Thermo Scientific HAAKE RotoVisco 1, HAAKE RheoStress 1 Instruction Manual

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Page 1

Instruction Manual

HAAKE RotoViscoHAAKE RotoVisco

HAAKE RotoVisco

®®

1 1

HAAKE RheoStressHAAKE RheoStress

HAAKE RheoStress

®®

1 1

version 2.3

“Translation of the original instruction manual“

Page 2

Page 3

Table of Contents

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.................

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Table of Contents

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

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.

Indicates 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

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Information concerning the CE sign / WEEE compliance

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 confirms that the apparatus meets all relevant essential requirements of the directive, the defined relevant protection requirements.

The conformity assessment procedures were performed following a defined methodology according to each applicable directive.

The council decision 93/465/EEC shall be authoritative concerning the modules of the various phases of the conformity assessment procedures and the rules for the affixing 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 tested according to the EMC requirements for emission and immunity for electrical equipment for measurement, control and laboratory use.

Compliance with the protection requirements areas (domestic establishments and establishments directly connected to a low voltage power supply network which supplies buildings used for domestic purposes) and industrial areas is ensured.

Our strict standards regarding operating quality and resulting considerable amount of time and money spent on development and testing reflect our commitment to guarantee the high level of quality of our products even under extreme electromagnetic conditions.

Practice however also shows that even electrical equipment which bears the CE marking such as monitors or analytical instruments can be affected if their manufactures 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.

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Information concerning the CE sign / WEEE compliance

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 symbol:

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 Scientific products which may assist the detection of substances subject to the RoHS Directive are available at www.thermo.com/WEEERoHS

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Quality Assurance/Contacts at Thermo Fisher Scientific

2. Quality Assurance

Dear customer, Thermo Fisher Scientific implements a Quality Management System certified according to ISO 9001:2008. This guarantees the presence of organizational structures which are necessary to ensure that our products are developed, manufactured and managed according to our customers expectations. Internal and external audits are carried out on a regular basis to ensure that our QMS is fully functional. We also check our products during the manufacturing process 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. +49(0)721 4094--444 Fax +49(0)721 4094--300

support.mc.de@thermofisher.com 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

Page 9

Warranty

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 initial 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 required.

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

5. Safety Notes and Warnings

The Rheometer corresponds to the relevant safety regulations. However you are solely responsible for the correct handling and proper usage of the instrument.

This instrument exclusively determines the rheological behavior 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 guaranteed 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 control stand.

This unit should only be used for the applications it was designed for.

The rheometer is designed for use with a rotor. All existing safety devices are based on the correct installation of the rotor. Is the lift (of the measuring table) used without 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 electrostatic charging resulting in a defect of the electronic circuit boards.

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! !

Safety Notes and Warnings

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 substance 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 personnel. Considerable damage can be caused by incorrect repair work. The Thermo Fisher Scientific service department is at your disposal for any repairs you may require.

Have the unit serviced by specialists at regular intervals.

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, depending 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 serious burns can result if they come into contact with the skin.

Thermo Fisher Scientific recommends shielding the rheometer 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 possible danger (burn injury).

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Safety Notes and Warnings

We do not know which substances you intend to test using 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

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 t he ends of the glass pane.

Use the transport handles provided for the instrument when unpacking.

The instrument must be carried by two persons.

Unpacking the instrument and putting it into operation 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

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Unpacking / Ambient conditions

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

Page 15

Unpacking / Ambient conditions

6.2.2 Sensor Systems

Various sensor systems are available for the Rheometer which differ also in their temperature control specifications.

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 circulators 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

Page 16

230 V

115 V

230V

115V

Unpacking / Ambient conditions

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:

Use the mains cable according to your local mains voltage ( see chapter “Contents of delivery”).

Insert the fuses according to your local mains voltage below the mains connection 6.

For 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

Insertion of the fuses: Pull out the fuse holder from the mains socket and

insert the fuses. Reinsert according to the marked voltage.

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 respectively. maximum conduction pressure 0.5 bar. (RheoStress are cooled by the outgoing air of the air bearing.)

1.0 m

0.85

Rheometer

Circulator

Page 17

Unpacking / Ambient conditions

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/m3air,

-- 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 damage 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 levels). 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 materialprocessing 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 admissible 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 controller 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

Page 18

Unit Description

7. Unit Description

lntroduction

The viscoelastic behavior of a fluid or a soft solid can be characterized in two ways; either the fluid is deformed and the resulting stress is measured (CR mode), or the stress is applied and the deformation monitored (CS mode). The principle 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 RheoWin Software or with one of 10 pre--programmable measuring procedures by the display unit. The results are available for further processing on a PC with the HAAKE RheoWin 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 available.

Page 19

Unit Description

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 controlled or can be loaded as procedure in the display and control 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 RotoVisco1 these tasks can be taken over by the PC which controls t he 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 measured 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

Page 20

Unit Description

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 dependence 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 dynamic 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.

Page 21

Unit Description

7.3 Temperature control:

TCO Glass plate with a Pt100 temperature sensor

(not temperature controlled).

TCL/Z Liquid temperature controlled receptacle for cylinder

measuring systems with direct contact of the thermal fluidfrom--40upto200C.

TCL/P Liquid temperature controlled measuring plate for

parallel plate or cone & plate measurements (with external circulator from --20 up to 300C).

TCP/P Measuring plate with Peltier temperature control for TCP/PE parallel plate or cone & plate measurements from

--40 up to 180C (external heat transfer required).

TCE/P Electrically temperature controlled measuring plate for

parallel plate or cone & plate measurements from

-- 2 0 Cupto350C.

TCE/PC Electrically temperature controlled measuring plate for

parallel plate or cone & plate measurements with electrical cone heating from --40Cupto350C.

SHRP Special temperature controlled system utilizing

thermal liquid as standardized for asphalts and bitumen. Temperature range: 0C(--25C)... +90C (for HAAKE RheoStress 1)

Page 22

Unit Description

7.4 Main features of the HAAKE rheometers:

 Quick fitting sensor with a high precision even if not

perfectly clean.

 Remote and manually controlled lift with variable

speed to preserve the fluid’s structure and ensure reproducible test conditions.

 Microprocessor controlled positioning of the sensor to

ensure the highest accuracy for routine tests.

 Standard temperature range of --40 to 250 C using a

heating circulator; utilizing electrical cone heating extends this up to 350 C.

 Controlled rate mode for characterizing rheologically

complicated fluids (HAAKE RotoVisco 1 and HAAKE RheoStress 1).

 Controlled stress mode for characterizing sensitive

substances (HAAKE RheoStress1).

