VV Micro - John Morris Scientific

VV Micro
Betriebsanleitung
Instruction manual
Mode d’Emploi
1
IDI
IEI
IFi
DEUTSCH
Seite
3 - 17
ENGLISH
page
18 - 31
FRANCAISE
page
32 - 47
2
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Thank you for purchasing a Heidolph Instruments product. This item has been designed,
made and inspected in compliance with DIN EN ISO 61010 for long performance and
continuous operation.
SUMMARY
SUMMARY ........................................................................................................................18
STANDARD ITEM PLUS OPTIONS .................................................................................19
GENERAL .........................................................................................................................19
SAFETY INFORMATION ..................................................................................................20
SET-UP..............................................................................................................................21
1. DRIVE UNIT ..........................................................................................................22
2. VAPOR SUPPORT TUBE AND EVAPORATION FLASK ...................................................22
3. CONDENSER ........................................................................................................22
4. INLET TUBE ..........................................................................................................23
5. COLLECTION FLASK ..............................................................................................23
6. SETTING UP FOR NORMAL DISTILLATION ..................................................................23
7. SETTING UP FOR REFLUX DISTILLATION ...................................................................23
8. COOLING WATER AND VACUUM CONNECTIONS .........................................................23
9. PART LIST GLASS SET V-mICRO .............................................................................24
CONTROLS AND OPERATION........................................................................................24
INFORMATION ABOUT DISTILLATION SETTINGS .......................................................25
10. ROTARY SPEED OF EVAPORATOR FLASK ..................................................................25
11. TEMPERATURE DIFFERENCE BETWEEN HOT BATH AND VAPOR ....................................25
12. TEMPERATURE DIFFERENCE BETWEEN VAPOR TEMPERATURE AND COOLANT ...............26
13. SOLVENT DATA .....................................................................................................26
CLEANING AND MAINTENANCE ....................................................................................28
DISASSEMBLE, FORWARD & STORE ...........................................................................28
DISPOSAL ........................................................................................................................28
TROUBLESHOOTING ......................................................................................................29
SPECIFICATIONS.............................................................................................................29
WARRANTY, LIABILITY & COPYRIGHT .........................................................................30
FAQ / REPAIR WORK ......................................................................................................30
CE-DECLARATION OF CONFORMITY............................................................................31
Important information
Advice about power cord / mains supply
Caution: mandatory action
Caution: fire- and explosion hazard
Caution: hazard of burns, hot surface
Advice about maintenance / repair
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STANDARD ITEM PLUS OPTIONS
Item
Description
1
1
1
Order number
Order number
230/240V 50/60Hz
115V 50/60Hz
511-10400-00
511-10400-07
511-10300-00
511-10300-02
513-10000-00
513-10000-00
1
1
1
1
1
23-09-03-01-01
22-03-02-01-03
515-01000-00
24-03-07-01-02
11-008-010-10
23-09-03-01-01
22-03-02-01-03
515-01000-00
24-03-07-01-02
11-008-010-10
1
01-005-001-58
01-005-001-58
Qty
2
3
Heating bath VV-Micro
Drive VV-Micro
Glass set V-Micro
loose parts:
9
Screw collar
10
Spring tension ring
11/12 PTFE seal 16 VV-micro
7
Support rod 7mm
15
Clamp complete
Instruction manual
Accessories (optional)
Description
5 liters bath liquid
Order number
515-31000-00
GENERAL
Unpack your item carefully.
Inspect for damage and report such damage or missing parts to your supplier
immediately.
Read your Instruction Manual carefully. Take the time to read the manual
which will save time while working with your product. Make sure that every
user has read and understands the Instruction Manual.
Please store the Instruction Manual in a place easily accessible to every
user.
IF ALL ELSE FAILS, READ THESE INSTRUCTIONS !
A so-called EURO-plug (DIN 49441 CEE 7/VII 10/ 16 A 250 V) is standard on
all of the products.
For the Continental US they feature a US-standard plug (NEMA
Pub.No.WDI.1961 ASA C 73.1 . 1961 page 8 15A 125V).
