Laser Particle Sizer Analysette 22 NanoTec / MicroTec / XT
Contents
1. Movement of the measuring cell is initiated according to the setting of the measuring range e g if the smallest measuring range is selected the measuring cell moves to the upper stop When the largest measuring range is set it moves to the lower end point Select Background Meas urement and press Start Measurement The measuring cell moves Instructions for selecting the program and adjusting the settings can be found in the software manual analysette 22 NanoTec MicroTec Seite 29 _ FRITSCH 4 2 Selection of the Liquids The measuring liquid in the device supply and measuring unit only comes into contact with materials that are largely chemically resistant Certain organic liquids or saturated inorganic salt solutions may be used briefly without damaging the device The measuring fluid comes into contact with stainless steel glass Tef lon Viton FPM and FKM and PA60 Nylon The standard connection hoses are made of Viton For measurement of samples not compatible with water an appropriate liquid can be selected from the following list e Mono di or tryhydric alcohols except for methanol e g ethyl alcohol isopropyl alcohol glycol or glycerine e Benzines petroleum ether test benzine kerosine e Mineral and organic oils such as petroleum and soy oil nut oil olive oil e Cyclic aromatic compounds ring hydrocarbons toluene only briefly rinse out after the measurement e Alkanes e Hexane hepta2. Transport safety device ccccccsseeeeceeeeeeceeeeaeeseeeeeeueeeseesseaeeeeseesaaees 23 Accessory CaSC ccccccccsssseececcceeceaeesseeceeeeeesaeeeeeeeeeeseauaaseeeeeeseessaeeaeees 24 Electrical Connection 25 Electrical FUSes nnnnennnnnnnn nennen nennen nennen fii 25 Stability of the Power Supply cccccccccceceeseeeeeeeeeeeeeseeeeeeessaeaeeeeeeeneaaaees 25 Adapting to the Power Network 25 BONNECIONE i eat eee encens ee 26 Preparing the Computer AUS 27 Data Connections 27 Switching on the Device 22uuusssssnnnnnnnnnnnennnnnnnnnnnnennnnnnnnnnnnnnnnnnnen 27 Checking the Communication 27 Function Check 5 28 Liquid Dispersing UN it 1ccccsssccsnsccenncsenensneensensecensssenenssnnnenes 29 Installing Hose Connections 29 Selection of the Liquids 2 30 Cleaning RS 31 Cleaning the Device i 31 Cleaning the Measuring Cell 31 Service Position 31 Preparation 2 022422002400000 nnnennnnnnnnnnnnnn neuen nennen nennen ME 31 Preparation se A 32 Disassembling the Measuring Cell 33 Cleaning EEE 35 Cleaning the Window 35 Loose Window TS 35 Flange Window aeea 37 Installing the Measuring Cell 38 analysette 22 NanoTec MicroTec als FRITSCH Table of Contents Page 4 4 Filling the Measuring Cell 39 4 4 1 Liguid Dispersing UNI nun ee 39 4 4 2 Filling t
3. ss 3 8 Preparing the Computer See the software operating manual 3 9 Data Connections Connect the 9 pin connector on the rear of the device to the Com1 or Com2 port of your computer with the included RS232 cable After checking all connections the plug of the power strip may be con nected to the power network as the final step 3 10 Switching on the Device Switch the device on with the main power switch on the front lower right of the device The internal control then performs an initialisation routine Any measuring cells positioned within the beam path of the laser are moved to the park position and the entire measuring cell is positioned at its reference point All filter wheels for transmitting or blocking the laser beams are moved to the reference point The initialisation routine may last a few seconds 3 11 Checking the Communication After you have established the serial connection between the measuring device and the computer you must check the communication To do this open the associated program analysette 22 for Windows and select the item Set System Configuration in the Configuration menu In the dialog Set System Configuration select your version of the analysette 22 In the dialog that appears next to the lower right se lect the RS232 port of your computer to which you have connected the cable to the measuring device If you do not receive any communication in the following steps this is usual
4. the dry left side or liquid dispersion unit right side are located underneath the stainless steel covers Combination versions contain both the liquid and dry dis persion units Depending on the model the measuring cells for measurement in sus pension or for measurement of dry solids with a nozzle arrangement for dispersing the sample and a suction device are installed separately or in the combination devices together on separate guide rails Switching of the measuring cell and therefore switching of the dispersion type takes place automatically The multi element detector with 80 individual elements and the associ ated preamplifier are situated in a protected housing on the top end of the optical bench The measuring device also contains the drive system for sliding the measuring cell or the nozzle arrangement to the two end positions analysette 22 NanoTec MicroTec Seite 3 FRITSCH se The liquid dispersion unit has an approximately 300 ml stainless steel container to hold the samples which is designed as an ultra sound bath The ultra sound output is approximately 70 Watts at 36 KHz and can be switched on or off as desired An optical fill level sensor monitors the liquid level in the ultra sound bath A centrifugal pump with flange connection beneath the ultra sound bath pumps the suspension through the entire measuring circuit Due to the high flow rate of the suspension even larger particles with high density
5. 2 4 Fraunhofer Mie Theory The energy distribution measured in radially positioned sensor elements is evaluated and used to calculate the particle size distribution In the analysette 22 this calculation can be performed according to either the Fraunhofer or the Mie theory The Fraunhofer theory named after German physicist Josef von Fraun hofer and based on diffraction at the particle edges applies only to fully opaque particles and small diffraction angle For particle sizes in the range of the wavelength and below the Fraun hofer assumption of a constant extinction coefficient no longer applies To account for the optical particle properties the analysette 22 makes use of the Mie theory named after German physicist Gustav Mie It describes the radiation in and around a ho mogenous spherical particle in a homogenous non absorbing medium for all spatial dimensions The particles can be transparent or completely opaque The Mie theory states that light diffraction is a resonance phenomenon If a light beam with a specific wavelength encounters a particle the par ticle performs electromagnetic oscillations in the same frequency as the stimulating light regardless of the relationship of the light wavelength to the particle diameter and the refractive index of the particles and me dium The particle is tuned to the reception of specific wavelengths and reemits the energy like a relay station within a defined spatial angle dis tributi
6. Small quantity liquid dispersing unit 22 6300 00 Liquid mini vessel 22 2910 00 Software for particle shape recognition analysette 22 NanoTec MicroTec Seite 14 2 Operating Safety 2 1 General Safety Instructions Read the operating instructions carefully The device may only be used for the purpose described in Section 1 3 Brief Description of the Device Use only original accessories Failure to adhere to this may jeopardize the protection of the machine All operators must be familiar with the contents of the operat ing instructions For this purpose always keep the operating instructions within easy reach Do not remove the instruction labels Care to prevent accidents must be taken during all work Independent conversions of the device negate the conformity with European directives declared by Fritsch and void the warranty When measuring oxidisable substances such as metals or ganic substances wood coal plastics etc the risk of spon taneous combustion dust explosion exists if the fine portion exceeds a certain percentage For this reason special safety measures e g measurement in suspension must be taken and the work must be supervised by a specialist In addition the MAK values of the pertinent safety regulations must be observed and sufficient ventilation must be ensured or the device must be operated under a hood The device is not designed with explosion protection and is not suitable for mea
7. and calculation of the particle size distribution can be satisified for every multiple meas urement by simply inputing the desired number of measurement chan nels yourself After specifying an upper and lower limit the measurement is distributed among up to ten adjacent measurement areas the sample is introduced only once before the start of the test The result of a measurement performed in this way is characterised by a resolution in up to 570 measurement channels In this way wide and highly inhomogeneous samples distributed over the entire measuring range can be measured precisely The high resolution displays fine de tails that remain hidden to other measurement methods This extreme resolution is particularly interesting in the finest particle range during multiple measurement within narrow limits between 0 01 um and 60 um the sample can be measured for instance in 155 true measurement channels or more and calculated 1 3 3 1 Liquid Dispersing Unit The liquid dispersing module offers fully automatic pumping of the sus pension Through the use of a motor driven 4 2 way valve the pumping takes place without dead space With the integrated ultra sound bath approx 500 ml volume 50 Watts output even difficult to disperse samples can be measured without additional instrument work The digi tal ultra sound generator keeps the specified output optimal and con stant The powerful centrifugal pump with 100 Watt output also pump
