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Pilot freeze dryers types L and LN Liver extract, hormones, enzymes, sera", plasma and derivatives, antibiotics, diagnostic and injectable Pharmaceuticals and fine chemicals are some examples of the many substances with widely differing characteristics which can be freeze dried in EDWARDS KNIESE pilot plants. Some of these materials are delicate and require freeze drying plant of high performance with accurate control. Type L or LN freeze dryers provide the conditions to process these delicate materials. They can be enclosed for laboratory use or open sided for installation through a wall in a sterile room. The pilot freeze dryers are also suited to small scale production. When the automatic control system (optional) is built into the pilot plant the control programme is generated on the plant and can be directly transferred to the controller of a suitably equipped production plant. The standard pilot freeze dryers can be adapted to special requirements. For example, measurement and control can be manual, semi- or fully automatic. In addition, the number of shelves and their spacing can be varied. The type L dryers include an ice condenser of higher capacity which is separated from the vacuum chamber. In type LN dryers, a condenser of normal capacity is provided at the rear of the drying chamber.
Drying Chamber The drying chamber and shelves are both of stainless steel. The standard chamber is cylindrical, rectangular hambers can be supplied on request. fhe silicone heat transfer fluid circulates rapidly through the shelves and provides uniform and accurately controlled temperatures throughout the process. A radiation plate ensures uniform drying conditions everywhere including on the top shelf. The number and position of the shelves in each model gives a wide choice of container size. Plants with increased chamber size are available so that the distance between the shelves can be increased for special requirements. For units with a vial stoppering facility, the shelves are adjustable and the gap can be closed down to 35 mm. The central shelf can be simply and easily removed and stored on the top or bottom shelf to increase the distance between the shelves up to 180 mm: The drying chamber contains ports for vacuum gauge heads, temperature sensors and for the entry of the heat transfer fluid. The convex door of the vacuum chamber is of acrylic material, giving a wide-angled view inside. Prefreezing is carried out in the vacuum chamber.
Condenser for Type L The stainless steel condenser is designed to ensure uniform ice deposition. A water spray (up to 90°C) is used for defrosting, and a high vacuum valve allows drainage. The drying chamber and condenser are connected by a ISO 100/150 flange joint, which can accommodate a vacuum isolation valve. The high capacity condenser allows two or three drying cycles before defrosting is necessary. A radiation shield inside the condenser chamber reduces heat gains and eliminates the need for external insulation. The lowest condenser temperature is normally —70°C. However a temperature of —80°C can be achieved by using refrigerant R13b1. The condenser can befitted with a catchpot for volatiles like alcohol which can be collected without affecting the vapour pressure in the system. Condensates can be drained separately before the condenser is defrosted.
Condenser for Type LN The condenser is at the rear of the shelves in the drying chamber and is defrosted by water spraying. There is a shield between the shelves and the condenser.
Refrigeration system A semi-hermeticaily sealed two-stage compressor, ortwo single-stage compressors in series, cool the condenser and the shelves. Compressors may beair-orwater-cooled as required. The system can be fitted with a manifold and the condensing capacity can be optionally increased. The refrigeration system isfitted with all necessary control and safety devices. For shelf temperatures of—40°Candcondensertemperatures of - 7 0 ° C, refrigerant R22 or R502 is used. R13b1 must be used when temperatures of —50° C (shelves) and —80°C (condenser) are required. The compressor must then be water-cooled.
Vacuum System The vacuum chamber is evacuated by an EDWARDS two stage, direct drive, rotary pump which is extremely quiet and vibration-free. The operating pressure is 10~3 mbar, the pump itself having an ultimate vacuum of 10~4 mbar without gas ballast (10~2 mbar with gas ballast). The pump has a integral vacuum isolation valve to isolate the chamber when the pump stops. The vacuum system has a separate manual isolation valve and an admittance valve to conrol the entry of an inert gas into the drying chamber. The addition of a diffusion pump to the system is possible.
