞

∑

and

{ }S nn n

g b an n n n nn

21

2 11

( )( )

(cos ) (cos )θ π θ τ θ=++

⋅ +=

∞

∑


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πn and τn are the classic Legendre functions of Lorenz-Mie theory, an and bn the Mie scattering coefficients. They depend from the optical characteristics and the size of the particles. The coefficients gn are defined by the beam profile of the used laser. The intensity distribution in the focal plane is defined as

IR

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and

IR

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4sin

6.3.3.3 Complex Refractive Index By solving the Maxwell equations for transmission of electromagnetic waves through materials one gets the complex refractive index N of the material

( ) ( )λλ kinN ⋅−=

with the wavelength dependent real part n(λ) and the wavelength dependent imaginary part k(λ). From this the most important material characteristics can be derived.

The real part of the complex refractive index is the refractive index known from geometrical optics. It defines the change of expansion direction of radiation passing from one to another material of different optical density. Normally n marks the passage from air to material.

From the imaginary part of the complex refractive index the absorption coefficient of the material follows:

( ) ( )λ

λπλβ k⋅⋅=

4

For materials with finite transmission the absorption is no longer only a surface feature. The incoming radiation flux will be reflected to a part ρ directly at the surface. The rest will penetrate the material and will be absorbed during his way through the material. It can be shown experimentally that the absorbed radiation per layer dΦ is proportional to the incoming radiation Φ and the layer thickness:

dzd ⋅Φ⋅−=Φ β

The proportional constant β ist the absorption coefficient of the material. It has the unit of a reciprocal length. The reciprocal value ξ=β-1 is called radiation penetration depth. The absorption coefficient is wave and temperatur dependent und must be determined experimentally.


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The solution of the above mentioned differential equation is the decay curve of the radiation flux

( ) ( )

−⋅Φ=−⋅Φ=Φξ

β zzz expexp 00

The radiation flux entering the material at z=0 is Φ0. For a layer with thickness z the transmission factor τ(z) is given by

( ) ( ) )exp(0

zzz ⋅−=ΦΦ

= βτ

After crossing a material with thickness z only a fraction exp(-βz) of the original radiation leaves the material, the rest is abosrbed.

6.3.4 Application of Fraunhofer or Mie Small particles with diameters in the range of the wavelength of the used light source should be calculated with Mie theory. Also particles with low refractive index and/or low abosrption coefficient should be calculated by means of Mie theory. If the optical parameters are low you shuld use Mie theory calculation also for coarse particles with diameters more than the wavelenth. Of course, computation of the particle size distribution in accordance with Fraunhofer theory can be used for fine samples with unknown optical constants. The diffraction patterns with maxima and minima, which also occur in the region of the Mie dispersion, make it possible for measurements of the size distribution in accordance with the diffraction theory also to be made in the boundary region between Fraunhofer and Mie theory (particle size equal to or slightly less than the wavelength). Experience has shown that results which are relatively correct and absolutely repeatable can be computed down to a particle size of 0.2 µm. This justifies, for example, the measurement of a sample with the "analysette 22" using the Fraunhofer diffraction theory in the instances in which the materialspecific constants are unknown or when mixtures of different material composition are to be measured. This applies in particular when the coefficient of absorption of the sample is greater than 1.0 - i.e. the sample is relatively "opaque", its refractive index is greater than 1.5 and the measurement can be performed in water.

6.4 Reset to Fraunhofer Resets the program to Fraunhofer calculation


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6.5 Set Measuring Range COMPACT

Depending on the size range of the sample select the appropriate Measuring range by clicking on the corresponding option button. Ok stores the measuring range, Cancel keeps the old range.

6.6 Set Measuring Range COMFORT The COMFORT version offers a larger measuring range and an improved resolution by creating multiple measurements during one measurement cycle. You can use command switches to preselect the cell positions and the corresponding measuring range.

You bring the measuring cell (resp. its symbol) into the desired position by clicking on the pushbuttons pointing to the right or left in the current window. You will find the limits of the related measuring range below the position indicator. Clicking on pushbutton <OK> causes the auto-ranger to move the measuring cell into position.


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For a larger, expanded measuring range you will have to switch from individual measurement to multiple measurement. To do so you need merely click on one of the command switches with the arrow symbol on the right-hand or left-hand side. These then multiplize by themselves: Resolution (number of measuring channels)

Setting of measuring range (multiple measurement) With one click on these doubled arrows you can change the measuring range as you wish. To this end, the measuring range is displayed with a fork in the upper area of the window; on the next line you will see the position of the measuring cell in the unit which is adjusted manually or automatically, depending on the unit version. You can select the number of measuring channels with the operating switches in the centre of the window. The numbers always present a multiple of the number of sensor elements on the sensor (31). During the multiple measurement of at least 62 measuring channels with up to 310 channels, you can therefore set a significantly higher resolution in your measurement for each selected measuring range.

Measurement at high resolution (<310 measuring channels)

To do so, the program of the C-Version automatically places the measuring cell at intermediate positions and performs a measurement for each. When calculating the particle size distribution, all x . 31 measuring signals are taken into account and your result is determined with a matrix calculation especially for your application.


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6.7 Beam Alignment COMPACT After selecting Beam Alignment you can see the current beam adjustment of the measuring unit laser. The "analysette 22 COMPACT" has an auto-alignment, so that there is no need for manual adjustment of the laser beam. Select Auto Alignment if you wish to achieve automatic positio-ning of the laser beam on the detector. At this time the pump au-tomatically switches itself on. During the beam adjustment the central beam is shown in red along with the 31 channels of the detector. The Y axis is divided into steps of 256. The central be-am (red) should, after auto-alignment, be greater than 2000 units and the remaining channels lower.

When the optics are well-adjusted and the clean measuring cell is in the path of a laser beam, the majority of the beam strikes the sensor directly in the centre. Very little light strikes the neighbouring sensor elements; the signals received there are low. When a laser beam is

not well-adjusted, at least the sensor elements immediately to the right of centre indicate a relatively high intensity. The first bar in the graph, the one for the central beam, indicates a relative intensity of about 2/3 of the possible overall height, which represents a value of 3000 units. The height of the neighbouring bars is lower (approx. 1 to 2 mm high); it may be slightly higher at the right-hand end. (Apart from an estimation of the alignment of the laser beam, the graphics from this program also permit an estimation of the beam intensities measured on the individual rings of the sensor.)

Caution: If your measuring cell is dirty this can lead to higher intensi-ties on the external channels or result in the sensor chan-nels being shown alternately as high and low. The auto-alignment may in this case no longer function. The glasses must be cleaned.


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6.8 Beam Alignment COMFORT The unit was carefully adjusted prior to delivery. The adjustment of the laser beam must be checked prior to initial use and readjusted if necessary. Following a total of approx. 10 minutes "Warm-up Time" after being switched on, the laser beam has stabilized and the check can begin. When the dry dispersing unit is used the measuring cell for suspensions must be removed (it is necessary to install the nozzle system)! This procedure is also utilized in the standard measurement program to check the beam adjustment. The measuring cell must be filled with clean measuring liquid for all measurements with dispersing units for suspensions, even when the mini-cell is used. The hood of the unit is closed The measuring cell is at approximately the 200 mm position. Click on the switching area with the icon for adjustment in the tool bar in the main menu. The window with the channel intensity symbols will open up:

When the optics are well-adjusted and the clean measuring cell is in the path of a laser beam, the majority of the beam strikes the sensor directly in the centre. Very little light strikes the neighbouring sensor elements; the signals received there are low. When a laser beam is not well-adjusted, at least the sensor elements immediately to the right of centre indicate a relatively high intensity. The first bar in the graph, the one for the central beam, indicates a relative intensity of about 3/4 of the possible overall height. The height of the neighbouring bars is lower (approx. 1 to 2 mm high); it may be slightly higher at the right-hand end. (Apart from an estimation of the alignment of the laser beam, the graphics from this program also permit an estimation of the beam intensities measured on the individual rings of the sensor.)


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In the event that the laser beam or supply unit is not activated, the message window appears, with acoustical signal:

After the laser and supply unit are activated and you have clicked on OK, this message disappears and the window with the intensity display again becomes the current window. This message also appears if a laser beam is poorly adjusted. In this case, opening the measuring unit and clicking at OK cancels the acoustical warning and you can update the window for checking the adjustment. (If need be, the light from a pocket torch will also be of assistance.) When the hood is open, only a few lines to the right of red first line are short. They are used to adjust the beam. The subsequent lines cannot be evaluated until the hood is closed. In the event that lines more than about 10 mm long are then still visible, particularly in the middle area, this indicates that the cell or measuring liquid is dirty or that the lenses are damaged. This does not influence the adjustment; this can also be carried out when a cell is slightly dirty. Before a measurement, however, the cell has to be flushed or the measuring liquid exchanged, whichever applies. If the lines cannot be shortened by flushing either, the lenses of the cell have to be cleaned (see Instruction Manual). To readjust the beam carefully turn the adjusting screws on the right-hand side of the lens holder flange with the hood open.

The two adjusting screws are set such that the intensity of the central beam (length of the first bar) is increased and length of the neighbouring lines decreases. The adjusting screw in front of the lens system shifts the beam horizontally: screwing it in moves the beam to the right side of the sensor. The screw over the lens system shifts the beam vertically: screwing it in moves the beam upward.

screw for verticall

screw for horizontal


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The following is a tried-and-tested method for doing so:

The following image might present itself after you open the window:

You then attempt to form the rear bars into a falling line by turning the front screw. As a result, when your efforts are completed, you may see the image displayed on the following page:

If you were able to approximately simulate this representation, for examine, try to further improve the adjustment. To do so, turn the top screw clockwise such that the high bars on the left which are still high are reduced in size until you see a red bar rising on the left-hand side. The first two bars

to the right of this will assist your during the fine adjustment. Both can be reduced in size by carefully turning both adjusting screws until the representation on the screen is very similar to the one below:

Please recheck the adjustment with the unit closed. During normal lab operation you do not have to secure the adjusting screws with the fastening screws across from them. They only function as a shipping brace.


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7 Main menu setup NanoTec and MicroTec

7.1 Parameters for measurement

7.1.1 Parameter 1 The comments and measurement numbers entered here are related to the subsequent measurement. If the entries are not changed, they will remain valid for all the subsequent measurements. If you select File, Page setup and enable the control box Comment for measurement, the entries are printed, provided that the font for printing was defined (see File, Page setup).