 Forced oscillation tests at very low frequencies and

very low strains allow destruction free measurements (HAAKE RheoStress 1).

 Sophisticated application software packages with

userfriendly window menus and an on-line help key.

Page 23

Installation

8. Installation

8.1 Setting up the Rheometer

Lift the Rheometer out of the package and place onto a stable, level table. Do not lift the unit at the glass pane or at the measuring head ! For sensible measurements a plane table is recommended.

In the base of the measuring instrument, there are four feet which can be screwed in or out for levelling the unit.Upon completion of the preliminary visual levelling, exact precision levelling can be carried out using the spirit level supplied.

The spirit level:

 is put on the measuring plate at temperature control

unitTCL/P;TCE/P;TCE/PCandTCP/P.

 is put into connection with a vessel at temperature con-

trol unit TCL/Z.

 is put on the measuring plate in the vessel at tempera-

ture control unit SHRP.

 is not used at temperature control unit TCO.

Adjust the feet so that the air bubbles remain in the center of the spirit level.

This adjustment process should be repeated at least once a week.

Page 24

Installation

8.2 Connecting up

Make sure that the unit has been switched off before you connect or disconnect the cables.

The cable connections between the sensor system, the control unit, the PC and the printer have to be established ( see. chapter Pin Wiring)

Measuring Instrument

Air

supply

unit

Heating

Bath

and

Circulator

Control

unit

Printer

and/or

Temperature Control Units

RS 232

Centronics

Display

Luft / Air

PT100 ( output )

PT100 ( input )

Shielded RS232 cable with ferrite core

e.g. filter unit 222-1211 or compressor 222-1435

(RheoStress 1)

222-1490

222-0572

8.2.1 PT100 connection

PT100 (input) socket for external PT100 sensor only

when using TCO

PT100 (output) socket for PT100 sensor only when using

TCL/Z and TCL/P

The connections are described in chapter “Pin Wiring”.

Page 25

Installation

8.3 Hose connections

8.3.1 Temperature control unit (with liquid):

 The temperature control unit with liquid temperature

control is connected with hoses to a heating bath and circulator.

While fastening the hose connections at the connecting nozzles (14) of the temperature control unit the connecting nozzles must be held up by wrenches.

Direction of flow of the liquid

Temperature range up to 150 C:

Viton hoses

Hoes nozzle -Set 222--1492

Temperature range of 100 Cupto350 C:

Metal hoses 333-0294

Hoes nozzle -Set 222--1492

Liquid temperature control:

Temperature range up to 100 C:

Thermal liquid in the temperature range between --50 C and 30 C: water with anti-freeze. Temperature range from 5 Cto90 C: distilled water.

Distilled water

Normal mains water causes cable deposits and frequently requires the unit to be descaled.

In principle, water up to 95 C can be used. However, above 80 C, so much water evaporates that it requires frequent topping--up.

Water with anti--freeze

If you intend working at temperatures below 5 C, anti--freeze must be added to the water. The added amount of anti--freeze should be sufficient for a temperature that is about 10C lower than the intended working temperature. This prevents the freezing of water on the evaporator coil of the cooling circuit, the surface of which is always much colder than the

Page 26

Installation

working temperature. However, too much anti--freeze worsens the temperature constancy due to its high viscosity.

Temperature range from 100 Cto200 C:

Silicone oils or other suitable liquids are used as thermal liquid.

8.3.2 Air bearing (measuring unit)

 The air bearings of the measuring units HAAKE

RheoStress1 require cooling air at port 9 (see “Requirements for the air supply”).

Page 27

Functional Elements

9. Functional Elements

9.1 Temperature control units

Rheometer Temperature control units

TCO TCL/Z TCL/P TCE/P

TCE/PC

TCP/P SHRP

HAAKE RotoVisco1 X X X X X HAAKE RheoStress1 X X X X X X

Page 28

Functional Elements

9.2 External filter

An external filter is part of the standard range of items supplied with the temperature control units for Series 1 TCP/P (Peltier-Temperature control system), TCE/P (electrical temperature control unit), TCL/PO (liquid temperature control unit for HAAKE RheoScope) and the UTCP/P (Peltier-Temperature control system for HAAKE RSXXX units). It consists of the filter itself, a plastic cone contained inside it, and clamps. Using this filter enables the interior of the relevant temperature control unit to be protected against any impurities carried in by the temperature liquid. The external filter represents an additional protection. On the standard model a sieve is built in to the intake of each temperature control unit.

As shown in Fig. X, the filter is installed in the intake hose leading into the temperature control unit between the thermostat and the measurement instrument. The intake and outlet directions must be noted (IN and OUT on the filter). It is fastened with the clamps that are supplied with it. Hoses with a diameter of 8 mm can be installed and fastened with the clamps supplied. The plastic cone on the inside of the filter serves as a direction of flow indicator, and its movements show the through-flow of the tempering liquid. If there are impurities in the filter it can be taken out, cleaned, and used again. The use of the external filter is recommended because any impurities can be recognised and removed more readily than with the sieve that is built in to the temperature control unit. The screw-in sieve (internal) must of course be checked for impurities from time to time in order to ensure t he functional capability of the temperature control unit.

Order numbers: 003-5266 Screw-in sieve (internal) for TCL/P, TCP/P,

TCE/P, TCL/Z

222-1667 External filter for TCP/P, TCE/P, TCL/PO

Page 29

Functional Elements

9.3 Measuring Instrument with no

temperature control unit.

Front

1. Measuring unit

3. Quick cut-off switch

4. Green LED display: operational

Page 30

Functional Elements

Rear

7 8

A. Caution: Read the instruction manual

6. Mains switch with mains socket and fuses

7. RS 232 interface (PC)

8. Connection for printer

9. Connection for cooling air (RheoStress1 for the air bearing)

10. PT 100 Connection

11. Connection for display unit

12. Reset switch

13. Switch for bootstrap loader

Page 31

Functional Elements

9.4 Measuring Instrument with TCL/Z -- temperature control unit.

Front

A. Caution: Read the instruction manual

Glass pane can heat up! Use safety gloves!

1. Measuring unit

2. Temperature control unit

3. Quick cut-off switch

4. Green LED display: operational

5. Yellow LED display: heating

18. Clamping lever

When using a circulator for temperature control, this must be located lower than the measuring device, other via the temperature control liquid will flow back in to the measuring beaker location and over the measuring device.