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Edwards Kniese
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EDWARDS KNIESE types L and LN pilot freeze dryers combine modern appearance with easy access for servicing. The main difference between the two types is the location and size of the condenser: at the rear of the chamber in type LN (see layout on this page); separated from the chamber, and of higher capacity in type L
Edwards Kniese 1. Control panel Stoppering mechanism Polished stainless stell high capacity condenser 4. Adjustable shelves Stainless steel chamber 6. Connexions for air-admittance, cooling water, process fluids, electrical supply, pump exhaust.
7. Refrigeration system. Separate water or air-cooled compressors for shelves and condenser.
8. Two-stage, direct drive vacuum pump.
9. Main electronic/electrical panel with relays and plant protection circuits.
Temperature control of the heat transfer fluid The fiuid transfer system regulates the temperature of the shelves. The shelf temperature can be selected at any level between —40° C and +60° C by balancing continuous cooling and electrical heating. A multi-point controller indicating both pre-set and actual temperatures is included in the control system. However, the use of a programme controller instead of the multipoint controller is becoming more popular.
tion is augmented by convection and the drying time is minimised. Because of this control, and the minimal leak rate of the equipment, the4 vacuum pump is only in continuous operation during the final drying process, when the end vacuum required is a function of the condenser temperature.
Vacuum pump on. Vacuum pump off, or air admittance on/off. 4
Controls All switches and indicator lights are mounted in a control panel at the front of the plant. The main electronic/electric panel is located at the side for easy access. A six-trace recorder indicates and records the most important temperatures and the pressure in the chamber. A temperature or programme controller monitors the temperature of the heat transfer fluid and the switching to further process stages. The pressure controller, in combition with the Pirani vacuum gauge indicates and records ...a chamber pressure (in plants with full automatic control). Manual switches are fitted to control the various sub-systems. Each one has complementary indicating lamps to display normal operation or malfunction. The control system can be pre-programmed to provide automatic changeover from pre-freezing to main drying as a function of time and/or product temperature, as well as the automatic changeover from main to secondary drying. EDWARDS KNIESE recommend fitting of the fully automatic controls when intensive use for production runs is intended. The automatic controller not only controls the whole process but also provides automatic protection of the product.
Automatic control The programme and pressure controllers are the basis of the automatic control for the complete process which ^erates by comparing the desired and actual conditions. 3 system controls pre-freezing, a recrystallisation phase and the changeover to secondary drying. Stoppering and defrosting can also be controlled automatically. The system pressure is adjusted during the primary drying so that heat transfer to the products by contact and radia-
3
Alarm activated when 2\ \1 required pressure exceeds limit after first pump-down.
3
{[ U
2
10" 10" 12 4 6 6 I 1.5 2 I I I I I I
Restart of programme controller.
I
I
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6 8 I 1,5 2 I
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0
2
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6
8
10
mbar x 100 = Pa Actual pressure.
Typical process cycle Switching values 1 and 4 are not visually indicated onthe pressure regulator, but are nevertheless pre-set to activate when pressure drops significantly below point 3; or rises significantly above point 2. Set value 1 and 2 are adjusted to the partial watervapourpressure (in most cases assumed to be the total plant pressure). The corresponding temperature as given in the water vapour curve lies approximately 10° C below the Eutectic point of the product to be dried. For example, if the freezing point of the product is—10° C, value 1 will be set at—20° C, represented by a pressure of 0,1 mbar. The pressure is maintained between values 3 and 4 during the main drying phase. If a fault occurs it usually results in a pressure rise, which will first exceed value 2 and then value 1.At point 2, the programme controller is switched off and the supply of refrigerant to the shelves is switched on. At point 1 the alarm (signalling pressure rise above pre-set maximum) is activated. These controls prevent thawing or deterioration of the product. When the pressure returns to the specified value, the programme controller is re-activated. Points 3 and 4, which control the vacuum pump and the air-admittance valve during the main drying phase, are pre-set close to points 1 and 2.
Trace 1 The freezing process ends at the s*- ~* of trace 1. (The control of the erature for the initial freezing process is taken from different parameters, not shown in this example). At the beginning of trace 1: — the programme drive motor is switched off. — condenser cooling circuit is switched on. — the vacuum pump starts. — the shelf cooling continues. When the vacuum chamber pressure is first decreased below points 1 and 2 (opposite diagram): — the programme is switched on. — temperature control of the shelves is activated. — all shelf cooling is switched off. Trace 2 Indicates the duration of pressure control in the vacuum chamber. The end of the trace shows when the pressure controller is overridden and the vacuum pump is in permanent operation (final drying).