8. are measured correctly The centrifugal principle also handles mechani cally sensitive samples as gently as possible The supply and discharge of the suspension and the automatic rinsing and filling are performed automatically by electro mechanical control valves and ball valves Do not use any highly flammable burnable liquids such as alco hols ketones benzines etc Do not allow any liquids to flow into the device Parts coming into contact with liquid are made of PA66 Nylon Vi ton Teflon and stainless steel analysette 22 NanoTec MicroTec Seite 4 FRITSCH ss 1 3 2 Function Analysis devices for determination of particle size distribution with laser deflection make use of the physical principle of the scattering of electro magnetic waves Particles in a parallel laser beam deflect the light at a defined angle that depends on the diameter of the particles A convergent lens focusses the scattered light in a ring on a sensor mounted in the focal plane of the lens Undiffracted light always converges at the focal point on the optical axis With the help of complex mathematics the particle size distribution of the particles diffracting the light can be calculated from the intensity dis tribution of the diffracted light As a result one obtains a particle diame ter from the laser diffraction that is equivalent to that of a ball with identi cal diffracted light distribution Average volume diameters are measured a
9. cell has angled surfaces on the side facing the detector so that light can leave the measuring cell even with large diffraction an gles The window on this side is firmly attached to the metal of the measuring cell The opposite window is loosely inserted into a slot in the measuring cell and can be removed for cleaning N conventional sensor for scattered light CAS sample back scattered light Normal measurement using laser 1 Illumination from back side using laser 2 4 3 2 1 Service Position In the Setup program under NanoTec MicroTec Control Window select the item Service Position The measuring cell is then moved to the opening area of the doors and the measuring cell is swivelled to the outside so that it is located outside the device This prevents any liquid used during cleaning from flowing into the device 4 3 2 2 Preparation Lay out the following e Tool for cell disassembly e Measuring cell storage tool analysette 22 NanoTec MicroTec Seite 31 _ FRITSCH Assemble the tool for disassembly of the measuring cell and place the cell storage tool in a handy location 4 3 2 3 Preparation In the Setup program under NanoTec MicroTec Control Window select the item Open 4 2 way valve to discharge The liquid in the sys tem then drains out analysette 22 NanoTec MicroTec Seite 32 _ FRITSCH 4 3 2 4 Disassembling the Measuring Cell Although the measuring cir
10. not be disabled or removed 2 4 1 Laser Emissions The laser emissions are not directly accessible because the laser is al ways blocked off by mechanical shutters after a properly completed measurement Sudden uncontrolled opening of the doors by the user also does not lead to a hazardous state because built in electronics to gether with the light sensitive silicon detector immediately detect an in crease in the residual light the measurement is halted and the laser is blocked by the mechanical shutters This state remains in effect until the doors are closed Then a new measurement cycle must be started with Start Measurement For this reason the analysette 22 NanoTec and MicroTec are classi fied as laser safety class 1 2 4 2 Pinching Danger Sudden uncontrolled opening of the doors by the user does not lead to a hazardous state because the built in electronics together with the light sensitive silicon detector detect an increase in the residual light and any movement by the measuring cell is immediately halted This state re mains in effect until the doors are closed Then a new measurement cycle must be started with Start Measurement 2 5 Danger Points Pinching danger at the cell holder when moving the measuring cell Do not operate the device with open doors Laser emitter with 7 mW output laser class 3b do not look into the beam Only operate the device in an open state while wearing safety goggles 2 6 Electrical S
11. on the interior of the measuring device as well as extreme humidity gt 85 e During operation of the device the ambient temperature may not exceed 35 C or fall below 10 C Storage between 1 C and 40 C is possible If it is expected that the temperature will fall below the permissible temperature range e g for a planned transport it is essential that the entire suspension circuit dispersion unit hoses and measuring cell in the measuring device first be rinsed thoroughly with ethanol and the liquid then completely removed e The device may not be switched on while cooled below the permissible temperature e After the device has been cooled to temperatures below 10 C you must wait for the device to warm to ambient tem perature before switching it on condensation in the device can lead to disruptions and damage analysette 22 NanoTec MicroTec Seite 22 _ FRITSCH FRITSCH E e You will be able to see characters and graphics on the screen A more easily if you select a setup location such that sunlight or artificial light do not fall directly on the image tubes Some times simply turning the monitor out of the light will help partial shadow increases the contrast and helps to prevent eye fatigue e Easy accessibility should be ensured during setup so the de vice can be operated without difficulty When opening the measuring device you must be able to reach the measuring cell easily e The setup locat
12. see chapter 4 3 2 3 Prepa ration 2 Put the liquid measuring cell to the park position please see chapter 4 3 2 5 Cleaning 3 Release the tubes from the liquid measuring cell and press the delivered plastic stoppers 3 on the tube openings Al gt 4 Release the screws 1 at the holding device 2 with the de livered tools 5 Putthe liquid measuring cell on the measuring cell holder 4 The tubes stay in the instrument i un u ns gi da analysette 22 NanoTec MicroTec Seite 55 _ FRITSCH 6 Then put the small volume dispersing unit on the hood space on the right hand side of the tower housing N Put the tubes with the measuring cell behind the tower hous ing on the left hand side of the instrument where the holes for the plug in of the measuring cell tubes are located 8 Now take the measuring cell of the small volume dispersing unit and fix it with the screws 1 to the holding device 2 9 Then plug the tubes which lead to the measuring cell of the small dispersing unit through the holes which are located at the side of the housing Please pay attention to the position control clips AN 10 The connection of the small volume dispersing unit is effected as described in chapter 6 2 1 Connection of the small vol ume dispersing unit analysette 22 NanoTec MicroTec Seite 56 FRITSCH se 7 Maintenance The analysette 22 NanoTe
13. the choke valve to set the pressure according to the material The optimal working range of the nozzle is between 3 and 4 bar For sensitive samples 1 bar may already be sufficient Do not set the compressed air to a lower value because the system does not function with lower pressures A pressure that is too high pro duces more water in the circuit which should be avoided Before setting the pressure you must pull on the black button on the front of the con troller analysette 22 NanoTec MicroTec Seite 44 FRITSCH sen FRITSCH ss 5 2 Cleaning the Measuring Cell Windows of the Dry Dispersing Unit Please check the Beam Alignment after about every 20 measurements to control the light intensities If you discover increasing channels in the fine area in the right section of the window toward Beam Alignment with a total level of more than 50 then the windows should be cleaned 5 2 1 Service Position In the Setup program under NanoTec MicroTec Control Window select the item Service Position The measuring cell is then moved to the opening area of the doors and the measuring cell is swivelled to the outside so that it is located outside the device This prevents any liquid used during cleaning from flowing into the device 5 2 2 Disassembly of the Measuring Cell The cell windows consist of saphire glass Perform the cleaning care fully although the surface normally cannot be scratched Beca
14. CH The dispersing units for measuring in suspensions or of dry solids con tain independent processor controls for all functions of sample prepara tion and feeding All of their functions can be accessed on the screen using the mouse or keyboard If you wish the computer and processor controls work together so that an individually programmed measurement cycle consisting of e background measurement e sample feeding e measurement single or multiple measurement e documentation of the results and e cleaning is executed fully automatically e g as a routine measurement that can be repeated at the push of a button The small dispersing unit is available as a special accessory for prepara tion of small sample quantities in suspension With this accessory you can perform a complete measurement with a small quantity of liquid approx 100 ml Between the smallest measuring range from 0 1 um to approx 53 um measuring cell at the smallest possible distance from the sensor and the largest measuring range between 7 um and 1000 um largest dis tance between measuring cell and sensor you can freely select any intermediate range The optical bench is constructed of high quality components in a vertical design to save space Two independent guides for liquid and dry meas urements allow fully automatic changing of the dispersing unit within seconds The fibre coupled robust 7 mW double laser diodes with polarisation preserving
