Leica EM CPD300 Operating Manual
Contents
1. Page 25 Operating Manual Leica EM CPD300 06112 7 3 Programming the EM CPD300 procedure Before placing the sample into the pressure chamber program the EM CPD300 protocol Switch to the program screen panel and follow the instructions under Program Panel see page 17 25 Do not forget adjustment of the pressure threshold for the bottle empty function see page 38 39 7 4 Filling the Sample Chamber with exchange fluid Open the screw on cover of the sample chamber by turning cover counter clockwise Sample Container with quick release pin Before filling the sample chamber with exchange fluid place the magnetic stirrer rod in bottom of the chamber Fill exchange fluid into the sample chamber until the stirrer is covered Then fill the sample container with exchange fluid to such a level that the sample holder and specimen will be completely submerged when inserted 7 5 Inserting Specimen into Sample Container Open lid and transfer prepared specimen into a suitable sample holder The sample holder must be filled with exchange fluid prior to transfer Insert the sample holder into the sample container and fill sample container with exchange fluid until the sample holder is covered Transfer the sample container into the sample chamber and check if sample holder is still covered with exchange fluid Adjust container volume if required with fillers or additional sample holders If sample holders with the v2. Code 10E11 10E12 10E13 10E14 10E16 10E17 100E3 100E4 100E5 Warning Com connection default Lid open Separator missing Separator full Heatup error Timeout CO IN Pressure sensor failure Pressure fault Temperature sensor failure Cause Process can not start if lid open Process can not start or continue if separator is missing Process can not start or continue if separator is full Pressure too low CO bottle empty or poral inlet filter is clogged Poral outlet filter blocked Page 49 Operating Manual Leica EM CPD300 06 12 Action Call Leica service Close lid Insert separator Empty separator Check CO bottle Check CO bottle or exchange poral inlet filter Call Leica service Exchange poral outlet filter Call Leica service fin MICROSYSTEMS EC Declaration EC Declaration of Conformity EG Konformit ts Erkl rung D claration CE de Conformite We Wir Nous Leica Mikrosysteme GmbH Hernalser Hauptstrasse 219 A 1170 Wien Austria declare in exclusive responsibility that the product erkl ren in alleiniger Verantwortung dass das Produkt d clarons sous notre seule responsabilit que le produit Model EM CPD300 Modell EM CPD300 mod le EM CPD300 Type Typenbezeichnung type EM CPD300 to which this declaration relates is in conformity with the following standards auf das sich diese Erkl rung bezieht mit den folgenden Normen ber
3. Living up to Life Leica EM CPD300 Operating Manual 167180032 Version 06 2012 MICROSYSTEMS Important Note Leica Mikrosysteme GmbH reserves the right to change technical specifications as vvell as manufacturing processes vvithout prior notice Only in this vvay is it possible to con tinuously improve the technology and manufacturing techniques used to provide our customers with excellent products Any copyrights of this document are retained by Leica Mikrosysteme GmbH Vienna Any reproduction of text and illustrations or any parts thereof by printing photocopy ing or other methods including electronic systems and media requires express prior permission in writing Issued by Leica Mikrosysteme GmbH Hernalser Hauptstrasse 219 A 1170 Vienna Leica EM CPD300 Operating Manual Leica EM CPD300 Serial Number Date of purchase For the instrument serial number please refer to the name type label on the back of the instrument Please read this instruction manual carefully before operating the instrument Forevvord This technical documentation is intended to provide essential information about the proper operation and servicing of the Leica EM CPD300 critical point dryer Service and operating staff must familiarize themselves with all components of the system before commissioning Particular attention must be paid to the aspect of safety Please retain this operating manual for future referenc
4. Page 14 Operating Manual Leica EM CPD300 06 12 Programm Screen Panel foi D Program Name MICROSTSZSTEME Progr rams CO IN Exchange Gas OUT Auto Speed Fillers Delay Speed Cycles Heat Speed fast med med fast fast fast fast fast SIN slow med fast KA se Pr He He Ho dra 1 Activates key pad to enter program name 2 Activated program is marked green 3 Stirrer on off with speed control 4 Activation of auto version If not highlighted manual version is active Only selectable in automated version 5 Sets speed of CO influx in pressure chamber Three possibilities slow medium fast 6 Switch to filler and holder panel Display of filler and holder status Sets delay time after influx of CO and before starting exchange process 8 Sets exchange speed from 1 10 9 Sets exchange cycles 12 cycles means one chamber volume is completely exchanged Minimum is 12 cycles 10 Sets heating speed for critical point Three possibilities slow medium fast 11 Sets gas out speed Possibilities slow medium fast Slow speed can be decreased up to 20 of its normal speed 12 Scrolls programs from 1 10 13 Confirms activated program Switch to main screen Page 15 Operating Manual Leica EM CPD300 06 12 Filler Holder Panel Program Name 1 Filler and holder panel 2 Status display of fillers and holders 3 Sets specific holder and fillers Combination of holders and fillers depends on thei