7.1.2 Enable measurement elongation ratio If you have the optional software for shape identification, you can enable the measurement in this window.

7.1.3 Parameter 2 In Parameter 2, you can set the parameters required for the measurement and for saving the result. If you select Write fixed values in ASCII file, the date, time and measurement comment are written in a sequential ASCII file named ASCII.DAT, located in the FRITSCH directory. For up to 100 values for the percentage volume, the corresponding particle sizes are saved separately with quotation marks. You can load this file with a database such as Superbase or with Excel; by using the corresponding import functions. Selecting Write values in database opens a database window, if a current measurement result has been saved. You can enter additional information in the database window for administering the results from the point of view of ISO 9000. The percentage volume digits are also saved in this database along with the relevant particle sizes in 1 percent stages. Selecting Print after measurement prints the result with the layout defined under Page setup. On selecting Save result after measurement, the measurement is saved directly after a measurement process.


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On selecting the User parameters card, you can enter user-specific parameter (e.g. the user name or a serial number of the unit). These details are printed out if Print measurement comments is selected in the File, Page setup window. Other parameters such as First name or key term are saved in the database, so as to simplify the administration of the result files. If, for example, “Stacking test XR40-E” is selected as key term 1, each file, which was saved with Write values in database enabled, can be easily searched in the database with key term 1 same as “Stacking test XR40-E”.

7.1.4 Other parameters The parameter files for calculating the particle size distribution are shown on the index cards. Attention: these parameter files are saved while saving the measurement. Changes in the parameters yield indefinite results. This option may only be used by experienced users with relevant knowledge and proper training from Fritsch employees.

Always the used parameters preset in the factory. Do not change the parameters.

7.2 Parameters for calculation You can define the parameters for calculating the results in the window Parameters for calculation.

7.2.1 Calculating interpolation values For calculating the interpolation values, you can select fixed particle sizes or fixed percentage volumes from the transient or residual sum total curve.

7.2.2 Selecting preset table values The individual interpolation values can be displayed by clicking the Information button. A window opens, in which the fixed values are displayed in rows containing up to 100 values, or you can select an appropriate value for the current calculation. Depending upon the selected interpolation values, the programme automatically displays only columns with fixed particle sizes or fixed percentages. Please enter the values in this sequence – precise to rough. You can save the newly generated fixed values in the databases.

7.2.3 Calculation methods for filters Here you can select whether you want to filter a distribution as mono-modal distribution. Limiting values to the left and right of the maximum are then set to zero so that only the main maximum of distribution is shown. This can be useful for precise tests, since peaks are often seen in the rough range due to disturbances in the measurement signal, which can then be filtered with this function. Likewise, you can also enable a RMS filter, which eliminates fluctuations in the distribution of the particle size, pertaining to only one channel.


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7.3 Mie Parameter The programme of analysette 22 uses the complete Lorenz-Mie theory for calculating the particle size distribution. Depending upon the optical constants the matrixes are calculated in real time. After the calculation, these matrixes are saved in the memory and can be used later. The absorptions and calculation index of the sample and the suspension liquid affect the elements of the matrix used for calculating the particle size distribution. A new matrix is to be calculated for every possible combination of these three volumes based on the material and the distance between cells. The programme calculated this matrix while determining the particle size distribution, without significantly extending the measurement time required for the purpose.

In the textboxes, enter the material constants for calculating the Mie matrix. Combo Boxes are arranged below the text fields for entering the names of solid materials and fluids; these show an alphabetical list of all names already included in the database. On selecting a material, the entries from the database are transferred to the text input field. On entering optical values, the programme automatically calls the Mie theory. The matrix covers all combinations of the refraction index and absorption coefficient, which are found in practice. The programme itself does not need more than one minute for this. The matrix thus determined is saved to the hard disk for subsequent calculations, so that future measurements and calculations for these materials can be made with the previously calculated matrix in a very short period of time. During a subsequent measurement, the programme “identifies” a matrix saved on the hard disk on the basis of these constants. The parameters depending upon the material should be known with an accuracy of three decimal places. These should be entered as soon as the relevant routine for this is called. After the abovementioned test of the memory, the matrix is either calculated or read.


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The changeover of demands Database for solids / Database for liquids opens the databases and enables the entry of your optical constants. These databases enable the entry of the refraction index and absorption coefficient of your sample and of the refraction index of the liquid. These solid and liquid matters are not saved in an alphabetical sequence. However, entries can be searched and their refraction index and absorption coefficient read.

Attention: The programme does not check whether the names of the solid or liquid matter are repeated. While entering the name, ensure that these are not already existing.

A new solid or liquid matter can be entered simply by clicking on the command button New. Enter all the relevant data in the corresponding entry fields. If you click on the command button Update, your entry will be accepted in the database and arranged alphabetically. To delete data from the database, select a solid or liquid matter and then click the command button Delete.

7.4 Resetting as per Fraunhofer Resets the programme to a calculation as defined by Fraunhofer.

7.5 Setting the measuring range The NanoTec and MicroTec version offers a larger measuring range and increased resolution by generating superimposed measurements. In this menu item, you can pre-select the cell position and the corresponding measuring range with the command buttons.

Bring the measuring cell in the desired position by clicking on the buttons in the current window pointing to the left or right. Below the position display, you will find the limits of the corresponding measuring range.


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Click OK to initiate the automatic mode for bringing the measuring cell automatically into position. For a larger measuring range, you must change over from single measurement to multiple measurement – for this, simply click on one of the command buttons with the arrow symbol to the right or left. These will then multiply on their own: Resolution (Number of measurement channels)

Setting the measuring range (multiple measurement) You can change the measuring range as required by clicking on these double arrows. The measuring range is displayed in the upper area of the window with a fork;in the next line you will see the position of the measuring cell in the device, which you can set manually or automatically, depending upon the version of the device. You can select the number of measuring channels with the sliding switch in the centre of the window. The numbers always show multiple times the number of sensor elements on the sensor (up to 80). Thus, for every selected measuring range during the multiple measuremen t of at least 74 measuring channels having up to 630 channels, you can set a considerably high resolution during your measurement.

In the NanoTec and MicroTec version, the programme automatically brings the measuring cell in the intermediate positions and performs a measurement process every time. While calculating the particle size distribution, all x * 57 and/or 63 measuring signals are taken into account and your result determined with a matrix specially calculated for your application.


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7.5.1 Enable Nano option (only NanoTec wet dispersing)

You can extend the measuring range downwards by clicking on the “Enable Nano range measurement” control box. As the particle size becomes smaller, the scattered light contains lesser information. At the same time, the angle of dispersion becomes very large and the intensity of the scattered light increases severely. Hence, the measurement of Nano particles involves a larger instrumental expenditure. Forward scattering The light scattered in the measuring cell is scattered in the forward direction and recorded by the light-sensitive elements of the scattered light detector. In the centre of the detector is a micro hole, through which the laser beam is fixed on a photo diode for determining the total absorption. Concentric, light-sensitive elements are arranged around this micro hole, the surfaces of which increase constantly in the outer range for compensating the low scattering effect of smaller particles. In the inner range of the detector, the elements are very small, so that they can measure the scattered light of larger particles with high resolution. State-of-the-art production methods in the semi-conductor technology are used for separating the individual elements. The scattered light cannot leave the measuring cell at extremely large angles because there is total (internal) reflection during the transition from optically dense to thinner medium from a particular angle onwards. For this reason, the optical measuring cell glasses of “analysette 22” have prism-shaped wideangle, from which scattered light can be emitted even at large angles. This light is measured on the detector by special wideangle elements. In the forward direction (lower measuring limit ~0.1 µm), a scattered angle range of up to ca. 60° is recorded with this structure. Backward scattering A considerably larger angle range must be recorded for recording the scattered light of Nanometer particles. For this, “analysette 22” NanoTec uses a backward laser, which enters the detector through the same micro hole and causes the scattering of light in the measuring cell, which is recorded by the detector as backward scattering in the angle range of 60 – 180°. In addition to this, the optimised geometry of the detector records and assesses the varying scattering effect of Nano particles parallel and perpendicular to the direction of polarisation of the laser. The lower measuring limit is ~10 nm.


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Measuring principle With the extension of the measurement of the backward scattered light, “analysette 22” NanoTec records a scattered angle range of 0° up to approx. 180°. A unique feature of this model is a double laser diode for measuring scattered light in the forward and backward direction. This “Nano” option can be enabled with the module for wet dispersing. For extending the measurement in the Nanometer range, the forward laser is switched off and a laser released in the backward range. This enters the detector through the same micro hole and causes scattering of light in the measuring cell, which is accepted by the detector as polarisation-selective backward scattering in the angle range of 60 – 180°. The extinction of the backward laser is recorded by swinging a photo diode in front of the forward laser. The lower measuring limit is ca. 10 nm.

7.6 Beam adjustment The device is carefully adjusted before delivery. Before the first use, the setting of the laser beam must be checked and readjusted, if necessary. In the NanoTec versions, the programme offers automatic alignment for the forward and backward laser and for the MicroTec version, only for the forward laser. A backward laser is not integrated in the MicroTec. However, a manual alignment can also be selected.

