LABOROTA 20 Control Automatic Instruction

LABOROTA 20 Control Automatic Instruction
LABOROTA 20 control automatic
Betriebsanleitung
Instruction Manual
Mode d'emploi
BEDIENFRONT BASISGERÄT
CONTROL PANEL, BASIC SYSTEM
PANNEAU FRONTAL DE COMMANDE, APPAREIL DE BASE
2
BEDIENFRONT DESTILLATIONSAUTOMATIK
CONTROL PANEL, AUTOMATIC DISTILLATION
PANNEAU FRONTAL DE COMMANDE, DISTILLATION AUTOMATIQUE
248
DEUTSCH
Seite
4 - 63
D
ENGLISH
page
64 - 122
E
FRANCAIS
page
123 - 184
F
3
E
Thank you for buying a Heidolph Instruments product. This unit has been designed, made and
inspected in compliance with DIN EN ISO 61010 for long-term and flawless operation.
SUMMARY
CONTROL PANEL, BASIC SYSTEM ............................................................ 2
CONTROL PANEL, AUTOMATIC DISTILLATION........................................ 3
SUMMARY ................................................................................................... 64
PARTS AND ACCESSORIES SUPPLIED ................................................... 67
GENERAL .................................................................................................... 68
SAFETY INFORMATION ............................................................................. 69
LABOROTA 20 CONTROL AUTOMATIC, SPECIFICATIONS ................... 70
REMARKS ABOUT DISTILLATION ............................................................ 71
1.
General .....................................................................................................................71
2.
Select vacuum control mode..................................................................................71
3.
Solvent data .............................................................................................................72
LABORATORY SET-UP .............................................................................. 74
SET-UP......................................................................................................... 74
4.
Set-up .......................................................................................................................74
5.
Install vapor tube and PTFE-seal ...........................................................................75
6.
Install condensers and expansion vessel .............................................................76
7.
Assembly of screw joint KS 64 ..............................................................................77
8.
Install inlet pipe with valve and screwed cap .......................................................77
9.
Connection of PTFE tubing (G) ..............................................................................78
9.1 Inlet tube ..................................................................................................................78
9.2 Venting tube: condensate cooler – glass set........................................................78
10. Electric connection of cut-out sensor ...................................................................78
11. Connection of vacuum and cooling water tubing. ...............................................79
11.1. Connection scheme vacuum and cooling water ..................................................81
12. Electric wiring between automatic module and vacuum pump ..........................81
GLASS-SET –A AUTOMATIC II 15-300-006-32......................................... 82
WORKING WITH THE LABOROTA 20 CONTROL..................................... 83
AUTOMATIC DISTILLATION, FUNCTION PRINCIPLE .............................. 83
CONTROL PANEL ....................................................................................... 85
13. Master switch / EMERGENCY-CUT-OUT ...............................................................85
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14. Heating bath lift .......................................................................................................85
15. Speed setting...........................................................................................................86
16. Heater .......................................................................................................................87
17. Select vacuum control mode..................................................................................87
18. P const vacuum control mode ...............................................................................88
19. T auto vacuum control mode .................................................................................88
20. Calibrate Vacuum pressure sensor .......................................................................90
21. Auto Start Stop ........................................................................................................92
22. Timer ........................................................................................................................93
23. Safety cut-out in an overpressure situation..........................................................93
24. Safety cut-off in case of a defect in the vacuum system .....................................95
25. Safety functions ......................................................................................................98
TIMER AND RAMP-FUNCTION................................................................... 98
26. Set ramp values.......................................................................................................99
27. Display ramp values..............................................................................................103
28. Edit ramp values....................................................................................................103
29. Start ramp function ...............................................................................................103
30. Discontinue ramp function ...................................................................................103
31. Delete ramp............................................................................................................103
AUTOMATIC MODULE FUNCTIONS ........................................................ 104
32. Fill evaporator flask ..............................................................................................106
33. Distillation cycle ....................................................................................................108
34. End of product metering.......................................................................................108
35. End of distillation ..................................................................................................108
36. Flush vacuum pump .............................................................................................108
37. Cut-out-sensor.......................................................................................................109
INTERFACE ............................................................................................... 109
38. Connect interface ..................................................................................................109
39. Interface parameters .............................................................................................109
40. RS 232 interface ....................................................................................................109
41. RS 232 interface commands.................................................................................110
FUNCTIONS AND HANDLING .................................................................. 111
42. Protective enclosure .............................................................................................111
43. Drive lock ...............................................................................................................111
44. Tightening of Evaporator Flask............................................................................111
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45. Flask supports.......................................................................................................112
46. Automatic water refill (water bath model only)...................................................113
47. Vacuum and water distribution ............................................................................114
48. Pt100 temperature sensor, chiller........................................................................115
HEATING BATH FUNCTION AND HANDLING......................................... 116
49. Fill heating bath (water bath only) .......................................................................116
50. Drain heating bath (water bath only) ...................................................................116
51. Condensate drain (water bath only) ....................................................................116
52. Heating bath over temperature protection ..........................................................116
OPTIONS.................................................................................................... 117
53. Temperature sensor for vapor .............................................................................117
54. Temperature sensor for T auto vacuum mode ...................................................118
CLEANING & SERVICING ......................................................................... 118
UNINSTALL, FORWARD & STORE .......................................................... 119
DISPOSAL.................................................................................................. 119
TROUBLESHOOTING ............................................................................... 119
WARRANTY, LIABILITY & COPYRIGHT .................................................. 120
QUESTIONS / REPAIR WORK .................................................................. 121
CE-DECLARATION OF CONFORMITY..................................................... 122
Legend:
Important information
Advice about power cord / mains supply
Caution: mandatory action
Caution: fire- and explosion hazard
Advice about maintenance / repair
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PARTS AND ACCESSORIES SUPPLIED
Scope of supply
Your LABOROTA 20 cartons contain the parts and accessories as listed below. Before disposing
of the carton, check the contents for all items on the below parts list.
We recommend to keep packing material for future use.
Item
P/N
LABOROTA 20 S A control automatic
qty.
for more details
refer to page
518-17100-00
1
LABOROTA 20 S A O control automatic
518-17200-00
1
LABOROTA 20 E A control automatic
518-27100-00
1
LABOROTA 20 E A O control automatic
LABOROTA 20 S A control automatic
without vacuumpump
LABOROTA 20 S A O control automatic
without vacuumpump
LABOROTA 20 E A control automatic
without vacuumpump
LABOROTA 20 E A O control automatic
without vacuumpump
Glas set-A (control automatic II)
518-27200-00
1
518-17110-00
1
518-17210-00
1
518-27110-00
1
518-27210-00
1
15-300-006-32
1
page 82
Large coupling
11-300-003-71
1
Page 75, (1)
Large split ring
23-30-01-02-31
1
Page 75, (13)
PTFE O-ring
23-30-01-01-11
1
Page 75, (5)
PTFE-adapter
23-30-01-02-29
1
Page 75, (4)
PTFE-seal
23-30-01-01-51
1
Page 75, (6)
Backing ring
23-30-01-02-28
1
Page 75, (7)
Small split ring
23-30-01-02-27
1
Page 75, (11)
Small coupling
11-300-003-18
1
Page 75, (2)
Transportation rod
22-30-01-03-17
2
page 74
Cap
11-300-003-28
4
Page 74, (5)
Tube-Set
591-34000-00
1
Vapour Temperature Sensor
14-014-003-06
2
page 117 and 118
Vacuum Pump MD4C+AK+EK
591-07200-00
1
only pos. 1 - 4
Instruction Manual
01-005-004-36
1
or
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Accessories (optional)
Item
P/N
10 l evaporator flask
15-300-003-16
20 l powder flask
15-300-003-19
10 l powder flask
15-300-003-18
Base cart for LABOROTA 20 control
591-23000-00
5 liters bath liquid
515-31000-00
GENERAL
Unpack your LR20 control automatic carefully.
Inspect for damage and report such damage or missing parts to your supplier right away.
Read your Instruction Manual thoroughly. Make sure that every user has read and
understood the Instruction Manual.
Please keep the Instruction Manual in a place easily accessible to every user.
IF ALL ELSE FAILS, READ THESE INSTRUCTIONS !
For safety reasons, connect your LABOROTA 20 control automatic with a grounded outlet
only. (also refer to “Laboratory set-up” page 74)
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SAFETY INFORMATION
Please comply with all safety and accident-prevention regulations, as in force for
laboratory work !
Use extra care when working with rotary evaporators.
Use adequate eye protection and protective garments.
Use extra care when working with flammable substances; refer to safety data
sheets.
When connecting your unit with your local power supply, please make sure your
unit is designed for your local supply voltage; go by data plate on the unit.
Turn power switch OFF whenever the unit is not used, or before disconnecting the
plug.
Repair work is limited to technicians approved by Heidolph Instruments.
Use extra care when working in the vicinity of flammable and explosive substances.
Motors are of non-sparking type, the unit itself however is not explosion-proof.
The user is responsible for sufficient aeration.
Caution ! Severe burns may occur when running the heating bath over 50°C. Do
not touch hot metal rim of bath, evaporator flask or heating bath fluid.
Never run heating bath dry.
Your LABOROTA 20 needs a solid level stand.
Never attempt to work with damaged or worn-out PTFE gasket (6 page 75). Not
reaching vacuum pressure wanted may damage your rotary evaporator. Inspect
PTFE gasket (6 page 75) in regular intervals and replace on condition.
