Fisher Bioblock Scientific ALPHA 1-4 LD-2 User manual

Gefriertrocknungsanlagen
OPERATING MANUAL
Freeze Dryer
ALPHA 1-4 LD-2
(Best.-Nr. 101041 / 101141 / 101241)
ALPHA 2-4 LD-2
(Best.-Nr. 101042 / 101142 / 101242)
MAR T I N C H R I S T
Gefriertrocknungsanlagen GmbH

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 2
Operating Manual ALPHA1-4 LD-2 and ALPHA2-4 LD 2
Order Number:
Serial Number:
In case ofinquiries or repair please state the above numbers.
For service please contact:
MARTIN CHRISTGefriertrocknungsanlagen GmbH
An der unteren S se 50, D-37520 Osterode
Tel. [phone], Telefax(05522) 5007-12

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 3
Preface
Dear customer,
Congratulations on purchasinga CHRIST freeze dryer.
The freezedryer is equipped with user-friendlyoptions which makethe operation
easier for you.
The newlydesigned ALPHA 1-4LD-2 /ALPHA 2-4LD-2 is auniversallyusable
CHRIST freezedryer for laboratories, R&D departments and scientific institutes. The
well proven rangeofaccessories allowsapplication oriented configuration ofthe
equipment especiallyfor routine use. Apractical and universallyusable rangeof
accessories is available for almost all applications for dryingin round bottom flasks,
dishes, ampoules and injection vials.
Aspecial advantageis the user-friendlycontrol system LD (Lyo-display), the functions
ofwhich are explained on the control panel:
- LC displayshowingthe most important process data (temperature ofice
condenser, vacuum)
- Conversion oftemperature and vacuum in accordance with the vapour pressure
curve above ice
- RS-232 communications interface (PC) is available as an option.
Especiallyworth mentioningis the possible retrofittingofavacuum measuringsensor
(type TPR 265) which onlyhas to be plugged in at the backofthe unit. This freeze
dryer offers a wide range offunctions for a varietyofpractical applications.
Wethankyou for your confidence and wish you asuccessful application ofthe freeze
dryer.
MARTIN CHRIST Gefriertrocknungsanlagen GmbH
An der unteren S se 50 - D-37520 Osterode
Tel. [phone], Telefax+49 (0) 5522/5007-12
Internet: www.martinchrist.de, e-mail: inf[email protected]

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 4
Contents:
Page
1 General Information
1.1 Introduction
7
1.2 Application
7
1.3 Technical specifications offreeze dryer ALPHA1-4 LD-2 /
ALPHA2-4 LD-2
8
1.4 Standards and regulations
10
1.5 Safetyinstructions
10
1.6 Prohibited freeze dryingprocesses 11
2 Installation and Commissioning of the Unit
2.1 Site ofinstallation
13
2.2 Mains electricity
13
2.3 Fuses on site
13
2.4 Checkingthe Earth connection
2.5 Defrostingwater
13
14
2.6 Vacuum pump exhaust
14
2.7 Initial start-up
15
2.7.1 Connection ofvacuum pump and installation ofaccessory
components
2.7.2 Functional components and control elements
2.7.3 Preparation for evacuation
2.7.4 Evacuation
15
21
22
22
2.8 Error messages 22
^2.9 Error resolution 23

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 5
3 Control System LD-2
24
3.1 Mains switch
25
3.2 "°C mbar" button
25
3.3 " " Button
25
3.4 Connection ofthe vacuum measuringsensor TPR 265
26
4 General Information on Freeze Drying
27
4.1 Freezing
29
4.2 Main drying
30
4.3 Final drying
34
4.4 End ofdryingand venting
34
4.5 Defrosting 34
5 Description of the Freeze Drying Processes
5.1 Freezingseparatelyand dryingon shelves
35
5.2 Dryingwith sealingdevice
35
5.3 Freezingseparatelyand dryingin round bottom flasks
36
5.4 Freezingseparatelyand dryingin ampoules usinga manifold 36
6 Maintenance
6.1 Vacuum pump
38
6.2 Exhaust filter
38
6.3 Ice condenser chamber
38
6.4 Rubber valves
38
6.5 Condenser for coolingliquid
39
6.6 Adjustment ofthe vacuum measuringsensor TPR 265
39
6.7 Cleaning
40