7.6.1 Manual alignment After approx. 10 minutes "warm-up period", the laser beam becomes stable and the check can be initiated. The adjustment of the laser beam can be checked after the preparations are made. (This method is also used in the standard measuring programme for checking the beam adjustment. For all measurements with dispersing units for suspensions, the measuring cell must be filled with a clean measuring liquid.) The cover of the device is closed. The position of the measuring cell is approx.200 mm. By clicking on the symbol for beam adjustment, the window with the intensity symbols of individual measuring channels opens:


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If the optics are well-adjusted and the measuring cell is clean, the main laser beam directly falls on the centre of the sensor (red bar to the left). Less scattered light falls on the adjoining elements – the signals are smaller. If the laser beam is not very well adjusted, at least the red bars to the immediate right of the sensor elements show a higher intensity. The first bar - that of the central beam - shows a relative intensity of approx. 3/4 of the possible overall height. The height of adjoining bar is lesser (approx. 1 -2 mm); the size should increase slightly towards the right. (In the graphic resulting from this programme, the beam intensities that are measured on the individual segments of the sensor should also be assessed in addition to the alignment of the laser beam.) If the cover is opened, very few lines to the right of the first red bar are low. The beam is adjusted with these lines. The lines that follow can be assessed only if the cover is closed. If lengths more than approx. 10 mm are seen mainly in the central area, this indicates that the cell or measuring liquid is dirty or the glasses are damaged. This does not hamper the adjustment as this is possible even if the cell is slightly dirty. Before the measurement, the cell must be cleaned and/or the measuring liquid replaced. If the bar height does not reduce even after rinsing the cell, the cell glasses must be cleaned (see Operating instructions). For readjusting the beam, the arrows in the window should be adjusted such that the intensity of the central beam (length of the first bar) is increased and the length of the adjoining lines is reduced. The right and left arrows shift the beam in the horizontal direction. The up and down arrows shift the beam in the vertical direction. It is possible that you see the following picture on opening the window:


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You can then try to bring the bar in a descending line by clicking the horizontal and vertical arrows. Try to further improve the adjustment. Finally, the overall scene should look somewhat like this:

7.6.2 Auto alignment Select the auto alignment function for the forward and backward laser, so that the programme can automatically adjust the laser beam. If this does not take place within 10 minutes, an error message appears, following which you must either try to optimise the beam picture through manual alignment or subsequently select auto alignment. Attention: ensure that the measuring cell glasses are not dirty. This hampers the auto alignment or makes it simply impossible.

7.7 NanoTec check In this window, you can directly control the different functions of the devices. Here, you can open the 4/2-way valve via software till the suspension is drained out or switch the pump and ultrasound on and off.

7.8 Display elongation ratio (Optional)

7.8.1 Principle The shape of particles can be identified on the basis of diffraction structures. The diffraction picture created by the particles in the laser contains information on the shape of the particles. particle shapes create different diffraction patterns in the laser beam. Shape information can be extracted from this using appropriate methods.

Diffraction pattern of a circular particle


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Diffraction pattern of an ellipsoid particle

During a real measurement, several particles are found in the measurement volume with a random alignment and varied particle sizes. The resultant diffraction picture contains combined information about the particle size, spatial arrangement and shape of the particle

Diffraction pattern of a group of particles

With the help of neuronal network technologies, the sensor data is prepared in such a way that a statistical assessment is possible. The result of the measurement is average elongation, calculated on the basis of the axis ratio of an ellipsoid approximate to the particles.

Sketch of the sensor arrangement


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A simulated neuronal back propagation network is trained and used for assessing the sensor data. With this, you will get a largely material-independent shape calibration, which is shown in the diagram (Fig. 5). Tests have shown that the measured values determined on the basis of a certain number of measurements, largely correspond to the setpoint values.

Comparison of standard particle elongation with the measured sensor data

7.8.2 Measurement Go to “Measure parameter" and select “Enable measurement elongation ratio”. Programme your measurement process in the usual manner and press “Start measurement”.

Under any circumstances, do not select “Rinse after measurement”, otherwise your sample will be rinsed in the discharge before the elongation ratio is determined and you will have no sample left in the measuring circle.

After this, the measurement process is carried out in the usual manner. At the end of the measurement process, a dialogue box appears, which notifies the beginning of the process for determining the elongation ratio. Based on the measured d50 value of your distribution, a cell distance is calculated, for which the 2nd diffraction minimum lies exactly on the detector channels for shape identification. The measuring cell travels to this calculated cell position and starts the measurement. Since a background measurement is not available for this cell distance, the rinsing process is subsequently started. The measuring circle is cleaned and then the background measurement carried out at this cell position.

Attention: If you have enabled the measurement of the elongation ratio, the rinsing process is started automatically after the measurement, for determining the elongation ratio. Your sample is then washed out.


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If your d50 value is too small, because of which the measuring cell is brought closer than 20mm to the detector the determination for a higher dXX value is started for the minimum cell distance of 20mm. Hence, it is possible that you are able to determine the elongation ratio only for the d90 value for a sample with a d50 value of 10 micron. With this measurement, you will no longer record a large part of the particle.

7.8.3 Presenting the result

A display appears, which gives the average elongation ratio and the minimum and maximum value of the elongation ratio for explaining the fluctuation. You can rotate the picture to see a three-dimensional approximation. The presentation is made in a grid. You can print the diagram with the Print key. If elongation data is found, this data is also printed while printing the result. The elongation data, if available, is linked with the result file, if you save its result. If you load a result later, for which an elongation measurement has been carried out, all files are re-created and you can trace back the then measured raw/unprocessed data.


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8 Main Menu Results

8.1 Graphics

8.1.1 Graphs Specific, measurable physical properties of individual particles or elements are utilized to describe a disperse system. The particle size as a property is generally an "equivalent diameter" which is calculated from the measurements during grain size analysis. The equivalent diameter is defined as the diameter of a sphere which exhibits the same physical properties as the measured, irregularly formed particle while a specific particle characteristic is being determined. For the graphic presentation, the total complex is arranged according to a geometric dimension of the particles such as the equivalent diameter x and plotted on the abscissa of a coordinate system. The components which are allocated to the size of the individual elements and which indicate the participation of individual particle classes in the distribution as a whole are plotted on the ordinate.

A distinction is drawn between two measurements of quantity • the distribution sum Qr • the distribution density qr The cumulative curve of distribution Qr(x) indicates the standardized total quantity of all particles with equivalent diameters smaller than and equal to x. Each point on the distribution cumulative curve indicates the quantity component total of all particles between xmin and x. The distribution density curve qr(x) is the first derivation of Qr(x) after x. It often exhibits the bell shape shown, however distribution density curves with two or more peaks can also be measured. You have the option of displaying the distribution density curve as drQ(x) or as qr(x).


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In accordance with dQr(x) = qr(X) dx, qr(x) is the component of a quantitiy dQr(X) contained in the interval dx for the particles between x and x + dx. It follows for a random type of quantity r that

dxxdQ

xqx

xqxxq rn

ii

ri

r

r

i

)(

)(

)()(

10

0=

⋅

⋅=

∑=

When you click your mouse on one of the lines, the form of representation changes, for example from the • distribution density curve qr (x) to the • distribution cumulative curve Qr (x) or to a • combination of the two forms of representation. In addition, you can also select a representation in the • RRSB coordinate network or an • Gaussian distribution, an • exponential curve or • lin-lin scale. Selecting RRSB coordinate network also presents a linear regression curve showing n and d‘ values (see Calculation Parameters) as well as a weighted regression for a parameteric representation of dissolution rate curves based on RRSB distributions.

8.1.2 Edit 8.1.2.1 Insert Object It´s possible, to insert an OLE 2 Object (object linking and embedding) into your graphs. We have integrated one of our company logos which was generated under CorelDraw 3.0 directly into the representation of the results after clicking on the first line. You can link any object here with OLE capability. Object linking and embedding (OLE) is a technology that allows a programer of Windows-based applications to create an application that can display data from many different applications, and allows the user to edit that data from within the application in which it was created. In some cases, the user can even edit the data from within the application. An OLE object refers to a discrete unit of data supplied by an OLE application. An application can expose many types of objects. For example a spreadsheet application can expose a worksheet, macro sheet, chart, cell, or range of cellsall as different types of objects.You use the OLE control to create linked and embedded objects. When a linked or embedded object is created, it contains the name of the application that supplied the object, its data (or, in the case of a linked object, a reference to the data), and an image of the data. An OLE control can contain only one object at a time.


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8.1.2.2 Load Object Retrieves an OLE Automation object from a file. You need the full path and name of the file containing the object to retrieve. When this code is executed, the application associated with the specified file name is started (e.g. WORDPROC.EXE in this example) and the object in the specified file is activated. If the filename argument is set to an empty string (""), this function returns the currently active object of the specified type. If there is no object of that type active, an error occurs.

8.1.2.3 Insert from Clipboard The Clipboard object is accessed with this command, and is used to manipulate text and graphics on the Clipboard. You can use this object to enable a user to copy, cut, and paste text or graphics in your application. The Clipboard can contain several pieces of data as long as each piece is in a different format. For example, you can use a program to put a bitmap on the Clipboard, and then use another one to put text on the Clipboard. You can then use the program to retrieve the text or the picture. Data on the Clipboard is lost when another set of data of the same format is placed on the Clipboard either through code or a menu command.

8.1.2.4 Save Object Saves an OLE object to a binary data file. If the OLE object is linked, then only the link information and an image of the data is saved to the specified file. The object's data is maintained by the application that created the object. If the OLE object is embedded, the object's data is maintained by the OLE control and can be saved by your application. Normalising to a new maximum Generally, the results of analysette 22 are standardised to 100%. If, for a subsequent application of the results in other applications, e.g. for taking into account rough parts, you want a standardisation to another value, you can convert the result to e.g. 80% with this function. The transient sum total curve ends after this operation not with 100% but with 80%.

8.1.3 Transformation 8.1.3.1 Transformations For a quantity r the distribution density curve is defined as

For the description of a particle size distribution so called complete moments are introduced


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The 1. index describes the exponent of the particle size x, the 2. the choosen quantity. A distribution density curve q(x) with quantity r can be transformed into a q(x) with quantity t via

From

and

the final formula follows

which represents the transformation formula. Your click on the first line initiates a conversion of the current distribution into a number distribution, the second line converts into a length distribution, the third line converts into a surface distribution, and the fourth line converts into a volume distribution. You can also convert a distribution repeatedly, i.e. theoretically also transform "backwards", which will naturally not take you back to the original distribution. For more details see Chapter D-Values.

8.1.3.2 Undersize / Oversize The distribution sum curve Q(r) can either be shown as undersize or as oversize curve. Oversize ist calculated as (100 - Q(r)).

8.1.3.3 Changeover to q3 distribution Switches between the presentation of the dQ(x) and q(x) distribution. q(x) is standardised to the logarithmic class amplitude.

8.1.4 Style Colors Following a click on the first line you can adapt

the background and foreground colour on your screen and (colour) printer to your own taste.

Fill Bars Fills the bars of the density distribution. Pattern You can cross-hatch the bars as you wish,

vertically, on an angle or horizontally Empty Bars Empties the bars of the density distribution. Line Changes the bar chart representation of your

density distribution into a smooth density curve. Grid On Off Switch the grid in your coordinate network on or

off.