Page 32

Functional Elements

Rear

IN OUT

A. Caution: Read the instruction manual

6. Mains switch with mains socket and fuses

7. RS 232 interface (PC)

8. Connection for printer

9. Connection for cooling air (RheoStress1 for the air bearing)

11. Connection for display unit

12. Reset switch

13. Switch for bootstrap loader

14. Liquid cooling for temperature control unit

20. Connection for PT100 (output)

Page 33

Functional Elements

9.5 Measuring Instrument with TCL/P / TCE/P / TCP/P / TCP/PE

-- temperature control unit.

Front

A. Caution: Read the instruction manual

Glass pane can heat up! Use safety gloves!

1. Measuring unit

2. Temperature control unit

3. Quick cut-off switch

4. Green LED display: operational

5. Yellow LED display: heating

19. Measuring plate

Page 34

Functional Elements

Rear

OUT IN

A. Caution: Read the instruction manual

6. Mains switch with mains socket and fuses

7. RS 232 interface (PC)

8. Connection for printer

9. Connection for cooling air (RheoStress1 for the air bearing)

11. Connection for display unit

12. Reset switch

13. Switch for bootstrap loader

14. Liuid cooling for temperature control unit

20. Connection for PT100 (output) only at TCL/P

Page 35

Functional Elements

9.6 Measuring unit with TCE/PC-temperature stabilisation unit and cone heater TC1

Front side

A. Caution: Read the operating instructions!

Unit parts can get hot! Wear protective gloves!

1. Measuring unit

2. Temperature stabilisation unit

3. Emergency OFF switch

4. Green LED: Ready for operation

5. Yellow LED: Heating

19. Measuring plate

21. Cone heater TC1

Page 36

Functional Elements

Rear

OUT IN

A. Caution: Read the operating instructions!

6. Mains switch with mains socket and fuses

7. RS 232 interface (PC)

8. Connection for printer (Centronics)

9. Connection for cooling air (RheoStress1 for the air bearing)

11. Connection for display unit

12. Reset switch

13. Switch for bootstrap loader

14. Liuid cooling for temperature control unit

20. Connection for PT100 (output)

22. Fuse T1.25A

23. Fuse T8.0A

24. Fuse T3.15A

25. Connection for cooling air (for TC1)

Page 37

Functional Elements

9.7 Measuring Instrument with SHRP -- temperature control unit.

Front

A. Caution: Read the instruction manual

Glass pane can heat up! Use safety gloves!

1. Measuring unit

2. Temperature control unit

3. Quick cut-off switch

4. Green LED display: operational

5. Yellow LED display: heating

17. Influx control

Page 38

Functional Elements

Rear

A. Caution: Read the instruction manual

6. Mains switch with mains socket and fuses

7. RS 232 interface (PC)

8. Connection for printer

9. Connection for cooling air (RheoStress1 for the air bearing)

11. Connection for display unit

12. Reset switch

13. Switch for bootstrap loader

14. Liquid cooling for temperature control unit

16. Overflow port

Page 39

down

MenuEnter

Tast e 4Tast e 1 Tast e 2 Tast e 3

Tast e 5

Tast e 6

Nr.(HEADER)

(Status)

Functional Elements

9.8 Display unit (optional)

(Order no. 222--1472)

DOWN

MENÜ

ENTER

Tas t e 4

Tas t e 1 Tas t e 2

Tas t e 3

Tas t e 5 Tas t e 6

Nr.MENÜ

Status

General display screen splitting

Header gives the display title

see mask number on the right;

Keys1to6 are reserved differently under each display

title

Up/Down increase or decrease e.g. number values;

short pressing - small increments, long pressing - increasingly higher increments;

Enter is the confirmation of an entry or selection; Menu goes back to an overview display; Status shows date/time, internal store capacity

for measurements, help texts

Page 40

Functional Elements

9.9 Menu tree of the display unit

Page 41

Temp. controlDiagnosis Time / Date Display

Language

Lift

100CONFIGURATION

OperatorConfiguration Jobs Lift

Sample name

010MENU

Status

OperatorConfiguration Jobs Lift

Sample name

010MENU

Status

Operating

10. Operating

10.1 Switching on

When all connections have been established and the supply lines are active, switch--on the mains switch 6:

 The green display 4 on the measuring table of the

rheometer indicates the ready state for operation.

The following operation sequence should be used to be able to make the measurements at short notice:

-- Instrument:

 Automatic device initialization  Raises the lift. Never switch off the unit during lift move-

ment.

In case of loss of power during the lift movement, the unit has to be initialized again.

 Then the following display appears:

-- Operator: Insert sensor if necessary

-- Instrument: Lowers the lift for zero point determination.

Due to the rotation of the pin spots can appear on the measuring plate. This is normal and does not constitute any damage to the unit.

Then move the lift again to cleaning position (i.e. up), the instrument immediately shows the MENU selection window (A) for defining, if necessary,the operator, sample name etc.

10.2 Working with the display unit

In MENU activate CONFIGURATION by pressing the key.

Pressing the key leads directly into the submenu.

Page 42

Full Print

200DIAGNOSIS

Status

203DATA MEMORY

Status

Start

Change

Cancel

Date: xx xx xxxx Time: yy:yy:yy

201TIME /DATE

Status

Online displayContrast Units Country

Online graph

202DISPLAY

Status

Enter

Operating

Diagnosis

FULL-DIAGNOSIS:

-- The complete device diagnosis contains all internal tests which are possible at present;

HARDCOPY:

-- Sends a diagnosis report to the printer.

Date / Time

Display

Pressing each key leads directly into the respective submenu:

CONTRAST Contrast number: xx increase or decrease

UNITS Switch over facility for

Temperature: Cor F Viscosity: Pas or mPas

COUNTRY SETTINGS Choice of one of two available date formats.

ON-LINE-VALUES ONE predefined display mask with 6 fields (3x large fields on left and 3x small fields on right, respectively assigned to the keys) appears. On pressing a key at the respective field, this field is activated and any desired physical parameter can be assigned to it. Fields with no parameter assigned to them do not appear during the measurement.

ON-LINE-GRAPHICS Twoy--axes and one x--axis can here be assigned to any desired respective physical parameters.

Data memory

Page 43

SpanishGerman English French

204LANGUAGE

Status

OperatorConfiguration

Jobs

Lift

Sample name

110MENU

Status

Batch ID

Open Together Stop

110LIFT

Status

Contact

Measurement

Sensor

Operating

Language

Measure

The measurement sequence as a whole is described under ”Measuring sequence”.

Lift

LIFT activation takes place in MENU by pressing the key.

Pressing the key leads directly into the submenu: OPEN

-- The lift raises to t he top position and stops there (cleaning position).

CONTACT

-- The lift moves down to t he contact point (zero point)

-- and then up again to the cleaning position with status message reporting successful zero point determination.