Avoid overpressure in the glassware kit while distilling low-boiling solvents.
Overpressure in the glassware kit may damage the evaporator or even blow-up
parts of the glassware kit.
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LABOROTA 20 CONTROL AUTOMATIC, SPECIFICATIONS
Supply voltage
Power rating
Rotation speed (electronic control)
Heating bath
Level control, water bath
Temperature range, water bath
Temperature range, oil bath
Heating power
Bath lift
Over temperature & dry
running protection
Boil temp. sensor: display range
Evaporator flask
Aeration valve, vacuum valve and
vacuum sensor
Timer operation
suction gauge
pumping capacity, vacuum pump
Cooling water consumption
Dimensions ( width x depth x height )
Weight
3 x 400 V 50 Hz or 3 x 230 V 60 Hz
5000 watts (includes 4,000 W of heating power)
6 - 160 1/min
400 mm dia., V2A, 17 liters capacity, when using a
20 liter evaporating flask
float switch plus automatic refill valve
0 - 100 ° C
0 - 180 ° C
4000 watts
motorized
separate safety circuit
0 - 150°C
20 liters;
10 liters optional
standard
0 – 99:59 h
1 - 1200 mbar
3.0 m3/h
150 - 350 l / h
970 mm x 620 mm x 1600 mm
(with front panel protrusion: 690 mm)
135 kg approx. (does not include glassware kit and
vacuum pump), vacuum pump: 14 kg.
glassware kit: 40 kg
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REMARKS ABOUT DISTILLATION
1. General
Using rotational evaporators for thermal breakdown of substances needs some basic
considerations about optimizing the distillation process. Parameters stipulated below are to be
considered for making optimal settings.
•
Rotational speed, evaporator flask
Increasing rotational speed will increase rate of distillation. Shorter distillation time preserves
thermal stability of your substances to be distilled.
•
Difference between heating bath and vapor temperatures:
This temperature difference should not be less than 20° C to maintain proper rate of distillation.
As long as your substances in distillation allow, you may even chose a higher temperature
difference.
Rule of thumb: doubling actual temperature difference doubles rate of distillation.
•
Temperature difference between vapor temperature and coolant:
To maintain adequate condensation rates, we recommend a 20° C temperature difference
between the solvent vapor temperature and coolant. A low temperature difference will affect
solvent recovery. For substances with high evaporation heat, you should increase temperature
difference.
2. Select vacuum control mode
2.1. p
const vacuum
control mode
The pconst mode includes the following features:
•
•
•
•
•
One of the most important modes of control
Selective distillation of different substances within the scope of their physical properties
Distillation of solvent mixtures need manual pressure settings
High recovery rates
Requires knowledge of thermodynamic substance data
first choice for all standard processes
•
For operation & parameter settings refer to page 88
•
•
Pressure (set vacuum) and hysteresis Δp (set Δp) need to be set
Select pressure p as to locate boiling point of the substance to be distilled between bath
temperature and coolant temperature, make reference to General Notes. For more information
refer to table and chart on page 74.
Δp (hysteresis) value defines max. pressure rise in mbar to open the vacuum valve.
•
Extended open valve times results in high rates of solvent loss due to extensive gas
transfer.
Low-boiling substances require a higher Δp-value (5 – 10 mbar), high-boiling substances a lower
value (1 – 5 mbar)
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2.2. T auto vacuum control mode
•
•
•
•
•
•
•
The T auto mode includes the following features:
(Temperature sensor needs to be installed)
Selective distillation of substances does not need manual pressure setting
Easy to reproduce
Easy setting
No need to know about thermodynamic substance data
first choice for low-pollution / zero-loss distillation.
Due to its location, the temperature sensor detects coolant temperature as an approximate
only. Set ΔT auto values of 2 – 8°C above coolant temperature for optimum reproducibility.
Increasing this temperature span results in a higher rate of distillation with a decrease in
reproducibility.
3. Solvent data
•
•
Examples for using table and chart:
The table displays essential substance data, the chart makes reference to the relationship
between pressure and boiling point of some solvents. In this case, 1/T is plotted as a function
of log p in accordance with the Clausius-Clapeyron equation.
a) Distillation of a solvent contained in the table:
• on the LABOROTA 20 control set the value from column “vacuum for set point at 40°C“ as
reference value for Set Vacuum.
b) Distillation of a solvent contained in the chart, with a boiling point other
than 40°C:
• Mark the boiling point desired on the temperature axis of the chart
• Draw a line to the right to get an intersection with the solvent
•
Vacuum pressure required for this one situation is found by drawing a vertical line from this
intersection down to the horizontal axis.
c) Distillation of a solvent not contained in the table or chart:
• The following notes may be helpful to determine the appropriate vacuum pressure:
• The line gradient is a function of enthalpy of evaporation. It is similar for chemically related
substances with boiling points close to each other. Hence, the plotted lines may be used as a
guide for substances with slightly different boiling points.
• Using a water-jet or diaphragm-type pump, you may lower boiling point by approx. 100°C.
• Rule of thumb: decrease pressure to a half will lower boiling point by approx. 15°C.
Avoid overpressure in the glassware kit while distilling low-boiling solvents. Aerate
glassware kit as required. Overpressure in the glassware kit may damage the evaporator
or even blow-up parts of the glassware kit.
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Solvent
Aceton
Acetonitril
Total
formula
C3H6O
Benzol
n-Butanol (Butylalkohol)
tert.-Butanol (tert.-Butylalkohol)
2-Butanon (Methylethylketon)
tert.-Butylmethylether
Chlorbenzol
Cyclohexan
1,2-Dichlorethan
1,2-Dichlorethylen (cis)
1,2-Dichlorethylen (trans)
Dichlormethan (Methylenchlorid)
Diethylether
Diisopropylether
Dimethylformamid
1,4-Dioxan
Ethanol
Ethylacetat
Heptan
Hexan
Methanol
3-Methyl-1-Butanol (Isoamylalkohol)
Pentachlorethan
Pentan
n-Pentanol (Amylalkohol)
1-Propanol (n-Propylalkohol)
2-Propanol (Isopropylalkohol)
1,1,2,2-Tetrachlorethan
Tetrachlorethylen
Tetrachlormethan (Carbontetrachlorid)
Tetrahydrofuran
Toluol
1,1,1-Trichlorethan
Trichlorethylen
Trichlormethan (Chloroform)
Wasser
Xylol (Isomeren-Gemisch)
C2H3N
C6H6
C4H10O
C4H10O
C4H8O
C5H12O
C6H5CI
C6H12
C2H4CI2
C2H2CI2
C2H2CI2
CH2CI2
C4H10O
C6H14O
C3H7NO
C4H8O2
C2H6O
C4H8O2
C7H16
C6H14
CH4O
C5H12O
C2HCI5
C5H12
C5H12O
C3H8O
C3H8O
C2H2CI4
C2CI4
CCI4
C4H8O
C7H8
C2H3CI3
C2HCI3
CHCI3
H2O
C8H10
MW
MW
ΔHvap
[g/mol]
[°C]
[J/g]
58,08
41,05
56,5
81,8
550
833
78,11
74,12
74,12
72,11
88,15
112,60
84,16
98,96
96,94
96,94
84,93
74,12
102,20
73,09
88,11
46,07
88,11
85,09
86,18
32,04
88,15
202,30
72,15
88,15
60,10
60,10
167,90
165,80
153,80
72,11
92,14
133,40
131,40
119,40
18,02
106,20
80,1
117,5
82,9
79,6
55,0
132,2
80,7
82,4
59,0
47,8
40,7
34,6
67,5
153,0
101,1
78,4
77,1
98,4
68,7
64,7
130,6
160,5
36,1
137,8
97,8
82,5
145,9
120,8
76,7
66,0
110,6
74,1
86,7
61,3
100,0
137-143
549
619
588
473
236
25
130
243
177
19
98
182
375
389
336
320
313
373
392
318
36
235
210
479
751
atm.
atm.
375
11
107
175
240
120
335
337
14
13
atm.
11
67
137
35
53
271
357
77
300
183
474
72
25
27
176
158
134
563
atm.
atm.
281
8
80
131
180
90
251
253
11
10
atm.
8
50
103
26
40
203
268
58
225
137
356
54
19
406
879
394
439
370
1225
593
203
382
593
787
701
247
233
225
425
251
265
263
2259
390
Conversion factor [mbar] to [mm(Hg)]: [mm( Hg )] ≈ 3 [ mbar ]
4
73
Vacuum for
Boiling point
at 40°C
[mbar]
[mm(Hg)]
556
387
230
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LABORATORY SET-UP
SAFETY INFORMATION:
THIS APPLIANCE IS NOT EXPLOSION-PROOF. USE EXTREME CARE WHEN USING IN THE
VICINITY OF FLAMABLE OR EXPLOSIVE SUBSTANCES.
When connecting this product with your local power supply, make sure you got the right
thing ! Check VOLTAGE DATA on DATA PLATE (located in the rear).
This product has to be wired with your local 3-phase network by a skilled electrician.
Wire code:
GREEN/YELLOW
BLUE
BROWN
BLACK
BLACK
= protective ground (PE)
= neutral (N)
= phase (L)
= phase (L)
= phase (L)
SET-UP
Carefully unpack all parts, inspect for missing parts by packing list.