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8.1.5 Options 8.1.5.1 Export This dialogue is only required for Office applications, which do not originate from Microsoft. For directly exporting certain values, please use the export functions described later for direct export to Excel.

8.1.5.1.1 DDE Dialog Excel After a click on DDE Dialog Excel you can communicate via DDE (Dynamic Data Exchange), for example with the spreadsheet EXCEL. Afterwards you can select a specific number of cells in columns and lines and prepare your results for postprocessing in EXCEL. Do not misuse, improper use of this DDE capability could corrupt your results. A22 program's DDE features enables your application to directly and continuously exchange data with other Windows-based applications that support DDE. These data exchanges are called conversations. Under DDE, a destination (or client) application sends commands through DDE to the source (or server) application to establish a link. Through DDE, the source provides data to the destination at the request of the destination or accepts information at the request of the destination. When you use DDE with Windows version 3.0 or 3.1 based applications, the source and destination applications are both located on the same computer. You start data exchanges by establishing DDE links, which can be created at run time. • Your application can start the other application before

initiating a conversation. • You can trap and handle errors. • Your application can choose under what circumstances

updates of data between linked controls actually occur. The procedure below is as an example of how to establish a DDE conversation between a-22 program and Excel for Windows. First, create the source spreadsheet in Excel: 1. Start Excel, and a document titled "SHEET1" will be created

by default. 2. From the File menu, choose Save As, and save the document

with the name SOURCE.XLS into your applications directory. 3. Exit Excel. For this example to function properly, Excel must

not be loaded and running. One of the windows mysteries is, that on some computer this works also with Excel running.

4. Next, create the DDE Link from the a22 program. It informs the source that information is being sent.

If you do not specify the right path to your Excel application this procedure will crash. If you do not specify the right short letters for row and column this procedure will crash (i.e. English Version of Excel: Row („R“) Column („C“) / German Version Row („Z“) Column („C“) )


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8.1.5.1.2 OLE Dialog Excel After a click on OLE Dialog Excel you communicate via OLE (Object Linking and Embedding) with EXCEL. Excel is opened, the Excel sheet SOURCE.XLS is opened and values are written to the corresponding rows. After finishing the communication Excel is closed and the a-22 program is reactivated. If Excel was already running before it will not be closed after data exchange. This will cause trouble when calling the procedure again. So please close any Excel instance before starting this OLE communication.

8.2 Statistical Values Apart from numerous graphics and other options, the "analysette 22" also furnishes the user with statistical values which can provide further useful information to evaluate the particle size distribution. This item offers a direct export function of the displayed values to Excel (Export Excel). The most important values are the "complete moments of distribution".

MM x q x M

Mk r

ri

i

n

ik r

r

k ri,

,

,

,( )= = =+

=

+∑10 1

00

0

The first index is always the exponent of grain size x; the second index is the quantity-type of distribution measured r=0: number distribution r=1: length distribution r=2: surface distribution r=3: volume distribution

The arithmetic mean diameter, for example, is derived from these moments.

∑

∑

=

=

∗

== n

ir

n

iri

rr

i

i

q

qxxM

1

1,1,1

Based on a volume distribution received with the laser particle sizer the following Statistical values are calculated with

∑=

=n

ii

qN1

3

8.2.1 Arithmetical Mean

N

qxx

n

ii i∑

=

∗= 1

3


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8.2.2 Geometrical Mean

Nn

i

qi

ixx ∏=

=1

3

8.2.3 Square Mean

∑=

∗∗=n

ii iqx

Nx

13

21

8.2.4 Harmonic Mean

∑=

= n

i ii

qa

Nx

13

1

8.2.5 Cauchy theorem Square > arithmetical > geometrical >harmonic Mean Diameter

8.2.6 Median Value The Median value represnts the grain size at which the Qr curve posesses 50% of its value.

8.2.7 Modal Value The Modal value represents the grain size at which the qr curve achieves its maximum.

8.2.8 Specific Surface Area A further value derived from the moment equation is the volume-related specific surface. It is an important, common criterion of material production, which is described in units of mass or volume of base material, is systematically reduced and is usually eventually reduced to a minimum in the finished product. The surface based on the unit of volume has the dimension area/volume and is designated as the specific surface of the substance. The product of specific surface and surface energy of the solid multiplied by the dimension energy/area defines an energy. In thermodynamic terms this is a free energy referred to the mass of the solid or the volume of the solid. It contributes significantly to the driving force of the sintering process, hence a simplification of sintering in the sense of a reduction of time and/or temperature is directly associated with the fineness of the raw product, i.e. the magnitude of the specific surface.

O k MM

kM

kx

v = = =2 0

3 0 1 2 1 2

1 1,

, , ,


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You can enter the density of the sample and [g/cm³] in the “Density” field. The surface-related Specific Surface [cm²/cm³] is directly converted to the mass-related Specific Surface [cm²/g] by division. By entering a form factor, the calculation of the specific surface can e.g. be adapted to the results from BET measurements. Attention: the calculation of the specific surface is based on smooth circles, whereas e.g. BET records measurements on the basis of the surface porosity. The results should be interpreted accordingly.

8.2.9 Span It is often useful to be able to use a number to describe how wide the distribution is scattered around the mean. One measure of this is the span.

50

1090

dddSpan −

=

Further values to describe this width are the lower and upper quartiles (25% and 75%), the interquartiles (75% to 25%) or the standard deviation:

( ) ( )∑=

∗−∗−

=N

iirri xqxx

N ir

1

2

11

σ

8.2.10 Skewness If the distribution density curve is shaped like a Gaussian distribution, the mean, median and modal value are at the same point. However, most distributions have more material on one side than on the other; they are skewed. The skew is defined as follows:

3

3

1

)(100

)(

MSD

xxxq

S

n

iri

ri∑=

−∗=

If more material is in the coarse range, the distribution has a positive skew; if more material is on the other side, a negative skew.

8.2.11 Kurtosis A further value, the kurtosis, describes the shape of the maximum. A distribution with a pointed maximum is referred to as being leptokrutic, a distribution with flattened maximum as being platykurtic.

K

q x x x

MSD

ri r

i

ni

=⋅ −

=∑ ( ) ( )

10 01

4

4


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8.2.12 Folk & Ward Special values based on Folk & Ward are

Mean: 3

845016 xxxM ++=

Standard deviation: 6.64

5951684 xxxxS −+

−=

Skewness: ( ) ( )595

50595

1684

501684

22

22

xxxxx

xxxxxS

−∗∗−+

+−∗

∗−+=

Kurtosis: ( )2575

995

44.2 xxxxK−∗

−=

8.3 Show d-Values

The Show d-Values window shows all relevant tabular values of your results. In addition to the fixed values of particle sizes which you have predefined and related percentages, you will also find weighted mean diameters in these tables. This item offers a direct export function of the displayed values to Excel (Export Excel). There is maximum confusion about the use of different d values. Hence, this topic is dealt with in a detailed chapter in this manual. DIN 66141 also acts as an excellent supplement and gives further explanation. Unfortunately, DIN uses the so-called x values; also, the nomenclature is different. Inspite of this, DIN is extremely useful for understanding the moment of distributions.


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8.3.1 Diameters If we look at a particle under the microscope we are looking at some 2-D projection of it and there are a number of diameters that we can measure to characterise this particle. If we take the maximum length of the particle and use this as our size, then we are stating that our particle is a sphere of this maximum dimension. Likewise, if we use the minimum diameter or some other quantity like Feret‘s diameter, this will give us another answer as to the size of our particle. Hence we must be aware that each characterisation technique will measure a different property of a particle (max. length, min. length, volume, surface area etc.) and therefore will give a different answer from another technique which measures an alternative dimension. Thus we can only seriously compare measurements on a powder by using the same technique. This also means that there cannot be anything like a particle size standard for particles like grains of sand. Standards must be spherical for comparison between techniques. However we can have a particle size standard for a particular technique and this should allow comparison between instruments which use that technique.

8.3.2 D[4,3] and other means What is the average size of three spheres of diameters 1,2,3 units ? On first reflection we may say 2.00. How have we got this answer? We have summed all the diameters (Σd=1+2+3) and divided by the number of particles (n = 3). This is a number mean, (more accurately a number-length mean) because the number of the particles appears in the equation:

nd

erMeanDiamet ∑==++

= 00.23

321

In mathematical terms this is called the D[1,0] because the diameter terms on the top of the equation are to the power of (d1) and there are no diameter terms (d0) on the bottom of the equation. Catalyst engineers will want to compare these spheres on the basis on surface area because the higher the surface area, the higher the activity of the catalyst. The surface area of a sphere is 4πr2. Therefore to compare on basis of surface area we must square the diameters, divide by the number of particles, and take the square root to get back to a mean diameter:

( )nd


=2222

16.23

321

This is again a number mean (number-surface mean) because the number of particles appear on the bottom of the quotation. We have summed the squares of the diameter so in mathematical terms this is called the D[2,0]- diameter. Terms squared on the top (d2), no diameter terms on the bottom (d0).


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Chemical engineers will want to compare the spheres on the basis of weight. Remembering that the weight of a sphere is 4/3*π*r3*ρ then we must cube the diameters, divide by the number of particles and take a cube root to get back to a mean diameter.

( )nd


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29.23

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Again this is a number mean (number-volume or number-weight mean) because the number of particles appears in the equation. In mathematical terms this can be seen to be D[3,0]. This is what industry usually understands by the Volume Mean Diameter (VMD). Academics normally prefer the D[4,3]. Stepping back to our particle of arbitrary shape, then the sphere of equivalent volume to our particle is in mathematical terms the D[4,3] and the sphere of equivalent surface area is the D[3,2j or Sauter Mean Diameter (SMD). These would be calculated as follows:

[ ]∑∑==

++++

= 3

4

333

444

72.23213213,4

dd

D

[ ]∑∑==

++++

= 2

3

222

333

57.23213212,3

dd

D

Note that the number of particles does not appear in the numerator or denominator of the equation. Techniques like laser diffraction which measure a distribution proportional to D3 do not need to know the number of particles in order to get an answer for the mean result.