15. CH The following window cleaning method has proven successful Rinse the window using the spray bottle of distilled water until no large contamination is visible Then place the special paper against the inside of the window and moisten it with distilled water and one drop of tenside Pril so that the paper adheres to the glass sur face To wipe off the surface slide the paper off parallel to the surface without pressing the paper against the glass You may need to repeat this wiping process on the glass surface with fresh paper until contamination can no longer be seen Sample residue that adheres very strongly can be softened with a tenside e g Pril and very carefully wiped a little with the special paper Then rinse the window clean with the spray bottle and dab it off carefully onto the dry special paper You should carefully keep the window cov ered until it is installed again in the measuring cell The spacer disk must be handled carefully It is manufactured to be plane parallel with an extremely low tolerance and may not be subjected to any mechanical stresses A bent spacer disk cannot be used You can rinse the spacer disk under flowing water Brush off any adhering parti cles very carefully with a soft brush The seal rings can be rinsed under flowing particle free distilled water and then dried with lint free soft paper Assembly of the measuring cell is performed in reverse order insert the loose gl
16. T ere ee MN eae eee E 3 FONGO sed ee ebene 5 The Conventional Design of the Parallel Laser Beam 5 The Inverse Fourier Design Convergent Laser Beam 6 HR OO ste ee ee ee ee An ee ge enge 6 Fraunhofer Mie Theory ss 7 Measuring in the Nanometre Range Us 7 Forward DIINaClHON nee sde seen 8 Backward DINPACHON 3 2 EPIT O RS E EEE 9 NanoTec MicroTec Device Description 9 Liquid Dispersing OAI se au 11 Dry Disp rsing OR ea a eiaa 12 Combination Unit for Dry and Liquid Dispersing ss442244000B2en nennen 12 Technical Data 12 ORO LP SR EE A A E T E AET 12 NanoTec 22 2000 00 MicroTec 22 4000 00 MicroTec XT 22 4900 00 12 Operating Safety ssannnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnnn 15 General Safety Instructions 15 Device Safety Instructions 16 RTE PR ER EP RER CESR NE TEE TE PNR ET PORN RER RER AIG 16 Ulitra sound BAR enee na OA EE AE EE a 17 Moving the Measuring Cells 17 PE O ee ee en ee eee 17 Safety Equipment ss 18 Laser EMISSIONS tances ne Aaen DRO r En naani 18 Pinching Danger een nee 18 Danger Points sise 18 Electrical Safety 18 GOTO al EINEN T E NS SEET EE TEE E TAE 18 Overload Protection ss 18 OVS TAN ATI OWN ee en en a E Ri 19 Transpo eccirni a en a EE Ee E A a 19 Unpacking ssl 19 SC LL OR ae ee a ne a ee ee ee 22
17. Tec Seite 58 FRITSCH ss Example Weakly magnetic materials In general particle size distributions of magnetic substances cannot be measured in suspensions due to the mutual attraction of the individual particles However due to the high sensitivity of the analysette 22 very low concentrations in other words relatively large distances between the individual particles can be used on one hand and on the other substances can also be suspended with high viscosity liquids due to the high power of the centrifugal pump If larger particles or particles with higher density must be measured the share of glycerine can be increased up to a ratio of 7 3 In general liq uids up to a viscosity of 30 cPoise can still be pumped without problems by the pump system of the dispersing unit 9 4 Dispersing of Poorly Wettable Samples Hydrophobic samples can be dispersed despite their water repulsing properties if they are first mixed into a paste with a fluid tenside Pril and then dispersed in water under constant stirring Agglomerates are also dispersed more easily and more quickly in an ultra sound bath because the entire sample is subjected to the ultra sound In the circuit of the dispersing unit only the quantity in the bath is in the area of the ultra sound For soil samples 0 1 0 5 sodium pyrophosphate solution is recom mended as a dispersing aid for example The sample prepared in this way in an ultra sound bath e g labore
18. Warnan y PERS RER N EEE RENE EE Te 57 9 Troubleshooting nenne 57 9 1 lg 0 ee E era 57 9 2 Transferability of Measurement Results 57 9 3 Selection of Liquids for SUSPENSIONS cccseeeeeeeeeseeeeeeeeeaeeeeeeeeees 58 9 4 Dispersing of Poorly Wettable Samples 59 9 5 Measurement of Weakly Soluble Samples nenne 59 analysette 22 NanoTec MicroTec FRITSCH FRITSCH ss 1 General Introduction 1 1 Notes about Operating Instructions e Fritsch GmbH Laborgeratebau retains the copyright to these technical documents e These operating instructions are not to be reprinted or copied without the express approval of Fritsch GmbH e Read the operating instructions carefully e All operators must be familiar with the contents of the operat ing instructions e Please follow the notes for your safety e The laser particle sizer was designed from the perspective of user safety however some risks could not be excluded Fol low the advice in these instructions to avoid risks to users e The symbols in the right hand margin highlight the risks de scribed in the text Some symbols may also be found on the device and warn against possible hazards existing there Warning symbols are surrounded by a triangle e These operating instructions do not constitute a complete technical description They describe only the details required for safe operation and maintenance for usage u
19. _ FRITSCH Operating instructions Laser Particle Sizer analysette 22 NanoTec MicroTec XT Fritsch GmbH Laborger tebau Industriestra e 8 D 55743 Idar Oberstein Phone 06784 70 0 Fax 06784 70 11 Email info fritsch de URL http www fritsch de Fritsch GmbH Laborger tebau was certified by the T V Zertifizierungsge meinschaft e V on 21 11 2003 ELUA Care DIN EN ISO 9001 Wo Based on an audit report Fritsch GmbH has been awarded the certificate of compliance to the requirements of DIN EN ISO 9001 2000 The enclosed conformity declaration specifies the directives fulfilled by the laser particle sizer analysete 22 NanoTec MicroTec in order to carry the CE symbol NanoTec model numbers 22 2000 00 22 2800 00 22 850 00 22 2900 00 MicroTec model numbers 22 4000 00 22 4400 00 22 4500 00 22 4950 00 MicroTec XT model numbers 22 4900 00 22 4940 00 22 4960 00 applies as of serial number 0001 Edition 06 2004 Index 004 _ FRITSCH A w w w w ho D D D D D ES ND 3 2 5 3 3 3 AA No ee ee eS eS Se ND 4 1 4 2 4 3 4 3 1 4 3 2 4 3 2 1 4 3 2 2 4 3 2 3 4 3 2 4 4 3 2 5 4 3 2 6 4 3 2 6 1 4 3 2 6 2 4 3 2 Table of Contents Page General INtrOAUCTION 111cccccneecenecnenseneenennensenennensenennennenanens 1 Notes about Operating Instructions 1 SV DOS SOG atone en ee 2 Brief Description of the Device 3 D SIR sere ay
20. afety Attention Connect the measuring device to a power supply line protected with a residual current circuit breaker 2 6 1 General The power switch disconnects the machine from the supply at both poles 2 6 2 Overload Protection The power supply protection provides overload protection analysette 22 NanoTec MicroTec Seite 18 FRITSCH E uf SE 3 Installation 3 1 Transport Transport over larger distances only in a transport box 3 2 Unpacking Compare your order with the delivery In the event of incomplete delivery and or transport damages inform the shipper and FRITSCH GmbH within 24 hours Later complaints can no longer be accepted Only open the boxes while the arrows point upward Remove the trans port packaging as shown in the following pictures analysette 22 NanoTec MicroTec Seite 19 FRITSCH of e re a LA LA LA analysette 22 NanoTec MicroTec Seite 20 FRITSCH of analysette 22 NanoTec MicroTec Seite 21 Unscrew the carry grips from the base plate and insert the grips into the fixtures in the accessory case provided for this Close the screw holes in the base plate with the closing plugs from the accessory case 3 3 Setup e Place the device indoors on a flat stabile surface It is not necessary to fasten the device in place e Please avoid intense heat sunlight heaters etc dusty envi ronments and their effects
21. alculated The vibration dosing channel automatically sets the dosing rate as a vibration amplitude and the quantity as a distance between the funnel and the vibration channel The quantity is set as low as possible and the dosing rate as high as possible This ensures the supply of a thin sam ple layer to the nozzle and results in optimal conditions The dry dispersing unit is a fully automatic system To apply initial settings to the dosing select the functions Setup NanoTec MicroTec Control Window to configure specific set tings These settings are overwritten during the measurement With an absorption setting of 2 to 5 per cent the vibration dosing chan nel supplies as much sample material as possible to fulfill this require ment First the quantity is increased and after the value 6 is reached the amplitude is also increased by steps of one The settings for this measurement are saved in the results file and can be reloaded analysette 22 NanoTec MicroTec Seite 50 FRITSCH se To add sample material add your sample material into the funnel After clicking on Start Measurement the measurement is performed The sample moves forward on the dosing channel Because at the be ginning no sample is conveyed into the laser it may occur that the measuring device control quickly increases the transport rate However this is very quickly corrected when sample is first transported Observe the flow behav