5. oo oo 100 a2 ae a Touch Flowrate Flowrate Separatorfull CO bottle empty max min Sanat wen 25 Page 42 Operating Manual Leica EM CPD300 06112 14 Software Update Insert USB stick with EM CPD300 software Leica Rare Connect service data stick to USB port Update date Software Part ID Cur Version New Version Update Update Update Update Software modules will be automatically recognized by the system Choose the module you want to update Leica MICROSYSTEMS Choose Software and click Update U date Software Part ID Cur Version New Version User Interface 6613 31 910 01 01 10 01 01 10 Update CPD Board 6613 31 901 01 02 03 01 02 03 Update Page 43 Operating Manual Leica EM CPD300 06 12 After software update press back were Updating Chamber Controller Software Pari ID Cur Version New Version User Interface 6613 31 910 01 01 09 01 01 09 Update Update c gt CPD Board 6613 31 901 01 02 03 01 02 04 Update Update Page 44 Operating Manual Leica EM CPD300 06 12 15 Service Notes 15 1 Gas Out filter maintenance Cooling temperature C Units Fo mu ud V dmg Heat temperature C CI psi Performed RUNS Www ug WU 100 Stirrer speed Advanced SLOW Gasout m in d M ali og Under Chapter 14 Maintenance the poral filter replacement is described Page 45 Operating Manual Leica EM CPD3
6. Year Month Day 2011 07 20 Or set the timer with the keypad 4 The timer function is activated if watch symbol is green 5 system Time aaa Hour Minute Second e nn a Year Month Day pen ere emm Gu wm a EE el eist Year Month Day iia m Second ER 2j ke Gac re Year Month Day 2017 07 19 e NEM R 6 1 6 Year Month Day mn om Page 29 Operating Manual Leica EM CPD300 06112 Press OK and settings vvill be saved 7 System Time Hour Minute Second 13 31 05 Year Month Day Start Time Hour Minute Wu ar Month In the main screen the green watch symbol beside the local time indication shows that time is activated 8 By activating the timer no programming or other changes are possible aai CPD300 AUTO ricer Filler 100 To cancel timer settings press stop 9 Page 30 Operating Manual Leica EM CPD300 06 12 then pause 10 CPD300 AUTO nas Filler 10074 and cancel 11 CPD300 AUTO uw Filler 100974 m zasdctniamk CPD300 AUTO nicer Filler 100 Page 31 Operating Manual Leica EM CPD300 06 12 and touch starting time to check finishing time 13 m audcniamk CPD300 AUTO mm le d CEP Page 32 Operating Manual Leica EM CPD300 06 12 8 Manual Operation of EM CPD300 8 1 Screen
7. 8870 3500 2 9878 1055 Austria Vienna 443 1 486 80 500 1 486 80 50 30 Belgium Groot Bijgaarden 32 2790 98 50 2790 98 68 Canada Concord Ontario 1 800 248 0123 847 405 0164 Denmark Ballerup 45 44540101 4454 0111 France Nanterre Cedex 33 811 000 664 156 05 23 23 Germany Wetzlar 49 6441294000 6441294155 Italy Milan 39 02574 861 02 574 03392 Japan Tokyo 81 3 5421 2800 3 5421 2896 Korea Seoul 182 25146543 251465 48 Netherlands Rijswijk 31 70 4132 100 70 4132 109 People s Rep of China Hong Kong 852 2564 6699 2564 4163 Shanghai 86 21 6387 6606 21 6387 6698 Portugal Lisbon 351 21 388 9112 21 385 4668 Singapore 65 67797823 6773 0628 Spain Barcelona 34 93 494 95 30 93 494 95 32 Sweden Kista 46 86254545 86254510 Switzerland Heerbrugg 441 117263434 117263444 United Kingdom Milton Keynes 444 800 298 2344 1908 246312 USA Buffalo Grovellllinois 1 800 248 0123 847 405 0164
8. Inserting Specimen into Sample Container ua aaa nana aaa nae enen e eee ea eee dani eee eee re ne eee kene eee ee veni 26 7 6 Preset of Cooling Temperature of the Sample Chamber 27 7 6 1 CO2 Bottle Temperature Pressure Function aaa aaa aaa nanen dan eee ek eee eee tere e kce ser eeate 27 Lf Starting the EM CPD300 auto procedure cosas anta iron PHE OE ebUt 28 7 8 Time and timer NCO NE ETE 28 8 Manual Operation of EM CPD300 nan naaaaannnnn nana ere ERKENNEN eren es nenes rene sere nes rene skenes eses see meme n se 33 US Gon o agote ee mm 33 8 2 Filling the chamber with exchange fluid AE 35 8 3 Inserting of Specimen into Sample Chamber 35 8 4 Coolingofthe Sample Chamber e netos 39 3 5 Filling the CO EE 36 3 6 Mixing the two liquid ne EE 36 3 7 Exchange media mixture from Sample Chamber 36 3 8 Heating the Sample Ee e 37 8 9 Releasing gaseous CO from Sample Chamber 37 9 REMOVING Dried Specimen vid as var din dr suas tuu j onu EENEG EG 37 10 Switching off the Unit eC nnne 37 11 Setting M En SEE TIT 38 12 CO Bottle Temperature Pressure Function nun ERKENNEN ane enen serine e rene nenes rene e rene rene ee mee 39 13 Adjustments of Pressure Threshold for Bottle Empty Function 40 14 Software Update e t A 43 139 S0 CS NOTOS emet rr todo 45 15 1 Gas Our filter maintenance ne dor oros 45 15 2 General EEN le