4. Set-up
•
•
•
•
•
•
6
The LABOROTA 20 control with its transportation rods is
bolted to the pallet. Remove these screws and carry the
unit to its place of installation (CAUTION: 2 persons
needed; in this configuration, unit’s weight is about 110 kg).
Place the LABOROTA 20 control on a stable level stand. In
ready-to-go configuration, unit’s weight will be about 174 kg
! Ideal stand height above ground is 60 cm, this enables
easy access to all controls. We recommend the optional
LABOROTA 20 base (P/N 591-23000-00).
Remove transportation rods and keep for later use.
Through-holes for carrying rods are plugged with caps (5).
Install protective cabinet (6) on table (7), door pointing
towards operator. Use screws (8) pre-installed in attaching
holes.
The vacuum pump can be placed in a space-saving way
within the base frame (591-23000-00). The front panel (10)
is snapped–on and can be removed easily.
8
7
5
5
9
74
10
E
5. Install vapor tube and PTFE-seal
Unscrew large-size (1) and small (2) coupling rings. Lock driveshaft by turning drive lock (3)
9
8
2
1
3
10
11
7
6
4
13
5
12
clockwise (lock) to ease loosening and tightening of large-size ring (1).
• Remove PTFE-adapter (4) with built-in PTFE-O-ring (5) and PTFE-seal (6)
• Install backing ring (7) and vapor tube (8) in drive head. Put sandwich gasket (9) on vapor tube
coupling flange
• Slide small ring (2) over coupling flange of distributor (10). Expand small split ring (11) and
slide over distributor (10) coupling flange, shoulder pointing forward
• Secure assembly (10, 2, 11) tight with small coupling ring (2).
Slide PTFE seal (6) on vapor tube (8), sealing lip pointing inward
Never attempt to work with damaged or worn-out PTFE gasket (6). Not reaching vacuum
pressure wanted may damage your rotary evaporator. Inspect PTFE gasket (6) in
regular intervals and replace on condition.
•
•
•
•
Slide PTFE-adapter (4) with built-in PTFE-O-ring (5) into
drive module.
Slide large-size coupling (1) over evaporator flask (12)
coupling flange. Expand large split ring (13) and slide
over evaporator flask (12) coupling flange, shoulder
pointing forward.
Set flask support tubes to 10 liter or 20 liter mark and
lock with knobs (14); (I = 10 l, II = 20 l)
Locate evaporator flask on flask lift support tubes (15),
tilt flask neck towards drive head, center connecting
flange in drive head, so that connecting flange rests
against PTFE-O-ring (5) located in PTFE-adapter (4).
75
15
14
16
E
•
Screw large-size ring (1) tight. When evacuating, double-check for firm seat.
Refer to page 111
Return flask lift support tubes to initial position (16), CAUTION: basic position uses electronic
monitor circuit. Leaving this position will freeze all electric functions of the LABOROTA 20
control. This situation is reported by an LED on the control panel (flask support).
6. Install condensers and expansion vessel
•
•
•
•
•
Loosen thumbscrew (2), lift bracket (1)
completely and secure with
thumbscrew (2)
Place rubber side of washer (3) on
lower bracket (4), line up holes. Put
one more washer (3) with rubber side
pointing up on upper neck of condenser
or expansion vessel (5)
Plug lower neck of condenser or
expansion vessel (5) through cutout in
bracket (4) and washer (3), and tilt to
an upright position
Loosen thumbscrew (2) and slide
bracket (1) over upper neck of
condenser or expansion vessel. Make
vertical adjustment with bracket (4)
Rotate thumbscrew (2) tight when
condenser or expansion vessel are in
an exactly upright position.
3
1
2
5
3
4
6
3
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7. Assembly of screw joint KS 64
The screw joint KS 64 (A) secures the connections of cooler, expansion vessel and vacuum
connector (ref. Fig. 1). For assembly screw knurled screws (B) to top.
Like indicated in Fig. 2, press knurled screws (B) down and slide screw joint onto glass joint (C).
Fasten knurled screws (B) like indicated in Fig 1.
Fig 1
A
C
Fig 2
D
B
A
B
Attention: Make sure that washer (D) is installed properly. White PTFE cover must
face towards the pan of the connection.
8. Install inlet pipe with valve and screwed cap
4
1. Valve sealing point is adjusted by turning a
screw clockwise with the screw driver (4)
supplied.
2. Slide threaded ring (5) and gasket kit (5) over
PTFE inlet hose (1), as shown. Secure inlet pipe
(2) on distributor (6) with threaded ring (5).
3
2
1
L
G
77
M
5
6
E
9.
Connection of PTFE tubing (G)
9.1 Inlet tube
For the connection of the inlet tube (G) with inlet pipe (2) slide on screw cap (L) and locking ring
(M) on the feeding tube (G). Screw cap (L) on inlet tube (2).
D
L;M;G
M
L
G
9.2 Venting tube: condensate cooler – glass set
For connection of venting tube with elbow of the glass set slide on screw cap (L) and locking ring
(M) on venting tube (G). Screw cap (L) on screw connector.
10. Electric connection of cut-out sensor
Cut-out sensor (11) is mounted to Y-connector (J) (also refer to page 82). After mounting of glass
ware according to figure on page 82, connect the plug (12) of cut-out sensor to the back-side of
automatic module and secure it with retaining ring by turning it to the right.
J
12
11
Attention: Make sure that the cylindrical body of the cut-out sensor (11) is
mounted in a horizontal position.
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11. Connection of vacuum and cooling water tubing.
8
16
6
13
5
17
15
4
The rear panel of the unit contains a vacuum / water distributor. The central water distributor
supplies the cooler T auto, the condensate cooler and the emission condenser of the vacuum
pump with cooling water. Refer to picture (page 81) when connecting the water hoses (ID=8 mm).
They are installed within the cooler housing and connected to the cooler via screw connector.
The central connection for cooling water is set up with a ball valve (4) for flow regulation.
The central cooling water return pipe is attached to connection (15).
The different consumers are connected as follows:
Connection 17: Flow cooler T auto
Connection 13: Return cooler T auto
Connection 5: Flow condensate cooler and emission condenser
Connection 6: Return condensate cooler and emission condenser
Ball valve (5) regulates the flow of the condensate cooler and emission condenser. Ball valve (6)
has to be open fully open.
Connection of vacuum distributor and glass set is achieved via joint (8). Vacuum pipe is installed
within the housing.
Connection of automatic water supply for heating bath is done via connector (16).
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Attention: Never install a valve in main return line of cooling water. A closed
valve leads to pressure build-up in the glassware which can lead to damage of
glass.
correct !
valve
supply line
Chiller
return line
No valve in
return line
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11.1.
Connection scheme vacuum and cooling water
vacuum
cooling water
12. Electric wiring between automatic module and vacuum pump
1.
2.
3.
Connect automatic module with terminal box (with cover) located on the rear panel of the basic
item, close to the power cord fairlead.
Connect vacuum pump with outlet in the rear panel of the automatic module. Turn vacuum
pump's power switch to "ON".
Automatic function requires both components connected with their outlets, and vacuum
pump's power switch in "ON" position.
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GLASS-SET –A AUTOMATIC II 15-300-006-32
Components of the "A" automatic II glassware kit
A
B
C
D
E
F
G
H
I
I1
J
K
L
M
N
O
R
S
T
U
V
W
X
Z
15-300-001-12
15-300-002-31
15-300-001-09
15-300-002-65
15-300-002-29
15-300-003-17
23-30-01-03-15
11-300-003-78
15-300-002-54
04-03-01-06-02
15-300-002-69
15-300-002-41
23-09-03-01-22
23-30-01-01-56
11-300-003-25
15-300-002-45
23-30-01-02-64
23-09-03-01-23
23-09-03-01-24
11-300-002-94
15-300-001-15
23-30-01-01-09
23-30-01-03-31
11-300-003-76
condenser, T auto (A)
vacuum fitting
expansion vessel
elbow
vapor tube, ground
evaporator flask, 20 l
PTFE pipe 6 x 8
filter assay
inlet pipe
hose, PTFE 6.5x0.5
Tee
distributor, to expansion vessel
coupling ring GL14 / Ø10
union ring
GL25 coupling kit
valve GL18
nipple for GL18
coupling ring GL18
screwed cap GL18
threaded joint KS 64, coated
secondary condenser
sandwich gasket 50 / 69 / 3
spacer sleeve
GL25 coupling kit / Ø12
L;M;G
R;S
D
U
C
T
O
T
L;L1;X
N
B
J
Z
F
L;M;G
E;W;K
V
L;M;G
R;S
Z
Use this list when checking your shipment for completeness.
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WORKING WITH THE LABOROTA 20 CONTROL
Use rotary evaporators with appropriate care. Comply with standard laboratory safety practices.
Be cautious when working with flammable solvents; motors and limit switches are of non-sparking
type but we cannot guarantee that the unit is explosion-proof.
SAFETY INFORMATION:
WHEN CONNECTING YOUR UNIT WITH YOUR LOCAL POWER SUPPLY, PLEASE
MAKE SURE YOUR UNIT IS DESIGNED FOR YOUR LOCAL SUPPLY VOLTAGE; GO
BY DATA PLATE ON THE UNIT.
CONNECT YOUR ROTARY EVAPORATOR WITH A GROUNDED OUTLET ONLY.
AUTOMATIC DISTILLATION, FUNCTION PRINCIPLE
LABOROTA 20 control automatic is able to automatically distil high quantities of a product.