22. ass with the bluish shimmering anti reflex coating to the out side arrows are located on the window edges see picture arrow tips pointing to the outside to the anti reflex layer You can identify the anti reflex layer by holding a window at an angle to a fluores gt cent lamp If you see the inner border of the N window shimmer in a bluish colour the re flex layer is facing up The coated side is also marked with an arrow on the edge of the glass If the inner border appears whitish the reflex layer is facing down be cause the light entering into the window does not appear coloured by the anti reflex layer Then position the spacer disk such that the sample supply and discharge is not covered then carefully place the two halves of the measuring cell together The screws must be tightened carefully in a cross pattern analysette 22 NanoTec MicroTec Seite 36 FRITSCH se You must take care that you close the two halves evenly with the four screws The spacer disk situated between the two windows holds the windows in an exactly parallel position Any contamination remaining between the windows and the spacer disk must absolutely be re moved first A particle remaining between the glass and the spacer disk can lead to breaking of a glass when screwing the cell together It also prevents the windows from being perfectly parallel When moving or sliding the measuring cell to adjust the measur ing
23. asuring Cell 4 4 1 Liquid Dispersing Unit Select the measurement process Rinse Before Measurement and press Start Measurement The ultra sound bath then rinses itself and fills itself with clear measuring fluid The fill level sensor automatically closes the valve 4 4 2 Filling the Measuring Cell When Using the Small Quantity Dispersing Unit Emptying and filling of the small quantity dispersing unit is performed manually Turn the valve lever to Drain Fill With the supply opened fresh sus pension liquid then flows into the glass container through the connected In hose The liquid level rises while the pump is switched off analysette 22 NanoTec MicroTec Seite 39 FRITSCH ss 4 5 Setting the Measuring Range for Calibration The calibration of the laser beam is performed with the measuring cell in a middle position approx 200 mm Inspection of the calibration takes place at the positions 385 mm MicroTec 290 mm and 9 mm If you enter Set Measuring Range change the measuring cell dis tance and close the dialog with OK the measuring cell does not move immediately but only after you have started a new measuring cycle with Start Measurement You can directly halt this with Stop Measurement To inspect the calibration at 20 and 385 or 290 mm simply activate a multiple measurement in Set Measuring Range with 20 mm and 385 or 290 mm Select Background Measurement and press Start Measurement The meas
24. ata 1 4 1 General Operating Noise The noise level is 42dB A Voltage Single phase alternating voltage 90 230V 10 1 4 2 NanoTec 22 2000 00 MicroTec 22 4000 00 MicroTec XT 22 4900 00 Current consumption The maximum current consumption is 0 5 A Power consumption The maximum power consumption is 125 W Electrical fuses Electronic fuses in the interior of the device on the switched power sup ply and beneath the wet connection combination analysette 22 NanoTec MicroTec Seite 12 ss FRITSCH Device MicroTec MicroTec XT Tete TE Combination device for liquid and dry measur ing 22 2000 00 Device for liquid mea suring 22 2800 00 Device for dry measu ring 22 2900 00 Small quantity liquid dispersing unit 22 6750 00 or 22 6700 00 Tete TE Combination device for liquid and dry measur ing 22 4000 00 Device for liquid mea suring 22 4400 00 Device for dry measu ring 22 4500 00 Small quantity liquid dispersing unit 22 6 50 00 or 22 6700 00 analysette 22 NanoTec MicroTec Liquid Dispersion 0 1 600 um Measu ring Time dry approx liquid 10s approx 0 1 2 liquid approx 10s cm in 500 ml liquid Dry Liquid Sample Quanti ty Liquid Volume dry 5 50 cm Dry Liquid liquid approx 0 1 2 cm in 500 ml approx 10s 100 ml liquid Measu ring Time Sample Quantity Liquid Volume liq
25. c and MicroTec requires no maintenance apart from the regular cleaning Before starting the work in the device switch off the measuring device and unplug the power cord 8 Warranty The warranty card enclosed with the device upon delivery must be com pletely filled out and returned to the delivering factory so that the war ranty can enter into effect The company FRITSCH GmbH Laborger te bau Idar Oberstein and its Technical Application Laboratory or the corresponding national representatives will be glad to offer advice and assistence Indication of the serial number imprinted on the type plate is required with any questions 9 Troubleshooting 9 1 Error List Error _ Possible Cause Lamp Plug in the power plug missing Does not light Switch on the main switch Replace the mains fuse 9 2 Transferability of Measurement Results lf a measurement of particles is intended to determine which of their assumed properties are true the measurer is not only an observer and the measuring device is not only his tool rather both participate actively in the process In the determination of particle size distributions both are active in generating the result and determining its nature In the development of measuring devices the designer strives to elimi nate the influence of the operator as much as possible However the effects of the physical measurement process applied and its realisation in the device cannot be ignored If f
26. cuit should now be completely without liquid it may be that residual liquid remains in the measuring cell itself There fore you should have a paper towel or something similar ready to di rectly collect any liquid escaping Unscrew the four screws on the underside of the measuring cell Be careful to hold the bottom parts of the measuring cell and the front measuring cell glass firmly while doing so Attention After removing the last screw the top measuring cell glass falls onto the lower part If the measuring cell is very dirty it is possible that you must also apply light pressure from above with paper towel analysette 22 NanoTec MicroTec Seite 33 FRITSCH se Place the flange on the cell storage tool Attention NEVER place the lower part of the measuring cell with the glass face down on an unprotected surface This could scratch the opti cal glass or destroy the anti reflex coating This can make your en tire measuring cell unusable Place the loose window with the outside down on the optical paper CRE EC analysette 22 NanoTec MicroTec Seite 34 __ FRITSCH 4 3 2 5 Cleaning It is normally sufficient to rinse the measuring cell with a clear liquid To remove stubborn residues you can also add a cleaning agent to the cleaning liquid Usually a few drops of a surface active household cleaner cleanser e g Pril or liquid soap is sufficient Mechanically adhering co
27. device to a power supply line protected with a residual current circuit breaker 3 6 1 Electrical Fuses The device has two device fuses beneath the power connection assem bly The internally required stabilised direct current of 24 V is provided by an integrated switched power supply with internal electronic short circuit and surge protection 3 6 2 Stability of the Power Supply Devices with electronic components demand stabile supply voltages 5 deviation For weak power networks or networks not safe against errors voltage peaks due to inductive load changes or switched mode power supplies we recommend connecting a voltage stabiliser and filters between the power supply and device order no 20 600 00 3 6 3 Adapting to the Power Network Manual switching of the voltage ranges on the device is not necessary because the device can be operated with 90 230 V The switching is performed automatically analysette 22 NanoTec MicroTec Seite 25 FRITSCH u 3 7 Connections ET b ei di Connection control box 8 for vacuum dry dispersing Main power supply Suspension liquid supply water connection at least 2 bar Suspension liquid discharge Compressed air supply 7 m h at least 5bar dry dispersing Connection for vacuum dry dispersing RS232 connection to the computer Control box for vacuum dry dispersing ONE ee analysette 22 NanoTec MicroTec Seite 26 FRITSCH
28. e of explosive or flammable liquids is forbidden they may not be used The following summary serves only to indicate the chemical com patibility of the device in relation to liquids Mono di or trihydric alcohols except for methanol ethyl alcohol isopopyl alcohol gylcol or glycerine Mineral and organic oils such petroleum and soy oil nut oil olive oil Before the planned use of other measuring fluids the factory must first be consulted The following may not be used Ketones acetone propanone butanone cyclohexanone Ether fluorochlorohydrocarbons Amines freon 21 32 Methanol aniline benzine Chlorohydrocarbons Ethanoic acid and its derivatives Undiluted acids and bases Even samples present in oil e g oils similar to machine oil do not also have to be measured in oil Example Toner in machine oil The sample is first dispersed in ethylene glycol with a drop of tenside Pril in the ultra sound bath Then a mixture is created 1 1 with water and this is added to the ultra sound bath of the laser particle sizer ana lysette 22 Example Raw cocoa mixture Raw cocoa mixture is typically measured in acetone or benzine Known from the sieving process Measurement in the analysette 22 can also be performed in peanut oil for instance Because peanut oil is suitable for use with food the waste oil can also be used as a lubricant on the rollers solving the disposal problem analysette 22 NanoTec Micro