9. descriptions Initialization screen Touch screen after initialization EM CPD300 MANUAL Version 01 01 11 Main Screen before start 1239 Set Leica E ee MICNHOSTEZTEMSE CPD300 1 MANUAL Te Pc 1 0bar Le We Dark gray buttons can be activated light gray buttons are inactive Page 33 Operating Manual Leica EM CPD300 06 12 Main Screen after start 1241 Set MICHOSTYTSTEMS CPD300 MANUAL 1 Version of the EM CPD300 2 Status display temperature pressure 3 Switch to Settings see Page 37 4 Light on off 5 Process Start Stop 6 Stirrer on off Is controlled in setting panel see Page 37 7 Cooling temperature to keep CO fluid 8 Sets speed of CO influx in pressure chamber Three possibilities slow medium fast To inactivate press again 9 Sets exchange speed Speed from 1 10 Shows opening status of the needle valve To inactivate press again 10 Sets heating speed for critical point Three possibilities slow medium fast To inactivate press again 11 Sets Gas out speed Possibilities slow medium fast Slow speed can be decreased up to 20 of its normal speed Adjustment under Settings advanced slow Gas Out see page 37 12 Sets Time see page 27 Page 34 Operating Manual Leica EM CPD300 06 12 8 2 Filling the chamber with exchange fluid Do not forget adjustment of the pressure threshold for the bottle empty function See page 38 39 Open the scr
10. must be maintained The manufacturer will not accept liability for damage caused by misuse of the system or its use for purposes other than the intended use nor for damage caused by work on the system that is not described in this manual Page 8 Operating Manual Leica EM CPD300 06 12 4 Method 4 1 Critical Point Drying Method Drying water containing biological and material specimens in air or under vacuum can drastically alter their structures or even destroy them completely by tangential forces caused by surface tension of the water A The surface tension is a quality of surfaces between a liquid and a gas and the tangential forces appears by boundary crossing from liquid to gaseous phase Phase diagram P bar solid phase i supercritical fluid liquid phase 3 Bf BR ei d C Pt A gaseous phase t T C P Critical Point P Triple Point A Air drying phase boundary crossing B and C Critical point drying no phase boundary crossing Page 9 Operating Manual Leica EM CPD300 06 12 For biological and most micro electro mechanical MEM samples critical point drying cannot be performed with water Water s critical point is at 374 C and 228 5bar Every biological and MEM sample would be destroyed at this temperature and pressure Therefore the use of CO as transitional fluid is the first choice for critical point drying It is liquid at room temperature at a comparative low pressure of GObar lts c
11. 00 06 12 15 2 General maintenance Cooling temperature C Units lum F mu S mv Heat temperature K Performed RUNS amp mm 500 Stirrer speed Advanced SLOW Gasout i T NE Program 2 n se CA ELE CPD300 Page 46 Operating Manual Leica EM CPD300 06 12 16 User Maintenance chamber the CO5 bottle has to be closed and the CO connection to the EM U Before starting the maintenance the pressure has to be released in the sample CPD300 has to be disconnected 16 1 Poral filter replacement Remove front cover Use a 17 size wrench to open the nut in the valve block Page 47 Operating Manual Leica EM CPD300 06 12 Remove poral filter vvith spring from the nut Remove spring from poral filter Exchange poral filter with the correct size Poral filter 0 5 um for CO Inlet left and Poral filter 75 100 uim for CO Outlet right Reassemble poral filter in to the nut and screw nut in valve block Page 48 Operating Manual Leica EM CPD300 06 12 16 2 Cleaning All surfaces can be cleaned with aqueous reagents or 6096 ethanol and a clean cloth 17 Warnings and Troubleshooting The list below summarizes Warnings W Regarding most of the displayed information just follow the instructions in the case of error messages contacting your local Leica Service is required
12. e Texts schedules and tables may not be copied reproduced or divulged to third parties without the express consent of Leica Microsystems In addition all generally applicable legal and otherwise binding regulations for preventing accidents and protecting the environment must be observed by the user and communicated to all users Page 1 Operating Manual Leica EM CPD300 06 12 Table of contents E E 3 E E 4 2 1 Safety concept of Leica MIKroSysteme GEnDPI sun de em rire o tesa eoe pi 4 3 Installation and Warranty Ga Mcd EN ioUPO TUA UU SN SERE S IPLE RIA iia 6 SAN nn P m 6 SM MICA Um 3 T Et E E H Aa Cru cal Pont Drying i is o EU A 9 5 Description and Specification na nana nannnananne nanen ose rene e skenes eres e sere ese rene e eren eene nena anus ese e nese ee nes rene ee m se 11 5 1 Technical specifications aaa aaaa aa aaaa ene a nenen eee e eee ke ea teke ee teren eee eee ee tere teren ene re teke nnne nnns eee eee eene 11 6 Preparation of SpecimensS nanauuuananna nana ne na s nenen kene arres es rene se rene s eren es rene sere neser enes rene skenes eres es ee mese n se 12 7 Automatic Operation of EM CPD3O00 un naaunnnnnnne nanen nse kene skenes eres es eren e esen e eren sere nese eme es rene eee 13 MEME rita ce dai E 13 7 2 Programming by example m 17 7 3 Programming the EM CPD300 e een IEN 26 7 4 Filling the Sample Chamber with exchange fluid oomccccoccconcconnocccoconoccononcononcnnnnnns 26 7 5
