Thermo Scientific HAAKE RotoVisco 1 User manual

Instruction Manual
HAAKE RotoViscoHAAKE RotoVisco
HAAKE RotoViscoHAAKE RotoVisco
HAAKE RotoVisco®®
®®
®11
11
1
HAAKE RheoStressHAAKE RheoStress
HAAKE RheoStressHAAKE RheoStress
HAAKE RheoStress®®
®®
®11
11
1
version 2.3
“Translation of the original instruction manual“

Table of Contents
1
1. Key to Symbols 3...........................
1.1 Symbols used in this manual 3.................
1.2 Symbols used on the unit 3....................
1.3 Information concerning the CE sign 4...........
1.4 WEEE Compliance 5.........................
2. Quality Assurance 6........................
3. Your Contacts at Thermo Fisher Scientific 6..
4. Warranty 7.................................
5. Safety Notes and Warnings 8................
6. Unpacking / Ambient conditions 11...........
6.1 Transportation damage? 11....................
6.2 Contents of Delivery 11........................
6.2.1 Standard Delivery Rheometer 11...........
6.2.2 Sensor Systems 13......................
6.2.3 Accessories for the Temperature Control
Units 13
6.2.4 Application software 13...................
6.3 Space Requirements 14.......................
6.4 Mains supply 14..............................
6.5 Cooling air for the measuring head
(HAAKE RotoVisco 1) 14.......................
6.6 Requirements for the air supply 15..............
6.7 Pipes in the building 15........................
6.8 Air compressors 15............................
6.9 Ambient conditions according to EN 61010 15....
7. Unit Description 16..........................
7.1 HAAKE RotoVisco1 17........................
7.2 HAAKE RheoStress1 18.......................
7.3 Temperature control: 19........................
7.4 Main features of the HAAKE rheometers: 20......
8. Installation 21...............................
8.1 Setting up the Rheometer 21...................
8.2 Connecting up 22.............................
8.2.1 PT100 connection 22.....................
8.3 Hose connections 23..........................
8.3.1 Temperature control unit (with liquid): 23....
8.3.2 Air bearing (measuring unit) 24............
9. Functional Elements 25......................
9.1 Temperature control units 25...................
9.2 External filter 26..............................
9.3 Measuring Instrument with no
temperature control unit. 27....................
9.4 Measuring Instrument with
TCL/Z -- temperature control unit. 29.............
9.5 Measuring Instrument with
TCL/P / TCE/P / TCP/P / TCP/PE
-- temperature control unit. 31...................
9.6 Measuring unit with TCE/PC-temperature
stabilisation unit and cone heater TC1 33........
9.7 Measuring Instrument with
SHRP -- temperature control unit. 35.............
9.8 Display unit (optional) 37......................
9.9 Menu tree of the display unit 38.................

Table of Contents
2
10. Operating 39................................
10.1 Switching on 39...............................
10.2 Working with the display unit 39.................
10.3 Starting the software 45........................
10.4 The ”Upload Mode” for the Display Unit
(RheoWin 2.6 or higher) 46.....................
10.5 Quick Cut-off 55..............................
11. Temperature control units 56.................
11.1 Temperature control unit TCO 56................
11.2 Temperature control unit TCL/Z 57..............
11.3 Temperature control unit TCL/P 59..............
11.4 Temperature control unit TCE/P 60..............
11.5 Temperature control unit TCP/P and TCP/PE 61..
11.6 Temperature stabilisation unit TCE/P with
cone heater TC1 67..........................
11.7 Cone heater TC1 67...........................
11.7.1 Correct application of the ceramic rotors 67.
11.7.2 Operation 68............................
11.7.3 Compressed air distributor for TC1 69......
11.8 Temperature control unit SHRP 70..............
12. Sensor Systems 78..........................
12.1 Cylinder Sensor Systems 82....................
12.2 Cylinder Sensor Systems Z-DIN 82..............
12.3 Cylinder Sensor System Z 88...................
12.4 Double Gap Cylinder Sensor DG43
according to DIN 53544 93.....................
12.5 Solvent trap for Z10, Z20, Z31,
Z34, Z38, Z41 und DG43 97....................
12.6 Solvent trap for Z43 98........................
12.7 Cone-Plate and Plate-Plate Sensor Systems 99...
12.8 Cone-Plate Sensor Systems 99.................
12.9 Plate-Plate Sensor Systems 115.................
12.10Platter--platter measuring equipment with
profiled surface. 119............................
12.11 High Shear Cylinder Sensor System HS 122.......
12.12SHRP Plate-Platte Sensor System PP 1 mm 126...
12.13Immersion Sensor System FL 129................
13. Optional sensor systems 132..................
14. Hints on Measurement 133....................
14.1 Temperature programs with Series 1 units 133.....
14.2 Range Limits in Oscillation 134..................
14.3 Correction of Dynamic Measurement 135..........
14.4 Determination of the massmoment of inertia 137...
15. Maintenance 138..............................
15.1 Maintenance Instructions HAAKE RheoStress1 139
15.2 Maintenance Instructions HAAKE Rotovisco1 140..
15.3 Filter unit 141..................................
15.4 Flat sieve 142.................................
15.5 Repairs 143...................................
16. Pin Wiring 144................................
17. External Connections 146.....................
18. Technical Specifications 147...................
19. Terms of Rheological Measurements 149.......