29. e valve Lay the hoses without kinks The 18 mm pipe connector with the designation In upper connection should be connected directly to your building water connection It serves to fill the measuring apparatus The device has an internally integrated pressure reducer that is permanently set to 1 5 bar In order to ensure that the rinsing process can be completed prop erly you must therefore provide at least 2 bar from your water sup ply lf you connect the supply connection In e with demineralised filtered water or e aliquid storage tank that supplies a pressure less than 2 bar more liquid will be discharged than can be supplied In this case you must reduce the cross section of the discharge hose e g with hose clamps until the rinsing process once again functions properly Reduction of the discharge hose cross section always leads to a less effective cleaning because the liquid in the ultra sound bath no longer discharges completely and is therefore only diluted fur ther This increases the risk of residues in the sample and therefore carry over The hose connections must be connected pressure tight with hose clamps You should check the position of the supply hoses in the device before the first measurement To do this move the cell from the top to the bot tom position Risk of injury A risk of injury by pinching exists for the operator while the posi tioning drive is operating and the door is open
30. fibre good temperature stability high beam quality and long service life radiate in the visible range A newly developed diffracted light detector on a ceramic base made in Germany according to state of the art manufacturing methods offers the best mechanical and thermal stability analysette 22 NanoTec MicroTec Seite 10 __ FRITSCH With the expansion for measurement of backward diffracted light the analysette 22 NanoTec covers a diffracted angle range from 0 to approx 180 It has a double laser diode for diffracted light measure ments in the forward and backward directions To expand the measure ment in the nanometre range the forward laser is switched off anda laser in the reverse direction is activated This generates light diffraction in the measuring cell that can be captured by the detector as polarisa tion selective backward diffraction in the angle range 60 180 The extinction of the backward laser is captured by a photodiode swivelled to a position in front of the forward laser The nano option can be acti vated in connection with the module for liquid dispersion For the cell distance of 20 mm this expands the measuring range of the device down to 10 nm You can make use of the full scope of the extremely large measuring range from 0 01 um to 1000 um in a single measurement process through controlled coupling of up to 10 individual measurements Your wish for a higher resolution in the measurement
31. from 60 180 In addition the optimised geometry of the detector makes it possible to capture and evaluate the various diffractive effects of nano particles par allel and perpendicular to the polarisation direction of the laser The lower measuring limit with this design is 10 nm I R N Pos Lee ee Da y 1 3 3 NanoTec MicroTec Device Description The NanoTec version is a device combination offering maximum user comfort The analysette 22 NanoTec offers everything that a user of modern laser particle sizers expects High quality optical mechanical and electronic components combined with modern flexible software for calculation of the Mie components the particle size distribution and the resulting parameters guarantee a state of the art analysis instrument The measuring range is 0 01 to 1000 um The analysette 22 MicroTec is the measuring instrument for samples in the micron and submicron range The reduced optical bench allows a very compact and inexpensive design The MicroTec is the little brother of the NanoTec All hardware and software components are identical with those of the analysette 22 NanoTec except for the nano expansion The measuring range is from 0 1 to 600 um MIcroTec XT 0 1 to 2000um As a new feature world wide Fritsch offers optional software for shape recognition for the models analysette 22 NanoTec and analysette 22 MicroTec analysette 22 NanoTec MicroTec Seite 9 _ FRITS
32. gly large surfaces in the outer area to com pensate for the small diffraction angle of smaller particles In the inner region of the detector the elements are very small so that even the dif fracted light of large particles can be measured with high resolution The separation of the individual elements from each other is performed using state of the art semiconductor manufacturing processes dr a LIN 71 TS F EO The diffracted light cannot leave the measuring cell at arbitrarily large angles because total reflection occurs at a specific angle upon transition from an optically more dense to less dense medium The optical meas uring cell glasses of the analysette 22 are therefore given prism shaped wide angle surfaces from which diffracted light can escape at a large angle This light is measured on the detector by special wide angle elements In the forward direction lower measuring limit 0 1 um a diffraction angle range to approximately 60 is covered with this design analysette 22 NanoTec MicroTec Seite 8 _ FRITSCH 1 3 2 5 2 Backward Diffraction To capture the diffracted light of nanometre particles a significantly lar ger angle range must be covered To accomplish this the analysette 22 NanoTec uses a backward laser that passes through the same mi cro hole in the detector and generates light diffraction in the measuring cell that is then detected by the detector as backward diffraction in an angle range
33. he Measuring Cell When Using the Small Quantity Dispersing Unit 39 4 5 Setting the Measuring Range for Calibration 40 4 6 Mounting instructions Measuring Range Extension Kit WET 41 5 Dry Dispersing UDUE u nennen 43 5 1 Preparing the Dry Dispersing Unit 43 5 1 1 Dry Dispersing Nozzle and Measuring Cell 43 5 1 2 Connecting the Measuring Device 43 5 1 3 Compressed Air Technical Data ccccccccsseeecccceeeceeeeeeeeeeeeeeeeeeeeeessaaaaeees 43 5 1 4 Connection to the COMpUuter 4 iasnissnasncesuancesinateaseedesinssndanesaesiidnsasasiateaseanictes 43 5 1 5 Connecting the Vacuum ss 44 5 1 5 Vacuum Technical Data ii iiiiiissssssseseeeseeessnss 44 5 1 6 Selling Ihe Pressure u uuseren sne aan 44 5 2 Cleaning the Measuring Cell Windows of the Dry Dispersing Unit 45 5 2 1 SJENICE PO WON A en a seen eo EE NE ra h 45 5 2 2 Disassembly of the Measuring Cell 45 5 2 3 Assembly of the Measuring Cell 49 5 3 Measuring with the Dry Dispersing Unit 50 5 4 Mounting instructions Measuring Range Extension Kit Dry 52 6 PRC COS SOIC S vase sector nee as ie de 54 6 1 analysette 22 WINDOWS Program 54 6 2 Small Quantity Dispersing Unit 54 6 2 1 Connection of the small volume dispersing unit 54 6 2 2 Small volume dispersing unit for manual change of the measuring cell liquid 55 7 IMAINIEHANLCE me a nan eee 57 8
34. indow The cleaning process is the same as de scribed for cleaning of the liquid measuring cell There are no seals to be cleaned in the dry measuring cell The seal is created by the metal metal glass metal and glass ceramic surfaces Above all make certain that no dust particles are located on the ceramic surfaces All surfaces must be perfectly clean Dust particles on the surface cause the measuring cell to no longer function properly and the beam loses its calibration upon moving of the measuring cell 5 2 3 Assembly of the Measuring Cell Reassemble the measuring cell in reverse order analysette 22 NanoTec MicroTec Seite 49 FRITSCH ss 5 3 Measuring with the Dry Dispersing Unit After the measurement starts the vacuum above its control cabinet is first switched on Then the compressed air and finally the vibration dos ing channel is switched on To stop the measurement repeat the steps in reverse order The dosing channel does not operate during the back ground measurement The background measurement takes about 20 seconds because the measuring cycle is always cleaned first Immediately after the back ground measurement and still before the actual measurement the dos ing channel is switched on and regulated such that the previously con figured value for the beam absorption is maintained After the measure ment is completed the data is then automatically loaded and the particle size distribution c
35. involved with laser emitters before using it Do not remove information and warning signs Laser devices of laser classes 3B and 4 are hazardous to the human eye even an exposure time of 0 25 s is sufficient t0 cause permanent damage to the retina For this reason any person operating the device with opened doors must wear suitable safety goggles The safety gog gles must be suitable for the wavelengths of the laser used for example safety goggles that protect against a green laser fail against a red laser The wavelength of the built in laser is 655 nm For laser devices of laser safety class 3B or 4 laser safety officers must be appointed in accordance with GUV 2 20 analysette 22 NanoTec MicroTec Seite 16 FRITSCH ss 2 2 2 Ultra sound Bath The ultra sound bath built into the liquid dispersing unit has an output of 70 Watts PZT ultra sound oscillators fastened to the oscillating trough convert electrical energy into mechanical vibrations Fritsch ultra sound baths cause the liquid to vibrate at 36 KHz This causes the formation of tiny vacuum bubbles that implode cavitation This cavitation principle destroys agglomerations Liquids contain dissolved gasses e g oxygen Freshly added liquids or liquids remaining in the oscillating trough for longer periods of time should be exposed to ultra sound for approx 5 to 15 minutes before use During the degassing period the cavitation noise alters loud de gassing noise
