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Page 42 Operating Manual EM CPD300 12/18

13. Adjustments of Pressure Threshold for Bottle Empty

Function

The bottle empty function was developed to protect the samples if the CO

2

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

2

temperature. See list below. Green marked values indicate

optimal working temperature and pressure range.

CO

2

-Temperature (°C)

Recommended

threshold for pressure

(bar)

Pressure of full CO

2

-

Bottle (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

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44
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Содержание EM CPD300

Страница 1: ...From Eye to Insight OPERATING MANUAL EM CPD300 167180032 Version 12 18 ...

Страница 2: ...d 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 Haupt...

Страница 3: ... 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 For Research use only ...

Страница 4: ...s of the system before commissioning Particular attention must be paid to the aspect of safety Please retain this operating manual for future reference 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 protect...

Страница 5: ...illing the Sample Chamber with exchange fluid 28 7 5 Inserting Specimen into Sample Container 28 7 6 Preset of Cooling Temperature of the Sample Chamber 29 7 6 1 CO2 Bottle Temperature Pressure Function 29 7 7 Starting the EM CPD300 auto procedure 30 7 8 Time and timer function 30 8 Manual Operation of EM CPD300 35 8 1 Screen descriptions 35 8 2 Filling the chamber with exchange fluid 37 8 3 Inser...

Страница 6: ...CO2 Bottle Temperature Pressure Function 41 13 Adjustments of Pressure Threshold for Bottle Empty Function 42 14 Software Update 44 15 Service Notes 46 15 1 Gas Out filter maintenance 46 15 2 General maintenance 47 16 User Maintenance 48 16 1 Poral filter replacement 48 16 2 Cleaning 50 17 Warnings and Troubleshooting 51 ...

Страница 7: ...pair Following these instructions will help to prevent hazards reduce repair and downtime costs and prolong the system s service life Symbols 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 c...

Страница 8: ...ens 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 mem...

Страница 9: ...uipment 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 maintenanc...

Страница 10: ...ssure gas hose a free space of 150 mm has to be provided on the backside of the instrument Connection of CO2 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 It is important here to ensure that the CO2 Container is not equipped with a residual pressure valve In order to preven...

Страница 11: ...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 ...

Страница 12: ...ion 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 The environmental conditions that were agreed contractually and determined at the time of installation must be maintained The manufacturer will not accept liability for damage...

Страница 13: ... 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 Pc Critical Point Pt Triple Point A Air drying phase boundary crossing B and C Critical point drying no phase boundary crossing T C solid phase liquid phase gaseous phase...

Страница 14: ...ater in the cell is replaced by an exchange medium like acetone or ethanol which unlike water are very soluble with liquid CO2 After the replacement of the water by an exchange fluid this exchange medium is substituted with liquid CO2 through serial dilution steps Thereafter by increasing the temperature the pressure is increased proportionally and will transfer the CO2 through its critical point ...

Страница 15: ... Critical point drying with the EM CPD300 is the optimal method 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 31 kg Sample chamber Chamber dimension Ø 60 mm x 62 mm Volume 185 ml in empty chamber Pressure Safety bursting membrane 105 bar at 20 C 10 Software ...

Страница 16: ...ion Gas inlet M 12 x 1 5 Gas outlet Ø 8 mm inner diameter Requirements Transitional fluid Carbon Dioxide chemical formula CO2 CO2 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 ...

Страница 17: ... 12 18 7 Automatic Operation of EM CPD300 7 1 Screen descriptions Initialization screen Touch screen after initialization Main Screen Dark gray buttons can be activated light gray buttons are inactive 1 2 3 4 5 6 13 12 11 9 10 8 7 14 15 ...

Страница 18: ... of programmed process In auto version buttons have no function 8 Cooling temperature to keep CO2 fluid can be changed under settings page 37 9 CO2 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 dis...

Страница 19: ...flux of CO2 and before starting exchange process 8 Sets exchange speed from 1 10 The number relates to the setting of the needle valve during exchange 1 means a small opening and staying open for longer slow flowing speed 10 means a big opening for a short amount of time fast flowing speed The parameters where set in a way that after a minimum of 12 exchange cycles only liquid CO2 is left in the c...

Страница 20: ...Page 17 Operating Manual EM CPD300 12 18 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 ...

Страница 21: ...00 12 18 Filler Holder Panel 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 their volumes 4 Confirms filler and holder setting 1 2 3 4 ...

Страница 22: ...Page 19 Operating Manual EM CPD300 12 18 7 2 Programming by example Press Programs Press Program Name Type Program name ...

Страница 23: ...Page 20 Operating Manual EM CPD300 12 18 Activate stirrer Press OK to confirm program name Select stirrer speed Speed display will disappear after 4 sec ...

Страница 24: ...Page 21 Operating Manual EM CPD300 12 18 Activated stirrer symbol becomes green Set CO2 IN speed Press Fillers Program Filler Holder combination Example 1 2 Holder with 1 6 and 1 3 Filler ...

Страница 25: ...Page 22 Operating Manual EM CPD300 12 18 Press OK to confirm Filler Holder settings Press Delay Set Delay time Example Set to 2min ...

Страница 26: ...Page 23 Operating Manual EM CPD300 12 18 Press OK to confirm Press Exchange Speed Set Exchange Speed Example set to 5 Exchange Speed display will disappear after 4 sec ...

Страница 27: ...Page 24 Operating Manual EM CPD300 12 18 Press Exchange Cycles Set Exchange Cycles Example set to 12 ...