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Key to Symbols
3
1. Key to Symbols
1.1 Symbols used in this manual
Warns the user of possible damage to the unit, draws
attention to the risk of injury or contains safety notes
and warnings.
Denotes an important remark.
1Indicates the next operating step to be carried out and

what happens as a result thereof.
Draws attention to the risk of injury.
1.2 Symbols used on the unit
Caution: Read the instruction manual!
Caution: danger of injury your hands
Caution: Unit becomes hot
Connection for cooling air support
Display operationa
Display heating

Information concerning the CE sign / WEEE compliance
4
1.3 Information concerning the CE sign
Thermo Scientific electrical equipment for measurement,
control and laboratory use bears the CE marking.
The CE marking attests the compliance of the product with
the EC-Directives which are necessary to apply and con-
firms that the apparatus meets all relevant essential requi-
rements of the directive, the defined relevant protection
requirements.
The conformity assessment procedures were performed
following a defined methodology according to each appli-
cable directive.
The council decision 93/465/EEC shall be authoritative
concerning the modules of the various phases of the con-
formity assessment procedures and the rules for the affi-
xing and use of the CE marking, which are intended to be
used in the technical harmonization directives.
To confirm compliance with the EC-Directive 2004/108/EC
Electromagnetic Compatibility (EMC) our product was te-
sted according to the EMC requirements for emission and
immunity for electrical equipment for measurement, con-
trol and laboratory use.
Compliance with the protection requirements areas (do-
mestic establishments and establishments directly con-
nected to a low voltage power supply network which sup-
plies buildings used for domestic purposes) and industrial
areas is ensured.
Our strict standards regarding operating quality and resul-
ting considerable amount of time and money spent on de-
velopment and testing reflect our commitment to guaran-
tee the high level of quality of our products even under ex-
treme electromagnetic conditions.
Practice however also shows that even electrical equip-
ment which bears the CE marking such as monitors or
analytical instruments can be affected if their manufactu-
res accept an interference (e.g. the flickering of a monitor)
as the minimum operating quality under electromagnetic
compatibility phenomena. For this reason we recommend
you to observe a minimum distance of approx. 1 m from
such equipment.

Information concerning the CE sign / WEEE compliance
5
1.4 WEEE Compliance
This product is required to comply with the European
Union’s Waste Electrical & Electronic Equipment (WEEE)
Directive 2002/96/EC. It is marked with the following sym-
bol:
Thermo Fisher Scientific has contracted with one or more
recycling/disposal companies in each EU Member State,
and this product should be disposed of or recycled
through them. Further information on Thermo Fisher
Scientific compliance with these Directives, the recyclers
in your country, and information on Thermo Fisher Scienti-
fic products which may assist the detection of substances
subject to the RoHS Directive are available at
www.thermo.com/WEEERoHS