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This trace activates the relay to switch off the programmer. The programmer is then not in operation and the plant continues operating in a steady state until changed by hand operation.
Edwards Kniese | Trace J
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Example of programme control
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77 /
Stoppering of small bottles
Manifold
Equipment can be supplied with a hydraulic or mechanical stoppering mechanism on request.
EDWARDS KNIESE pilot freeze dryers can be supplied with various manifolds so that large bottles, small bottles, ampoules etc., can be externally connected.
Steam sterilisation
Other accessories
All pilot plant is optionally available with steam sterilisation. The sterilisation temperature is usually between 120°Cand 136°C. The calculations and design principles are approved by the appropriate authorities and the equipment itself subjected to pressure test. Instead of an acrylic door, a stainless steel door with bayonet closures is fitted and is supplied with safety devices.
Accessories forthe loading and unloading of the product, e. g. racks, carriers, trays, can be provided to meet special requirements. Forthe type 'U freeze dryer a stainless steel freezing bath can be built in on request. The bath temperature can be regulated to—40°C. Substances can also be shell or spin frozen when a variable speed geared motor is fitted.
Vacuum chamber and shelves: Diameter of vacuum chamber Shelf dimensions No. of shelves Distance between shelves ?hen no. of shelves is
1 2 3 4
L1
L2
mm mm
350 250 x 350 1/2
Qoo 500 600 350 300 x 400 400 x 500 250 x 400 1/2/3 2/4 1/2
500 700 300 x 450 450 x 450 2/3/4 1/2/3
mm mm mm mm
150 75
180 120/60 60
120/60 60
L3
LN 1
LN2
LN3
130
150 75
1 0,360
65 1 0,800
1 0,200
1 0,400
ca. 28
ca. 28
ca. 4
ca. 8
ca. 16
-40/+70 <-70 ^50/+70 <-85
-40/+70 <-70 -50/+70 <-85
-40/+70 <-70 -50/+70 <-85
-40/+70 <-70 -50/+70 <-85
-40/+70 <-70 -50/+70 <-85
180
240/80 160/80/80 80 1
Condenser ice capacity
kg
1 0,175 ca. 18
Temperature using: Refrigerant R 502 - shelves - condenser Refrigerant R13b 1 - shelves -condenser
°C °C °C °C
-40/+70 <-70 -50/+70 <-85
Vacuum pump throughput
m 3 -rr 1 7,0
14,6
20,5
7,0
7,0
14,6
Services: Electrical power consumption Water consumption (water cooled systems only)
kW
ca. 4
ca. 6
ca. 8
ca. 4
ca. 6
ca. 8
l-h- 1
120-180
250-300
450-700
120-180
250-300
450-700
kg m m m
600/800
700/1150
850/1300
500/700
600/850
750/1000
1,7 1,0 1,75
2,20 1,05 2,0
2,20 1,05 2,0
1,2 1,0 1,8
1,4 1.0 2,0
1,5 1.0 2,0
Radiation shield is Shelf area
m2
Weight nett/gross Packed dimensions:
length width height
0,800
A B D E F
LN 1
LN 2
LN 3
1575
950
1100 1650
1300 1750
780 743 852
780 743 877
790 743 922
1690
1820
1920
/I \
Types LN r~
1
I i
p-1 '
jI 1 I ^
1
A B C D E F
L1
L2
L3
1520 1650 753 852 1550 810
2000 1905 753 952 1800 840
2000 1955 763 952 1800 850
wards Kniese
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Types L