36. ion must be protected against water If there exists the risk that a water layer could form on the setup sur face in the event of an error you must select another setup location If no other location is available the entire device must be elevated use riser blocks 3 4 Transport safety device To avoid damanges of the laser diode during the transport it is secured by a protecting cap MicroTec model Please remove this before the first measurement analysette 22 NanoTec MicroTec Seite 23 3 5 Accessory Case FRITSCH se 7 ne The accessory case contains Agents and tools for cleaning the optical glass elements cleaning liquid cleaning cloths compressed air etc Replacement screws and hose clamps for the measuring cell A storage tool for the front flange of the measuring cell with glass Tool for assembly and maintenance A CD ROM with software A micro fibre cleaning cloth for metal and glass surfaces Internal particle size standard F500 F70 Cell storage tool Closing plugs and carry grips analysette 22 NanoTec MicroTec Seite 24 FRITSCH ss 3 6 Electrical Connection Connect the measuring device the computer with monitor and the printer to a power strip each with separate power cables The enclosed power cable is intended for the measuring device It is a special design with electronic filter that was selected to ensure error free operation Attention Connect the measuring
37. ior of the sample For samples that do not flow well you should further configure the limits of the beam absorption Samples that flow well can be measured for example with a minimum beam absorption of 2 and a maximum beam absorption of 3 The more difficult the sample is the more you should extend the limits for instance up to a maximum beam absorption of up to 6 The fluctuations that you permit in this way directly affect the re producibility of your measurement If you would like to keep the limits low with a sample that does not flow well you need signifi cantly more sample analysette 22 NanoTec MicroTec Seite 51 FRITSCH US 5 4 Mounting instructions Measuring Range Exten sion Kit Dry 1 Configuration Set Configuration NanoTec MicroTec System Use Option for extended Measuring Range Please note the software instructions 2 Take the Measuring Extension Kit dry from the accessories case and remove lens caps analysette 22 NanoTec MicroTec Seite 52 FRITSCH of 3 Introduce the body of the tube with locating pin 1 into the drilling planned for it 2 in the profile of the optical bench Insert the measuring range extension kit in such a way that the signature cell shows towards the measuring cell Put the rider on the profile and tighten the knurled thumb screw 8 4 Ready 5 For the disassembly of the measuring range extension kit pro ceed in rever
38. ly the result of a missing or non functional RS232 port on your computer In this case always check the hardware of your computer analysette 22 NanoTec MicroTec Seite 27 _ FRITSCH 3 12 Function Check Select the version of your NanoTec MicroTec and the liquid dispers ing for combination devices Enter Measuring Range Setting and select a cell distance of 190 mm Enter the Beam Adjustment You will not immediately see signals from the detector you will see signals only after you have selected Manual Adjustment and clicked on one of the arrows Then one data record is sent from the measuring device to the computer Check whether the beam adjustment is accurate see here the operating manual Select only Background Measurement as the measurement process Press Start Measurement The measuring cell must now move to a distance of 190 mm and you must see the signals of the background measurement on the screen Now perform a measurement with the Fritsch internal standard sample Instructions for this can be found in the Fritsch reference manual analysette 22 NanoTec MicroTec Seite 28 FRITSCH ss 4 Liquid Dispersing Unit 4 1 Installing Hose Connections The liquid dispersing unit has two pipe connectors in the rear for hoses with 18 mm inner diameter The 18 mm pipe connector with the designa tion Out lower connection serves to release used measuring and rins ing fluid through the discharg
39. nce be tween the measuring cell and the detector is equivalent to the focal length of the convergent lens in conventional applications one obtains the same diffraction image as with a conventional design without the disadvantages of reconfiguration in order to change the measuring range the measuring range can be changed by simply moving the measuring cell as with a zoom lens The user has full control over the local frequencies of the Fourier optics e Large distance between measuring cell and detector TELE gt Measuring of coarse particles e Small distance between measuring cell and detector MACRO gt Measuring of small particles down to the submicron range The laser particle sizer analysette 22 is the only instrument with which the measuring cell is moved along the optical axis to adjust the measur ing range without the need to change the lens The sample is therefore always measured with the greatest dynamic and optimal conditions 1 3 2 3 Resolution The inverse Fourier optics also allow measurement of a particle size distribution with extremely high resolution With the fully automatic com puter controlled positioning of the measuring cell within the convergent beam a super matrix of up to 520 measurement channels can be cre ated for calculations using the models NanoTec MicroTec and Micro Tec XT The total measuring range is available without limitation analysette 22 NanoTec MicroTec Seite 6 __ FRITSCH 1 3
40. nd the resulting particle size distribution is a volume distribution 1 3 2 1 The Conventional Design of the Parallel Laser Beam The diffraction image in the focal plane can be mathematically described with the help of Fourier optics The measurement principle is based on the unique property of a convergent lens of performing a two dimensional Fourier transformation on the incoming field For this rea son the convergent lens situated in the parallel laser beam is also called a Fourier transformation lens The local frequencies of the Fourier components are directly proportional to the focal width of the convergent lens Changing the measuring range therefore always requires changing the lens involving reconfiguration of the device Many manufacturers have therefore adopted an alternative measurement design in recent years one that was invented by the FRITSCH company analysette 22 NanoTec MicroTec Seite 5 FRITSCH aia 1 3 2 2 The Inverse Fourier Design Convergent Laser Beam The analysette 22 offers an alternative optical design that is both state of the art and impressively simple The design which was included in ISO 13320 1 under the term Inverse Fourier Optics has long been known as a part of Fourier optics How ever the advantages for particle size distribution measurement were first recognised utilised and patented by FRITSCH The sample is placed within a convergent laser beam The dista
41. nder normal conditions analysette 22 NanoTec MicroTec Seite 1 _ FRITSCH 1 2 Symbols Used Attention Warning against danger spot Observe operating instructions Attention Mains voltage Attention Hazard of explosion Attention Inflammable substances Attention Warning against laser beam Wear safety goggles Spraying with water forbidden Warning against hand injury analysette 22 NanoTec MicroTec Seite 2 _ FRITSCH 1 3 Brief Description of the Device The laser particle sizer analysette 22 model NanoTec and model Mi croTec are universally usable devices for determination of particle size distribution in suspensions emulsions solids and aerosols They are primarily used in research and development and in quality and process inspections The analysette 22 NanoTec and Micro Tec models utilise the FRITSCH patent on a convergent laser beam for determination of particle size dis tribution 1 3 1 Design The measuring device of NanoTec contains two semi conductor lasers wavelength 650 nm laser power mW laser class IIIb The measuring device of MicroTec contains one semi conductor lasers wavelength 650 nm laser power mW laser class IIIb Warning labels for laser radiation are located on the inside of the device All optical and electrical components are situated in a vertically aligned aluminium profile Depending on the feature variant
42. ne only briefly rinse out after the measure ment because the connecting hoses will be damaged e Formaldehyde e Saturated solutions of inorganic salts Before the planned use of other measuring fluids the factory must first be consulted In principle we warn against the use of liquids that are explosive combustible or hazardous to health they cannot be recom mended The above summary serves only to indicate the chemical compati bility of the device in relation to liquids The measuring device and dispersing units are not designed with explosion protection The liquid consumption is significantly reduced through the use of the small quantity dispersing unit The following may not be used Ketones acetone propanone butanone cyclohexanone Ether fluorochlorohydrocarbons Amines freon 21 32 methanol aniline benzene Chlorohydrocarbons such as ethanoic acid and their derivitives undiluted acids and bases When using measuring liquids hazardous to health always follow the applicable safety regulations MAK values and place the meas uring unit and dispersing units in ventilated safety zones if re quired analysette 22 NanoTec MicroTec Seite 30 FRITSCH ss 4 3 Cleaning 4 3 1 Cleaning the Device The device can be wiped with a moist cloth or the micro fibre cloth from the accessory case Do not allow any liquids to flow into the device 4 3 2 Cleaning the Measuring Cell The measuring