Distillation pressure is automatically controlled with either mode P const or Mode T auto.
Mode P const controls the pressure to a chosen level within the range of an adjustable hysteresis.
Mode T auto finds and controls the distillation pressure according to a temperature probe, set up in
the condenser. The system reacts on changing vapour pressure of the product mixture in an ideal
way. Speed of distillation can be set by the parameter ΔT auto.
For continuous operation the LABOROTA 20 control automatic comprises of an automatic for
charging of product and discharging the condensate.
Automatically discharging from the vacuum system works in a quasi-continuous way. Several times
per minute the processor-controlled valve matrix sluices out a small volume of condensate. The
aeration of this small volume has nearly no effect on the vacuum of the system.
The automatic product charging unit is responsible of refilling the evaporation flask according to the
amount of solvent distilled off. This makes it possible to distil large amounts in 24h-operation.
Moment of metering is detected by a weight sensor measuring weight of the evaporator flask fill.
Such weight is defined by the user, accounting for different product densities and sizes of the
evaporator flask.
Moreover, you may adjust fill capacity of the evaporator flask.
A product sensor detects whenever no product is available and stops the refilling process. A
concentration can be achieved by terminating the distillation by hand, by terminating with the buildin timer or when reaching an adjustable end pressure (only with Mode T auto).
To remove solvents from the vacuum pump after distillation, various modes to flush the vacuum
pump are available.
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solenoid valve
scavening
vacuum pump
solenoid
valve
scavening
air reflux
aperture
aftercooler
produkt - sensor
fitting
cooling
water
separator
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CONTROL PANEL
13. Master switch / EMERGENCY-CUT-OUT
Emergency CUT-OUT
Master switch
The Master switch disconnects all wires from power supply, and serves as a RESET button. (after
Emergency CUT-OUT).
The Emergency CUT-OUT discontinues operation of the rotary evaporator immediately.
• Stop rotation
• Lowers heating bath
• Opens aerating valve (vacuum valve closes)
• Turns OFF heating circuit
• Product feed and condensate discharge is cancelled
• Buzzer sounds
• Emergency LED turns ON
CAUTION: if entry of ambient air causes unwanted reactions, take adequate action
(inert gas, or keep aerating valve closed).
System re-starts after an Emergency CUT-OUT situation requires system RESET. Make sure the
problem is fixed before resetting. See an expert, if required.
To Reset, turn Master switch OFF & ON.
14. Heating bath lift
Heating bath lift RAISES, as long as the Lift UP
key is held depressed.
Heating bath lift LOWERS, as long as the Lift DOWN
key is held depressed.
At upper and lower limits, lift motion stops automatically.
Water bath only:
The LABOROTA 20 control automatic WB (water bath)
features a fully automatic water refill system with float switch.
85
Lift UP
Lift
DOWN
E
Exceeding the max. fill mark (about 30 mm below tank rim, monitored by float switch), the Lift UP
motion is discontinued automatically.
float switch must be connected
As water in the heating bath evaporates, the heating bath itself travels up in small increments for
compensation, until reaching the upper stop.
If max fill level is not sensed at the upper stop, the water will be refilled automatically.
Oil bath only:
The LABOROTA 20 control automatic OB (oil bath) features neither refill or float switch.
15. Speed setting
Display
Act Speed LED
Select key
Start key
Stop
Rotation LED
Set Speed LED
increase
Change between Act Speed and Set Speed display with
Select key. Act Speed LED or Set Speed LED illuminate.
Select LED Set Speed for speed setting.
Nominal speed (rpm) appears in the display.
Change nominal speed with Set keys.
5 seconds after last entry, display will change to “Act”, last
entry will be saved.
Start rotation with Start Stop key.
Hit this key once more to stop rotation.
CAUTION: for safety reasons, start rotation at low speeds.
Rotational speed can be increased during operation.
decrease
Never exceed a speed of 100 rpm, while working with a 20 l
evaporation flask.
If rotation does not start with the Start Stop key, please check for illumination of one or more of the
Safety Cover, Flask Support or Rotation Stop LED’s.
If this occurs check if the enclosure is open, flask support not in one of its extreme positions, or the
drive lock engaged.
For more information refer to safety functions page 98.
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16. Heater
Display
Act Bath LED
Set Bath LED
Select
key
Start / Stop
key
Act Chiller LED
Heater LED
Heater control LED
Change between Act Bath, Set Bath and Act Chiller with
increase
Select key. Act Bath, Set Bath or Act Chiller LED turns
ON.
Act Chiller is the actual coolant temperature, which is the
basis for the T auto vacuum control mode.
To set heating bath temperature, select Set Bath LED.
Display now shows the heating bath’s nominal temperature
with a 1/10 of a degree C resolution.
Change heating bath temperature with the Set keys.
Not pressing one of these keys for 5 seconds will cause the
display returns to “Act” mode. The last figure entered is
saved.
The Start Stop key turns the heater ON.
decrease
Pressing the key once more will discontinue heating.
The Heater LED illuminates as long as the heating mode is kept active, the Heater control LED
illuminates as long as heating current flows. (Act Bath < Set Bath)
Should the Heater LED remain dim after pressing the Start Stop key, please check to see if the
Over temperature Protection LED is ON or flashing. For more information refer to safety
functions page 98.
17. Select vacuum control mode
Vacuum control requires the optional vacuum valve and –sensor.
The Mode key changes between p const and T auto
vacuum control modes. p const or
T auto LED illuminates.
You may change between these vacuum control
modes during operation. For more information about
vacuum control modes please refer to solvent data
page 72.
P const
LED
Mode key
T auto LED
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18. P const vacuum control mode
In this mode, a vacuum level once selected will be maintained. Set Vacuum key sets the level and
Set Δp your control span Δp (hysteresis)
Start Stop key
Display
Act Vacuum
LED
Set Vacuum LED
Select key
Δp LED
Aeration LED
LED
Vacuum
Valve LED
increase
Change between Act Vacuum, Set Vacuum and Set
Δp with Select key. Act Vacuum LED, Set Vacuum
LED, or Set Δp LED will illuminate.
Select Set Vacuum LED for setting the nominal
vacuum level.
The nominal suction pressure in mbar appears in
your display.
Change nominal suction pressure level with the Set
keys.
Not pressing one of these keys for 5 seconds will
return the unit to “Act” mode. The last figure entered
is saved.
decrease
Select Set Δp LED for setting hysteresis of Δp.
Use SET keys as required.
The Start Stop key starts evacuation.
Press the key for an instant to interrupt evacuation without opening the aerating valve, Valve LED
flashing; one more brief press on this key continues evacuation.
Extended actuation of the Start Stop key discontinues evacuation, the aerating valve opens, and
the vacuum valve is closed.
Vacuum LED illuminates, when “vacuum control” was selected with the Start Stop key.
Ventilation LED illuminates, when the aerating valve is open.
Valve LED illuminates, when the vacuum valve is open.
Valve LED flashes, when evacuation was interrupted without aeration.
19. T auto vacuum control mode
In this mode, vacuum pressure level is controlled by an optional temperature sensor. For
installation refer to Options Section (page 118).
T auto is a low-pollution mode. This special vacuum control allows very low quantities of solvents
to be extracted by the vacuum pump.
The T auto temperature sensor detects temperature in the middle of the condenser.
For cooling water temperature, the LABOROTA 20 control automatic uses a separate temperature
sensor (act Chiller).
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E
Set Δ T auto is set to 2 – 10 °C (temperature difference from cooling water).
A high Set Δ T auto value results in high-speed distillation, whereas a low value renders a slow
and controlled distillation process.
When reaching the temperature difference (in the condenser) once set with Set Δ T auto, the
vacuum valve closes; as soon as the temperature drop equals Set ΔVapor (hysteresis), the valve
will open once more. A current Set ΔVapor setting is 0.5°C.
Display
Act Vapor LED
Act T auto LED
Select key
ΔT auto LED
Δ Vapor LED
Pressing the Select key changes display
reading between Act Vapor, Act T auto,
Set ΔT auto and Set ΔVapor.
The Act Vapor, Act T auto, Set ΔT auto or
Set ΔVapor will illuminate.
increase
Act T auto shows command temperature in
the condenser for mode T auto, i.e. at point
5 (see page 118), as soon as the
temperature sensor is installed and
connected with #4 plug connector (T auto
temperature sensor) (see page 118).
decrease
Act Vapor shows vapor temperature in the
elbow, i.e. point 1 (see page 117) as soon as the temperature sensor is installed and connected
with #3 plug connector (boiling temperature sensor) (see page 117).
For Set ΔT auto you need to select the Set ΔT auto LED. Use Set keys as required.
Next step is entering final pressure; exceeding this value automatically discontinues distillation.
After about 5 seconds, "Endp" appears in display II, at this point select final pressure. Final
pressure selected appears in the display I.
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E
Reaching this final pressure during distillation, will discontinue distillation right away. Also refer to
Display I
Display II
Taste Select
Taste Start Stop
125
EndP
Auto Start Stop function (see page 92)
If distillation should not be discontinued, enter "1" in "Endp mode", which never can
be reached by physical condition.