1 ' 1
•
Ordering details Edwards Kniese Pilot Freeze Dryers types L and LN: L2
L3
LN1
LN2
Model
L1
Freeze dryer, cabinet enclosed, with watercooled refrigerating system, 220/380 V, 3 ~, 50 Hz as above, but with aircooled refrigerating system
22-K001-01-001 22-K002-01-001 22-K003-01-001 22-K101-01-001 22-K102-01-001
22-K103-01-001
22-K001-01-002 22-K002-01-002 22-K003-01-002 22-K101-01-002 22-K102-01-002
22-K103-01-002
22-K001-02-001 22-K002-02-001 22-K003-02-001 22-K101-02-001 22-K102-02-001
22-K103-02-001
22-K001-02-002 22-K002-02-002 22-K003-02-002 22-K101-02-002 22-K102-02-002
22-K103-02-002
Freeze dryer, open version for wall mounting in sterile room, with watercooled refrigerating system, 220/380 V,3~,50 Hz as above, but with aircooled regrigerating system
LN3
Isolation valve between drying chamber and condenser
22-K500-10-001 22-K500-10-002 22-K500-10-003
Mechanical stoppering mechanism for small bottles
22-K500-20-001 22-K500-20-002 22-K500-20-003
22-K500-20-101 22-K500-20-102 22-K500-20-103
Manifold with 4 connections dia 32 mm as above, with 6 connections as above, with 8 connections as above, with 12 connections
22-K500-30-104 22-K500-30-106 22-K500-30-108 22-K500-30-112
22-K500-30-104 22-K500-30-106 22-K500-30-108 22-K500-30-112
22-K500-30-204 22-K500-30-204 22-K500-30-204 22-K500-30-206 22-K500-30-206 22-K500-30-206
Gas admittance valve Refrigerating system and condenser of increased capacity Electronic 4 point controller for automatic pressure control during the drying process
22-K500-30-104 22-K500-30-106 22-K500-30-108 22-K500-30-112
22-K500-40-000 22-K500-40-000 22-K500-40-000
22-K500-40-000 22-K500-40-000 22-K500-40-000
22-K500-50-001 22-K500-50-002 22-K500-50-003 36-K500-90-000 36-K500-90-000 36-K500-90-000 36-K500-90-000
36-K500-90-000 36-K500-90-000
6 colour recorder with 1 pressure and 5 temperature connections 36-K500-91-000 36-K500-91-000 36-rK500-91-00036-K500-91-000 36-K500-01-000 36-K500-91-000 Programme controller with 1 traces
-36-K500-92-000 36-K500-92-000 36-K500-92-000
36-K500-92-000 36-K500-92-000 36-K500-92-000
Edwards, Kniese&Co. Hochvakuum GmbH Postfach1569 D-3550 Marburg (OTMichelbach, Am Wall) Tel. 06420/415 Telex 04 82 375
EDWARDS Edwards Kniese
Ordering details Edwards Kniese Pilot Freeze Dryers types L and LN: Model
L1
L2
L3
LN 1
LN2
LN 3
Freeze dryer, cabinet enclosed, with watercooled refrigerating system, 220/380 V, 3 ~, 50 Hz as above, but with aircooled refrigerating system
22-K001-01-001
22-K002-01-001
22-K003-01-001
22-K101-01-001
22-K102-01-001
22-K103-01-001
22-K001-01-002
22-K002-01-002
22-K003-01-002
22-K101-01-002
22-K102-01-002
22-K103-01-002
22-K001-02-001
22-K002-02-001
22-K003-02-001
22-K101-02-001
22-K102-02-001
22-K103-02-001
22-K001-02-002
22-K002-02-002
22-K003-02-002
22-K101-02-002
22-K102-02-002
22-K103-02-002
22-K500-10-001 22~K500-10-002
22-K500-10-003