Quality Assurance/Contacts at Thermo Fisher Scientific
6
2. Quality Assurance
Dear customer,
Thermo Fisher Scientific implements a Quality Manage-
ment System certified according to ISO 9001:2008.
This guarantees the presence of organizational structures
which are necessary to ensure that our products are deve-
loped, manufactured and managed according to our cu-
stomers expectations. Internal and external audits are car-
ried out on a regular basis to ensure that our QMS is fully
functional.
We also check our products during the manufacturing pro-
cess to certify that they are produced according to the
specifications as well as to monitor correct functioning and
to confirm that they are safe. The results are recorded for
future reference.
The “Final Test” label on the product is a sign that this unit
has fulfilled all requirements at the time of final manufacturing.
Please inform us if, despite our precautionary measures,
you should find any product defects. You can thus help us
to avoid such faults in future.
3. Your Contacts at Thermo Fisher Scientific
Please get in contact with us or the authorized agent who
supplied you with the unit if you have any further questions.
International / Germany
Thermo Fisher Scientific
Dieselstraße 4
D-76227 Karlsruhe, Germany
Tel. [phone]
Fax [phone]
[e-mail]
www.thermoscientific.com/mc
The following specifications should be given when product
enquiries are made:
Unit name printed on the front of the unit and specified on
the name plate.
Typ: Order No. (e.g.: 557--3001)
Ser.:Nr.:
_ ___________
_Manufacturing order no.: ( 1--9)
__ Manufacturing year ( e.g. 09)
______
Production order no.:
(000001 --99999)
___ Serial--number
Mains voltage in V / power input:
e.g. 115 V/ 50 Hz/ 2 A

Warranty
7
4. Warranty
For the warranty and any potential additional warranty, the
user shall have to ensure that the devices are serviced by
an expert at the following intervals:
The maintenance is required after approx. 2000 operating
hours, at the latest, however, twelve months after the in-
itial operation or the last maintenance, respectively.
Two thousand operating hours are achieved:
at an operating period of eight hours daily (five days
a week)
about once a year
at an operating period of more than eight to sixteen
hours daily
about every six months
at an operating period of more than sixteen hours
daily
about every three months
We recommend to have the maintenance carried out by
Thermo Fisher Scientific or by staff authorised by Thermo
Fisher Scientific as special knowledge and tools are requi-
red.
The maintenance and calibration work carried out has to
be recorded by certificates in conformity with ISO 9000 ff.

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Safety Notes and Warnings
8
5. Safety Notes and Warnings
The Rheometer corresponds to the relevant safety regula-
tions. However you are solely responsible for the correct
handling and proper usage of the instrument.
This instrument exclusively determines the rheological behav-
ior of fluid and half-solid materials. These materials may not
be tested if people can be hurt or devices be damaged.
Do not lift or move the unit at the ends of the glass pane.
Do not measure / temperature control any materials that
may give off dangerous vapours or may be inflammable
within the working temperature range of the rheometer.
The device may not be operated if there are any doubts
regarding a safe operation due to the outer appearance
(e.g. damages).
A safe operation of the instrument cannot be guaran-
teed if the user does not comply with this instruction
manual.
Ensure that this instruction manual is made readily
available to every operator.
Do not bend connection and/or mains cable, do not
subject cables to stress or high temperatures (higher
than 70 C).
Check cables visually at regular intervals.
The operator must have an uninterrupted view of the
machine and its surroundings.
The rheometer must be fully visible from the PC con-
trol stand.
This unit should only be used for the applications it was
designed for.
The rheometer is designed for use with a rotor. All exist-
ing safety devices are based on the correct installation
of the rotor. Is the lift (of the measuring table) used with-
out a rotor installed injuries may occur when reaching in
the lift area.
Make sure that the unit has been switched off before you
connect or disconnect the cables. This is to avoid elec-
trostatic charging resulting in a defect of the electronic
circuit boards.