For hysteresis setting select LED Δ Vapor. Use Set keys as required
20. Calibrate Vacuum pressure sensor
•
•
•
Install separate calibrated vacuum gauge in vacuum
line close to condenser
Unplug power plug of automatic module from socket
of base unit
Unplug power plug of vacuum pump from socket of
the backside of automatic module and plug into plug
on the backside of base unit
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Display I
Display II
Select key
Taste
Start /Stop
750
1
CAL
VAC
•
•
•
•
•
•
•
•
•
•
•
•
•
Display Time
Display Speed
Turn vacuum pump ON
Turn LABOROTA 20 control automatic Master switch (Power) OFF
Depress Select and Start Stop keys next to display I together and hold for 5 seconds, turn
master switch ON, release keys
Display Speed shows “CAL”, display Time “VAC”.
Display I to show 750 and display II 1 (1st step)
Increase/decrease separate vacuum gauge reading of in display I with Set key
Confirm with Start Stop key
Display I to show “50” and display II “2” (2nd step).
LABOROTA 20 control automatic automatically is going to turn its vacuum pump ON, and
continues evacuating to max. limit (limit defined by vacuum
increase
pump's power). To this end disconnect aerating valve
control wire. (Vacuum gauge display won't change any
more).
Increase/decrease vacuum gauge reading in Display I
with Set key
Confirm with Start Stop key located next to Display I. As
confirmation for the accepted calibration values, „0“
appears in Display I and Display II
Turn main switch OFF and ON
Connect aerating valve control wire again
decrease
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•
•
•
Calibration is complete
Unplug power plug of vacuum pump from socket on backside of base unit and plug it into
automatic module (original state)
Unplug power plug of automatic module and plug it into socket on the backside of the base unit
(original state)
21. Auto Start Stop
With Auto Start Stop fully automatic distillation is started or stopped. Before such action, enter all
distillation parameters and start the following functions with the Auto Start Stop key:
• Lift UP
• Rotation ON
• Heater ON
• Vacuum pump and vacuum controller is activated
• Product feed and condensate discharge is activated
• Start timer (LED Act Time flashing)
An LED next to the Auto Start Stop key confirms such action.
CAUTION: if one or more functions are already active, e.g. heater, only the remaining functions will
be started.
The Time display shows time elapsed from pressing the Auto Start Stop key.
Pressing the Auto Start Stop key once more will reset the functions started:
• Lift DOWN
• Rotation OFF
• Heater OFF
• Aerating valve OPEN, vacuum control OFF and vacuum pump OFF
• Product feed and condensate discharge is cancelled
During this automatic mode, all distillation parameters may be changed!
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22. Timer
Select key
Display
Act Time LED
Set Ramp Time
LED
Set Time LED
Start Stop key
Set Ramp Value LED
Timer LED
The timer function allows ending distillation after a pre-selected period of time has expired. After
the time has elapsed, the following actions will be taken:
increase
• Lift DOWN
• Rotation OFF
• Heater OFF
• Aerating valve OPEN, vacuum control OFF and
vacuum pump OFF.
• Product feed and condensate discharge is
cancelled
• Buzzer sounds for 10 seconds
Turn timer ON and start
Select Set Timer with Select key.
Set hours and minutes with Set keys.
Start timer with Start Stop key, Timer LED flashes
Time remaining appears in display
decrease
Turn timer ON and start, after having started with Auto Start Stop before
Pressing Start Stop Timer, Set Timer LED illuminates.
For more settings refer to above paragraph.
23. Safety cut-out in an overpressure situation
The LABOROTA 20 control has been designed for distillation under vacuum. All of its gaskets and
seals have been optimized for this vacuum atmosphere. Product feeding also only works under
vacuum.
In particular situations, overpressure may build-up in the glassware kit. Please understand that our
sealing system has not been designed for such overpressure situations.
In adverse overpressure situations, solvent may get into the drive module and hence damage
bearings.
Moreover LABOROTA 20 control features an electronic overpressure monitoring circuit;
"Emergency function" will disconnect the item to avoid overpressure damage.
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Description:
A vacuum sensor, installed to display and regulate distillation pressure, monitors pressure in the
glassware kit either. Pressure rise above e.g. 1,100 mbar will disconnect the LABOROTA 20
control by activating the „Emergency“ function:
Hot bath lift rises automatically,
heater and rotation are disconnected,
vacuum controller off, aeration valve open and vacuum pump off,
system is aerated,
a buzzer sounds continuously,
Emergency LED lights, Akt Vacuum LED flashes.
To reset Emergency-function, turn power switch OFF and ON.
Limit value:
Depending on local atmospheric pressure, limit value may be adjusted. In the factory, a standard
value of 1,100 mbar was set, you may do your own settings between 900 and 1,200 mbar.
Rule of thumb:
The higher your local elevation, the lower your limit value. Make reference to the pressure in the
aerated system, as displayed, plus about 50 mbar.
Edit limit value:
Turn LABOROTA 20 control OFF with "power" switch.
Depress Select and Start Stop keys in the „Time“ block
the same time, hold depressed and turn power switch
to "ON". Wait for all of the LEDs are lighted and release
Select and Start Stop keys.
Select key
Start Stop key
Display I shows the actual limit value, e.g. 1,100 mbar.
Use arrow keys to edit this value.
increase
Display II shows the emergency cut-out function active or
not by „ON“ or „OFF“. Use Mode key to select „ON“ or
„OFF“.
decrease
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Do not override this safety feature except in very rare cases ! Your
LABOROTA 20 might be damaged !
Display I
Display II
Mode key
Confirm this action by turning the power switch OFF.
24. Safety cut-off in case of a defect in the vacuum system
The LABOROTA 20 control has a special monitoring function for the vacuum.
Disconnected vacuum hoses, broken glass parts, defective vacuum pump, and lack of vacuum
from the central vacuum supply are recognized during distillation. These are recognized when a
previously set pressure limit value is exceeded. When this limit value is exceeded, distillation is
stopped by the „Emergency“ function.
Description:
The vacuum sensor, which is installed to display and regulate the distillation pressure, is used for
monitoring the pressure in the glass set. If the pressure rises above a limit value of 900 mbar, for
example, with the vacuum regulation activated, distillation is stopped by the „Emergency“ function:
The heating bath lift automatically moves downward,
The heater and rotation stop,
The system is aerated,
Continuous buzzer,
Emergency LED illuminates, Akt Vacuum LED blinks, and “SAFE” is shown in the Vacuum Display
alternating with the actual pressure.
Reset the Emergency-Function by switching the master switch on and off again.
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Limit value:
Depending upon the desired vacuum, at which distillation should occur, it can be advantageous to
adjust the limit value. From the factory, the limit value is set at 900 mbar. The limit value can be
changed from 0 to 1200 mbar.
Pay attention that the limit value is never set lower than the value, at which
distillation should occur, as an „Emergency“ will be triggered otherwise.
Change limit value:
Switch off the LABOROTA 20 control with the master
switch „Power“.
Simultaneously press the Select key and the Start Stop
key in the „Speed“ field and switch on the master
switch „Power“. Wait until all LED´s light up and then
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Display I
Display II
Mode
900
ON
SAFE
Display Speed
Select key
Start /Stop
key
release the Select key and the Start Stop key.
„SAFE“ appears in the Display Speed
Whether or not the safety cut-off is active (ON) or switched off (OFF) is shown in Display II (Temp
Vapour) with „ON“ or „OFF“. You can change from „ON“ to „OFF“ with the Mode key.
Switching off the safety cut-off is the sole responsibility of the user.
This function does not work during distillation without vacuum! Here, the safety
cut-off offers protection in case of excess pressure.
Even when using the auto function, the function only activates after the limit value
is exceeded. Ensure by experimentation that the set limit values are never reached!
The current limit value is shown in Display I (vacuum)
e.g. 900 mbar. The limit value can be changed with the arrow
keys.
Increase value
The process must be concluded by switching off the master
switch „Power“.
Decrease value
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25. Safety functions
•
•
•
•
•
•
All of the following cause LED ON situations.
The Safety Cover LED tells you that the enclosure is
open. Rotation won’t start, or rotation is going to stop.
Close hood and hit Start Rotation key.
Flask Support LED : Flask support is not in its extreme
position (either side). Rotation won’t start, or rotation is
going to stop, lift won’t work.
Move flask support to extreme position (both sides) and
secure with knurled knobs (7, page 112).
LED Rotation Stop LED: Drive lock engaged, rotation
can’t start. Release lock by turning knob CCW.
Overheat Protection LED: Bath temperature beyond
acceptable limits. Heater won’t start, heater is disconnected. Check heater for possible
problems.
Overheat Protection LED flashing: After response, over temperature protection enters
Emergency mode (refer to next paragraph).
Heater won’t start, heater is disconnected.
Possible reasons: heating bath level insufficient, heating bath dry; refill.
Heater is broken.
After repair action allow bath to cool off and reset over temperature protection by depressing
little button with screwdriver.
Emergency LED: Emergency CUT-OUT actuated, over temperature protection response (refer
to paragraph above) or the safety sensor responded.
Heating bath lift descends automatically;
Heater and rotation OFF;
vacuum is turned OFF and system aerated.
Continuous buzzer
Reset with master switch OFF and ON
The Emergency LED being lighted and the Act Vacuum LED flashing the same time means
the safety circuit detected an overpressure situation (refer to page 93).
Heating bath lift descends automatically;
Heater and rotation OFF;
vacuum is turned OFF and system aerated.
Continuous buzzer
Reset with master switch OFF and ON
TIMER AND RAMP-FUNCTION
Time- and ramp-functions allow setting time ramps for bath temperature and rotational speed. A
maximum of 10 ea. steps may be programmed for every parameter. A maximum of 20 time
settings are accepted by the system.