Freeze dryer, open version for wall mounting in sterile room, with watercooled refrigerating system, 220/380 V, 3 ~, 50 Hz as above, but with aircooled regrigerating system Isolation valve between drying chamber and condenser Mechanical stoppering mechanism for small bottles
22-K500-20-001
22-K500-20-002
22-K500-20-003
22-K500-20-101
22-K500-20-102
22-K500-20-103
Manifold with 4 connections dia 32 mm as above, with 6 connections as above, with 8 connections as above, with 12 connections
22-K500-30-104 22-K500-30-106 22-K500-30-108 22-K500-30-112
22-K500-30-104 22-K500-30-106 22-K500-30-108 22-K500-30-112
22-K500-30-104 22-K500-30-106 22-K500-30-108 22-K500-30-112
22-K500-30-204 22-K500-30-206
22-K500-30-204 22-K500-30-206
22-K500-30-204 22-K500-30-206
22-K500-40-000
22-K500-40-000
22-K500-40-000
22-K 500-40-000 22-K500-40-000
22-K500-40-000
22-K500-50-001
22-K500-50-002
22-K500-50-003
Gas admittance valve Refrigerating system and condenser of increased capacity Electronic 4 point controller for automatic pressure control during the drying process
36-K500-90-000 36-K500-90-000
36-K500-90-000 36-K500-90-000 36-K500-90-000 36-K500-90-000
6 colour recorder with 1 pressure and 5 temperature connections 36-K500-91-000 36-K500-91-000
36-K500-91-000 36-K500-91-000 36-K500-01-000
Programme controller with 3 traces
36-K500-92-000\ 36-K500-92-000 36-K500-92-000 36-K500-92-000
36-K500-92-000 36-K500-92-000
36-K500-91-000
Edwards, Kniese&Co. Hochvakuum GmbH Postfach15 69 D-3550 Marburg (OTMicheibach, Am Wall) Tel. 06420/415 Telex 04 82 375
EDWARDS Edwards Kniese
Page 1 of 2 Pascal Van Dam From:
Pascal Van Dam
Sent:
woensdag 27 oktober 2010 13:25
To:
Sebastiaan Schipper
Cc:
Lenard Bezemer; Sebastiaan Schipper
Subject: reparatie edwards vriesdroger Meetrapport Edward Freeze dryer. Compressor burn-out, Deze vervangen en koudemiddel en oiie als vervuild afgevoerd. 6.5 kg vervuilde r404a naar cilinder 001457 4.5 liter vervuilde poly-esther oiie afgevoerd. Geleverd: 6.5 kg R404a uit cilinder 146114. Na 24 draaiuren koudemiddel en poly-esther oiie uit systeem gehaald en als vervuild afgevoerd. 6.5 kg vervuilde R404a naar cilinder 23975. 4.5 liter vervuilde poly-esther oiie afgevoerd. Geleverd: 6.5 kg R404a uit cilinder 146114(4.5 kg) 161646(2.0 kg 4.5 liter poly-esther oiie. Na in bedrijf stellen bijgaand een meetrapport. Meting uitgevoerd bij condensor temperatuur van -75 en schappen temperatuur van -38. Persgastemperatuur: 88 graden Persdruk: 14 Bar. Vloeistoftemperatuur: 26.8 graden. Onderkoeling: 5.2 graden. Zuigdruk: -0.6 Bar. Zuiggastemperatuur: -55.8 graden. Oververhitting: 6.3 graden. Opgenomen amperage L1 -3.5 A L2 -3.4A L3 -3.4A Oliedruk Low pressure 1.1 Bar Controle van diverse componenten: HP prestostaat. LP prestostaat. Oliedrukverschil prestostaat. Condensordrukregeling. Waterregelventiel. Carterverwarming. Vloeistofklep. Installatie draait naar behoren en is volgens STEK eisen geinstalleerd en in bedrijf gesteid. Tevens kenplaat.instructiekaart en logboek compleet gemaakt. Ik hoop u hiermee voldoende geTnformeerd te hebben.