13. e 20 Operating Manual Leica EM CPD300 06 12 Press OK to confirm Press Exchange Speed Set Exchange Speed Example from 5 to 7 Page 21 Operating Manual Leica EM CPD300 06 12 Exchange Speed N Exchange _ if display will ir ee E Fillers Delay Speed C Heat Speed disappear after 4 CM mo K t Ge GU Wm sec Press Exchange Cycles Set Exchange Cycles Example from 16 to 12 Page 22 Operating Manual Leica EM CPD300 06 12 Press OK to confirm Set Heating Speed Example from medium to fast Set Gas out Speed Example from fast to slow Page 23 Operating Manual Leica EM CPD300 06 12 T Programs Select slow CO IN xchange Gas OUT 7 speed setting N 2 XU E EE TOT y He peri Example from 100 to 75 slow Slow Gas out Speed display will disappear after 4 sec Press OK to confirm a da d i gat D Se Ae T S E n E d 7 d Tast Kai a4 asi Ar Le d ig p SS L 1 1 e d DES J GR E Ga e E R num a Um um med EE Se Ki 3C med a Kg Page 24 Operating Manual Leica EM CPD300 06 12 Press Start to activate program Test een noo ei CPD300 AUTO em E qp a E ME Eet p H J i
14. einstimmt auquel se r f re cette d claration est conforme aux normes EN 61010 1 EN 61326 1 following the provisions of directive gem ss den Bestimmungen der Richtlinie conform ment aux dispositions de directive 2004 108 EC Electromagnetic compatibility Elektromagnetische Vertr glichkeit 2006 95 EC Low Voltage Equipment Niederspannungsrichtlinie V2 Wien 17th June 2011 Dr Reinhard Lihl Entwicklungsleiter R amp D Manager Chef du service d veloppement Leica Microsysteme GmbH Tel t43 1 48899 Hernalser Hauptstrasse 219 Fax 43 1 48899 350 A 1170 Wien www leica microsystems com www leica microsystems com CLCCL MICROSYSTEMS The statement by Ernst Leitz in 1907 With the User For the User describes the fruitful collaboration with end users and driving force of innovation at Leica Microsystems We have developed five brand values to live up to this tradition Pioneering High end Quality Team Spirit Dedication to Science and Continuous Improvement For us living up to these values means Living up to Life Leica Microsystems operates globally in four divisions where we rank with the market leaders LIFE SCIENCE DIVISION The Leica Microsystems Life Science Division supports the imaging needs of the scientific community with advanced innovation and technical expertise for the visualization measurement and analysis of microstructures Our strong focus on understanding scientific application
15. ellow box If the poral filter is clean and the bottle is not empty the reason for the warning is the CO temperature bottle which is cooler than the chamber temperature This means due to the low temperature difference the pressure of the CO in the bottle is not sufficient to fill up the chamber The temperature of the bottle can be estimated by measuring the bottle surface with a thermometer The CO temperature is then about 2 C cooler than the bottle surface Decrease the chamber temperature according to the list below and fill again The green marked values indicate the optimal working temperature and pressure range Example If the bottle surface temperature is 22 C the estimated CO temperature is 20 C the cooling temperature of the chamber should be set to 15 C Recommended pressure chamber CO Temperature C cooling temperature C 14 9 15 10 16 11 18 13 20 15 22 17 24 19 25 20 26 21 28 29 Page 39 Operating Manual Leica EM CPD300 06 12 13 Adjustments of Pressure Threshold for Bottle Empty Function The bottle empty function was developed to protect the samples if the CO bottle becomes empty during a run When the warning occurs all valves will be closed so that the pressure chamber is sealed and the empty bottle can be exchanged with reduced possibility of sample damage The threshold for this function has to be adapted to the CO temperature See list below Green marked values indicate optimal working te
16. ew on cover of the sample chamber by turning counter clockwise Spacer with magnetic Stirrer Before filling the sample chamber with exchange fluid place the magnetic stirrer rod together with the spacer into bottom of the sample chamber Fill exchange fluid into the sample chamber until the stirrer and spacer is covered Fill the sample chamber with exchange fluid to such a level that the specimen holder with specimen will be completely submerged when inserted 8 3 Inserting of Specimen into Sample Chamber Open lid and transfer prepared specimen into a suitable sample holder Quickly insert the sample holder with the specimen into the sample chamber filled with exchange fluid Check if sample holder is still covered with exchange fluid 8 4 Cooling of the Sample Chamber After tightly closing the screw on cover of the sample pressure chamber press Start Press the cooling button and wait until pressure chamber cools up to the preset cooling temperature 15 C factory setting The cooling temperature depends on the bottle temperature Please see sub chapter 7 6 1 CO2 Bottle Temperature Pressure Function to select the appropriate cooling temperature The cooling unit automatically keeps the temperature at the preset cooling temperature or below Page 35 Operating Manual Leica EM CPD300 06 12 8 5 Filling the CO into Sample Chamber Wait until the sample chamber temperature has reached 15 C Once this temperature is reached c