TOGETHER

-- The lift runs max. (if STOP is not actuated before) to the contact point and stops there.

STOP

-- Stops the lift immediately.

MEASURING POSITION

-- Runs from the current position (usually the cleaning position) to the measuring position.

Page 44

OperatorConfiguration Jobs Lift

Sample name

010MENU

Status

Batch ID

SchleimTei g #1 Teig #2 PE-Lösung

010SAMPLE NAME

Status

OperatorConfiguration Jobs Lift

Sample name

Batch ID

010MENU

Status

Muster

115OPERATOR

Status

Operating

Operator

In MENU activate OPERATOR by pressing the key.

Pressing the key leads directly into the submenu:

-- The list of OPERATORs is defined in RheoWin and downloaded from there.

Sample name

In MENU activate SAMPLE NAME by pressing the key.

Pressing the key leads directly into the submenu:

-- The list of SAMPLE NAMEs is defined in RheoWin and downloaded from there.

Page 45

OperatorConfiguration Jobs Lift

Sample name

Batch ID

010MENU

Status

Polyethyl. CreepSnap-shot test Manual Measurement Multiwave

Linearitätstest

105JOBS

Status

Aushärtungstest

SampleMethode: Sensor: Multiwave:

210MEASUREMENT DEFINITION

Status

125BATCH ID

Status

OperatorConfiguration

Jobs

Lift

Sample name

Batch ID

010MENU

Status

ID: ABC87--D2/F

ABCDEFGHIJKL MNOPQRSTUVW

down

MenuÜbersicht ausdrucken

Batch ID:

Sample number

Start test

Operating

Batch ID

In MENU activate BATCH ID by pressing the key.

Pressing the key leads directly into the submenu:

-- Batch ID must be entered on the display unit.

Measuring sequence

In MENU activate MEASURE by pressing the key.

Pressing the key leads directly into the submenu: (The names of the jobs are defined by the user in the RheoWin--Software.) ”Snap--Shot Test” and ”Manual measurement” are permanently assigned.

Pressing a key leads directly to the ”Measurement definition screen”.

-- If all specifications are correct, the operator can press ”START TEST”.

Page 46

Stop JOB

Stop element

320TEST RUN

Status

Start test

321TEST STOP

Status

Lift

Operating

-- After the operator has started the measurement, the job starts and the display shows the predefined online form.

-- The operator waits until the job is completed or discontinues the job or the current element (jumps to the next element).

On completion or discontinuation of the job, the following display appears:

The operator sees the results of the job on the display and has 3 options for continuing:

Insert new sample: Press LIFT (lower lift), display No. 110 appears, replace old sample with new one and then continue.

Next measurement (same job) with same sample but possibly other parameters: Press STARTNEW MEASUREMENT. Any existing parameter place holders of this job are shown again for editing.

General continuation of operation of the instrument via MENU.

Page 47

Operating

10.3 Starting the software

Switch on the PC and load MS Windows.

In the Windows Program Manager double-click t he RheoWin Job Manager icon.

 RheoWin is started.

Click the Device Manager icon in the menu bar.

Select the connected unit in the Device Manager and check the connection with ”Test”.

For extensive operation please read the instruction manual of your software.

Page 48

Operating

10.4 The ”Upload Mode” for the Display Unit

(RheoWin 2.6 or higher)

The rheometers can be operated by the software RheoWin in ”direct mode” or it can be loaded by special functions measuring programs in the store of the measuring device. By that, the measuring device gets independent of the PC and it is only connected for programming or data transfer. The measuring programs (”JOBs”) are started after the corresponding programming with the display unit.

For programming or data transfer the Rheometer must be connected to the PC via RS232 cable as usual and Thermo Fisher Scientific Haake software RheoWin must be loaded.

After installing the rheometer two versions per model can be found in the device manager . The device e.g. RotoVisco1 is running in the software direct mode as usual. Model RV1 (Upload mode) has already been pre--defined as independent device.

The characteristic ”Upload Mode” is transferred to the device driver on the following card which can be found under ”Edit”. So you can give the device driver the characteristic ”Upload” or ”Software” mode. For practical reason it is advisable to define a new device for each operation.

Page 49

Operating

Other options on the device record card are:

Torque Compensation

When the torque compensation is activated, the present value of the torque display is set on zero ”0” right before the measurement so that possible faults (offset faults) can be reduced. This is always advisable when samples without ”yield point” are to be measured. In case of doubt it is measured first without ”Torque Compensation” and after that it is decided whether the function can be used.

Inertia of Masses Correction Ramp

If fast speed ramps (< 180 s) are driven, the dampening set at the sensors (usually 30%) and also the inertia of the masses of the measuring device (motor and rotor) enter the result. Fast ramp speeds make up a hysteresis curve which does not come from the sample but from the test conditions and the measuring device. The influence can be seen qualitatively in the following diagram. It is recommended to drive measurements with ramp times of less than 120s without correction only in special cases. With correction, the influences of the inertia of masses are compensated. This can be tested individually at examples relating to practice.

Page 50

Operating

Communication Record

This function has been installed for service use. If this function is activated, all commands between the measuring device and the PC are recorded in a file named Driver.log (RV1.log, RS1.log,) and are managed in the directory \rheo-

win\driver\.

Upload

Under ”Upload” you can find the present data for user, sample and sensor. These data are entered with RheoWin and are read out . In the display unit these exact terms can be selected. If you are connected to the measuring device at the running time the present level of the store is read out with ”READ” and is displayed. Changes can be made. They are transferred to the measuring device while leaving the menu and are available now. If the device has not been programmed yet (state at delivery) all lists are empty.

Now the three record cards can be filled with information. With the mouse and the cursor the first position is clicked and e.g. a name is entered. After that the second line can be clicked and other entries can be made.

Page 51

Operating

When all names of possible users are entered, the names of the samples which are to be measured can be entered. Only these names can be recalled from a selection list.

In principle the same is valid for the sensors of the rheometer. It is recommended to enter only the sensors which are really in existence from the list of all variants to keep the display clearly organized.

Page 52

Operating

The sensors of the right window are transferred to the measuring device if you leave the menu with <OK> . With Cancel the existing adjustments are kept. If the factors are changed, e.g. after a calibration, the values of the sensors can be renewed with <READ> after the reading of the store.

Drawing up JOBS for Uploading

JOBs or measuring and evaluation procedures are drawn up with the RheoWin Job manager. The distinction takes place before the drawing up of a JOB at the selection of the measuring device. If existing JOBs are changed afterwards unexpected reactions can take place. The following proceeding is recommended:

First the measuring device is selected. After that the procedure is drawn up.