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Safety Notes and Warnings
9
Once the probe attains appropriate viscosity, cylindrical
tube (Order no. 222--1394) protectors that prevent
probe’s radial exit must be used when measuring. An
operational error when using the measuring device can
lead to the probe’s radial exit from the measuring gap; it
is therefore recommended to wear protective goggles.
Do not operate the unit with wet or oily hands.
Do not immerse the unit in water or expose it to spray
water.
Do not clean the unit using solvents (fire danger!) -- a
damp cloth applied with a household cleaning sub-
stance is often sufficient.
Complete separation from the mains is required when
repairs or maintenance work is about to be carried out.
Suitable personal protective gear, consisting of lab
coat, protective eyewear and safety gloves, must be
worn at all times when working with the instrument
Repairs, alterations or any work involving opening up
the unit should only be carried out by specialist person-
nel. Considerable damage can be caused by incorrect
repair work. The Thermo Fisher Scientific service depart-
ment is at your disposal for any repairs you may require.
Have the unit serviced by specialists at regular inter-
vals.
RheoStress1: The pressure of the air supply for the air
bearing must not exceed 4 bar. Higher pressure will
damage the air bearing permanently!
For applications at elevated temperatures above 250C
it is a must to switch the fan for the air bearing cooling
on stage 2 (on the rear) and use ceramic shafts only.
Furthermore use the cone heater TC1 as thermal shield
to prevent the heating up of the air bearing housing!
Severe skin burns can be caused by contact with hot
unit parts!
The rheometer can reach temperatures up to 350 C, depen-
ding on the temperature control unit installed. This can result
in parts of the rheometer heating up to such an extent, even
when taking the cooling and insulation into account, that se-
rious burns can result if they come into contact with the skin.
Thermo Fisher Scientific recommends shielding the rheome-
ter when operating at high temperatures and handling it only
with high temperature proof gloves and safety glasses.
A danger symbol on the glass plate warns the user of possi-
ble danger (burn injury).

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Safety Notes and Warnings
10
We do not know which substances you intend to test us-
ing this unit. Many substances are
inflammable, easily ignited, explosive
hazardous to health
environmentally unsafe
i.e.: dangerous
You alone are responsible for your handling of these
substances!
Our advice:
If in doubt, consult a safety specialist
Read the product manufacturer’s or supplier’s
“EU SAFETY DATA SHEET”
Read the REGULATIONS CONCERNING DANGER-
OUS MATERIALS
Observe the “Guidelines for Laboratories”

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Unpacking / Ambient conditions
11
6. Unpacking / Ambient conditions
6.1 Transportation damage?
Notify carrier (forwarding merchant, railroad,
post office) etc,
Compile a damage report.
Before return delivery:
Inform dealer or manufacturer
(Small problems can often be dealt with on the spot).
Do not lift or move the unit at the ends of the glass
pane.
Use the transport handles provided for the instru-
ment when unpacking.
The instrument must be carried by two persons.
Unpacking the instrument and putting it into ope-
ration is part of the installation and is carried out by
trained personnel from Thermo Scientific.
6.2 Contents of Delivery
6.2.1 Standard Delivery Rheometer
The Rheometer is delivered in a recyclable package
with the following accessories:
HAAKE RotoVisco 1
Part.No. TCO TCL/Z TCL/P TCE/P
TCE/PC
TCP/P
Connection cable
conntry specific 1 1 1 1 1
Instruction Manual ger. 003--5212 1 1 1 1 1
Instruction Manual uk. 003--5213 1 1 1 1 1
RS232 cable to PC, 9 pole 222--1490 1 1 1 1 1
Protection ring 222--1394 1 1 1
Splashboard 003--5172 1 1 1
Lever for cylinders 222--1639 1
Fuses 230V/T1.6A 087--0532 2 2 2
Fuses 230V/T3,15A 087--0533 2 2
Fuses 100/115V/T3.15A 087--0533 2 2 2
Fuses 100/115V/T5A 087--3353 2 2
Leveling indicator 002--4696 1 1 1 1

Unpacking / Ambient conditions
12
HAAKE RheoStress 1
Part.No. TCO SHRP TCL/Z TCL/P TCE/P
TCE/PC
TCP/P
Connection cable
conntry specific 1 1 1 1 1 1
Instruction Manual ger. 003--5212 1 1 1 1 1 1
Instruction Manual uk. 003--5213 1 1 1 1 1 1
RS232 cable to PC, 9 pole 222--1490 1 1 1 1 1 1
Compressed air hose 10m 082--2451 1 1 1 1 1 1
Protection ring 222--1394 1 1 1
Splashboard 003--5172 1 1 1
Ring for Peltier tempera-
ture control unit 222--1720 1
Lever for cylinders 222--1639 1
Fuses 230V/T1.6A 087--0532 2 2 2 2
Fuses 230V/T3,15A 087--0533 2 2
Fuses 100/115V/T3.15A 087--0533 2 2 2 2
Fuses 100/115V/T5A 087--3353 2 2
Leveling indicator 002--4696 1 1 1 1 1