17. f the CO in the bottle is not sufficient to fill up the chamber The temperature of the bottle can be estimated by measuring the bottle surface with a thermometer The CO temperature is then about 2 C cooler than the bottle surface Decrease the chamber temperature according to the list below and fill again The green marked values indicate the optimal working temperature and pressure range Example If the bottle surface temperature is 22 C the estimated CO temperature is 20 C the cooling temperature of the chamber should be set to 15 C Recommended pressure chamber SOTEM ey cooling temperature C 14 9 19 10 16 11 18 13 20 15 22 17 24 19 25 20 26 21 28 23 Fully open the shut off valve of the CO bottle Page 27 Operating Manual Leica EM CPD300 06 12 7 7 Starting the EM CPD300 auto procedure After programming go back to the main menu and press start 7 8 Time and timer function Press timer function 1 m zasdcniamk CPD300 AUTO us Filler 100 Es 1 8 5 ec J WW LINE i System Time Hour Minute Second 13 31 os Year Month Day 2011 07 19 Start Time Hour Minut t9 Year Month 2011 07 20 Page 28 Operating Manual Leica EM CPD300 06 12 Now you can change the local time 3 System Time Gi EN H Hour Minut Second 13 05 au Lage Cau site Start Time ko Heur Minute 13 31
18. he backside of the instrument Connection of CO Container It is absolutely necessary to use a pressurized gas container with a pipe feed pipe so that the medium CO2 can reach the specimen pressure chamber in liquid form T In order to prevent accidents the CO pressurized gas container must be AN securely fastened in an upright position Screw the high pressure gas hose onto the CO IN connection Page 6 Operating Manual Leica EM CPD300 06 12 Connect the other end of the high pressure gas hose to the gas pressure container The high pressure gas hose and seal are included in the accessory set of the unit Electrical Connection Check assigned connecting voltage of the unit Connect power cable to wall socket Page Operating Manual Leica EM CPD300 06 12 3 2 Warranty The EM CPD300 is covered by a WARRANTY in accordance with the conditions of sale If functional errors should occur or if the components of the system sustain damage that is subject to warranty coverage during the warranty period the manufacturer will repair or replace the faulty components following examination thereof The manufacturer warrants for the system in its original configuration Only original replacement parts may be used The manufacturer accepts no liability for damage caused by use of other replacement parts Caution AN The environmental conditions that vvere agreed contractually and determined at 4 the time of installation
19. hod to prevent the damaging effects of the above mentioned forces by bringing the liquid to the gas phase without boundary crossing 5 1 Technical specifications Dimensions Weight Empty weight Sample chamber Chamber dimension Volume Pressure Safety bursting membrane Software controlled cut off Max operating pressure Software controlled Temperature Heating range Software controlled cut off Heating time Slow Heating time Medium Heating time Fast Page 11 Operating Manual Leica EM CPD300 06 12 31 kg 60 mm x 62 mm 185 ml in empty chamber 105bar at 20 C 80bar 9bar 10 adjustable 30 C to 45 C gt 45 C 1 C min 2 C min 3 C min Cooling Cooling capacity Refrigerant Quantity Cooling range Cool down time Electrical Connection Voltage Frequency Power consumption Gas Connection Gas inlet Gas outlet Requirements 90 VV at 5 C 2500 1 min R134a 120 g adjustable 5 C to 25 C 2 0 C min 100 V 230 V 50 60 Hz 170 VA M 12x 1 5 8 mm inner diameter Transitional fluid Carbon Dioxide chemical formula CO CO pressure bottle with feed pipe Exchange fluid Acetone Ethanol 6 Preparation of Specimens Wash in a physiological salt solution Fix chemically with a suitable fixing agent Wash out fixing agent with a suitable buffer solution Dehydrate the chemically fixed specimen with acetone or ethanol Protocol examples are sho
20. l temperature and the critical pressure 31 C and 73 8 bar for CO have been passed the liquid CO is transformed into the supercritical status The system will stop at 35 C and 79 bar to be safe on the supercritical state The change of the physical state can be observed through the front viewing glass 8 9 Releasing gaseous CO from Sample Chamber After reaching the supercritical status choose the GAS OUT speed slow medium or fast and press the GAS OUT button The temperature will be constant at 35 C only when the valve is opening to release the COs which will change the physical status from supercritical to gaseous due to the pressure decrease under constant temperature 9 Removing Dried Specimen i Close the shut off valve of the CO bottle Open the screw on cover of specimen sample chamber Remove specimen holder with dried specimen from sample chamber for further processing Since the dried specimen is highly hygroscopic it has to be coated as quickly as possible with a thin metal or carbon film to protect it from atmospheric humidity If this is not possible it is recommended to keep the specimen in a desiccator until it is processed further 10 Switching off the Unit i Leave the sample chamber open Leave the CO bottle closed Switch off the main switch located on the unit Page 37 Operating Manual Leica EM CPD300 06 12 11 Setting Panel Dark gray buttons can be activated light gray buttons are inacti