For using the item in a country with deviating outlet / plug systems, we
recommend to use approved adapters or to have an electrician replace the
standard plug with one mating your local system.
As shipped, the item features a protective ground wire. When replacing the
original plug, make sure to reconnect this protective ground wire in the new
plug !
19
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SAFETY INFORMATION
Please comply with all safety and accident prevention regulations as in
force for laboratory work !
Use extra care while working with rotary evaporators.
Use eye protection and adequate clothing.
Use extra care while working with flammable substances; refer to safety
data sheets.
Use extra care while working close to flammable and explosive
substances. Motors are of non-sparking type, the item itself is not
explosion-protected.
Before connecting your item with the local power supply, make sure the
item has been designed for your local voltage; refer to data plate on
item.
Connect your item with a grounded outlet only.
Turn power switch to OFF when item is not in use, or before
disconnecting from mains.
Caution ! Hazard of burns when running the hot bath at temperatures
exceeding 60°C. Avoid touching hot edge of bowl, evaporator flask and
fluid in bowl. Use gloves when replacing evaporator flask.
Never run hot bath dry.
Repair work is limited to skilled personnel so authorized by Heidolph.
Your item needs a solid stand.
Locate the rotary evaporator on a smooth, horizontal table. Make sure not to
obstruct area around evaporator.
Avoid overpressure in the system. Explosion hazard. For reasons of
safety open aerating valve, when working at ambient pressure, in order
to avoid excessive overpressure.
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SET-UP
Please read the sections „General Information" and „Safety Instructions" before
you assemble the appliance.
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1.
Drive unit
Mount the drive on the support rod (1) with the clamping ring (4). The black screw collar
(9) must face inwards towards the heating bath and the electric power cable (6) must point
down.
Secure the clamping ring (4) with the drive unit by tightening the star grip (5) on the
support rod (1).
Insert the power cable with plug (6) in the correct socket on the rear of the heating bath
housing (2).
Screw the support rod (7) for the condenser in the threaded hole of the coupling (8).
2.
Vapor support tube and evaporation flask
Remove the black screw collar (9), the spring tension ring (10), the PTFE seal (11) and the
silicon ring (12) from the drive.
From the side with the red locking knob (14), insert the vapor tube (A) with the black
support ring (B) in the drive unit as far as the stop. Make sure the side outlet of the vapor
tube is parallel to the support rod (7).
From the bath side, slide the silicon ring (12) - curved
face first - on the vapor tube (A). Then slide the
13
PTFE seal (11) - sealing lip first - on the vapor
support tube as far as it will go.
Place first the screw collar (9) and then the spring
tension ring (10) on the neck of the evaporation flask
(C, D, E) or transition piece (F).
Slide the flange over the vapor support tube (A) and
into the drive up against the seal. Push the flask as
far as it will go and half tighten the screw collar.
To give the screw collar and flask sufficient hold,
press the fastening knob (13) to lock the gear.
3.
Condenser
14
The glass set is easier to mount when the condenser is in
upright position.
The support rod (7) should be vertical. If not, loosen the red
locking knob (14) and pull out the fastening knob (13) so that
the coupling (8) can be swivelled 180°. The fastening
knob (13) will then latch home again and the support rod will be
in upright position. Re-tighten the red locking knob (14).
Screw the butt flange (G) to the threaded socket on the side of
the vapor support tube (A) and insert the sealing ring (G1).
Place the clamp (15) on the support rod (7) and fasten the
condenser (H) to the support rod with the clamp. Make sure that
the condenser's water and vacuum connections are at the top
end. Using the butt flange (G), screw the condenser unit (H) to the vapor tube (A). The
red locking button (14) must be tight in order to provide a secure hold for the condenser
and support rod.
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4.
lnlet tube
Place the screw connection cap (I) and the seal (I1) on the inlet tube (K).
Then insert the inlet tube in the open end of the vapor tube and tighten the screw
connection cap (I). Inlet valve is made of PTFE, please do not grease.
5.
Collection flask
Screw the butt flange (G) on the open end of the condenser (H) and screw the sealing
ring (G1) and the collection flask (L, M, N) or vacuum cap (0) on the other end of the
unit (according to the intended method of distillation).