Page 53

Operating

After the selection of the measuring device, the sensor and a temperature control unit are selected. If no temperature control unit is selected, no temperature control can take place. No selection (--------)also means that the temperature control unit is switched off.

The measuring process is now composed according to the requirements of the application or of the user just as in the PC mode. There are some restrictions of the length of names and the selection of elements. These restrictions are visible only at editing.

After the drawing up of a JOB it can directly be started for a test or it can be uploaded to the measuring device. On this

Page 54

Operating

occasion a list gets visible that shows an empty list or already existing JOBs. The order or position of the list corresponds to the reservation in the measuring device. So you can make an allocation indirectly. Empty positions have to be avoided, because otherwise the following entries would be ignored.

Uploaded JOBs can be called in via the display unit and can be carried out directly.

Reading back uploaded JOBs from the measuring device

JOB’s can be read back from the measuring device with the RheoWin function /File/Open Job of Measuring Device/. This function corresponds to the reading of the hard disk.

If this function is selected, all installed unit drivers are called in and it is tested if a connection can be made. Drivers that are not installed correctly cause error messages and should be cancelled from the device list (device manager). If a measuring device with the possibility of managing JOBs responds it is selected and displayed immediately.

Page 55

Operating

In the white area the existing JOBs are listed for selection.

Measuring result

The measuring result is a chart with measuring and preset values according to the measuring definition. It can be transferred, if defined in the JOB, directly to a printer. The result is then shown as selected. Segments can be printed or ignored. The selection of the column contents takes place via the list menus:

Importing the measuring result in RheoWin

The last measuring result can also be imported directly to the RheoWin software (measuring device connected to PC and RheoWin active).For this the file in the DATA manager is opened.

Page 56

Operating

From the following list the device of your choice is selected for reading out the data. This is necessary because the software RheoWin can drive and read several units by multitasking.

After the selection the data are transferred via RS232 interface from the measuring device to the PC/RheoWin software. The data are treated like comparable values of the local hard disc or of the network.

Page 57

Operating

10.5 Quick Cut-off

The switch (3) at the top of the right column switches off the measuring drive, heating and lift.

Internal measuring jobs are interrupted.

Page 58

Temperature Control Units

11. Temperature control units

11.1 Temperature control unit TCO

The sample is in the measuring gap of the sensor system. The rotator is driven by a preset speed (n). Due to its viscosity, the sample is resistant against the rotation. This resistance gets active as (braking) torque (Md) at the measuring shaft of RV1. The torque is measured.

From the values of speed, torque and measuring system geometry (system factor) the installed PC calculates the the measuring values for

If a temperature sensor is connected, the temperature T (in C) is also calculated.

The results are shown on the display (operating panel) and and can be passed on to a computer (PC) or printer via interface connection RS232.

Page 59

open

closed

Temperature Control Units

11.2 Temperature control unit TCL/Z

Place the beaker into the temperature control unit and fix it with the clamping lever.

The sensor system and the temperature control unit require cooling according to load and temperature during the measurement.

Connect the rheometer to a Thermo Fisher Scientific Haake circulator with optional hoses ( 8 mm).

While fastening the hose connections at the connecting nozzles(14) of the temperature control unit::

-- ensure the correct flow direction (IN/OUT)

-- the connecting nozzles must be held secured using a wrench.

maximum conduction pressure 0.5 bar (water circulation). For the TCL/Z sensor system and the open--bath and heat-

ing circulators the necessary tubing hoses are not part of the standard accessories. They have to be ordered separately.

When the measuring beaker is inserted in the t emperature control unit, a valve is automatically opened as it is pressed in and temperature control liquid flushes the beaker. The valve is closed again when the beaker is removed. The displacement path of the valve means that the beaker must be moved 3mm. If the seal is missing or an incorrect closing screw has been fitted, the valve can remain closed and the temperature control function is inoperative. Remedy:

Fit a new seal, a correct closing screw or a

spacer.

The circulator must be located lower than the measuring device, other via the temperature control liquid will flow back in to the measuring beaker location and over the measuring device.

For the TCL/Z measuring unit and the open--bath and heating circulators the necessary tubing hoses are not part of the standard accessories. They have to be ordered separately.

The lever (222--1639) for cylinders is an accessory for t he RheoStress 1 and RotoVisco 1 rheometer models, which are equipped with a liquid temperature control unit (TCL/Z) for coaxial cylinder measuring geometries. The lever enables the removal of the measuring cup, e.g. for cleaning at the end of a measurement.

Page 60

Temperature Control Units

The following procedure is recommended:

Switch the circulator off, in order to reduce the low pressure of the temperature liquid.

Position the lever as illustrated in Fig. and move the lever upwards till the measuring cup is free to move.

The measuring cup can be now easily removed by hand.

Hendling of the lever

lever

measuring cup

Page 61

Temperature Control Units

11.3 Temperature control unit TCL/P

The temperature control unit has a holding for the measuring plate. The measuring plate is put on the thermal liquid heated temperature control unit and is fastened.

Cones and measuring plates should have the same diameter e.g. as cone C60/1 and the measuring plate MP60 or plate PP35 and measuring plate MP35. If not, huge measuring faults are the consequence !

For measurements at temperatures higher than 70Citis recommendable to use at least the sample protection shield (222-0608) to reduce the loss of heat. In any case, the application of measuring cones and measuring plates with a ceramic shaft that do carry off less heat is recommendable.

The sensor system and the temperature control unit need cooling that is dependent on the load and the temperatures during the measurement.

While fastening the hose connections at the connecting nozzles(14) of the temperature control unit::

-- ensure the correct flow direction (IN/OUT)

-- the connecting nozzles must be held secured using a wrench.

For the cooling of the temperature control unit hoses (with

 8mm) can be connected to a liquid circulator. maximum conduction pressure 0.5bar (water circulation).

Page 62

Temperature Control Units

11.4 Temperature control unit TCE/P

The temperature control unit has holding a for the measuring plate. The measuring plate is put on the thermal liquid heated temperature control unit and is fastened.

Cones and measuring plates should have the same diameter e.g. as cone C60/1 and the measuring plate MPC60 or plate PP35 and measuring plate MPC35. If not, huge measuring faults are the consequence !

For measurements at temperatures higher than 80Citis recommendable to use at least the sample protection shield (222-0608) to reduce the loss of heat. In any case, the application of measuring cones and measuring plates with a ceramic shaft that do carry off less heat is recommendable.

The temperature control unit is connected to a liquid circulator via hoses ( 8mm) .

For the TCE/P measuring unit and the open--bath and heating circulators the necessary tubing hoses are not part of the standard accessories. They have to be ordered separately.