21. mperature and pressure range Seinen Cle Pressure of full CO CO Temperature C threshold for pressure S Bottle bar bar 14 47 50 15 48 51 16 49 52 18 52 55 20 54 57 22 57 60 24 60 63 25 61 64 26 63 66 28 66 69 Page 40 Operating Manual Leica EM CPD300 06 12 Adjustments of Pressure Threshold Press Settings select Service enter password see operating manual and press ok 3 MICROSYSTEMS Cooling temperature I C In the advanced settings screen touch the CO bottle empty pressure threshold area Advanced settings Valve open Valve closed Finish Time NV position Time NV position Minimum Valve open see mm P sec mm X Cycles sec Teo 100 12 6 Touch Flowrate Flowrate Separator full CO bottle empty max min Sanam _brosaure PADIT 160 j EN Page 41 Operating Manual Leica EM CPD300 06 12 Change CO bottle empty pressure threshold value according to the list on page 45 The CO temperature can be estimated by measuring bottle surface with thermometer CO temperature is then about 1 2 C cooler then the bottle surface Leica Advances A Exc Valve open Valve Tim NY position Time ss N CO2 bottle empty preassure bar Press Back to confirm Advanced settings Exchange Valve open Valve closed Finish Time NV position Time NV position Minimum Valve open sec mm p sec mm Cyeles sec o
22. olume of 33 5096 are used more sample holders or fillers can be added to the pressure chamber up to 100 Fully open the shut off valve of the CO bottle Page 26 Operating Manual Leica EM CPD300 06 12 7 6 Preset of Cooling Temperature of the Sample Chamber The pressure chamber cools up to the preset cooling temperature 15 C factory setting The cooling temperature depends on the bottle temperature Please see chapter 7 6 1 CO5 Bottle Temperature Pressure Function to select the appropriate cooling temperature The cooling unit automatically keeps the temperature at the preset cooling temperature or below see subchapter 7 6 1 below 7 6 1 CO Bottle Temperature Pressure Function For correct filling of the pressure chamber with CO a temperature difference of 4 C minimum and a pressure difference of 5 bar is essential Therefore the pressure chamber has always to be minimum 4 C cooler than the CO Bottle see list bellow You can find the adjustment of pressure chamber temperature under settings see operating manual The factory preset cooling temperature of the pressure chamber is 15 C If the CO does not fill the chamber within a certain time Timeout CO IN shows in the yellow box If the poral filter is clean and the bottle is not empty the reason for the warning is the CO temperature bottle which is cooler than the chamber temperature This means due to the low temperature difference the pressure o
23. ompletely open the shut off valve of the CO bottle Press CO In with the selected speed slow medium or fast The pressure display shows the pressure in the sample chamber identical to the pressure in the CO bottle Fill the sample chamber up to the upper edge of the front viewing glass with liquid CO Fill up to here with liquid CO Press the CO In button again CO goes off The CO level in the sample chamber may rise slightly 8 6 Mixing the two liquid media Press the STIRRER key The magnetic stirrer is switched on The magnetic stirrer should not be used if the specimens are very delicate 8 7 Exchange media mixture from Sample Chamber Press the EXCHANGE button Drain the media mixture from the sample chamber until the specimen is barely covered by the liquid Press the EXCHANGE button again to close This procedure of filling mixing and draining needs to be repeated several times minimum 12 times before heating to remove all the exchange fluid from the specimens Multiple and or larger specimens require more changes Page 36 Operating Manual Leica EM CPD300 06 12 8 8 Heating the Sample Chamber Press the HEAT button and wait until sample chamber is heated up to 35 C The cooling unit automatically keeps the temperature of the pressure chamber at 35 C With the rising temperature the pressure in the sample chamber also increases as shown on the display At the time the critica