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 6
6.7.1 Cleaningofthe freeze dryer
40
6.7.2 Cleaningofaccessories
40
6.7.3 Maintenance ofthe condensate drain valve
41
6.7.4 Disinfection ofchamber and accessories
41
6.7.5 Operator checks
41
7 Instructions for Error Correction
7.1 Power failure
42
7.2 Insufficient vacuum
42
7.3 Unit does not function
43
7.4 Insufficient ice condenser temperature
44
8 Appendix
Declaration ofconformityfor ALPHA 1-4 LD-2 / 2-4 LD-2
…………………………………………………………………………………………
Explanation to the panels ALPHA 1-4 LD / 2-4 LD
Explanation to the panels ALPHA 1-4 LD-2 / 2-4 LD-2
…………………………………………………………………………………………
Operatingmanual ofthe vacuum pump (onlyin case ofdelivery)
Operatingmanual ofthe exhaust filter (onlyin case ofdelivery)
…………………………………………………………………………………………
……….Separate leaflat “The freeze dryer ofthe ALPHA-series”
Accessories leaflat “The accessoryfor freeze drying”
General leaflat “The program ofthe freeze dryers”
…………………………………………………………………………………………
Chemical properties ofPLEXIGLAS
(acrylic glass, material ofdryingchamber)
Disinfectant sprayINCIDUR
Return Declaration
Declaration ofContamination

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 7
1 General Information
1.1 Introduction
What is freeze drying?
Freeze drying means:Extraction ofwater from frozen material. The dryingprocess
takes place byavoiding the liquid state through sublimation, i. e. direct conversion from
ice to vapour. This happens under vacuum, when the temperature in the product is
less than -10°C.
The aim of freeze drying is to obtain an easilywater soluble product which will have
the same characteristics as the original product after addition ofwater.
As the drying process takes place in frozen state at verylowtemperatures it is possible
to drye. g.albumen which will remain water soluble. Also most ofthe other chemical
compounds will be qualitativelyand quantitativelyunchanged.
Freezedrying(lyophilisation) is also the most gentle process for preservingthe
biological properties ofsensitive tissue and tissue components.
Through freeze drying the product, mainlyofbiological origin - such as tissues, tissue
extracts, bacteria, vaccines and sera - is transformed into adryproduct. Duringthis
process enzymatic, bacterial and chemical changes are largelyavoided.
1.2 Applications
The freezedryer ALPHA1-4LD-2 /ALPHA2-4LD-2 is ahigh-performance, universal
laboratoryand pre-production unit for freezedryingofsolid or liquid products in
ampoules, bottles, glass flasks, wide-neckfilter bottles or dishes. All operations
necessaryfor freeze dryingare possible inside the unit:
− Freezing
− Freeze drying
− Final drying
The freezedryer ALPHA1-4LD-2 /ALPHA2-4LD-2 is suitable for dryingofe. g.
bacteria and virus cultures, blood plasma, serum fractions, antibodies, sera, vaccines
and pharmaceutical products such as chloramphenicol, streptomycin, vitamins,
ferments as well as plant extracts for biochemical tests.

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 8
1.3 Technical Specifications of Freeze Dryer
ALPHA1-4 LD-2 / ALPHA2-4 LD-2
Performance data:
Ice condenser capacity: max. 4 kg max. 4 kg
Ice condenser performance: max. 4 kg/24 h max. 4 kg/24 h
Ice condenser temperature:
Approx. -54°C approx. –84°C
Shelftemperature when freezinginside
the ice condenser chamber: Approx. -25°C approx. –50°C
Max. shelfsurface area when drying
outside the ice condenser chamber: 5xshelfsurface areas 360
Max. shelfsurface area when dryingin
injection vials (accordingto DIN) with sealing
under vacuum or nitrogen atmosphere:
Onlyoutside, with 4xshelf
surface areas 250
Dryingin round bottom flasks, e. g. each 300 ml: 24 pieces with additional
chamber
Other data:
Dimensions ofthe unit: width: 390 mm
height: 415 mm
depth: 540 mm
(incl. vacuum flange connection)
Weight: approx. 42 kg approx. kg
Noise emissions accordingto DIN 45635
Electromagnetic compatibilityaccordingto EN
55011:
dB (A) dB (A)
class B
Filling quantities:
Refrigerant: see label on the backofthe unit
Connection requirements:
Electric connection: 230 V, 50 –60 Hz
(others on request) and central
groundingconnection

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 9
Max. power consumption: 0,92 kVA 1,84 kVA
Max. current: 4,0 A 8,0 A
Safetyprecaution
6,3 AT 10 AT
Max. ambient temperature climate categorySN
+10°C to +32°C
(higher temperatures on request)
Equipment connections:
Vacuum connection: small flange connection
DN 25 KF
(ISO 28403, DIN 2861)
Condensate drain: hose nozzle DN 10 with
0.5 m silicon hose
(D=8 xs = 2mm)
Scope of supplyincludes:
1 tube high-vacuum grease
1 litre vacuum pump oil (ifpump is supplied)
1 operatingmanual and detailed technical documentation
0.5 m condensate drain hose (silicon 9 x12 mm)
Scope of supplydoes not include:
− Commissioningofthe unit will be carried out on request and charged at cost.
− Installation ofthe exhaust pipe ofthe vacuum pump (not necessarywhen usingan
exhaust filter).