8.3.3 Different techniques give different means. If we use an electron microscope to measure our particles it is likely that we will measure the diameters with a graticule, add them up and divide by the number of particles to get a mean result. We can see that we are generating the D[1,0] number - length mean by this technique. If we have access to some form of image analysis then the area of each particle is measured and divided by the number of particles - the D[2,0] is generared. If we have a technique like electrozone sensing, we will measure the volume of each particle and divide by the number of particles - a D[3,0] is generated. Laser diffraction can generate the D[4,3] or equivalent volume mean. This is identical to the weight equivalent mean if the density is constant as shown below. First take a cube of unit dimension X. The volume of this cube is obviously X.X.X. = X3 and the weight of the cube is X3*ρ. where ρ is the density. What are the spherical equivaIents of this cube ?


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8.3.3.1 Volume equivalent There is a sphere of diameter D1 which is the same volume as the cube

ρπ ⋅

31

234 D

From this we can calculate D1 if we know X3.

8.3.3.2 Weight equivalent There is a sphere of diameter D2 which is the same weight as the cube. This sphere will weigh

ρπ ⋅

⋅⋅

32

234 D

Therefore

ρρπ ⋅=⋅

⋅⋅ 3

32

234 XD

lt is easy to see that D1=D2 as the densities will cancel in the equation above. Thus the density of the material is irrelevant to a volume or weight equivalent. Extending this trivial example, it can be seen that for any shaped object of constant density the weight and volume equivalent will be the same. So each technique is liable to generate a different mean diameter as weIl as measuring different properties of our particle. No wonder people get confused! There are also an infinite number of ,,right“ answers. Imagine 3 spheres with diameters 1,2,3 units

[ ]

[ ]

[ ]

[ ]

[ ]

[ ]

[ ] wmvm

sv

lv

ls

nv

ns

nl

XDX

DX

DX

DX

DX

DX

DX

==++++

==

=++++

==

=++++

==

=++++

==

=++

==

=++

==

=++

==

72.22781811613,4

57.2941

27812,3

45.2321

27811,3

33.23219411,2

29.23

27810,3

16.23

9410,2

23

3210,1

3


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8.3.3.3 Number and volume distributions. The following example is adapted from an article in New Scientist (13 October 1991). There are a large number of man-made objects orbiting the earth in space and scientists track them regularly. Scientists have also classified them in groups on the basis of their size

Size (cm) Number of Objects

% by Number

% by Mass

10-1000 7000 0.20 99.96 1-10 17500 0.50 0.03

0.1-1.0 3500000 99.30 0.01 Total 3524500 100.00 100.00

If we examine the third column above we would conclude (correctuy) that 99.3% of all the particles are incredibly small. This is evaluating the data on a NUMBER basis. However, if we examine the fourth column we would conclude that virtually all objects are between 10 -1000cms. This is where all the MASS of the object is. Note that the NUMBER and MASS distribution are very different and we would draw different conclusions depending on which distributions we use. Neither distribution is incorrect. The data is just being examined in different ways. If we were making a space suit, for example, we could say that it is easy to avoid the 7000 large objects and this takes care of 99.96% of all cases. However, what is more important with a space suit is the protection against small particles which are 99.3% by number ! If we take a calculator and calculate the means of the above distributions we find that the number mean is about 1.6 cm and the mass mean about 500 cm - again very dif-ferent.

8.3.3.4 Inter conversion between number, length and volume/mass means.

If we are measuring our particles on an electron microscope we know, from an earlier section that we arc calculating the the number-length mean size. If what we really require is the mass or volume mean size we have to convert our number mean to a mass mean. Mathematically, this is easily feasible, but let us examine the consequences of such a conversion. Imagine that our electron measurement technique is subject to an error of 3% on the mean size. When we convert the number mean size to a mass mean size then as the mass mean is a cubic function of the diameter then our errors will be cubed or 27% variation on the final result. However, if we are calculating the mass or volume distribution as we do with laser diffraction then the situation is different. For a stable sample measured under recirculating conditions in liquid suspension we should be able to generate volume mean reproducibility of 0.5%. If now we convert this volume mean to a number mean the error of the number mean is the cube root of 0.5% or less that 1.0%!


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In practice this means that if we are using an electron microscope and what we really want is a volume or mass distribution, the effect of ignoring or missing one 10 micron particle is the same as ignoring or missing one thousand one micron particles. Thus we must be aware of the great dangers of inter conversion. The software will calculate other derived diameters but we must be very careful of how we interpret these derived diameters.

8.3.3.5 Measured and derived diameters. We have seen that the laser diffraction technique generates a volume distribution for the analysed light energy data. (Note that with Fraunhofer analysis, the projected area distribution is assumed but a volume distribution is generated). This volume distribution can be converted to any number or length diameter as shown above. However, in any analysis technique, we must be aware of the consequences of such a conversion (see immediately above) and also which mean diameter is actually measured by the equipment and which diameters are really calculated or derived from that first measured diameter. Other techniques will generate other diameters from some measured diameters. For example, a microscope will measure the D[1,0] and will/may derive other diameters from this. We can place more faith in the measured diameter than we can on the derived diameters. In fact, in some instances it can be very dangerous to rely on the derived property. For example, the analysis table gives us a specifid surface area in m2/cc or m2/g. We must not take this value too literally - in fact, if what we really want is the specific surface area of our material we really should use a surface area specific technique e.g. B.E.T. or mercury porosimetry.

8.3.3.6 Which number do wo use? Remembering that each different technique measures a different property (or size) of our particle and that we may use the data in a number of different ways to get a different mean result (D[4,3], D[3,2] etc.), then what number should we use ? Let‘s take a simple example of two spheres of diameters 1 and 10 units. Imagine that we are making gold. If we calculate the simple number mean diameter this will give us:

[ ] 50.521010,1 =

+=D

So we would assume that the average size of the particles in the system is 5.50 units. However, we must remember that if we are making gold we are interested in the weight of our material. For example, if we have a process stream we are not interested that there are 3 million particles in it, we are more interested that there is 1kg or 2kg of gold.


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Remembering that the mass mean is a cubic function of diameter, we would see that the sphere of diameter 1 unit has a mass of 1 unit and the sphere of diameter 10 units has a mass of 103 = 1000 units. That is, the larger sphere makes up 1000/1001 parts of the total mass of the system. If we are making gold then we can throw away the sphere of 1 unit bedause we will be losing less than 0.1% of the total mass of the system. So the number mean does not accurately reflect where the mass of the system lies. This is where the D[4,3] is much more useful. In our two sphere example the mass or volume mean would be calculated as follows

[ ] 991.91011013,4 33

44

=++

=D

This value shows us more where the mass of the system lies and is of more value to chemical process engineers. If we throw away the smaller 1 unit particle the weight or mass mean D[4,3] will only change from 9.991 to 10.000 which is very slight. However, let us imagine that we are in a clean room making wafers of silicon or gallium arsenide. Here, if one particle lands on our wafer it will tend to produce a defect. In this instance the number or concentration of the particles is very important because 1 particle = 1 defect. We would want to use a technique that directly measures the number of particles or gives us the concentration of particles. In essence this is the difference between particle counting and particle sizing. With counting we will record each particle and count it - the size is less important and we may only require a limited number of size classes (say 8). With sizing the absolute number of particles is less relevant than the sizes or the size distribution of the particles and we may require more size bands.


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8.4 Average Results In the window Average Results you can define a specific type of mean and the type of calculation (standard deviation, etc.). This item offers a direct export function of the displayed values to Excel (Export Excel). Initially, the right portion of the window remains blank. Your next step is to click on the pushbutton for selecting the result files (Select Files). In the Load Comparisons window subsequently opened you have the opportunity to mark and load the data carrier, the directory with your results and, finally, up to 100 files.

By clicking on Show Selected Files you see the selected curves. Clicking on Calculate starts the calculation and you can have a look at your mean curve from the preceding window. After selecting Ok you can store the mean value together with min-max curves or other options selected.

8.5 Control Card d-Values If the Load comparison curves was already selected, the programme shows the defined d values of all selected result files. This item offers a direct export function of the displayed values to Excel (Export Excel). Here, you can check the conformity of your measuring device with ISO 13320, since the programme also directly exports the ISO values and tolerance limits to Excel. If no files are selected the program will access the file \FRITSCH\ASCII.DAT and will present defined d-values based on the contents of this file. For more information see also Measurement Parameters.


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8.6 User Sizes

8.6.1 Enter Theoretical Values In the program section for entering a theoretic curve you can enter coordinate points in a table.

The programme uses this item for calculating a theoretical result - if you wish, also with the aid of a spline function with intermediate values to smooth them. Afterwards you can use this virtual measurement result as if it had actually been measured. This method is used in particular when specifying limiting, target or standard values. You can enter particle sizes and the related percentage volumes to produce your distribution curve, but the program also assists you to enter theoretical sizes quickly. • In the righthand portion you define the minimum and

maximum value for your particle size (e.g. 2 µm and 45 µm); if you did not do so, a reminder is issued.

• In the input field Channel you define the number of supporting points you are to enter.

• You can employ a calculating aid which calculates the same distances between your supporting points. To do so, activate a monitoring box for linearly same-size or logarithmically same-size classes. Likewise, you select a multiplication factor between your values or an ascending equal summation.

• Following a click on Calculate the program writes the particle sizes into the column on the lefthand side. All you have to do now is to enter the percentage associated with the particle sizes.

Afterwards you click to open a submenu in the menu line in which you save your distribution curve. You are familiar with the selection of the data carrier, directory and the assignment of a file name - the customary procedure is followed.


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You can also store the series of particle sizes just created in the same submenu so that you will not have to enter them later again. To load stored size classes, click on the first line to move to a window with the familiar options for selecting data carrier, directory and name (the suffix to the file name is "THE"). In the Import item, you can read a saved result and change it with the editor or you can read an ASCII file (separated by comma) with 3 values (consecutive number, corn size, sum total curve) and process further.

8.6.2 Enter User Sizes In the window Enter User Sizes you create classes or load classes you defined earlier. By clicking on Save File you can store under a name a class division you created if it is to be used later again. Likewise, after clicking on Load File you can call up prepared size classes.

8.6.3 Calculate User Sizes

In this program part you can convert the results you measured with the laser particle sizer analysette 22 into individual particle classes which you have defined. In the first step you determine up to 100 classes (see above); in the second step the program converts the results and shows them as if they had been measured in these classes.