43. ntamination can be rinsed out with the addition of approx 2 g of fine abrasive Household abrasive ATA VIM Oily residues can be rinsed out with a slightly alkaline cleaning agent lt can be necessary over time to clean the insides of the measuring cells as well This is necessary if with the measuring cell all the way to the left with activated laser beam you see many small points of light on the insides of hte window that cannot be removed by rinsing multiple times or if the window has become matte In the Setup program under Control NanoTec select the button Park Position The measuring cell is then moved to a distance of approx 150 mm so that It is located in the area of the door opening If the measuring cell was swivelled into the laser beam path it is now swivelled out to a park position In the Setup program under Control NanoTec select the button Service Position this swivels the measuring cell out of the device and you can perform the necessary steps outside of the device 4 3 2 6 Cleaning the Window 4 3 2 6 1 Loose Window Before disassembling the measuring cell and cleaning the windows the spacer disk and the seal rings place a spray bottle with distilled water and the lens cleaning paper from the accessory case on a clean work table Great care is required for cleaning the windows The windows may only be touched by hand on their edges analysette 22 NanoTec MicroTec Seite 35 _ FRITS
44. of your computer analysette 22 NanoTec MicroTec Seite 43 5 1 5 Connecting the Vacuum Connect the control box for the vacuum to the power network and insert the power plug of the vacuum system into the socket of the control box max 16A Vacuums frequently produce disruptions in the power network For this reason it is best to connect the control box to a different power supply than the rest of the equipment measuring unit com puter etc The control box of the vacuum can be delivered with an adapter so that the various power plugs of different countries will fit Insert the hose of the vacuum into the connection provided for this on the measuring device The connection has a diameter of 40 mm appro priate for typical commercial vacuums Should your vacuum not fit onto this connection you must obtain an appropriate adapter from your local accessory Store 5 1 5 1 Vacuum Technical Data The following information represents the minimum guiding values to be fulfilled and may differ depending on the vacuum used However the minimum values must be fulfilled Power consumption max 1100 Watts Air flow 40 I S Vacuum 23kPa Vacuum power 270 W Filter surface 2400 cm Dust bag capacity 9 0 5 1 6 Setting the Pressure A pressure reduction valve with manometer is located on the front side of the measuring device During the measurement an electrical valve opens and switches the compressed air to the nozzle Use
45. on According to the Mie theory multiple oscillation states of vary ing probabilities are possible and there exists a relationship between the optically effective cross section and particle size light wavelength and the refractive index of the particles and medium In order to apply the Mie theory the refractive index and absorption co efficient of the sample and the medium must therefore be known The software of the analysette 22 contains these constants for many mate rials within its database During measurement an appropriate diffraction matrix is selected or calculated within seconds upon entry of new con stants 1 3 2 5 Measuring in the Nanometre Range As the particle size decreases the diffracted light contains less and less information At the same time the diffraction angles become very large and the intensity of the diffracted light decreases significantly For this reason more elaborate instrument technology is required for the nano range analysette 22 NanoTec MicroTec Seite 7 _ FRITSCH 1 3 2 5 1 Forward Diffraction The light diffracted in the measuring cell is diffracted in a forward direc tion and captured by the light sensitive elements of the diffracted light detector The detector contains a micro hole in its centre through which the laser light encounters a photodiode to determine the total absorption Light sensitive elements are arranged concentrically around this micro hole These have increasin
46. or instance particle size distributions are determined according to the sedimentation process scanning photo sediment graph analysette 20 and through the evaluation of a diffraction image results that differ slightly from each other must be expected at the least In the measurement of particle sizes through the analysis of a diffraction image all dimensions of irregular particles are seen and correspond ingly taken into account in the result For instance the longitudinal ex tent of needle shaped samples are also determined here In a compari son or the transfer of particle size distributions from various measuring processes the particle shape must be taken into consideration analysette 22 NanoTec MicroTec Seite 57 FRITSCH ss 9 3 Selection of Liquids for Suspensions Because the measuring fluid in the entire device can come into contact with materials that are not chemically resistant certain organic liquids or saturated inorganic salt solutions cannot be selected The measuring fluid comes into contact with stainless steel glass Teflon Viton FPM and FKM and PA66 Nylon The standard connection hoses are made of Viton Only water is approved by Fritsch as a suspension liquid for the dispersing unit Before the planned use of other measuring fluids the factory must first be consulted For measuring samples incompatible with water a liquid can be selected from the following list In principle the us
47. ranges the calibration of the laser is disrupted by unparallel windows The calibration is no longer valid for the entire adjust ment range of the measuring cell due to the prism effect of the unparallel measuring cells 4 3 2 6 2 Flange Window The same applies to the window attached in a fixed position with the metal flange as for the loose window Handle the optical surfaces very carefully analysette 22 NanoTec MicroTec Seite 37 _ FRITSCH A Also clean all metal surfaces and seals very well Adhering grains can lead to the window not being optimally installed and the laser beam is brought out of calibration by moving of the measuring cell In extreme cases a glass can even break during installation 4 3 2 7 Installing the Measuring Cell After you have cleaned both windows and cell halves you must install the measuring cell again Lay the loose glass in the direction of the channels on the flow disk TE un gt i p e ie An A 27 f The groove in the picture above perfectly matches the groove in the op posite flange of the measuring cell Take care to ensure correct position ing analysette 22 NanoTec MicroTec Seite 38 _ FRITSCH Do NOT tighten any screw all at once Turn the screws a little tighter in alternation until all screws are tight If you tighten the screws unevenly the windows may break 4 4 Filling the Me
48. s disappear at the end of the degassing process the de vice operates noticeably more quietly A lower noise level does not mean any subsiding in the ultra sound output only the end of the de gassing process Caution e Do not operate the ultra sound bath without liquids e Do not use any flammable liquids e g benzine solvents and no chemicals that contain or give off chloride ions Some disin fectants household cleaners and dishwishing soaps for ultra sound cleaning in the stainless steel trough Do not use aggressive cleaning liquids e g acids salt solu tions Do not reach into the cleaning fluid during ultra sound clean ing The cleaning fluid heats up during longer periods of operation check the temperature 2 2 3 Moving the Measuring Cells Do not operate the device with open doors Due to the high torque of the motor for moving the measuring cell severe pinch ing or injuries can occur if the measuring cell is moved while the doors are open Always close both doors before initiating Start Measurement 2 3 Operators e The device may only be operated by authorised persons and maintained and repaired by trained experts e Persons under the influence of health impairments medica tions drugs alcohol or excess fatigue may not operate the device analysette 22 NanoTec MicroTec Seite 17 FRITSCH ss 2 4 Safety Equipment Safety equipment such as coverings must be used as instructed and may