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Unpacking / Ambient conditions
13
6.2.2 Sensor Systems
Various sensor systems are available for the Rheome-
ter which differ also in their temperature control specifi-
cations.
6.2.3 Accessories for the Temperature Control
Units
The temp. control units for liquid temp. control may be
operated with different hoses:
For the temperature control units, the open-bath circu-
lators and heating circulators the necessary tubing
hoses are not part of the standard accessories. They
have to be ordered separately.
Temperature range up to 150C:
Viton-hoses with quick coupling 222--0610
Hose nozzle set 222--1492
Temperature range of 100 up to 350C:
Metal hoses (150 cm each) 333-0294
Hose nozzle set 222--1492
Secure all hose connections using hose clamps!
6.2.4 Application software
HAAKE RheoWin Rheometer software for
Windows XP
Software RheoWin 
for HAAKE RotoVisco1 098--5003
for HAAKE RheoStress1 098--5004

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230 V
115 V
230V
115V
6
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Unpacking / Ambient conditions
14
6.3 Space Requirements
Good working conditions for a complete installation require
an area of about 1 x 0.6 meters. The two benches should be
rigid with a level surface and easy to clean. The circulator
used for temperature control should be located below the
rheometer on a separate bench to avoid backflow of thermal
fluid and possible mechanical oscillation.
A suitable laboratory bench must be provided for
the installation.
The circulator has to be located below the level of
the rheometer, otherwise the thermal fluid flows
back in the cup holder and flushes the instrument.
6.4 Mains supply
Only attach the units to mains sockets with a
grounded earth. Compare the local mains voltage
with the specifications written on the name plates
of the measuring instrument and the control unit.
Voltage deviations of 10 % are permissible.
Mains cable and unit fuses:
1Use the mains cable according to your local mains volt-
age ( see chapter “Contents of delivery”).
2Insert the fuses according to your local mains voltage
below the mains connection 6.
3For TCO, SHRP, TCL/Z, TCL/P:
230 V 2 x T1.6 A
100/115 V 2 x T3.15 A
For TCE/P, TCE/P, TCE/PC, TCP/P:
230 V 2 x T3.15 A
100/115 V 2 x T5A
4Insertion of the fuses:
Pull out the fuse holder from the mains socket and
insert the fuses. Reinsert according to the marked vol-
tage.
6.5 Cooling air for the measuring head
(HAAKE RotoVisco 1)
Compressed air is connected at nozzle 9 to avoid overheat-
ing under extreme load (high torque, high temperature
(200--350 C)) and at use of the measuring instrument at
temperatures > 100 C in the continuous operation respec-
tively.
maximum conduction pressure 0.5 bar.
(RheoStress are cooled by the outgoing air of the air bea-
ring.)
1.0 m
0.85
Rheometer
Circulator

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Unpacking / Ambient conditions
15
6.6 Requirements for the air supply
HAAKE RheoStress RS1 / RW1F
Pure air pressure is connected at nozzle for the air bearing
with a pressure by 2.5 bar (ideal way).
The air supply must have the following conditions:
-- max. 4 bar,
-- consumption approx. 10 dm3/minute
(1 dm3= 1 thousandth of a cubic meter),
-- no synthetic oil in the line,
-- max. oil contents 3mg/m
3air,
-- dry air with a residual moisture < 40 %
Use the filter unit (order no. 222-1211) or the HAAKE
compressor (order no. 222-1434 for 230 V and 222-1435 for
115 V).
HAAKE RheoStress1: The pressure of the air supply for the
air bearing must not exceed 4 bar. Higher pressure will dam-
age the air bearing permanently!
The air bearing reacts highly sensitive to dirt like particles (dust an
lint) or liquids (oil or water which condenses at high humidity lev-
els). It is therefore recommended to have new air compressors run
for a longer period of time (0,5 hrs.) without actually connecting
it to the Rheometer. In the case of internal supply systems polluted
air might have collected near the connection nozzle when the line
has not been used for some time. Therefore, we also recommend
to ”flush” this line for a period of approx. 0.5 hrs.
6.7 Pipes in the building
Oil is generally applied to air pipes in the buildings of material-
processing plants in order to prevent rusting in the workshops. By
means of complex filters the oil content may be reduced by rarely
so much that the air bearing does not suffer damage.
Thermo Fisher Scientific air bearings must not be used in plants in
which oil is added.
6.8 Air compressors
There are ”oil-free” and ”lubricated” versions of air compressors.
Only oil-free compressors (e.g. the HAAKE compressor) are ad-
missible for Thermo Fisher Scientific air bearings.
If the hose length is larger then 5 m (between compressor and
measurement unit), it must be separately attached pressure con-
troller located next to the measurement unit (see instruction
manual Air compressor Carat).
6.9 Ambient conditions according to EN 61010
It is recommended to run tests in an air-conditioned room,
(T = approx. 23C):
indoors, max. 2000 meters above sea level,
ambient temperature 15 ... 40C,
relative humidity max. 80%/31C(50%/40C)
excess voltage category II, contamination level 2