After you have clicked on New Calculation both curves

will be presented to you superimposed over each other. The results recalculated in this program can be stored like measured results if you do not wish to overwrite them - you can even store them under a new name. Just click Ok. This type of conversion does not take any differences in results into consideration which are caused by different measurement procedures: During the sifting of the same sample it is only in exceptional cases that you can anticipate a particle size distribution such as the one you see following the analysis of a diffraction image.


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8.6.4 Combine Oversize In the Combine Oversize window it is possible to combine a measurement result received with a different measurement method with the a22 measurement result. If the measurement range of the a22 is too small, you can make a sieving at the upper limit of the a22. Measure the fine particles and e.g. make a sieving with the coarse material. If you enter the sieving result into the a22 program, it is possible to combine these two measurements with this function. Just tell the program where you want to have the intersection point by clicking into the distribution curve window to the size where you want to have the cut. The new combined distribution will be calculated. It is also possible to import directly a measurement received with FRITSCH AUTOSIEVE program.

8.7 Revalidation of Results

8.7.1 Revalidation Function Different measuring methods produce different results when measuring a particle size distribution (PSD) of irregular, non-spherical particles. To determine a PSD, each measuring method utilizes a specific physical property related to the particle size. As a result the special equivalent diameter for the method is obtained. In general, the equivalent diameter is defined as the diameter of a sphere which, when a specific particle is determined, exhibits the same physical properties as the measured, irregularly shaped particle. Hence the diameter determined by means of sedimentation is the diameter of an (equivalent) sphere which has the same sinking speed as the irregularly shaped particle. Other methods are based on other fineness parameters such as the projection area of the particle, its volume, or the interference it caused in an electrical field. By definition, the form factor is the ratio between two equivalent diameters which were determined on the same particle with different measuring methods. With the aid of this program you can convert results obtained with the "analysette 22" such that they correspond to the equivalent diameter of the „strange“ method. For the conversion, the program forms a function whose major component consists of quotients of corresponding particle sizes. XLaser and XSieving are examples of diameters which are determined with the laser particle sizer "analysette 22" and by sieving. For the complete function, a quotient is calculated step by step from the different diameters. The "new" diameter is then obtained from XSieving = f *XLaser.


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8.7.2 Creating Revalidation Function

We start with the two cumulative result curves where the cumulative curve (2) is the result from sieving and the other one is the original „analysette 22“ result (Laser result file 215std28.dat, sieving result file 221std28.siv). Both curves are reproduced by means of a cubic spline function with double precision and an error limit of 0.0000001. From these we get two particle sizes XLaser (1) and Xsieving (2) for each percentage volume on the y-axis (starting at 0.1% in 0.1 % steps).

In the above picture (called revalidation function) both particle sizes (x-axis: Laser Sizes „analysette 22“; y-axis: sizes from different measuring method [Rev.Sizes], e.g. sieving) are shown.


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8.7.2.1 Revalidation Function File The revalidation function is stored as ASCII-file with the following contents: Revalidation File C:\A22WIN\FRITSCH\OUTPUT.DAT A:\221STD28.SIB 1 11.9796 .1 2 14.46748 .1753347 3 16.5174 .295096 4 18.13146 .46464 5 19.64834 .6825767 10 25.27047 2.268322 11 26.26962 2.647999 12 27.12046 3.040183 13 27.89738 3.44286 14 28.67431 3.854035 15 29.45124 4.271823 228 78.8947 53.84134 229 79.04187 54.00159 230 79.18905 54.16185 240 80.66077 55.76435 241 80.80795 55.92461 242 80.95512 56.08486 243 81.10229 56.24511 757 146.5115 124.7354 758 146.6662 124.8912 759 146.8209 125.0469 760 146.9756 125.2026 761 147.1304 125.3583 999 365.6213 218.7117 1000 -1 219.9055


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This file reads as follows: 0.1% laser size 11.9796 µm sieve size 0.1 µm 1.0% laser size 25.27047 µm sieve size 2.268322 µm 22.8% laser size 78.8947 µm sieve size 53.84134 µm 75.7% laser size 146.5115 µm sieve size 124.7354 µm 100% laser size NO VALUE sieve size 219.9055 µm Later we can calculate nearly 1000 form factors f = XSieving / XLaser from this revalidation function file. This enables us to fit laser results to a measuring method the revalidation function is based on. It is evident, that this revalidation only functions, if the measured result was received with the same material the revalidation function was created.

Note: 1. Normally we do have a 100% value for the laser

measurement, but because of rounding errors in the spline functions there is an uncertainty of 0.5%.

2. If the sieving result would start with 6% at 45 µm all values for sieving starting with 0.1% up to 5.9% will be set to –1. Even if the laser measurement starts with 0% at 0.1 µm all values up to 5.9% will not be considered. There is NO form factor between both result curves in this range.

3. The same thing happens if the cumulated curves stop before 100%. This normally happens if there is oversize for the last sieve. There also will be NO form factor between both result curves in this range.

8.7.3 Revalidation of Measurements In order to conduct a revalidation you need a revalidation function. You have either just created one or you can call a prepared function from your memory.

8.7.3.1 Selecting result In the „Revalidation of Results“, the program asks you to select a result. You can either select the actual one right away or select a stored result. Thereafter you can view the selection again - before the conversion.

8.7.3.2 Selecting revalidation function In the window you have can open a revalidation function file. After selecting the revalidation function there is an „Info Revalidation Function...“:


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In some circumstances the next message „Calculating Revalidation Hint...“:

shows a warning, that the size range of the result to be revalidated is larger than the size valid size range of the revalidation function.

Note: 1. The cumulative value for the a22 result for 10.15956 µm was

.040632%. The revalidation funtion started with 0.1% so the first value of a22 result was not considered.

2. The second value for the a22 result, 0.0981% at 11.92746 µm also was not considered.

3. The first value at 0.1% for a22 measurement was 11.9796 µm at 0.1%.

4. This resolution problem could be resolved, if we would not make 0.1% steps during creation of revalidation function, but 0.01% steps. The drawback is, that not 1000 values, but 10000 values would be stored to the harddisk with each revalidation function.

5. The resolution of 0.1% steps normally is sufficient. 6. The last valid value for a-22 at 99.9% was 365.6213 µm, last

valid value for sieving at 99.9% was 218.7117 µm.

8.7.3.3 Revalidation At last click on the pushbutton Revalidation and the recalculated result is displayed as the second one in the graphics. 1. First the Revalidation function is reproduced by means of a

cubic spline function with double precision and an error limit of 0.0000001.

2. Next all particle sizes from the „analysette 22“ result inside the valid range of the revalidation function from 11.9796 – 365.6213 µm are recalculated by means of the form factors stored in the now splined revalidation function.

XRevalidation = (Xoriginal sieving / Xoriginal laser) * XLaser >----- from Revlidation file -< >--- Measurement ---<

3. At last the revalidated curve is reproduced by means of a cubic spline and divided in logarithmical equally spaced size classes. This is the last spline function during the long process.

Values outside the valid range are NOT considered.


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The left curve is the revalidated result, the right one is the original a22 measurement result curve.

In the picture above one result curve is the original sieving result, the other result curve is the revalidated a22 measurement. The correlation between the original and the revalidated curve is significant and remarkable. After a click on Ok you can then assign a name for the new result and store it. As described at the beginning of this section, you can view the converted result on your monitor just like an original measurement result.

8.8 Recalculation A new particle size distribution is calculated based on the last measurement data, which always remains in computer memory. The measurement data is updated after measurement or after loading a stored result file.


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9 Main Menu Special

9.1 Winkler Three Phase Diagram This procedure is needed for special ceramics, gypsum and cement applications. There are three percentage axes ranging to predefined sizes. The values are presented in the grid relative to the opposite percentage volumes. For a long time now, the Winkler triangle is used in ordinary ceramics for assessing the usability. Also, similar to the T-Q-F diagram, the fractions < 2 µm, 2 to 20 µm and > 20 µm are entered as the measuring point in a corn size triangle. The data given by Winkler in 1954 was inspected by Schmidt [35] in 1979 on the basis of certain measurements and adapted to the new requirements of brick production. Besides, Schmidt specifies closer corn limit areas than Winkler, in which more than 80 % of the examined masses move. While using the Winkler triangle, the values specified by Schmidt should be used in future. The Winkler triangle alone cannot be referred to for assessing the usability, because only the corn structure of the mass is taken into account here and not the mineral composition. The following example gives a clear explanation. E.g., quartz sand can be ground in different ways and subsequently, the corn size fractions mixed such that a “roofing tile mass” is obtained on the basis of the assessment by the Winkler triangle. However, this “mass” will not contain any clay minerals and as a result, the strength of the roofing tile will not be sufficient. Since the minerals mainly exist in corn fractions and e.g. rough inclusions have to be avoided in roofing tiles, the granulometric data must also be taken into account for assessing the usability. Because of a statistical analysis, two undersize curves are obtained, whereby maximum bending tensile strength of the masses was detected on one hand and maximum compressive strength on the other. Roofing tile masses are located near the undersize curve for maximum bending tensile strength and lining brick masses near the undersize curve for maximum compressive strength.


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9.2 Tromp Calculation In a closed grinding circuit, the grinding process is strongly influenced by the separation. For the judgement of the grinding process it is necessary to judge in addition to the performance of the mill also the performance of the separator. The duty of the separator is to divide a material stream which has a certain grain size distribution into two streams. One stream should contain mainly coarse particles and the other one fine particles. The judgement of the quality of this separating action can be done by means of the three separator criteria: Circulating load, separator effielency and Tromp - value. For more information see appendix (this instruction is only availbable in english).

9.3 Mass Balance This function enables the assessment of a measurement of a mixture of two samples mixed at any desired ratio. For checking the efficiency, ISO 13320 also proposes the measurement of mixtures. If you mix two samples at different locations in a 50:50 ratio (absolutely same density of both the samples is required), the mixture more or less reflects the particle size distribution. This programme item supports in the process of assessment of the measurement. The theoretical mass centre of gravity, the measured mass centre of gravity and the deviation of the measured values from the theoretical mass centre of gravity in percentage form is calculated.

9.4 Chart In the programme, all selected curves, which have been loaded in “Load comparison curve", can be displayed as 3d diagrams. You can rotate the diagram by holding down the Ctrl key and clicking on the diagram with the mouse.