6.
Setting up for normal distillation
(Starting from the position for reflux
distillation)
For normal distillation the collection
flask has to point down. Slacken the
red locking knob (14), pull out the
fastening knob (13) and swivel the
condenser (with flask and support
rod) through 180° until the fastening
knob (13) latches in the second position. Then re-tighten the red locking
knob (14).
7.
Setting up for reflux distillation
(Starting from the position for normal
distillation)
For reflux distillation the condenser has to be in
upright position and a vacuum cap (0) is used
instead of the collection flask (L). To re-position
the condenser, loosen the locking knob (14),
pull out the fastening knob (13) and swivel the
condenser with flask and support rod through
180° until the fastening knob (13) latches home.
Then tighten the locking knob (14).
8.
Cooling water and vacuum connections
Join the cooling water connections (H2) and the
vacuum connection (H1) to the side of the
condenser and secure with hose clips (not
supplied).
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9.
Part list Glass set V-Micro
Order number
514-40000-00
514-72100-00
514-71100-00
514-70100-00
514-33000-00
514-45000-00
514-20000-00
514-46000-00
514-50000-00
514-82100-00
514-81100-00
514-80100-00
514-34000-00
Item
A+B
C
D
E
F
G + G1
H
I + I1
K + K1
L
M
N
O
Description
Vapor tube with Support ring
Evaporation flask 250 ml
Evaporation flask 100 ml
Evaporation flask 50 ml
Transition piece NS 14,5
Butt flange with Seal for butt flange
Cooler K-micro
Screw connection cap with Seal
Inlet tube with Valve
Collection flask 250 ml
Collection flask 100 ml
Collection flask 50 ml
Vacuum cap
Qty
1
1
1
1
1
1
1
1
1
1
1
1
1
CONTROLS AND OPERATION
Important:
It is imperative to read the section „Safety instructions" and „General
information" before you use the appliance for the first time.
Before connecting the appliance to the power supply, make sure that
your supply voltage is the same as that on the rating plate of the
appliance. Use plugs approved for your country. In this connection,
please read the note in the section „General" on page 19.
o
o
o
o
o
Check all components and make sure they are in working order!
Check all connections for leaks.
Add water, oil or bath liquid to the heating bath. Observe the
max/min level.
Run water or an alternative liquid through the condenser.
Add solution to the evaporation flask.
o
Use the locating knob (16) and
star grip (5) to position the
evaporation flask in the heating bath with a safety
clearance of at least 10 mm between the flask and the
bath wall (see detail view on page 14). The flask
rotation switch (17) is not to be used before this point.
o
The depth of immersion of the evaporation flask in the
bath liquid is set by vertical adjustment of the complete
drive. Holding the drive unit (3) securely, slacken the
star grip (5), move the drive up or down accordinqly
16
and retighten with the star grip.
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o
o
o
o
o
o
Use switch (18) to turn on the bath heater (the pilot lamp lights up). You can
select the bath temperature with knob (20).Caution: Risk of scalding when
using the heating bath!
When you are sure that the knob (19) is set to 0 (turn counterclockwise as far as the
stop), use the switch (17) to turn on the flask
18
17
19
20
rotation (the Pilot lamp lights up). Then you can
use the knob (19) to set the required speed.
You can add solvent to the evaporation flask
when the system is under vacuum. To do so,
connect the inlet tube (K) to a length of tubing
(dia 6 mm) and place the end of the tubing in the
solvent container. Use the valve (K1) to regulate
the required amount of solvent.
You can switch over the VV Micro from reflux
distillation to normal distillation while it is in
operation. Important: Fit a large enough
collection flask before beginning with the distillation. To switch over, release
the locking knob (14), pull out the fastening knob (13) and swivel the condenser
through 180° until the fastening knob (13) latches home. Re-tighten the locking
knob (14).
When the distillation is over, lift the evaporation flask out of the bath by undoing
the star grip (4 and/or 5) and moving the drive unit.
Before you use the appliance in the laboratory for the first time, please check
that its switches, knobs, drive etc. are in working order.