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E
Select key
Display
Act Time LED
Set Time LED
Start Stop key
Set Ramp Value LED
Set Ramp Time
LED
Timer LED
26. Set ramp values
Before programming a new ramp, make sure to have deleted the old one (refer to “delete ramp”,
page 103).
Procedure 1st step:
You need to program 00:00 for the first time.
Press the Select key next to the Display Time until Set Ramp Time LED illuminates.
Set Ramp Time LED ON. Display Time only is active, all other displays are blank.
Display shows time for the present ramp in hh:mm.
The time 00:00 should always be programmed as the first time (is preset).
Press the Set keys to alter time setting (forward & back).
Not pressing a key for 5 seconds, display will return to Act. Last value entered will be saved.
To program parameter values as a function of times selected, go to Set Ramp Value LED with the
Select key next to the Display Time. Set Ramp Value LED illuminates, Set Ramp Time LED
flashes.
Go to parameter desired with Select key next to the Display Time, Set LED illuminates:
the following parameters can be programmed:
vacuum (p const mode) Set Vacuum LED illuminates
ΔT auto (T auto mode) Set ΔT auto LED illuminates
bath temperature
Set Bath LED illuminates
speed
Set Speed LED illuminates
If one or more of the parameters listed above is not to be assigned a ramp function, leave this
parameter as „OFF“.
As shipped, no ramp functions are set. (“OFF“ displayed)
Values are programmed with the Set keys, as described.
Write value in memory by pressing the Select key once more.
Use the same procedure to program the next parameter.
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E
key Select for Set Vacuum
using p const
OFF
key Select for Set ΔT auto
using T auto
OFF
OFF
key Select for
OFF
key Select for
Set Speed
Set Bath
00:00
2nd step:
Now, select the LED Set Ramp Time by pressing the Select key next to Display Time repeatedly.
The time for the 2nd step of programming can be changed with the Set increase or Set decrease
keys.
After 5 seconds with no entry, the display returns to Act Condition. The last value is accepted.
Additional steps:
Additional steps can be programmed in the same manner as step 2.
Select Set Ramp Time LED to program the next time.
For complex ramps, we recommend you to use the form enclosed (for convenience). The same
page shows an example.
Note: Values only can be programmed that had been activated at 00:00 before.
Parameters, which were programmed as a ramp, cannot be changed during the process of the
ramp with the „Set Function“. Parameters that are not programmed as a ramp can be changed at
any time with the „Set Function“
100
Time
Set Ramp Time
Set Vac
Set T auto
Set Bath
Set Speed
Unit
hh:mm
mbar
°C
°C
rpm
1
2
3
4
5
6
7
8
9
10
Time
Set Ramp Time
Set Vac
Set T auto
Set Bath
Set Speed
Unit
hh:mm
mbar
°C
°C
rpm
11
12
13
14
15
16
17
18
19
20
Time
Set Ramp Time
Set Vac
Set T auto
Set Bath
Set Speed
Unit
hh:mm
mbar
°C
°C
rpm
21
22
23
24
25
26
27
28
29
30
Time
Set Ramp Time
Set Vac
Set T auto
Set Bath
Set Speed
Unit
hh:mm
mbar
°C
°C
rpm
31
32
33
34
35
36
37
38
39
40
101
Time
Set Ramp Time
Set Vac
Set T auto
Set Bath
Set Speed
Unit
hh:mm
mbar
°C
°C
rpm
1
0:00
1000
OFF
20
20
2
0:15
1000
3
0:20
700
4
0:30
400
5
0:40
200
6
0:50
150
7
1:00
100
8
2:00
9
50
30
1200
70
1000
60
50
800
40
600
30
400
20
200
10
0
0:00
10
0
0:15
0:30
0:45
1:00
1:15
1:30
1:45
102
2:00
2:15
2:30
2:45
3:00
Set Vac
Set Bath
Set Speed
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27. Display ramp values
Ramp values once programmed can be displayed and edited.
Hit Ramp key; Ramp on LED illuminates. Press the Select key (Time) until Set Ramp Value
LED illuminates.
First programmed time 00:00 and corresponding value are displayed.
Void parameters are marked OFF.
More times and programmed values are displayed with the Set keys.
28. Edit ramp values
To edit a value, select with Select key.
Now edit value with the Set keys.
Accept new value by pressing the Select key once more.
Program more times: refer to page 99, set ramp values.
29. Start ramp function
Program ramp values as described in page 99.
Press Ramp key, Ramp on LED illuminates.
Hit Auto Start Stop key, Auto Start Stop LED illuminates.
The following functions are started:
lift UP
rotation ON
vacuum ON
heater ON
All values programmed for a ramp are controlled automatically.
Display shows time elapsed from START.
Values between times programmed are interpolated.
30. Discontinue ramp function
Ramp function may be discontinued any time.
To discontinue hit the Ramp key, Ramp LED dims.
The very last ramp function values are kept.
A ramp once programmed will be kept in memory even during power-off times and can be
used and edited all the time.
31. Delete ramp
Ramp LED and Set Ramp Value LED must illuminate.
Press both SET keys at the same time and hold. After 5 seconds, “dEL” appears for 3
seconds, a buzzer sounds.
The ramp has been deleted.
With the ramp function activated, it is not possible to also activate the timer
function! If the timer function is activated during the ramp function, the ramp
function will be switched off and the current values of Set Vac, Set Bath, Set
Speed, and Set ΔT auto are accepted as Set-values. These can then be changed.
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AUTOMATIC MODULE FUNCTIONS
LABOROTA 20 control automatic features the following control components:
¾ Automatic product refill
o Product is sucked into evaporator flask by vacuum pressure.
o Refill system for the evaporator flask features solenoid valve for product tank.
o A weight sensor is monitoring min. and max. fill of the evaporator flask. Both
parameters are easy to adjust by the user.
o A product sensor monitors availability of the product in its feed line. As soon as all of
the product in the tank has been supplied to the evaporator flask, solenoid valve is
going to close automatically. This way, sucking ambient air into the evaporator flask
is impossible. Product may be distilled to the degree wanted.
o Flow rate of the product may be regulated by a valve installed in the feed pipe.
¾ Automatic product drain via valve matrix
o Discharging of product is organized by 4 valves situated on the condensate cooler.
o The condensate is chilled in the condensate cooler and kept there for a short time.
o After valves 1 and 4 are closed, valves 2 and 3 are opened and condensate can
flow out by gravity. To overcome greater distance to a container valve 3 can also be
pressurized (max. 0.5 bars).
o Seconds later valves 2 and 3 are shut again and valves 1 and 4 are opened,
allowing again condensate to run in to the condensate cooler.
¾ Manual pump aeration
o Vacuum pump can be aerated at any time from the panel
o Aeration is to clean the pump’s valves from condensated solvents to keep up full
functions.
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produkt - sensor
aftercooler
fitting
cooling
water
separator
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32. Fill evaporator flask
32.1
Weight sensor
The LABOROTA 20 drive head features a weight sensor to determine weight evaporator flask
and its contents. This way, evaporator flask can be filled to a certain mass all the time and start
refill at a certain weight defined before. Weight is displayed as „Solvent Level“, figure
displayed being relative, instead of the absolute weight in kg.
248
32.2. Accuracy of weight displayed
Weight displayed is a function of a variety of factors and may differ:
32.2.1. Evaporator flask weight
Depending on flask size (6 liters, 10 liters or 20 liters), weight is different.
32.2.2. Buoyancy in hot bath
Depending on flask size (6 liters, 10 liters or 20 liters), buoyancy is different.
32.2.3. Hot bath fill level
Rule of thumb: the higher fill level in the hot bath, the higher buoyancy of the evaporator
flask.
Talking about a water bath, featuring automatic water refill and fluid level control, fill
level is kept constant within very narrow limits. Hence, influence by fill level is rather
low.
Talking about an oil bath, not featuring refill mode, fill level depends on the user who is
going to fill it. Account for thermal expansion of the oil or heater fluid all the time.
Operational buoyancy will settle when reaching hot bath nominal temperature.
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32.2.4. Evaporator fill level
The more fluid filled in the evaporator flask, the higher the Solvent Level displayed is.
32.2.5. Display: hot bath in low position
Descending the hot bath, buoyancy in the hot bath fluid won't exist; hence, weight
displayed under Solvent Level will be higher ! For reproducible fill levels, it will be of
essence to run the hot bath against its upper mechanical stop all the time !
32.3.
Start filling
After having activated evacuation by pressing the Auto Start Stop button and with
vacuum pressure in the evaporator flask, you may start filling the evaporator flask.
32.3.1. rotate min-rheostat to its LH end, using a coin.
32.3.2. rotate max-rheostat to its LH end with coin.
32.3.3. Hit Start filling key (Start filling LED lighting) and keep depressed until reaching
the right fill level in the evaporator flask. By vacuum pressure in the evaporator
flask, product is fed into the flask through the inlet valve being open now. Flow rate
may be regulated with the inlet valve.
32.3.4. Display Solvent Level read-out
If necessary the evacuation can be halted by shortly pressing the Vacuum Start/Stop
button to prevent foaming during filling (ref. vacuum control page 88)
Control light Start filling is lit when product is detected in feeding line by product sensor.
32.4.
Set max. fill level
32.4.1.
32.4.2.
32.4.3.
32.5.