Unit Description
16
7. Unit Description
lntroduction
The viscoelastic behavior of a fluid or a soft solid can be char-
acterized in two ways; either the fluid is deformed and the re-
sulting stress is measured (CR mode), or the stress is ap-
plied and the deformation monitored (CS mode). The princi-
ple benefits of the CS mode are:
Software
Software control and evaluation with HAAKE RheoWinor
OS1 to program the display unit for production laboratories.
Measurements and evaluation
The Rheometers is controlled either by the HAAKE Rheo-
WinSoftware or with one of 10 pre--programmable mea-
suring procedures by the display unit. The results are avail-
able for further processing on a PC with the HAAKE Rheo-
WinSoftware. Alternatively up to 50 measurements can be
stored internally and be evaluated, displayed or printed out
for documentation purposes.
Sensors
For HAAKE RotoVisco1 and HAAKE RheoStress1 plates,
cones, coaxial cylinders and immersion systems are avail-
able.

Unit Description
17
7.1 HAAKE RotoVisco1
Thixotropy and flow curve
The determination of the flow behavior of a test substance
requires a speed ramp up, a holding time and a return curve
for the determination of the thixotropy. This hysteresis
method can like all other measuring procedures be PC con-
trolled or can be loaded as procedure in the display and con-
trol unit.
Time curve
Is the viscosity of a test substance changing with time this
can be monitored objectively with the HAAKE RotoVisco1.
This is especially important for substances which are curing
(adhesives, building materials), change their viscosity with
storage time or show considerable changes of viscosity after
shearing during the production process (cosmetics, paint,
food).
Temperature programs
Temperature programs are very time consuming when the
rheometer has to be operated and supervised. With the Ro-
toVisco1 these tasks can be taken over by the PC which con-
trols the rheometer as well as the temperature control units
-- everything without intervention of the operator.
Determination of the yield point
As soon as substances are strained beyond the Hookean
range they start to flow. This can be defined as yield point
and is an important characteristic value in quality control.
With the HAAKE RotoVisco1 this value can be established
relevant to practical applications, fast and easily by applying
a small deformation through extremely low speed values.
CD Mode
In the CD mode (speeds lower than 0.1 min–1 ) it is only mea-
sured at constant speeds. When ramps or steps are preset,
the following speed table is run:
Speed ( min–1 )
0.0125
0.0250
0.0375
0.0500
0.0630
0.0750
0.0875
0.1000

Unit Description
18
7.2 HAAKE RheoStress1
Flow curves
in CR and CS mode can be recorded as ramp or steps
(steady state).
Time curves
for reactions (e.g. curing) at constant temperature, shear
rate, shear stress or frequency.
Temperature programs
are software controlled to determine the temperature depen-
dence with controlled shear stress, shear rate or frequency.
Yield points
can be determined with creep/recovery tests or with stress
controlled ramps.
Viscoelasticity
of a fluid can be quantified by a creep/recovery test or by dy-
namic measurements in CD (Controlled Deformation) or CS
(Controlled Stress) mode.
Multiwave
even allows the determination of the frequency spectra as a
function of time or temperature by overlay within shortest
time.