27/10/2010
DenHartog
Tolboomweg 8 3784XC TERSCHUUR
t: +31 (0) 342-460040 f: +31 (0) 342-460045
ELiCOLA3 group
STEK
0
INSTALLATIERAPPORT Registratienummer R1851 Installatie-identificatienummer:
Nominale vulling van^de i n s t a l j ^ t i e : S / <~Type koudemiddel:
Reden werkzaamheden
• Nieuwbouw
n Nominale bijvulling
^Reparatie
• Periodiek onderhoud/service contract
o Afbraak
Omschrijving storing / reparatie:
I ifAAJt Vak'er voorgeko^en bij installatie:
t'nJJL &-A, YjUruA^mA^Xmji ja/fiee"j
Documenten/gegevens aanwezig Kenplaat installatie
Instructiekaart
fjajnee
a Volledige installatiecontrole
Logboek
(Silee
Drukbeproeving
Q Vacumeren
• Beperkte installatiecontrole
H Vullen
Drukbeproeving
Max. toegestane werkdruk LD zijde 0 bar
Max. toegestane werkdr. HD zijde 15 bar
Lekdichtheidscontrole
(H-Totale installatie
LD gedeeltebaif^O bii
HD gedeeltebar/20 bar)
D Evt. Losse onderdelen 24
Standtijd drukbeproeving
uur
minuten
Vacumeer en vulprocedure
Bereikte vacuumdruk:
Merk lekdetecton-T-'T Type: ( 7 v _ j I
Serienummer: \
5001
micron
1
uur
- minuten
Ukdatum:
: \j Q8 8 i'
I t l l t i t l Installatiecontrole
Standtijd
Hoogste werkdruk:
bar
Hoogste temperatuur:
oQ d ri
Laagste werkdruk:
bar
Laagste temperatuur:
_
Schakeldruk pressostaat h/d:
bar
Schakeldruk pressostaat l/d:
bar
°c
O/^ischrijvjng verriqhte wj^rkzaamhede,
Hoeveelheid koudemiddel
Type koudemiddel:
gekomen:
K
Hoeveelheid koudemiddel geleverd In installatie:
JwftTV C
Hoeveelheid bijgevuld emissie:
K
Type koudemiddel:
9
kOU a Type koudemiddel:
Advies corrigerende maja^tregelen
' g O iWSM, Naam monteunPascal van Bam
Stekregistratienummer:816739 landtekening klant (voor ontvangst
A. Datum:
document)
GECONTROLEERD 2 7 C";. 20' 0
DenHartog
Tolboomweg 8 3784XC TERSCHUUR t: +31 (0) 342-460040 f: +31 (0) 342-460045
group
STEK
INSTALLATiERAPPORT Registratienummer R1851 Installatie-identificatienummer:
ant: i -j
Type installatie: .*
Adres:
Merk/typekoelaggregaat:
Postcode en woonplaats:
Serienummer:
^ML
Telefoonnummer:
Nominale vulling van olfe installafie:
jjf
Contactpersoon:
r
Type koudemiddel: 17 ^
Reden werkzaamheden
n Nieuwbouw
H,Nominale bijvulling
S Reparatie
n Periodiek onderhoud/service contract
n Afbraak
Omschrijving storing / reparatie:
(Mtnm Vaker vojorgekomen bij installatie:
Documenten/gegevens aanwezig Kenplaat installatie
najjnee
Instructiekaart
^Volledige installatiecontrole
/jajhee
Logboek
! Drukbeproeving
jaftiee
K Vacumeren
• Beperkte installatiecontrole
BVullen
S Lekdichtheidscontrole
Drukbeproeving
Max. toegestane werkdruk LD zijde 0 bar
Max. toegestane werkdr. HD zijde 15 bar
aTotale installatie
LD gedeeltebar^O bar]
HD gedeeltebai^O barj
n Evt. Losse onderdelen 24
Standtijd drukbeproeving
uur
minuten
Vacumeer en vulprocedure
Bereikte vacuumdruk:
Merk lekdetectocr|",*pType: D y . | A
Serienummer:
f 500
7s micron
Standtijd
1
uur
- mfnuten
Ukdatum:
Installatiecontrole Hoogste werkdruk:
bar
Hoogste temperatuur:
Laagste werkdruk:
bar
Laagste temperatuur:
Schakeldruk pressostaat h/d:
bar
Schakeldruk pressostaat l/d:
bar
Omschrijving verrichte werkzaamheden:
Hoeveelheid koudemiddel retour gekomen:
Kg
installatie:
Kg
5 Hoeveelheid koudemiddel geieverd in b'Hl
Hoeveelheid
Type koudemiddel:
Flesnr.:
Type koudemiddel:
Flesnr.:
Type koudemiddel:
Flesnr.:
J
Kg Advies corrigerende maatregelen:
Li
0 VtAJUtu. Naam moniSunPasca van Dam Handtekening monteur:
on
Stekregistrall4nummer:816739 Handtekening klant (voor ontvangst
Datum:
document)
GECONTROLEERD
2 7 m . 201