Hit Set max Level key (max Level LED lighting); limit value is displayed; this limit
value may be edited with the max rheostat.
Set value (from para. 0) so displayed on max rheostat with coin.
Automatic product supply is discontinued automatically when reaching this value,
hence reaching the evaporator flask's max. fill level all the time.
Set min. fill level
32.5.1.
32.5.2.
32.5.3.
Hit Set min Level key (min Level LED lighting); limit value is displayed; this limit
value may be edited with the min rheostat.
Set max Level minus 10 - 50 units at min rheostat with a coin.
Automatic product supply is activated when reaching this value all the time.
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33. Distillation cycle
Distilling off, Distilling LED will light; feeding product is confirmed by the Refilling LED.
34. End of product metering
Product tank empty, a product sensor will trigger a solenoid valve in the product feed line.
From this moment on, the product can be distilled to whatever degree, as requested by the
user.
35. End of distillation
When reaching concentration wanted, distillation needs to be discontinued. Distillation is
discontinued by one of the three methods, as stipulated below:
35.1.
Manual
Hit Auto Start Stop key to run the following actions:
• descend lift
• rotation OFF
• heater OFF
• Aerating valve OPEN, vacuum control OFF and vacuum pump OFF.
• Product feed and condensate discharge is cancelled
35.2.
Timer
At the end of a certain period of time, as set with the timer before, the following actions are
taken:
• descend lift
• rotation OFF
• heater OFF
• Aerating valve OPEN, vacuum control OFF and vacuum pump OFF.
• Product feed and condensate discharge is cancelled
• buzzer sounds for about 10 seconds
35.3.
Termination by using final pressure EndP (only Mode T auto)
If final pressure End P is reached distillation is terminated with following action:
• descend lift
• rotation OFF
• heater OFF
• Aerating valve OPEN, vacuum control OFF and vacuum pump OFF.
• Product feed and condensate discharge is cancelled
36. Flush vacuum pump
At the end of a shift, we recommend to flush your vacuum pump with air. This way, solvent
residues are removed from pump body and valve area. This way, valves remain clear and
won't get stuck.
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To this end hit Pump ventilation key. Pump ventilation LED is lighting. After about a couple
of minutes, stop this operation by hitting the Pump ventilation key once again.
37. Cut-out-sensor
Automatic distillation is supervised
by cut-out-sensor (X).
If a failure in the automatic
discharging unit occurs and the
condensate can’t flow into the
condensate cooler, the Yconnection (J) will fill up with
condensate. To prevent solvent to
be drawn into the vacuum pump the
safety sensor activates an
emergency CUT-OUT which stops
the distillation (ref. page 85). If
CUT-OFF is provoked by sensor
you see only an emergency LED
blinking accompanied by
continuous buzzer.
J
X
Before resetting and restarting it is essential to remove the fault.
INTERFACE
38. Connect interface
Make sure the Unit is OFF before you attempt to connect the interface cable.
Use a cable with SUB-D 9 connectors and connect with the terminal connector located
underneath the LABOROTA 20 control automatic control panel.
39. Interface parameters
9600 Baud, no parity, 8 bits, 1 stop bit, no protocol
40. RS 232 interface
This interface allows you to specify all Set-values, move the lift up and down, open and close
aerating valve and vacuum valve.
All Act-values and status of safety functions may be recalled.
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41. RS 232 interface commands
query
Command
Act commands
VAC?
VAP?
BATH?
CHILL?
SPEED?
TIME?
COUNT?
Safety functions
SC?
FS?
RS?
OP?
EM?
action
remarks
Act Vacuum
Act Vapor
Act Bath
Act Chiller
Act Speed
Act Time
Act Time
elapsed time, continuous operation
time, timer mode
Safety Cover
Flask Support
Rotation Stop
0 = action; 1 = no action
0 = action; 1 = no action
0 = action; 1 = no action
OverTemperature
Prot.
0 = action; 1 = no action
Emergency
0 = action; 1 = no action
triggering
Command
Set commands
VAC=XXXX!
action
remarks
Set Vacuum
BATH=XXXX!
Set Bath
SPEED=XXX!
Set Speed
TIME=XXXX!
Set Timer
4-digit in mbar; range set 0000 to 1200
4-digit, in 1°C increments
range set 0000 to 1800 equals 0.0 to 180.0
3-digit, in rpm; range set 000 to 180
4-digit, in hh:mm
range set 0000 to 9959 equals 00:00 to 99:59
Actions
SVX!
VVX!
BVX!
SBX!
SSX!
STX!
LU!
LD!
Start Stop Vacuum
Valve
Ventilation
Start Stop Bath
Start Stop Speed
Start Stop Timer
SV0! = OFF ; SV1! = ON
vacuum valve; VV0! = CLOSE ; VV1! = OPEN
aerating valve; BV0! = CLOSE ; BV1! = OPEN
SB0! = heater OFF ; SB1! = heater ON
SS0! = rotation OFF ; SS1! = rotation ON
ST0! = Timer OFF ; ST1! = Timer ON
lift UP
lift DOWN
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FUNCTIONS AND HANDLING
42. Protective enclosure
8
The protective enclosure (1) is an extra safety
feature for the operator. Its large pane of a
special safety glass guarantees a clear view of
the rotating flask. A handle (2) on the front is
used for closing and opening. In both extreme
positions, it is held by a pneumatic strut.
Caution: Flask will not rotate unless the hood is
closed. Opening the enclosure during operation
will stop rotation.
Safety Cover LED (6) illuminates.
After closing the enclosure, rotation is restarted
by the Start Stop key.
1
6
2
43. Drive lock
picture on top.
The drive lock helps opening and closing the large coupling ring (3) holding the flask (4).
• To engage lock: turn knob (8) CW until “lock” appears.
Manually rotate drive head, until lock snaps into place. Rotation Stop LED (6) on front panel
illuminates.
• To release lock: turn knob (8) CCW until “unlock” appears.
Rotation Stop LED (6) on front panel dims.
44. Tightening of Evaporator Flask
Evaporator Flask must be sufficiently tightened with large coupling ring (X).
For this purpose the large coupling ring (X) is equipped with a torque indicator. As illustrated below
the coupling ring has to be tightened until the indicator point (Y) is aligned with point „1“ (Z). This is
accompanied by a „click“. For distillation without vacuum the ring has to be tightened until point (Y)
is aligned with point „2“ (A).
If rule is not followed leakage can occur during operation.
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X
Z
Y
A
45. Flask supports
8
1
2
4
5
7
The flask supports make flask (1) removal (even filled) an easy job for one person.
•
•
Uninstall flask: Open enclosure (2). Engage drive lock (8). Slide support pipes (4) to flask (1)
from both sides. Check for firm contact and lock support pipes in place by tightening
thumbscrews (5) CW. Unscrew large coupling ring (6, not shown) by turning CCW. Tilt flask
neck with large coupling ring (6) forward. Remove flask carefully (coupling ring to remain on
flask).
Install flask: Open enclosure (2). Engage drive lock (3). Move support pipes (4) (both sides) to
the respective flask size mark (center of thumbscrew = mark). Mark I = 10 l flask; mark II = 20 l
flask. Lock support pipes in place by tightening thumbscrews (5) CW. Put flask (1) , holding
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large coupling ring (6), on support pipes carefully. Swing flask axis with coupling ring in-line
with axis of rotation, until flange is centered in drive head. Secure PTFE-adapter (not shown)
with PTFE-O-ring tight by CW turn. Double-check for firm seat. Return support pipes to initial
position (7). Release drive lock (3). Caution: Basic position of support pipes is monitored by
the electronic circuit; when leaving this position, all electric functions of the system will freeze.
This situation is reported by the Flask Support LED on the control panel.
46. Automatic water refill (water bath
model only)
The LABOROTA 20 control WB features a
automatic water refill system with float switch.
The float switch (1) monitors water level in the
heating bath. When dropping below normal
level (about. 30 mm below tank rim), a
solenoid valve (2, next para.) opens the water
supply until reaching the normal fill level.
Cooling water is supplied to the heating bath
via pipe.
The float switch needs to be connected with
plug connector (3).
Caution: For technical reasons automatic refill
requires the heating bath lift to be at its upper
most position.
Upward lift travel is limited by the float switch.
Water control valve on the rear must be
connected.
1
3
The float switch may fail due to calcareous deposits, causing the hot bath to be overfilled
or overflow. We recommend to decalcify this float switch every 6 months.
To this end uninstall float switch (disconnect plug connector (3) and loosen float switch
(1) attaching screws with a screwdriver.
Use commercial grade decalcifying agent (go by instructions on the pack), and immerse
float switch until fluid level reaches coupling nut. For treatment time refer to instructions
on the pack.
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47. Vacuum and water distribution
11
10
8
9
12
16
6
13
15
5
17
4
The rear panel of the unit contains a vacuum/water distributor. A central cooling water supply
optionally works with:
1 chiller; 1 chiller plus 1 after-chiller, or 2 chillers. Refer to picture above when connecting the
water hoses (ID=8 mm). Hoses are routed in the chiller panel and attached to the chiller with hose
nipples. Inlet flow control uses a ball valve (4). When using 2 chillers, open ball valve (5) (lever inline); when using 1 only chiller, close ball valve (6) (lever out-of-line). The same applies to the
coolant return network. When using 2 chillers, open ball valve (6) (lever in-line), using 1 only chiller,
close ball valve (6) (lever out-of-line).