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 10
1.4 Standards and Regulations
Please refer to the enclosed EU-Statement ofConformity.
1.5 SafetyInstructions
1.5.1
CAUTION!Disconnect Mains Plug!
As current-carryingparts are accessible inside the unit the mains plugmust be
disconnected before the side panels are opened. For maintenance the unit must be
switched off with the mains switch.
1.5.2
CAUTION!Solvents!
Acidic products or products with ahighsolvent concentration cannot be dried without
special protectivemeasures and devices such as e.g.acoolingtrap for protection of
the vacuum pump (ifnecessarycheckwith our service department).
Special caution is necessarywhen using azides because adangerous explosive
develops in combination with copper or non-ferrous metals!It is absolutely
essential to consult our company!
1.5.3
ADVICE!Cleaning and Maintenance of the Unit!
For infectious, toxic, pathogenic and radioactivesubstances the correspondingsafety
regulations must be observed.
1.5.4
WARNING!Freezing of Limbs to surfaces!
Duringoperation ofthe freezedryer dangerous situations in the ice condenser
chamber mayarise. When puttingin the shelves takecare that limbs do not come into
contact with the condenser in the ice condenser chamber as the limbs maybecome
frozen to the surface. The limb can onlybe detached from the surface byapplying
heat. Liquid should not be used.

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 11
1.5.5
IMPORTANT!Transport instructions!
Please keep the packagingfor possible subsequent dispatch.
The freezedryer should be carried bytwopersons byholdingit underneath on both
sides.
WARNING! When transportingor puttingdownthe unit do not hold the plastic control
panel. Please note: When puttingthe unit downon asurface there is adanger of
squeezinghands or fingers.
1.6 Prohibited Freeze Drying Processes
1. Operation offreeze dryer when not installed correctly.
2. Operation without panels.
3. Operation bynon-authorised personnel.
4. Operation with shelves not installed properly.
5. Operation with verycorrosive substances which can cause damage to material and
affect mechanical strength ofchamber and shelves.
6. Operation with accessories not allowed bythe manufacturer, except for
commercial freezedryingvessels made ofglass or plastic. The user is explicitly
warned not to use poor qualitygoods. Breakingglass or burstingvessels can
cause dangerous situations duringfreeze drying.
7. Operation in locations with danger ofexplosion.
WRONGRIGHT

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 12
8. Duringoperation the freezedryer must not be knocked or moved. Leaningagainst
or restingon the freeze dryer is not allowed.
9. Do not place potentiallydangerous material, e. g.glass vessels containingliquids,
near the freeze dryer.
10. Products which could react to the supplyofhighenergyduringthe freezedrying
process must not be dried.
11. Do not freeze dryexplosive or highlyinflammable substances.
12. Substances which could damagethe material of the shelves or the chamber in any
waymust not be dried or mayonlybe dried when special safetymeasures are
observed. Infectious, toxic, pathogenic and radioactivesubstances must onlybe
dried in suitable vessels.

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 13
2 Installation and Commissioning of the Unit
2.1 Site of Installation
WARNING! Papers, cloths or similar items must not be put behind the unit as the air
circulation ofthe heat exchanger will not workanymore.
The freeze dryer should be positioned horizontally. The ambient temperature should be
within approx. +15°C and +25°C.
The refrigerator ofthe freezedryer is air-cooled. Sufficient air circulation must be
ensured. A distance ofat least 30 cm to the wall should be kept. The unit should not be
positioned near radiators or heat sources and direct insolation must be avoided.
In the event ofinsufficient air circulation or atoo highambient temperature pressure
and temperature in the refrigeratingsystem will increase.
The following connections are necessaryat the site:
2.2 Mains Electricity
The voltage given on the name-plate must correspond to the local supplyvoltage.
CHRIST freezedryers are units ofsafetyclass Iand include athree-conductor
connection cable and a shockproofplug.
2.3 Fuses on Site
The freeze dryer must be protected typicallywith a 16 A fuse.
2.4 Checking the Earth Connection
For checkingthe earth connection there is ascrewfor equalisingthe ground potential
on the backpanel ofthe freezedryer. The checkcan be carried out bymeans ofan
appropriate measuringdevice.