Страница 28: ...Page 25 Operating Manual EM CPD300 12 18 Press OK to confirm Set heating speed Example from medium to fast Set Gas out speed Example from fast to slow ...

Страница 29: ...Page 26 Operating Manual EM CPD300 12 18 Select slow speed setting Example Set to 100 slow Slow Gas out Speed display will disappear after 4 sec Press OK to confirm ...

Страница 30: ...Page 27 Operating Manual EM CPD300 12 18 Press Start to activate program Test ...

Страница 31: ...hen 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 co...

Страница 32: ...ling temperature of the pressure chamber is 15 C If the CO2 does not fill the chamber within a certain time Timeout CO2 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 CO2 temperature bottle which is cooler than the chamber temperature This means due to the low temperature difference the pressure of the CO2 in the bottle is not ...

Страница 33: ...rating Manual EM CPD300 12 18 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 The timer display pops up 2 1 2 ...

Страница 34: ...1 Operating Manual EM CPD300 12 18 Now you can change the local time 3 or set the timer with the keypad 4 The timer function is activated if watch symbol is green 5 Activated time fields become blue 6 4 3 6 5 ...

Страница 35: ...K and settings will be saved 7 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 To cancel timer settings press stop 9 8 7 9 ...

Страница 36: ...Page 33 Operating Manual EM CPD300 12 18 then pause 10 and cancel 11 Touch Process time field to check in the main screen the timer starting time 12 10 11 12 ...

Страница 37: ...Page 34 Operating Manual EM CPD300 12 18 and touch starting time to check finishing time 13 13 ...

Страница 38: ...0 12 18 8 Manual Operation of EM CPD300 8 1 Screen descriptions Initialization screen Touch screen after initialization Main Screen before start Dark gray buttons can be activated light gray buttons are inactive 1 2 3 4 5 6 7 8 9 10 11 ...

Страница 39: ...eed of CO2 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 ...

Страница 40: ...erted 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 Star...

Страница 41: ... again CO2 goes off The CO2 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 ...

Страница 42: ...he 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 CO2 which will change the physical status from supercritical to gaseous due to the pressure decrease under constant temperature 9 Removing Dried Specimen Close the shut off valve of the CO2 bottle Open the screw on ...

Страница 43: ...justing 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 ev...

Страница 44: ...not empty the reason for the warning is the CO2 temperature bottle which is cooler than the chamber temperature This means due to the low temperature difference the pressure of the CO2 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 CO2 temperature is then about 2 C cooler than the bottle s...

Страница 45: ... 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 CO2 temperature See list below Green marked values indicate optimal working temperature and pressure range CO2 Temperature C Recommended threshold for pressure bar Pressure of full CO2 Bottle bar 14 47 50 15 48 51 16 49 52 ...

Страница 46: ...re threshold see table above under the CO2 bottle empty pressure area Change CO2 bottle empty pressure threshold value according to the list on page 45 The CO2 temperature can be estimated by measuring bottle surface with thermometer CO2 temperature is then about 1 2 C cooler then the bottle surface Press Update to confirm ...

Страница 47: ...Page 44 Operating Manual EM CPD300 12 18 14 Software Update Insert USB stick with EM CPD300 software Software modules will be automatically recognized by the system Choose the module you want to update ...

Страница 48: ...Page 45 Operating Manual EM CPD300 12 18 After software update press back ...

Страница 49: ... Operating Manual EM CPD300 12 18 15 Service Notes 15 1 Gas Out filter maintenance After 100 runs are performed the following note appears Under Chapter 14 Maintenance the poral filter replacement is described ...

Страница 50: ...Page 47 Operating Manual EM CPD300 12 18 15 2 General maintenance After 500 runs a general maintenance is recommended ...

Страница 51: ...re has to be released in the sample chamber the CO2 bottle has to be closed and the CO2 connection to the EM 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 Remove nut which includes porous filter from the valve block ...

Страница 52: ...Page 49 Operating Manual EM CPD300 12 18 Remove poral filter with spring from the nut ...

Страница 53: ...h the correct size Poral filter 0 5 µm for CO2 Inlet left and Poral filter 75 100 µm for CO2 Outlet right Reassemble poral filter in to the nut and screw nut in valve block 16 2 Cleaning All surfaces can be cleaned with aqueous reagents or 60 ethanol and a clean cloth ...

Страница 54: ...tart if lid open Close lid 10E13 Separator missing Process can not start or continue if separator is missing Insert separator 10E14 Separator full Process can not start or continue if separator is full Empty separator 10E16 Heatup error Pressure too low Check CO2 bottle 10E17 Timeout CO2 IN CO2 bottle empty or poral inlet filter is clogged Check CO2 bottle or exchange poral inlet filter 100E3 Pres...

Страница 55: ... der Richtlinie conformément aux dispositions de directive Electromagnetic compatibility Elektromagnetische Verträglichkeit 2014 30EU Low Voltage Equipment Niederspannungsrichtlinie 2014 35EU RoHS directive RoHS Richtlinie 2011 65 EU declares in exclusive responsibility that the product erklärt in alleiniger Verantwortung dass das Produkt déclare sous sa responsabilité que le produit Model Modell ...

Страница 56: ...Leica Mikrosysteme GmbH Vienna Austria T 43 1 486 8050 0 F 43 1 486 8050 30 www leica microsystems com CONNECT WITH US ...

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