The cooling (liquid or gas) is controlled directly in the measuring device via the built-in solenoid valve according to the requirements. It is important that the cooling medium used is selected in the RheoWin software, as the control parameters (PID) are thus selected. The switching condition of the valve is „open“.

Utilizing the optional electrical cone heating extends the temperature range up to 350C.

Page 63

Temperature Control Units

11.5 Temperature control unit TCP/P and TCP/PE

The temperature control unit has a measuring plate  60, which is at the same time the location for other measuring plates. The measuring plate is put on the Peltier temperature control unit and fastened. The additional plates MPC are only necessary if the same cone--plate diameter is used for measuring.

Temperature control is carried out electrically via a Peltier element within a temperature range of --40 to 180C.

The Peltier process

The temperature control system is based on a component which uses the Peltier effect. This effect which is the reverse of the thermoelectric effect (e.g. used by thermocouples), was discovered in 1834 by the French physicist Jean Peltier.

Peltier elements consist of two semiconductor bridges of differing doping (p- and n-type). Stimulated by a (regulated direct-)current flow, the electrons transport heat from one connection point to the next.

Diagram of a Peltier module

n- and p-doped elements

contact bridges

electric insulation

Cold side

Hot side

The heat flow direction is dependent on the current flow direction. Peltier temperature control systems can thus be used for both heating and cooling depending on the current flow direction.

The heating or cooling capacity i.e. the transported heat quantity is proportional to the current strength depending on the semiconductor material used and the number of Peltier elements electrically connected in series within the Peltier module.

Page 64

Temperature Control Units

Peltier modules transport heat from one side of the module to the other and thus can be understood as the thermoelectric system of a solid state heat pump. Heat itself is scarcely absorbed during this process. The heat side is in any case exposed to the dissipated energy in addition to the transported Peltier heat which has the result of causing the heating and cooling measuring curves not to be identical. The maximum heating rate is therefore higher than the maximum cooling rate.

Operation

In the temperature control unit a cooling coil (with hose connections for liquid cooling) is built in to cool the Peltier element.

The connector nozzles of the heat exchanger may not be closed during operation. A high overpressure may exist during the heating up.

The temperature control plate is set in a plastic part (TEKAPEEK).

Recommended couling liquids are water or mixtures of water / alcohol as well as water / glycol.

The maximum for the temperature of the couling liquid is 100 C.

Cooling and Heating

Since the Peltier temperature control unit is cooled by circulating water the temperatures as well as the heating and cooling rates (times to reach t hose temperatures) depend on the temperature and of the flow through rate of the coolant.

By variation of the flow-through temperature and the flowthrough volume optimum conditions can be reached for every working range desired.

In general, the following applies:

 During heating the temperature control unit will reach

a max. temperature difference of abt. 100C between temperature control plate and the temperature of the coolant under optimum conditions.

 During cooling the temperature control unit will reach

a max. temperature difference of abt. 20--40C between temperature control plate and the temperature of the coolant under optimum conditions.

Page 65

Temperature Control Units

Heating

140

Final temp.

[ C]

600

t[s]

Cooling curve with water circulator (DC50--K20) of about 80C

Cooling curve with high temperature supply of about 100C

Cooling curve with room temperature coolant fluid

In general, the following applies for the heating:

 Increasing the temperature of the coolant will result in

higher final temperatures and higher heating rates (the final temperature will be reached faster).

 Decreasing the flow through volume will result in higher

final temperatures and higher heating rates. Example: With a preset temperature of 20C the Thermo Fisher

Scientific Haake circulator DC50-K20 will reach max. heating rates up to 1 K/s and a final temperature of about 100C after about 10 minutes.

Page 66

Temperature Control Units

Cooling

Cooling curve with high temperature of the coolant (room temperature)

Cooling curve with coolant water circulator (DC50--K20) (reservoir temperature 20C)

360

t[s]

Final temp.

[ C]

Cooling curve with low temperature of the coolant (reservoir temperature 5C)

-- 2 0

In general, the following applies for the cooling:

 Decreasing the temperature of the coolant will result in

lower final temperatures and higher cooling rates (the

final temperature will be reached faster).

 Increasing the flow through volume will result in lower

final temperatures and higher cooling rates. Example: With a preset temperature of 20C at the Thermo Fisher

Scientific Haake circulator DC50--K20, the Peltier system will reach max. cooling rates up to 1 K/s and a final temperature of 0C. Starting at +20C the final temperature of 0C will be reached after about 6 minutes.

 For a given ambient or room temperature there is a low-

est temperature which can be reached. This is usually

about 0C.

 lower temperature values can be realized if the loss of

cooling capacity is reduced by insulation.

Page 67

Temperature Control Units

Explanation for the cooling

The cooling rate is limited especially for a value when cooling below the ambient temperature. Therefore, the settings of the software have to be adapted in order to reach the temperature desired:

1. For the measuring definition of temperature ramps downwards the ”rising” will be tested -- for cooling negatively. That means that it has to be calculated according to the set values for start and end temperature as well as the duration using a formula to find out whether the cooling rate can be achieved. If it is not possible an error message shows the possible cooling rate.

2. At the beginning of a segment cooling down to the set starting temperature can be necessary. This coolingdown time will be calculated. In case the time being higher that 10 s the band width will be set from 0.0 to

0.1 to reach the desired start temperature. In this case a message window appears as always whenever the band width for the start temperature is unequal 0.0. The system waits until the band width of 0.1 has been reached. Attention: An abortion using the F7 key would also abort the cooling process. Then the segment would be measured with the temperature reached until then.

3. For temperature segments the waiting time set by the user might be too short to hold the possible cooling rate. In case the time being more than 10 s too short it will be set to the required value.

The sensor system and the temperature control unit require cooling that is dependent on the load and the temperatures during the measurement.

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Temperature Control Units

For the cooling of the temperature control unit hoses (with  8mm) can be connected to a liquid circulator.

While fastening the hose connections at the connecting nozzles(14) of the temperature control unit::

-- ensure the correct flow direction (IN/OUT)

-- the connecting nozzles must be held secured

using a wrench.

maximum conduction pressure 0.5bar (water circulation). For the TCP/P measuring unit and the open--bath and heat-

ing circulators the required tubing hoses are not part of the standard accessories. They have to be ordered separately.

Page 69

Temperature Control Units

11.6 Temperature stabilisation unit TCE/P with cone heater TC1

The temperature stabilisation unit has a holder for the measuring plate. The measuring plate is placed and secured onto the electrically heated temperature stabilisation unit.