INFORMATION ABOUT DISTILLATION SETTINGS
Using a rotary evaporator for thermal cracking of substances some basic consideration
should be made to achieve the best results possible. Optimize settings as described
below:
10. Rotary speed of evaporation flask
Raise distillation speed by raising rotational speed. This methods cuts distillation time and
protects the substances handled.
11. Temperature difference between hot bath and vapor
This temperature difference should at least be 20 K to reach adequate distillation speed. If
acceptable by thermal stability of the substances handled, you even may raise the
temperature difference.
Rule of thumb: double temperature to double distillation speed.
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12. Temperature difference between vapor temperature and coolant
This temperature difference should be no less than 20 K to guarantee adequate
condensation. Low temperature difference, effectiveness of solvent recovery drops.
Choose an as high as possible temperature difference in particular for high-boiling
substances.
13. Solvent data
Examples for using reference table and nomogram:
This reference table details substance data needed for distillation, whereas the nomogram
reflects relationship between pressure and boil temperature of some solvents. Go by the
Clausius-Clapeyron equation and plot 1/T against log p.
13.1. At boiling temperature of 40°C
Vacuumcontroller: in column "vacuum for boil temperature" use the "Set Vac" nominal
value as depicted for 40°C.
13.2. At boiling temperatures deviating from 40°C
1. On temperature axis of the nomogram mark boil temperature needed.
2. Draw a line to the right and determine intersection with the solvent line.
3. From this intersetion draw a straight line down to determine the vacuum pressure
neeed for this particular application.
13.3. Solvents not depicted
-
The following items might help in determining the right vacuum pressure:
1. Raise of the straight line is a function of evaporation enthalpy. It is similar for similar
chemical substances with similar boil temperature. Hence, straight lines depicted may
be used for rough reference to a lightly deviating boil point.
2. A water jet pump or diaphragm-type pump may lower boil temperature by about 100°C.
3. Rule of thumb: decrease pressure to ½ will decrease boil point by about 15°C.
26
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solvents
acetone
methyl cyanide
benzol
n-butanol (butanol)
tert.-butanol (tert.-butanol)
2-butanon (methylene-etylene-ketone)
tert.-butylmethylether
chlorobenzol
cyclohexane
1,2-dichlorethane
1,2-dichloroethylene (cis)
1,2-dichlorethylene (trans)
dichloromethanw (methylene chloride)
diethylether
diisopropylether
di-isoimethylformamide
1,4-dioxane
ethanole
ethylene-acetate
Heptane
Hexan
methanole
3-methylene-1-butanole (isoamylalcohol)
Pentachlorethanw
Pentane
n-pentanole (amylalcohol)
1-propanole (n-propylalcohol)
2-propanole (isopropylalcohol)
1,1,2,2-tetrachloroethane
tetrachloroethylene
tetrachloromethane (carbontetrachloride)
tetrahydrofurane
toluene
1,1,1-trichloroethane
trichloroethylene
trichloormethane (chloroform)
water
xylole (isomeric mix)
molecular
formula
MW
[g/mol]
boil point
[°C]
ΔHvap
[J/g]
C3H6O
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
58,08
41,05
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
56,5
81,8
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
550
833
549
619
588
473
27
375
389
336
320
313
373
392
318
406
879
394
439
370
1225
593
203
382
593
787
701
247
233
225
425
251
265
263
2259
390
vacuum for
boil point of
40°C
[mbar]
556
230
236
25
130
243
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
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CLEANING AND MAINTENANCE
For cleaning, wipe housing with a damp cloth (add some sort of mild liquid soap).
NOTE: To avoid damage to the surface finish, avoid using chlorine bleach,
chlorine-based cleaners, abrasive substances, ammonia, rags or cleaning
pads containing metallic particles.
Vapor tube (A+B, page 21) and PTFE seal (11/12, page 21) need regular
upkeep. To this end, remove, clean, and inspect vapor tube (A+B) and
PTFE seal (11/12) (sealing edge); replace PTFE seal on condition. To
reinstall vapor tube and PTFE seal, make reference to chapter 2.
The item is maintenance-free. Repair work is limited to engineers authorized to do so by
HEIDOLPH. So therefore get in touch with your local HEIDOLPH dealer or field
respresentative.