24. r 46 10 User Maintenance EE AT 16 1 Poral filter replacement E 47 MZ ne E 49 17 Warnings and TroubDleshoO llfig arse gege ao eiii 49 Page 2 Operating Manual Leica EM CPD300 06 12 1 Introduction In order to ensure the safety of service technicians and operators and to prevent any damage to the Leica EM CPD300 critical point dryer it is essential to carefully read this manual before beginning any work with the system This Operating Manual is intended to help the user understand the system more completely to use it within the specified limits of its working capabilities and to maintain in accordance with its physical parameters This user manual includes important information regarding proper installation operation troubleshooting and repair Following these instructions will help to prevent hazards reduce repair and downtime costs and prolong the system s service life oymbols in this manual and their meaning Danger All paragraphs in the Technical Documentation that contain instructions regarding possible hazards are identified with this symbol Non observance these alerts may result in serious injury Users of the instrument must comply with instructions at all times Caution AN This symbol alerts the user to important information which may endanger staff or result in damage to the system ifit is ignored Notel This symbol indicates further informa
25. r volumes 4 Confirms filler and holder setting Page 16 Operating Manual Leica EM CPD300 06 12 7 2 Programming by example Program tame Program 1 Press Programs wen ic e ln dr i CPD300 AUTO totor Filler 0 Exchange Gas OUT S CIS Press Program Name Speed Em Heat Type program name ip Ea 7 3 H F N I Page 17 Operating Manual Leica EM CPD300 06112 Press OK to confirm program name Activate Stirrer Et Fillers Delay Speed Cycles Heat mi E gt T gt 1 N F T mq t lt q s D am A r1 E Pee LPL A EN ICU T i TI i Ld d nae j z EI d Mi y me N z i T x E 7 7 B e sek g dp E as d wb m y ko wm E d L Ls TUE drams d stirrer Speed Cycles Heat We i med Speed display will disappear after 4 sec Page 18 Operating Manual Leica EM CPD300 06 12 Activated Stirrer Symbol becomes green Set CO IN speed Example from slow to fast Press Fillers Program Filler Holder combination Example 1 2 Holder with 1 6 and 1 3 Filler Page 19 Operating Manual Leica EM CPD300 06 12 Press OK to confirm Filler Holder settings Press Delay Set Delay Time Example changed from 120s to 100s Pag
26. ritical point is at 31 C and 73 8bar Technically these temperature and pressure requirements of the CO can be implemented relatively easily Hence the water in the cell is replaced by an exchange medium like acetone or ethanol which unlike water are very soluble with liquid CO After the replacement of the water by an exchange fluid this exchange medium is substituted with liquid CO through serial dilution steps Thereafter by increasing the temperature the pressure is increased proportionally and will transfer the CO through its critical point into a supercritical state B At constant temperature the controlled and carful depressurization converts the supercritical CO into its gaseous phase without crossing the phase boundary between liquid and gas C After coating the dried sample can be analyzed in a scanning electron microscope SEM Comparison between air and critical point drying Air dried sample Water flea Page 10 Operating Manual Leica EM CPD300 06 12 5 Description and Specification Introduction Biological specimens intended for investigation in a scanning electron microscope must be dried before being introduced into the microscope to allovv the specimen to be imaged If specimens with water content are dried tangential forces caused by surface tension of the water destroys the structures of the specimen as mentioned in the previous chapter Critical point drying with the EM CPD300 is the optimal met
27. s puts Leica Microsystems customers at the leading edge of science INDUSTRY DIVISION The Leica Microsystems Industry Division s focus is to support customers pursuit of the highest quality end result Leica Microsystems provide the best and most innovative imaging systems to see measure and analyze the microstructures in routine and research industrial applications materials science quality control forensic science inves tigation and educational applications BIOSYSTEMS DIVISION The Leica Microsystems Biosystems Division brings histopathology labs and researchers the highest quality most comprehensive product range From patient to pathologist the range includes the ideal product for each histology step and high productivity workflow solutions for the entire lab With complete histology systems featuring innovative automation and Novocastra reagents Leica Microsystems creates better patient care through rapid turnaround diagnostic confidence and close customer collaboration MEDICAL DIVISION The Leica Microsystems Medical Division s focus is to partner with and support surgeons and their care of patients with the highest quality most innovative surgical microscope technology today and into the future Leica Microsystems an international company with a strong network of worldwide customer services Active worldwide Tel Fax Australia North Ryde 61 2