The wedge and measuring plates should have the same diameter, for example like the taper C60/1 with the measuring plate attachment MPC60 and the plate PP35 with the measuring plate attachment MPC35. Otherwise unavoidable measuring errors arise!

11.7 Cone heater TC1

The high temperature system TC1 was developed for the measuring units with a TCE/P temperature stabilisation unit for rheological measurements at temperatures of > 0Cto 350C with and without external cooling. Inert gas should be used for cooling.

A PID controller is used to control the temperature, with the upper and lower heating elements being regulated separately and independently of each other. Each of the two systems has individual control parameters and its own control sensor. This enables the lower part to also be used separately for temperature control in order to improve the handling (albeit at the expense of the temperature stability) and so that the behaviour of the flowing sample material can be observed better. When the measuring element body is fitted, only tapers and plates with ceramic shafts can be used.

We generally recommend in the case of measurements over +60C that these special measuring geometries be used in order to minimise unwanted heat dissipation via the shaft.

11.7.1 Correct application of the ceramic rotors

We recommend the use of the tools supplied at the same time in order to ensure t hat the ceramic rotors are properly screwed in. Insert the Allen key supplied into the ceramic shaft opening above the cone heating and fasten the rotor. Tighten the union nut by hand.

Page 70

Temperature Control Units

11.7.2 Operation

The temperature stabilisation system TC1 is operated exclusively via the application software of the HAAKE rheometer being used.

As long as the system is hot, do not touch either the upper chamber or another hot part without wearing suitable protective gloves.

Parking position top or Measuring position bottom

From the parking position to the measuring position:

Swivel both halves outwards as far as possible and then lower them down. Fold together the TC1 and lower it down onto the measuring plate.

From the measuring position into the parking position:

Lift the TC1 approx. 2 cm in one movement without letting go TC1, swivel it out as far as possible, lift it up as far as it will go and fold together until both halves lie on the engaging pins.

The measuring unit and the temperature stabilisation unit require cooling, depending on the utilisation level and the t emperatures during the measurement.

When attaching the hose connections to the connection glands (14) of the temperature stabilisation unit,:

-- pay attention to the flow direction (IN/OUT)

-- use an open-ended spanner to hold the connec-

tion glands in position.

The TC1 can be cooled by compressed air or inert gas.

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Temperature Control Units

11.7.3 Compressed air distributor for TC1

The design of the compressed air distributor depends on the availability of a compressed air supply inside the building. If such a building connection is not available and if a HAAKE compressor is used instead, no adapter is required.

Using a compressed air supply inside the building

Adapter for building

To TCE/PC

lower meas. plate

To TC1 upper heater

Filter

To RS/RT air

Using a compressor for the compressed air supply

Adapter Filter

To RS/ RT air

instrument air

To TCE/PC lower meas. plate

Standard

To TC 1

upper heater

Compressor for

In both cases, the valves are actuated via the software.

Page 72

Temperature Control Units

11.8 Temperature control unit SHRP

Rheometer like HAAKE RheoStress with parallel plate sensor systems are suitable for the rheological testing of viscous and elastic behavior of bitumen and asphalt blends which are used as surfacing at road building. The rheological tests are usually used for more or less solid bitumen samples in the temperature range from about 5Cto85C .The samples are most of the time tested in the dynamic mode which subjects disk--like specimens placed into the gap between parallel plates -- alternatively a gap between an upper cone and a lower plate is possible, but rarely used for bitumen -- to a sinusoidal stress. The resulting response of the sample --a sinusoidal deformation--is measured in the form of the complex modulus G* related to the resistance of the mass against a sinusoidal deformation and the phase shift angle ”” which appears between the applied stress and the resulting strain. Making use of the angle ””the complex modulus G* can be broken up into the components G’ -- the storage modulus defining the elastic component -- and G’’ -- the loss modulus defining the viscous component in the rheological behavior of a sample subjected to such a dynamic test. The phase angle ”” defines the ratio of the two moduli. From the dynamic measurements with special sensor system for SHRP tests which are described in detail below tests of the viscosity of bitumen melts at temperatures of 120Cto 180C have to be distinguished. For these measurements sensor systems with a measuring gap between coaxial cylinders for the HAAKE rheometers named above are used. At these melt tests the shear stress in proportion to the viscosity of the sample is measured at given shear rate.

Bitumen and asphalt compounds are very sensitive to temperature variations in their r heological behavior., i.e. in t heir viscoelastic response to applied loads and stresses. When subjecting them in a DSR--rheometer to dynamic or to creep and recovery tests this t esting should be carried out in a wide temperature range that relates to summer/winter road pavement conditions. According to the American SHRP specifications measurements at temperatures of 0Cto 85C are desirable. At low temperatures the materials are tested for the likelihood of cracks as the result of a short and hard deformation of the more or less hard and brittle material. Under these conditions the road material may just split/crack unless it is sufficiently elastic to absorb temporarily sudden loads. At low temperatures the bitumen may also creep -- flow very slowly -- even as the result of much lower but longer lasting stresses such as caused by the pressure of car tires when the automobiles have to stop e.g. in front of red traffic lights. It is important to test such samples also at temperatures up

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Temperature Control Units

to 85C as they can occur on the surface of the road pavement in summer. In such cases the tires of trucks often leave lasting deformations.

Under the ”Strategic Highway Research Program” in the USA parallel-plate sensor systems of commercial, internationally available DSR-- rheometers were surveyed for their suitability for the testing of the rheological behavior of bitumen in the given temperature range. It was found that most sensor systems for these rheometers with electrically heated upper and lower plates provided atemperature control accuracy of considerably more than  0,1 C, while for these tests an accuracy better than  0,1 Cwas considered essential. This caused Thermo Fisher Scientific to develope a special thermal liquid heated sensor system”SHRP” with parallel plate measuring geometry for the HAAKE rheometers of series RV and RS. This sensor system meets the requirements set in the ”Standard Method for the Determination of Rheological Properties of Asphalt using a Dynamic Shear Rheometer (DSR) (AASHTO Designation: TP5)”.

The SHRP sensor system consists of an interchangeable upper and a fixed lower measuring plate. A cup--shaped vessel that encloses the two plates is part of the housing that bears the lower plate. During the rheological bitumen measurement the thermal liquid -- normally just water --flows permanently through this cup vessel. By that the two measuring plates and the sample enclosed between the plates can be heated constantly on each set temperature within the temperature range with an accuracy better than  0.1C. For this an external bath and circulator equipped with a built--in cooling unit and a highly accurate electronic temperature control accuracy of better than  0.05C is required. This circulator is connected to the sensor system and pumps the temperature controlled liquid in the cup vessel. During the measurement the liquid level in the cup vessel ascends over the upper measuring plate up to the upper circular ring of bore holes in the cup vessel. Through these bore holes the bath liquid is led to an overflow. Through the overflow the bath liquid is led back again to the bath and circulator via the second connecting hose. This highly precise thermal liquid temperature control by means of circulated water is acceptable for sample materials such as bitumen and their compounds which are not affected or dissolved/leached by water during the duration of such a test.