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10 Main Menu Configuration

10.1 Set Configuration In the Set Configuration window please choose your configuration and the connected RS232 port to communicate with the measuring unit. Also choose this window to change i.e. from dry to wet dispersing unit. The Settings frame of the main screen in that case changes from Settings Compact Dry to Settings Compact Wet and vice versa.

Only for COMFORT dry versions: You can enable an external trigger, which receives a definite log via the RS232 interface, evaluates and starts the measurement automatically. With this programme item, external sources such as a PLC control system can carry out an online measurement. After the measurement, certain values are available in the analysette 22 record, which can be read and evaluated by the connected PLC in a fully automatic manner.

Attention: The record must be adapted individually.

11 Main Menu Help

11.1 Service (only „COMPACT“) Two cards of the Service window give you an overview about the actual status of your measuring unit. In the third card you can carry out manual settings.

By selecting the RS232 Communication card you can see the currently performed measuring points at all times. The middle frame shows the received protocoll sent by the measuring unit (each 0,5 seconds) and the right frame shows the sent protocol from the program. This is only for your information.


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The card RS232 Protocoll contains a bit-based decoded information about the state of the measuring unit. Activated options show a green led, not activated options remain red. If i.e. in the Byte 3 frame the status led for Valve Pressure Air remains red during measurement either the valve is broken or you have to look at Byte 4 frame Pressure switch. If this led also is red there is no air pressure to the unit and you have to check your local installation. This is only for your information. In the Manual Settings card you can carry out possible manual

settings provided by the system. Above all here you have the possibility to adjust the feed rate and quantity of the analysette 22 dry dispersing unit feeder to your sample. After a click on Start the dust exhaust is switched on and the feeder starts working. You can set a suitable feed rate and quantity until your Sample Dilution bar shows the desired beam obscuration value. The cards two and three look a little different in design, but the functions are nearly the same.


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11.2 Printing system settings Here, you can print out the complete contents of the Registry entries of the a-22 programme; this information is important for service technicians or for telephonic error diagnosis.

11.3 Install sensor calibration (only COMFORT and ECONOMY) On the CD-ROM, you will find a directory with data for individual sensor calibration in the sub-directory to the a-22 installation programme. All the installed programme versions automatically receive a universally applicable sensor calibration. If this universal calibration is not sufficient (because e.g. the comparability of the devices must be adjusted among themselves and/or improved), an individual sensor calibration file can be enabled by the CD-ROM. For this, you need to read the number registered on the sensor and enable the file with the corresponding number of the CD-ROM. You will be asked twice, if you really want to continue. Attention: Selecting an incorrect sensor calibration file will yield incorrect measuring results.

11.4 About In this item, you will find a version history of the programme. All the errors and their elimination are listed here. If you want to know the current version of your programme, you will have to scroll down completely in the text box. The 32Bit programme version starts with Version 2.0; versions with in-built support for NanoTec and MicroTec begin with Version 3.0.


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12 Appendix

12.1 Tromp Calculation The circulation load is the ratio separator feed to separator fine fraction. The separator efficiency is applied to a determined grain size. lt shows the portion of the separator feed smaller this grain size, which goes into the fine fraction. The Tromp-value resp. Tromp-curve shows for each grain size of the separator feed to which portion the particles of this size are in the fine fraction or in the coarse fraction. The circulating load, the efficiency and the Tromp-value can be calculated. To get the basic figures for these calculations a separator test must be carried as follows: • Recording of separator data (e.g. Adjustment of separator,

mechanical condition etc.) • Sieve analyses of the samples • Measuring of quantity (either feed, coarse fraction or fine

fraction) • Evaluation of test i.e. calculation of circulating load, efficiency

and Tromp-values by means of the particle size analyses and the quantity. The results can then be compared with ideal values or other grinding installations of the same type and if necessary the separator can be adjusted accordingly. The optimum solution for every single step case must be found in several steps and the evaluation of each single step enables to estimate the direction and size of the next one.

12.1.1 Introduction The two main parts af a closed grinding circuit are the mill and the air separator (slurry classifier in case of slurry mill). The mill grinds the material to a certain particle size. The separator takes the discharge from the mill and selects the portion that will give the right quality (fine fraction). The rejected portion (coarse fraction) is sent back to the mill and reground. The separation itself has an essential influence on the grinding performance in the tube mill, and therefore it is necessary to be able to judge the functioning of the separator. The separator functioning is mainly infiuenced by: Separator adjustment and technical condition of separator, e.g. speed of distributing plate, number and position of Spin rotor blades, wear on fan and Spin rotor, air leakages etc. Separator feed. e.g. feed rate, particle size distribution, moisture content, density etc. Separating air, e.g. density, viscosity etc. The characterizing data and curves for the judgement and comparison of the functioning of the separators as well as the test procedure are explained in the following chapters.


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12.1.2 General Calculating Methods 12.1.2.1 Definition of a closed grinding circuit The operation of a closed grinding circuit is defined by the quantity and fineness of material entering and leaving the mill and the separator. The following symbols are used in this instruction manual:

Description Mass flow (weight) t/h

Fineness % passing

a sieve

Spec. Sur-face cm2/g

Blaine

Mill feed M - -

Separator feed = Mill discharge

A a BA

Fine fraction (Product)

F f BF

Coarse fraction (Tailings)

R r BR

12.1.2.2 Basic equations (Mass balance) The weight of the material fed to the separator is equal to the sum of the weight of the fine fraction and the coarse fraction.

RFA +=

The dimension is (t/h). The mass balance can also be made for a portion of the separator feed which is limited by a defined particle size x µm. This quantity is divided up into the fine fraction which contains f % of particles finer x µm and into the coarse fraction which contains r % of particles finer x µm. Hence lt follows the equation:

rRfFaA ∗+∗=∗


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The dimension again is (t/h).The values for a, f and r can be found by means of the particle size analysis. The mass balance can also be made for a fraction of the separator feed which is limited by two defined particle sizes x1 µm and x2 µm The separater feed contains ∆a % of particles which are between x1 and x2 µm in diameter. This quantity is divided up into the fine fraction which contains ∆f % of particles between x1 and x2 µm and into the coarse fraction which contains ∆r % of parlicles between x1 and x2 µm. Hence it follows the equation:

rRfFaA ∆∗+∆∗=∆∗

With the dimension (t/h). The values for ∆a, ∆f and ∆r can be found by means of the particle size analysis.

12.1.2.3 Circulating load The relation between the weight of the separator feed and the fine fraction is described as the circulating load u.

FAu =

The minimum value for u is 1 (if the complete separator feed gets into the fine fraction, i.e. if F = A), the maximum value for u is ∞ (if no material gets into the fine fraction, i.e. if F = 0). Both extreme values (u = 1 and u = ∞) are undesired for a proper separator operation. A very low u-value means that the change in the separator is only small, the particle size distribution in the fine fraction is very similar to the particle size distribution in the separator feed. A very high u-value means that the amount of the fine fraction is very small, and a large amount of tailings is recirculated. Possible reasons for high values are e.g. insufficiently prepared feed to the separator (poor mill performance), inproper functioning of the separator, high fineness of the finished product etc. The value of the circulating load is dependent on various factors, e.g. dimensioning of mill , product fineness etc., but as a guide the following values can be given:

• Cement mill small mill u = 2.0 to 3.0 large mill u = 1.5 to 2.0

• Raw mill u = 2.0 to 2.6

If a cement mill, designed for grinding normal cement, will be used for grinding high fineness cement then the circulating load will increase considerably. In the USA some cement mills are operated with a high circulating load of 5 — 6 (short mill).


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To calculate the circulating load u by means of above equation it is necessary to know the weight of the feed A to the separator and the weight of the fine fraction F. But in many cases only the weight of the fine fraction is known. If this is the case the circulating load must be calculated by means of the fineness of the separator feed, the coarse fraction and the fine fraction.

( )

rarfu

rruauruauf

rFFAa

FAf

FARRFA

rFRa

FA

FrRaAf

rRfFaA

−−

=

+∗−∗=∗−−∗=

∗−

−∗=

−=+=

∗−∗=∗−∗

=

∗+∗=∗

1

lt is necessary to take the u-value calculated by the fineness carefully, because even small mistakes in the particle size analysis values a, f. r influence the result considerably. This is most remarkable if the values a, f. r are low. In the USA the circulating load is defined in a different way, and the relation between uUSA and uEurope is as follows:

11

1

+=

−=

−=−

=

+=

=

USAEurope

EuropeUSA

USA

USA

uuuu

FA

FFAu

RFAFRu

12.1.2.4 Separator efficiency The efficiency of a separator can be calculated as follows:

100

1001

100

∗∗

=

∗∗=

=

∗∗∗

=

uafaf

u

FAu

aAfF

η

η

η


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From above the separator efficiency is the percentage of a defined fraction (0 - x µm) which gets from the separator feed into the fine fraction, or to express it in another way, it is the probability of a particle having a defined size to get into the fine fraction.

Remark: In some literature also the values ,,gain of material“ are used and the corresponding formulae are

afV

VFAu

AR

AFVV

VVARV

AFV

F

F

RF

FR

R

F

∗=

==

=+=+

=+

∗=

∗=

η

100

1100

100

100

100

12.1.2.5 Tromp value, Tromp curve The Information given by the η-value is not detailed enough because the defined fractions 0-x µm or <x µm (given by the a, f, r values) are wide. For a more detailed information the Tromp values (t) are used. The Tromp values can be calculated either for the fine fraction (tF) or for the coarse fraction (tR), and the used formulae are similar to the formula above. Tromp value tF

100

100

∗∗∆

∆=

∗∆∗∆∗

=

uaft

aAfFt

F

F


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The Tromp curve resulting from the Tromp-value tF shows for each individual particle size of the separator feed the percentage which gets into the fine fraction. Tromp value tR

( )

10011

1001

100

100

100

∗

−∗

∆∆

=

∗

∆∆

∗−∆∆

=

∗∆∗∆∗

−∆∗∆∗

=

∗∆∗

∆∗−=

∗∆∗∆∗

=

uart

ar

uart

raA

FraA

At

aArFAt

aArRt

R

R

R

R

R

The Tromp curve resulting from the Tromp value tR shows for each individual particle size of the separator feed the percentage which gets into the coarse fraction.