Connect #1 chiller with the fittings (13). Coolant return is connected with fitting (17).
Connect vacuum distributor with fitting (8) on glass kit. Vacuum hose is routed in the chiller panel
to glass kit fitting and attached with screwed nipples. The built-in aerating valve (9) is controlled
from the control panel.
The aerating valve (9) is connected with #3 terminal connector (6-pin) (11).
Water refill solenoid valve (12) is connected with the lower terminal connector (4-pin) (10).
The cooling coils of the cooler may only be exposed to a maximum cooling water
pressure of 2 bar. So that higher pressure can never develop, no valve and no
restrictor may be installed in the cooling water return.
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48. Pt100 temperature sensor, chiller
The chiller Pt100 sensor is connected with
the terminals (1); this sensor used to display
cooling water temperature (Act Chiller).
1
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HEATING BATH FUNCTION AND HANDLING
49. Fill heating bath (water bath only)
Using de-ionized or distilled water needs to add 0.2 % of Borax (Na2B4O7*10H2O)
(corrosion inhibitor)
Please note: The use of tabwater as heating media can lead to calcification which
can provoke crevice corrosion.Therefore the user is strongly recommended to
clean the heating bath with an adequate polish on a regular basis.
Heating bath water supply uses the vacuum/water distributor (refer to page 114).
Connect inlet end to fitting. Heating bath fill uses line (12) and is controlled by a solenoid valve
(12). Also refer to page 114.
50. Drain heating bath (water bath only)
1
The rear panel of the LABOROTA 20 control with water bath
features a drain valve (1). To close valve turn black lever
perpendicular to line.
This valve drains bath fill into a tank (not supplied).
Caution: Allow water to cool to ambient to avoid burns.
51. Condensate drain (water
bath only)
2
The LABOROTA 20 control (water
bath) features a condensate drain.
Water vapor from the hot bath is
condensed by the chiller coil (1) of
the condenser (2), and is collected in
a sump (3), which in turn is drained
through a nipple (4).
This nipple (4) accepts an elastic
hose (ID = 8 mm). The other end is
plugged in a collection tank.
1
3
4
52. Heating bath over
temperature protection
Once the over temperature protector responds (Over temperature Protection LED), allow the bath
to cool off and fix the problem.
Most possible reason: no water supply.
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Descend heating bath lift to LOW.
Turn master switch OFF.
Reset over temperature protector by introducing an insulated screwdriver through the little hole at
the lower right end of the unit. (remove black plastic plug to gain access through panel)
OPTIONS
1
53. Temperature sensor for vapor
To display vapor temperature on the control
panel, you’ll need the optional temperature
sensor (1) (P/N 14-014-003-06). To install,
remove cap from temperature fitting (2) of glass
kit. Its plug fits the rear #3 terminal connector of
the drive head. Secure in place.
3
4
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54. Temperature sensor for T auto vacuum mode
T auto vacuum control mode needs the optional
temperature sensor (5) (P/N 14-014-003-06).
To install, remove caps from condenser (6). When
running the T auto mode, connect temperature
sensor with the forward terminal connector (4) in the
rear of the drive head.
6
5
CLEANING & SERVICING
Cleaning: wipe housing clean with a damp cloth (add some mild liquid soap).
Note
To avoid damage to the surface finish, avoid using chlorine bleach, chlorinebased detergents, abrasive substances, ammonia, rags or cleaning agents
containing metal particles.
Rust stains appearing on the bottom of the hot bath after long-term use is
caused by foreign matter deposits (iron particles or rust particles).
Remove such rust stains and calcareous deposits with a conventional
phosphoric acid bathroom cleaner (decalcifying agent).
The float switch may fail due to calcareous deposits, causing the hot bath
to be overfilled or overflow. We recommend to decalcify this float switch
every 6 months.
To this end uninstall float switch (disconnect plug connector (3) and
loosen float switch (1) attaching screws with a screwdriver (refer to
page 113)
Use commercial grade decalcifying agent (go by instructions on the pack),
and immerse float switch until fluid level reaches coupling nut. For
treatment time refer to instructions on the pack.
Never attempt to work with damaged or worn-out PTFE gasket (6). Not
reaching vacuum pressure wanted may damage your rotary evaporator.
Inspect PTFE gasket (6) in regular intervals and replace on condition refer
to page 75).
The unit is maintenance-free. Repair work is limited to technicians approved or appointed by
Heidolph Instruments. Please call your local Heidolph Instruments Dealer or a Heidolph
Instruments Field Representative (also refer to page 121).
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UNINSTALL, FORWARD & STORE
Uninstall
Turn the item OFF and disconnect mains plug.
Forward & Store
1. We recommend to store the item and its components in its original box, or a similar container
that offers adequate protection against damage in transit. Tape the box securely.
2. Store the item in a dry place.
Caution
Do not jolt or shake the item during transport.
DISPOSAL
For disposal, please comply with your local or national regulations.
Separate by metal, plastic, etc.
Packing material to be treated as described above (material split).
TROUBLESHOOTING
•
Master switch won’t light when turning ON
check power cord
master switch broken (call service)
•
Display: Act Vacuum “0000“
vacuum sensor broken or not connected
•
Display: Act Vapor “----“
temperature sensor not connected or broken
•
Display: Act Chiller “----“
Cooling water temperature sensor not connected or broken
•
Display: Act Vacuum (aerated) differs from atmospheric
altitude correction factor not integrated.
Calibrate vacuum pressure sensor.
•
Poor vacuum pressure
inspect gaskets and fittings
check ground fittings, coat with vacuum grease, as required
PTFE seal installed the wrong way. Sealing lip needs to point towards drive head
check line to vacuum pump
•
Heating bath lift won’t travel up
float switch not connected or broken
also refer to safety functions section
lift mechanism broken
upper limit switch broken
•
Heating bath lift won’t travel down
lift mechanism broken
lower limit switch broken
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•
No rotation
also refer to safety functions section
motor broken
•
Aerating valve won’t work.
Aerating valve broken or not connected.
•
Product metering won't stop, Refilling LED being OFF
Open and clean solenoid valve; valve is clogged with foreign matter.
•
Vacuum pump won't start running when hitting Auto Start Stop or Start Stop key
Vacuum pump not connected with automatic module; Set Vacuum value higher than ambient.
Change Set Vacuum value to „0“ or final pressure wanted.
•
Distillation automatically discontinued (by accident)
EndP value incorrect; Set Time incorrect, cut-out sensor responded.
Also refer to safety functions (page 98)
Whenever facing a problem that cannot be fixed by the above information, call your authorized
Heidolph Instruments dealer right away.
WARRANTY, LIABILITY & COPYRIGHT
Warranty
Heidolph Instruments provides a three-year warranty on the products described here (with the
exception of glass and consumable parts) if registered with enclosed warranty card or via internet
(www.heidolph.com). Warranty starts with the date of registration. Without registration warranty
starts according to serial number. This warranty covers defects in materials and workmanship.
Transit damage is excluded from this warranty.
To obtain such warranty service, contact Heidolph Instruments (phone: +49 – 9122 - 9920-68) or
your local Heidolph Instruments Dealer. If defects in material or workmanship are found, your item
will be repaired or replaced at no charge.
Misuse, abuse, neglect or improper installation are not covered by this warranty promise.
Alterations to the present warranty promise need Heidolph Instruments’ consent in writing.
Exclusion Clause
Heidolph Instruments cannot be held liable for damage from improper use or misuse. Remedy for
consequential damage is excluded.
Copyright
Copyright in pictures and wording of the present Instruction Manual is held by Heidolph
Instruments.
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QUESTIONS / REPAIR WORK
If any aspect of installation, operation or maintenance remains unanswered in the present Manual,
please get in touch with the following address:
For repairs please call Heidolph Instruments (phone: ++49-9122-9920-68) or your local, authorized
Heidolph Instruments Dealer.
Note
You will receive approval for sending your defective unit to the following address:
Heidolph Instruments GmbH & Co. KG
Lab Equipment Sales
Walpersdorfer Str. 12
D-91126 Schwabach / Germany
phone: ++49-9122-9920-68 Fax: ++49-9122-9920-65
E-Mail: [email protected]
Safety Information
When shipping items for repair that may have been contaminated by hazardous
substances, please:
advise exact substance
take adequate protective action towards our parts receiving and service
personnel
mark the pack IAW Hazardous Materials Act
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CE-DECLARATION OF CONFORMITY
We herewith declare that the present product complies with the following standards and harmonized
documents:
EMC-Act:
EN 61326: 1997 + A1:1998 + A2:2001+ A3 2003
EN 61000-3-2: 2000
EN 61000-3-3: 1995 + 1997 + A1:2001
EN 61326: 1997 + A1:1998 + A2: 2001+ A3 2003
EN 61000-4-2:1995 +A1:1998+A2:2001
EN 61000-4-3:2002 +A1:2002
EN 61000-4-4:1995 +A1:2001 + A2:2001
EN 61000-4-5:1995 +A1:2001
EN 61000-4-6:1996 +A1:2001
EN 61000-4-11:1994 + A1:2001
Low-voltage Act:
EN 61010-1 + EN 61010-2-010
122
01-005-004-36-1
28/02/2007
© HEIDOLPH INSTRUMENTS GMBH & CO KG
Technische Änderungen sind ohne vorherige Ankündigung vorbehalten.
Technical changes reserved. Publication not mandatory.
Sous réserve de modifications techniques sans notification préalable.
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