DISASSEMBLE, FORWARD & STORE
Disassemble
o
o
Turn off the appliance and remove the plug from the socket-outlet (allow to cool).
Clear away all equipment from around the evaporator to provide easy access for
dismantling. Remove the glass set and dismantle the appliance and its components
in reverse order to their assembly.
Transport and store
1. Use orginal box or a similar pack to store your item in order to prevent damage in
transit. Tape box as required.
2. Store item in a dry place.
CAUTION: avoid shocks and vibration while in transit.
DISPOSAL
For disposal, please comply with your local or national regulations. Split by metal, plastic,
etc.
Packing material to be treated as described above (material split).
28
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TROUBLESHOOTING
The heater does not work:
o
Check the power cable
o
The capillary tube controller is defective
o
The On/Off switch is defective
o
The tubular heater is defective
The drive does not rotate:
o
No electricity at socket-outlet
o
Check the power cable and the connecting cable to the main unit
o
The setting potentiometer is defective
o
The On/Off switch is defective
o
The speed setting is too Iow
o
The black screw collar is too tight
o
The motor is defective
o
The motor capacitor is defective
Not enough vacuum:
o
Check the seals and the connection (a total of 6 points)
o
Replace worn seals where necessary
o
Make sure the seal is fitted properly (sealing lip on the appliance side, see the
drawing page 21)
SPECIFICATIONS
Model
Drive
Speed range (rpm)
Speed monitor
Heater rating (W)
Temperature range of heating bath (°C)
Control precision of heating bath (°C)
Bath temperature display
Material of heating bath
Diameter of heating bath (mm)
Supply voltage
Connected load (W)
Weight without glass set (kg)
Dimensions** (WxDxH) (mm)
Length of power cable (m)
Protection type
Permisible ambient conditions
Evaporation capacity (ml H2O / h)
Cooling area (cm²)
Order number
**Drive in top position, without glass set
29
VV-Micro
Capacitor motor with speed control
80 - 200
Scale
500
30 - 110
±5
Scale
Chrome steel
139
230 V / 50 Hz o. 115V/60Hz (others
available)
530
6,9
167x235x350
2
IP 21
0 - 40° C bei 80 % air humidity
approx. 250
270
511.12000.00
E
WARRANTY, LIABILITY & COPYRIGHT
Warranty
Heidolph Instruments warrants that the present product shall be free from defects in
material (except wear parts) and workmanship for 3 years from the date shipped from the
manufacturer’s warehouse.
Damage in transit is excluded from this warranty.
To file for such warranty service, contact Heidolph Instruments (phone ++49-9122-992068) 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.
Alterations to the present warranty 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.
FAQ / REPAIR WORK
If any aspect of installation, operation or maintenance remains unanswered in the present
Manual, please contact the following address:
For repair services 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 item 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]
Note
If you are based in the United States of America, please contact Heidolph US :
Heidolph Instruments, LLC
Lab Equipment Sales
2615 River Rd.
Cinnaminson, NJ 08077
Phone: 856-829-6160
Fax: 856-829-7639
E-Mail: [email protected]
30
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Safety Information
When shipping items for repair that may have been contaminated by
hazardous substances, please:
advise exact substance
take proper protective measures to ensure the safety of our receiving and
service personnel
mark the pack IAW Hazardous Materials Act
CE-DECLARATION OF CONFORMITY
We herewith declare that the present product complies with the following standards and
harmonized documents:
EMC-Guideline:
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 61000-4-3:2002 +A1:2002
EN 61000-4-5:1995 +A1:2001
EN 61000-4-6:1996 +A1:2001
EN 61000-4-8: 1993
EN 61000-4-11:1994 + A1:2001
Low-voltage Guideline:
EN 61010-1 + EN 61010-2-010
31
01-005-001-58-1
24/04/2006
© HEIDOLPH INSTRUMENTS GMBH & CO KG
Technische Änderungen sind ohne vorherige Ankündigung vorbehalten.
We reserve the right to make technical changes without prior announcement.
Sous réserve de modifications techniques sans avis préalable.

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