12.1.2.6 Characteristic data of the tromp curve The following formulae are based on the Tromp curve tR, but of course they are also valid tor the Tromp curve tF.


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12.1.2.6.1 Cut point (CTP) Cut point is defined as the limiting partlcle size or limiting particle diameter for which the probability to get into the fine fraction and the probability to get into the coarse fraction are equal. The majority of the particles coarser than dt gets into the coarse fraction, the majority of the particles finer than dt gets into the fine fraction.

Remark: If a separation is very unsharp already 50% of the very fine particles are in the coarse fraction. In such cases it is impossible to state the cut point.

12.1.2.6.2 Sharpness of separation For a good separator a sharp separation is desirable, that means that the coarse particles being over CTP should be cut off sharply, their amount in the fine fraction should be as low as possible. The fine particles below CTP should, on the contrary, get all into the fine fraction. An ideal (not realistic) sharpness of separation is shown in the following figure:


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Ideal separation: All particles <CTP go into fine fraction All particles > CTP go into coar-se fraction

For real conditions the following two figures above show examples of a sharp and a not sharp separation.

12.1.2.7 Additional criteria for the slurry classifiers The methods for the judgment of separators as presented in the previous chapters are also valid for the slurry classifiers. For the judgment of slurry classifiers mainly the two criteria efficiency η and final classifying effect t<x/t>x are used. The final classifying effect is normally not used for the judyment of air separators and therefore explained in this chapter. As basis for the calculation the values a and f for two screen openings are necessary. In most cases the sizes 200 µm and 90 µm are chosen, and the following values must be calculated:

100

100,100

100

100,100

*

*

*200

*200

*90

*90

200

200

90

90

20090

2000900

∗∗

=

∗∗

=∗∗

=

∗∗

=

∗∗

=∗∗

=

>

∞−∞−

<

−−

uaft

generallyorua

ftua

ft

andua

ft

generallyorua

ftua

ft

x

xf

ff

x

xf

ff

x

x

a and f are % passing (90 and 200 µm sieve) a* and f* are % residue (90 and 200 µm sieve) From these 4 values the final classifying effect is to be calculated (from 90 µm and 200 µm)

effecttionclassificafinaltt c

x

x =>

<


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From this formula the final classifying effect is the relation between (a) the probability of the particles being finer than x µm („desired“ particles) to get into the fine fraction and (b) the probability of the particles being coarser than µm („undesired“ particles) to get into the fine fraction.

*

*

*

*

*

* ,x

x

x

x

x

x

xx

xx

x

x

x

x

x

x

fa

af

tt

ufauaf

uafua

f

tt

∗=∗∗∗∗

=

∗

∗=

>

<

>

<

As can be seen from the formula above the final classifying effect can be calculated without knowing the value of the circulating load u (for calculation of efficiency or t-values the knowledge of u is necessary). lt characterizes the total change of the particle size distribution in the classifier. A higher value of the final classifying effect means a better separation. To characterize a classifier it is recommendable to calculate, additionally to the value of the final classifying effect t<x / t>x also the value of ηx (= t<x).

12.1.3 Test Procedure 12.1.3.1 Target of test and conditions The result of the separation is characterized by the weight and fineness of the coarse fraction and of the fine fraction. These values and the factors which are influencing the functioning of the separator (See introduction, e.g. separator adjustment, feed, separating air etc.) must be determined during the test. lt is of most importance that the operation of the mill is stable during the test. Since the separation is strongly influenced by the weight and the particle size distribution of the separator feed it is necessary to keep the separator feed constant during the test. That means the fresh feed to the mill must be controlled either by the power consumption of the bucket elevator or if a scale is installed in the return line (coarse fraction) of the separator by this scale. If there is no automatic control System installed the fresh feed to the mill must be regulated in such a way that the power consumption of the bucket elevator is constant.

12.1.3.2 Sampling and duration of test The most accurate determination of the amounts A, F and R can be done if two of the values can be measured (e.g. scales), and the third value is calculated by means of the first equation. In this case, the duration of the test is in the region of 10 minutes, and the samples should be taken in intervais of 1 to 2 minutes.


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lt is very often that only the fresh feed M to the mill can be measured. lt is assumed that the weight of the fine fraction F is equal to the mill feed M. The weight of the separator feed A and the coarse fraction R can only be determined by means of the circulating load, and the circulating load can be calculated by means of the sieve analysis of A, F and R. To get an accurate value of the circulating load it is necessary to extend the duration of the test to 3 - 6 hours, and depending on the duration of the test 10 to 20 samples (in equal intervals) should be taken on each sampling point.

Then the individual samples of each sampling point can be homogenized to one sample (i.e. sample for A, F and R). lt is recommended to check for each sample the percentage passing a medium sieve size (e.g. 30 µm) before homogenizing. Samples with e~treme values should be eliminated (e.g. due to unstable operation of the mill etc.). If two separators are operated in parallel it is rather seldom that the feed rate to both separators is the same. Therefore the two units cannot be treated as one unit and it is recommended to carry out the performance test for each individual separator.

12.1.3.3 Sieve analysis The sieve analysis for the three samples (A, F and R) has to be performed. In many plants it is only possible to carry out dry sieving tests where the lower limit of the measureable particle size is 30 µm. For an accurate separator judgment the particle size distribution for particles smaller than 30 µm must also be known. For the particle size analysis smaller 30 µm the wet sieving method is applied. A more advanced method would be the application of a laser beam analyzer to determine the particle size distribution.


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12.1.3.4 Evaluation of test results The further procedure is now according to chapter 2 „general calculating methods“ and is as follows: Calculation of: • Mass balance • Circulating load • Efficiency incl. graph • Tromp values incl. graph • Cut point and sharpness of separation The report on hand explains the basic methods how to carry out a separator performance test. These methods enable to define and evaluate the main operational characteristics of a closed grinding circuit, to compare them with other cases and with ideal values. The Optimum solution for every single case must be found in several steps, the evaluation of results of each single step enables to estimate the direction and the size of the next one. No universal method is available enabling to find the ideal solution at the writing desk without experiments.

12.1.3.5 Practical Calculation and Example Data of separator and mill Plant: A Date of test: 30.7.1981

Separator: Make, Type: Heyd, mechanical air separator Diameter: 4.2 [m] Motor power: 50 [kW], 500 [V] 975 [min-1] Speed fan and distribution plate: 210 [min-1] Fineness Regulation: Spin rotor, number and position of blades Year of Installation: 1960 Mill: Cement mill, no. 1 Type: Two compartment, end discharge Diameter, length: 2.6 m / 10 m Motor power: 650 kW Year of Installation: 1960 Mill feed: Weigh feeder Control: By power consumption bucketelevator


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During the test a Portland cement PZ 275 has been produced consisting of 96 % clinker and 4 % gypsum. The duration of the test was 5 hours. me measured quantity of the miii feed and the power consumption of the separator and the bucket elevator are shown in the table below.

Time Mill feed Power consumption Counter [t/h] M [t/h] Bucket ele-

vator [kW] Separator

[kW] 08.15 7642.7 -- 6.5 40 09.15 7666.7 24 6.0 38 10.15 7690.9 24.2 6.2 41 11.15 7715.0 24.1 6.5 42 12.15 7738.9 23.9 6.3 40 13.15 7763.2 24.3 6.2 39

120.5 24.1 6.3 40

Mill feed total: 120.5 t; hence it follows M = 120.5 / 5 = 24.1 t/h

Sampling and size analysis Sampling points: The sampling points are shown in the

figure above, marked * Number of samples: 16 sampies per sampling point have been taken Sieve analysis: Particles <30 µm — wet sieving Particies >30 µm — dry sieving


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The particie size distribution of the separator feed, coarse fractionl and fine fraction are listed in the table below and the corresponding graphs are shown next.

Particle Size [µm]

Separator feed a [%]

Fine Fraction f [%]

Coarse Fraction r [%]

2 3.5 5.5 2.0 4 7.8 10.8 4.5 8 12.5 17.9 6.1

15 24.6 30.3 17.9 20 31.5 43.0 18.1 30 38.2 53.6 20.1 40 49.3 72.1 22.5 60 65.2 86.0 36.5 90 77.1 97.1 58.4

120 89.5 99.6 77.5 150 95.5 100.0 90.0 200 97.2 100.0 93.8

Sum 591.9 t715.9 1447.4

Remark: The values for a, f and r are % passing.

Blaine values: • separator feed BA = 2090 [cm2/g] • coarse fraction BR = 1120 [cm2/g] • fine fraction BF = 2810 [cm2/g]

Evaluation Circulating load u Since only the weight of the miii feed M was measured the circulating load must be calculated by means of the fineness a, f and r.

rarfu

−−

=

The circulating load for each individual particle size (e.g. 2, 4, 8 µm etc.) can now be calculated and then the mean value of the circulating load u can be determined. A simpler form is to calculate the sum of a, f and r as shown in the table above and then to calculate u by means of the formula:

86.15.4479.5915.4479.715

=−−

=

−

−=∑ ∑∑ ∑

u

u

rarf

u


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Separator feed A The mill feed M is known and is equal to the fine fraction F. The separetor feed A can now be calculeted by means of equation

]/[8.441.2486.1htA

AuMuFA

FAu

=

∗=∗=∗=

=

Coarse fraction R The weight of the coarse fraction R can be calculated according to equation

]/[7.201.248.44htR

RFARRFA

=

−=−=+=

Efficiency The efficiency is calculated as

100∗∗

=uafη

The calculated values are listed in the table below and the corresponding graph is shown later (it is to state that for the calculation the mean value for u = 1.86 has been used). Tromp Value The Tromp-value is calculated as

10011 ∗

−∗

∆∆

=ua

rtR

The calculated values are listed in the table below and the corresponding graph is shown later.

Cut point The cut point particle size is CTP = 55 µm

Sharpness of separation The Sharpness of separation is calculated as

35.147

5.63

35

65 ===ddk


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Conclusion The evaluation of the separator performance test shows that the separator efficiency is medium, but the sharpness of the separation can be considered as good.

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Instruction Manual FRITSCH team/fritsch/Fritsch data/A22... · 2007-03-02 · edition 04/2002 index 001 programme manual "analysette 22“ fritsch zerkleinern partikelmessen teilen