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 14
2.5 Defrosting Water
The defrostingwater is drained via the condensate drain valveon the leftside ofthe
unit. To drain the water place the hose supplied with the unit onto the nozzle. The
defrostingwater is collected in a vessel.
The defrostingwater can also be drained directlyvia this hose. The defrostingwater
must be able to drain freely.To achievethis the hose must haveasteadydownward
slope. It must be ensured that water does not collect in anypart ofthe hose. The end
ofthe hose alwayshas to be abovethe level ofthe liquid in the vessel for the
discharged defrostingwater. Otherwise there is the riskofwater and dirt residues
beingsucked into the condenser chamber ifthere is avacuum when openingthe
condensate drain valve.
2.6 Vacuum Pump Exhaust
Duringthe main dryingphase the vacuum pump must be operated with open gas
ballast valve. The oil mist which is produced must be removed.
A ½"hose is connected to the exhaust flange ofthe vacuum pump RZ-2 or RC-5 and a
¾"hose is connected to the exhaust flangeofthe vacuum pump DUO 005 or DUO
010. The hose either leads into the open air or into a vent.
Duringinstallation ofthe pipe care must be taken that condensate cannot flowback
into the pump. With upward leadingpipes it is safest to use aseparator (Woulfe's
bottle or wash bottle) in the pipe.
Ifdrainingofthe oil mist should not possible werecommend that an exhaust filter (oil
mist separator) is fitted. This filter prevents air pollution byoil mist which is emitted by
the vacuum pump in smaller or larger quantities dependingon the workingpressure.
The filter is fastened to the exhaust flange ofthe vacuum pump.
The filter is equipped with apressure control valvewhich indicates the saturation ofthe
filter. Cleaningor replacingofthe filter insert must be carried out at the latest when the
pressure control valveis activated. The collected oil is visible in the inspection glass
and is drained via the dischargingscrew.
(Please refer to separate operating manual of the vacuum pump!)

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 15
2.7 Initial start-up
CAUTION! Ensure that the freezedryer is correctlymounted and installed before
initial start-up (see point 2.1 Site and followingpoints).
2.7.1
Connection of vacuum pump and installation of
accessorycomponents
The accessorycomponents are connected up to the freeze dryer ALPHA1-4 LD-2 /
ALPHA2-4LD-2 accordingto the process flowdiagram above. Centeringringsand
clampingflanges with wingnuts are used as connectingelements (small flange
connections accordingto ISO 28403 respectivelyDIN 2861, see followinginstructions)
In addition the plugofthe vacuum measuringsensor must be inserted into the socket
“Vacuum measuringsensor”on the backofthe unit (see point 3.4 connection of
vacuum measuringsensor TPR 265).
1 ALPHA 1-4 LD-2 / 2-4 LD-2
2 Vacuum measuring sensor
3 Vacuum release valve
4 Manual stop valve
5 Vacuum hose
6 Vacuum pump
6
4
3
3
5 2
1

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 16
Instructions on connecting centering rings and clamping flanges
Vacuumhose
Centeringring
Clampingflange
Vacuumreleasevalve
(separateaccessory)
Lay-outassemblyof
vacuum connections.
Place centeringringon
oneside ofsmallflange
connection
(e.g.vacuum hose).
Connectsecondflange
(thecenteringringmust
bepositionedcorrectly!)
and placeclampingflange
overtheconnection and
presstogether.
Tighten the screwof the
clampingflangebyhand.
A B
C D

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 17
Other ordered accessories (e.g.dryingchamber, shelves and connections for round
bottom flasks) are added accordingly.
Example: Accessoryfor dryingon
5unheated shelves as well as
individuallysealable rubber valves
for round bottom flasks.
Example: Accessoryfor dryingon
2unheated shelves with sealing
device for injection vials.

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 18
Schematic diagram of accessories
ALPHA 1-4 LD-2
ALPHA 2-4 LD-2
Drip tray
Base plate
Drying chamber 300
with 12 connections
Rubber valve
Ampoule manifold
Drying vessel, e.g.
ampoule
Product dish
Ground-in stopper
Drying vessel, e.g. injection vial
Drying vessel,
e.g. round bottom
flasks
Additional chamb
er 300
with 12
connections
Drying vessel, e.g. injection vial
Stoppering device with 1 shelf,
250, unheated, max. 4
shelves can be used
Drying chamber 300
3 or 5 shelves
265, unheated

Operating Manual Freeze DryerALPHA1-4 LD-2 / 2-4 LD-2, Version 0203, Page 19
ALPHA 1-4 LD-2
ALPHA 2-4 LD-2
Lid 300
Rubber valve
Drying chamber, e.g.
round bottomflaks
Drying vessel, e.g. injection vial
Drying vessel, e.g..
wide neck filter
Manifold, different versions, max.
24 rubber valves