28. s responsible for her his own health Only instructed users authorized by the customer are allowed to work at or with the system For all interaction with the EM CPD300 the user must wear protective clothing prescribed in the respective environment It is strictly prohibited to alter or remove protective equipment or covers of any kind Every user must be trained in safe handling of the process gases and fluids that are utilized in the EM CPD300 unit After every repair the user technician must verify a flawless state of the system by a test run Leica can guarantee full operation of the system only if original spare parts according to the part lists are used Careful operation and preventive maintenance of the EM CPD300 reduces maintenance costs and assures reliable operation By means of frequent checks and prompt rectification of even small damages considerable damage can often be avoided Observation of this operating manual and all notes installed on the system serves your own safety Page 5 Operating Manual Leica EM CPD300 06 12 3 Installation and Warranty 3 1 Installation Required space for setting up the unit width 340 mm depth 583 mm Operating room temperature 20 35C at 1bar CO bottle limit Relative humidity 5 90 To allow adequate intake of cooling air required for the refrigeration unit and due to the inflexibility of the high pressure gas hose a free space of 150 mm has to be provided on t
29. tion relating to a previous explanation which does not have a safety critical function However it is important to follow this information to ensure that the system functions optimally Page 3 Operating Manual Leica EM CPD300 06 12 2 Safety Warning The EM CPD300 critical point dryer can be operated simply and safely if the system is operated according to the operating manual 2 1 Safety concept of Leica Mikrosysteme GmbH The use in accordance with regulations of the EM CPD300 critical point dryer consists of critical point drying of biological or industrial samples with minimal deformation of the specimens for subsequent SEM analysis Any other application without written approval of the manufacturer can lead to damages and injuries of instrument and user The manufacturer refuses to take any responsibility for damage caused thereby The sample pressure chamber with a maximum working pressure of 150bar is secured with a Software and Hardware Cut Off function Hardware controlled cut off Bursting membrane at 105bar at 20 C 10 Software controlled cut off Pressure at 80bar and temperature at 45 C For safe operation it is absolutely necessary to set up and connect the device according to the instructions in Chapter 3 Page 4 Operating Manual Leica EM CPD300 06 12 General safety regulations Generally the following safety regulations apply to the handling of the EM CPD300 critical point dryer Every user i
30. ve Leica Settinas Cooling E C Units Volume _ f Dk E d be Performed RUNS mun ole Advanced SLOW Gasout 1 Sets cooling temperature to keep CO fluid Not recommended to change 2 Sets heating temperature to reach the critical point Not recommended to change 3 Sets stirrer speed recommended adjusting to sample sensitivity 4 Press Main to switch to main screen 5 Press update for software updates USB 6 Service Panel just for Service technician see Service Manual 7 Adjustment of Gas out speed at slow Function under settings only in the manual version accessible In the auto version the advanced slow Gas out speed adjustment is accessible under program display see page 15 8 System counts every complete run for maintenance advices see page 40 9 Volume change 10 Physical unit change Page 38 Operating Manual Leica EM CPD300 06112 12 CO Bottle Temperature Pressure Function For correct filling of the pressure chamber with CO a temperature difference of 4 C minimum and a pressure difference of 5 bar is essential Therefore the pressure chamber has always to be minimum 4 C cooler than the CO Bottle see list bellow You can find the adjustment of pressure chamber temperature under settings see operating manual The factory preset cooling temperature of the pressure chamber is 15 C If the CO does not fill the chamber within a certain time Timeout CO IN shows in the y
31. wn in the EM CPD300 Application booklet Page 12 Operating Manual Leica EM CPD300 06 12 T Automatic Operation of EM CPD300 7 1 Screen descriptions Initialization screen Touch screen after initialization Version 1 01 15 CPD300 AUTO hoger Filler 0 Tc 17 C M PN Se Pc 1 0 bar Heat slow 35 C ER Process time 1 20 40 Gas OUT l slow 100 Dark gray buttons can be activated light gray buttons are inactive Page 13 Operating Manual Leica EM CPD300 06 12 1 Version ofthe EM CPD300 2 Switch to program panel see page 15 3 Status display of fillers and holder in the sample chamber Programmable under programs 4 Status display temperature pressure and time to finish the process last point only with auto function 5 Switch to settings see page 37 6 Light on off 7 Status display of programmed process In auto version buttons have no function 8 Cooling temperature to keep CO fluid can be changed under settings page 37 9 CO influx speed in pressure chamber Programmable under programs 10 Exchange speed 1 10 and status of finished exchange cycles Programmable under programs 11 Heating speed and heating temperature for critical point Programmable under programs 12 Status display gas out speed Programmable under programs 13 Process start after defining program 14 Timer function see page 27 15 Program name of activated program see page 15
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