49. s parti cles with higher specific gravity and is suitable for long term operation The entire liquid volume can be completely pumped once within three seconds with the powerful pump This makes the measurement inde pendent of inhomogeneities in the sample The pump rotation speed and ultra sound output can be adapted to the properties of the sample All parts in contact with the liquid are of stainless steel Viton and PA60 All functions can be controlled by computer analysette 22 NanoTec MicroTec Seite 11 1 3 3 2 Dry Dispersing Unit The dispersing module for dry samples prepares agglomerates using mechanical and pneumatic forces The dosed sample is supplied by a new amplitude controlled vibration dosing channel The dispersing takes place in a two phase annular gap nozzle through air fins with aerody namic wave formation at the nozzle outlet and high flow speed in the nozzle channel To operate the dry dispersing unit a connection for oil water and parti cle free compressed air with a pressure of at least 5 bar and a flow rate of at least 8 m h is required The fully automatic measuring sequences can be freely programmed and saved The entire functional process is controlled by an integrated microprocessor 1 3 3 3 Combination Unit for Dry and Liquid Dispersing The combination device contains the module for both liquid and for dry dispersing The desired dispersing type can be selected with a software command 1 4 Technical D
50. se order analysette 22 NanoTec MicroTec Seite 53 _ FRITSCH 6 Accessories 6 1 analysette 22 WINDOWS Program With the software package analysette 22 for WINDOWS all functions of the COMPACT COMFORT ECONOMY Nano Tec and MicroTec ver sions can be programmed and controlled see user manual analysette 22 for Windows 6 2 Small Quantity Dispersing Unit 6 2 1 Connection of the small volume dispersing unit The small quantity dispersing unit is connected directly to the measuring cell in the measuring device It has four hose connections labelled with e FROM CELL e TO CELL e IN e OUT FROM CELL and TO CELL must be connected with the measuring cell Kleinmengen Dispergiereinheit small Dispersing Unit Von Drehzahlregulierung Pumpe und R hrer Speed Control Pump and Stirrer IN on the dispersing unit serves to fill the measuring apparatus and is connected either to a central supply line with for instance demineral ised filtered water or to a storage tank with measuring fluid OUT serves to discharge the measuring and rinsing fluid Attention The maximum water pressure in the device is 0 5 bar analysette 22 NanoTec MicroTec Seite 54 _ FRITSCH 6 2 2 Small volume dispersing unit for manual change of the measuring cell liquid For the conversion to the small volume dispersing unit you need to per form the following steps 1 Drain off the hole system please
51. surement the dry measuring cell swivels automatically into the beam path after pressing Start Measurement If the liquid measuring cell was swivelled in this is automatically swivelled out first The sample hose a compressed air hose and the hose for suction are already connected to the dry dispersing unit 5 1 2 Connecting the Measuring Device The dry dispersing unit has rear connections for all required hoses Connect your external compressed air supply with the included hose 3 m compressed air hose with compressed air connector On the rear side of the device you will find connectors for all electrical connections Connect the measuring unit to the main power supply with the included cable Attention NEVER operate the dry dispersing unit without the vacuum In this case the glasses of the measuring cell will become very dirty and may become unusable Connect the control box for the vacuum to the dry dispersing unit round connector 5 1 3 Compressed Air Technical Data The compressed air must be oil free particle free and dry If this is not the case the measurement results will be inaccurate The compressed air supply must be capable of providing an air flow of at least 7 m h approx 120 l min We recommend using at least a particle oil and water filter with a filter effect in the micron range 5 1 4 Connection to the Computer Connect the measuring unit with the included 9 pin data cable to an RS232 port
52. suring explosive combustable or fire promoting substances The device may not be used in an electrically conducting dust containing or moist environment Do not allow any liquids to flow into the device Do not use any highly flammable burnable liquids such as al cohols ketones benzines etc analysette 22 NanoTec MicroTec Seite 15 ss FRITSCH _ FRITSCH 2 2 Device Safety Instructions 2 2 1 Laser The measuring unit of the analysette 22 contains a semi conductor laser with 7 mW output and a wavelength of 655 nm The laser of the analysette 22 NanoTec and MicroTec is therefore classified as Class 3b EN 60825 1 11 2001 and may only be operated in compliance with the corresponding safety instructions of EN 60825 Part 1 and 2 with re gard to the laser emitter in the purview of the safety regulations of the German Trade Supervision The user must familiarise himself with the hazards involved with laser emitters before using the device Warning labels regarding the laser emissions are located on the inner doors of the device Caution Never look into the laser beam Never place reflective objects within the laser beam Wear appropriate safety goggles during maintenance or cali bration work on the open laser emitter lt 10 mW 655 nm The device equipped with a laser emitter may only be oper ated by authorised personnel The user of the device must familiarise himself with the haz ards
53. tte 17 can be measured in pure water 9 5 Measurement of Weakly Soluble Samples Even samples that are weakly soluble in liquid can be measured with the laser particle sizer analysette 22 To do this preparation of a saturated measuring liquid is recommended In this liquid the particle size cannot change by dissolving the measurement results therefore remain inac curate However the saturated solution must be filtered before use For very expensive products it is sometimes worthwhile to identify a replacement substance that takes over the task of saturating the measuring liquid analysette 22 NanoTec MicroTec Seite 59
54. uid approx 0 1 2 cm in 500 ml liquid dry approx liquid 10s liquid approx 10s dry approx 10s approx 0 1 2 cm in 500 ml liquid 0 1 0 5 cm in 100 ml liquid approx 10s FRITSCH se Dry Dispersion 0 1 1000 um 0 1 600 um 0 1 2000 um 0 1 2000 um Dimen sions 80 x 65 x 122 cm net 105 kg 80 x 65 x gross 140 kg 122 cm net 105 kg 80 x 65 x gross 140 kg 122 cm net 8 kg 14x 14x 32 cm gross 10 kg Dimen sions 80 x 65 x 94 cm 80 x 65 x 94 cm 80 x 65 x 94 cm 14x 14x 32cm net 105 kg gross 140 kg net 90 kg gross 125 kg net 75 kg gross 125 kg net 76 kg gross 125 kg net 8 kg gross 20 kg Seite 13 FRITSCH miig Module Dry Measu Sample Quanti Dimen Liquid ring ty sions Time Liquid Volume Combination device for dry approx dry net 105 kg 80 x 65 x liquid and dry measur liquid 10s 5 50 cm gross 140 kg 122 cm ing 22 4900 00 liquid approx 0 1 2 cm in 500 ml Device for liquid mea liquid approx approx 0 1 2 net 105 kg 80 x 65 x suring 10s cm in 500 ml gross 140 kg 122 cm 22 4940 00 iqui Device for dry measu dry approx net 105 kg 80 x 65 x 22 4960 00 Accessory NanoTec Dry MicroTec XT MicroTec XT S cb r fe c amp Liquid Dry 22 6900 00 Small quantity liquid dispersing unit 22 6750 00 Small quantity liquid dispersing unit 22 6700 00
55. uring cell is then moved to the re spective positions analysette 22 NanoTec MicroTec Seite 40 FRITSCH E uf SE 4 6 Mounting instructions Measuring Range Exten sion Kit WET 1 Configuration Set Configuration NanoTec MicroTec System Use Option for extended Measuring Range Please note the software instructions 2 Take the Measuring Extension Kit wet from the accessories case and remove lens caps analysette 22 NanoTec MicroTec Seite 41 FRITSCH 3 Introduce the body of the tube with locating pin 1 into the drilling planned for it 2 in the profile of the optical bench Insert the measuring range extension kit in such a way that the signature cell shows towards the measuring cell Put the rider on the profile and tighten the knurled thumb screw 3 4 Ready 5 For the disassembly of the measuring range extension kit pro ceed in reverse order analysette 22 NanoTec MicroTec Seite 42 FRITSCH ss 5 Dry Dispersing Unit 5 1 Preparing the Dry Dispersing Unit 5 1 1 Dry Dispersing Nozzle and Measuring Cell The dry dispersing nozzle with dry measuring cell is mounted on the right guide rail while facing the device This measuring cell also swivels automatically into the beam path of the laser To do this select the item Select Dry Dispersing Unit in the program for the NanoTec MicroTec After you have selected the option Background Adding Sample or Mea
56. use the windows are treated on their outside surfaces with an anti reflex coating you must still handle them very carefully A scratch in the anti reflex coating has the same effect as a scratch in glass Attention The anti reflex coating is very soft even cleaning with normal pa per tissues can damage the windows Always use lens cleaning paper from the accessories case Take the required tool from the accessory case and lay it ready analysette 22 NanoTec MicroTec Seite 45 FRITSCH se Remove the two screws on the upper cover plate of the dry measuring cell analysette 22 NanoTec MicroTec Seite 46 nd the upper measuri J u i Remove the upper cover plate a ng cell window Then you can remove both ceramic end pieces that are inserted as par allel stops for the measuring cell windows analysette 22 NanoTec MicroTec Seite 47 FRITSCH se _ FRITSCH Now clean the upper window The cleaning process is the same as de scribed for cleaning of the liquid measuring cell Now unscrew the front screw of the cover plate facing down Only loosen the rear screw You can then turn the lower cover plate around this screw to be able to remove the lower glass Attention When turning the cover plate make certain that the window does not fall out of the holder analysette 22 NanoTec MicroTec Seite 48 _ FRITSCH 4 Now clean the lower w
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