Page 74

141514

OUT

Temperature Control Units

Installation

The temperature control unit is connected to the bath and circulator placed at disposal (not shown in the picture). The circulator should be equipped with a pressure and suction pump. Connection OUT/IN 14

While fastening the hose connections at the connecting nozzles(14) of the temperature control unit::

-- ensure the correct flow direction (IN/OUT)

-- the connecting nozzles must be held secured

using a wrench.

For the cooling of the temperature control unit hoses (with

 8mm) can be connected to a liquid circulator.

maximum conduction pressure 0.5bar (water circulation).

For the SHRP sensor system and the bath and circulator the required hoses are no standard accessories. They must be ordered separately.

The ball valve (accessories) is placed at the outlet port of the bath and circulator. The valve setting is done by means of a screwdriver to regulate the rate of flow of the bath liquid so that the liquid level in cup vessel 6 can ascend to the upper circular ring but not above. When connecting the circulator first time to the SHRP unit the ball valve must be in the ”closed position” to prevent a sudden overflow in cup vessel

6. The ball valve should be gradually opened to adjust the

proper flow rate. In this phase of the installation valve 8 is maintained in the open-valve position. For placing new sample disks into the gap between the parallel plates and for the removal of these samples at the end of a test, the liquid level in the cup vessel 6 can be lowered by closing the valve 8:the liquid in 6 is sucked back to the circulator via hose 11 and cup vessel 6 is emptied. The inflow and flowing off of the bath liquid is only controlled by valve 8.

Liquids that flow over the cup vessel during the measurement are collected in the underside of the housing and are led back to the bath and circulator via overflow 16 (for hose  8mm).

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Temperature Control Units

 In case of extreme load (high torque, high operating

temperature of about 200--350C) cooling air for the motor is needed.

Devices with air bearing:

 For measurements at temperatures of 200-- 350C

cooling for the measuring head is needed. For this the compressed air connection 9 on the underside of the temperature control unit is used.

Description of HAAKE SHRP sensor system -- Fig. 1:

Fig. 1

3 lower measuring plate with a diameter of

8 mm (optional) or 25 mm

4 inlet tubing for the bath liquid 5 overflow tubing allowing the return of the bath liquid

back to the bath and circulator

6 cup vessel with circular ring of overflow holes through

which the level of the bath liquid in the vessel is controlled

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Temperature Control Units

The temperature of the liquid surrounding the parallel plates and equally the sample being tested is measured by means of a temperature sensor placed into the lower measuring plate from underneath -- not shown in Fig. 1 --. The measured temperature is displayed on the computer screen during the measurement and has an accuracy of  0.1C. According to this actual temperature value of the sensor system the set value must be corrected at the bath and circulator until the actual value of the temperature sensor is conform to the required measuring temperature. The accuracy of the rheological test data depends heavily on the temperature accuracy of the thermal liquid provided by the bath and circulator. In order to maintain a preset temperature level in the tested bitumen specimen of  0.1Casrequired by the SHRP standard, the bath and circulator must guarantee a temperature tolerance of better than or equal to  0.05 C. The actual temperature of the thermal liquid surrounding the parallel plates and thus the specimen should be counter checked by means of a calibrated external thermometer graded with a  0.05 C scaling.

Bitumen being characterized by its low thermal conductivity normally requires some 5 min. to reach any test temperature. Operators may check the actual time requirement for reaching a temperature equilibrium by running dynamic tests in the ”time mode”, i.e. check how long it takes after having raised the liquid level above the parallel plates to reach a time-constant value of i.e. G*.

The specimens placed into the gap between the parallel plates must be preshaped in a separate work step into suitable disks of the right diameter and height prior to their installation in the gap:

a) diameter of 25 mm and 1 mm thick test disks for tests at

higher test temperatures and for the measuring plate with a diameter of 25 mm

b) diameter of 8 mm and 2 mm thick disks for tests at lower test

temperatures -- 5C--usedincombinationwiththe8mmplate. The tests can be run at different constant test temperatures.

a.) with programmed variable shear stresses in ”Controlled

Stress (CS)” mode of the rheometer or

b.) alternatively with programmed variable frequency in

”Controlled Strain (CR)” mode of the rheometer. If tests are to be run according to the SHRP standard the re quired standards have to be kept. Please see the added copy of these standards.

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Temperature Control Units

Tests at constant shear stress or frequency as function of programmed variable measuring temperatures are also usual: see example in Fig. 2.

Fig.2: the rheological behavior of a bitumen in dependence on the the temperature

The upper measuring plates for the SHRP sensor system has shafts with a ceramic segment to minimize heat losses up or downwards. Attention: these ceramic shafts can break! These special measuring plates with ceramic shaft segments are longer than the standard measuring plates of the HAAKE rheometers. This overlength necessitates the use of an elongation (standard accessories) of the micrometer shaft -- at least while using former rheometer models. For this the end piece of the shaft is screwed off, the elongation piece is screwed in and after that the end piece is put on again.

The SHRP sensor system must be adjusted to a gap width of h=0 before starting a test series. This should be done at measuring temperature which means it should be done while the the bath liquid already floats the two measuring plates adjusted to set temperature.

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Temperature Control Units

The cup vessel 6 can be moved up an down by turning it at the brim. By that it is moved in a thread opposite to the housing. The bottom of cup vessel 6 that is cut out in a circular shape slides close to the outer rim of the lower measuring plate when the cup vessel is moved. In the upper position the the hole in the bottom of the cup vessel makes up a good centering for the disk--like bitumen sample. So the sample can be positioned precisely on the lower measuring plate. Before starting the actual test, the cup vessel must be moved down until its bottom is clearly under the surface of the lower measuring plate and the sample disk cannot be touched by the bottom of the cup vessel. After ending the test or at the end of a working day cup vessel 6 can be removed by screwing it off to be cleaned inside and outside from dirt particles that can possibly be floated from the circulator to the sensor system.

For the SHRP sensor system and the bath and circulator the required hoses are no standard accessories. They must be ordered separately.

Page 79

Temperature Control Units

measuring plate

Page 80

Immersion Disc ISO 2555

Immersion Cylinder ISO 2555

Coaxial Cylinder DIN 53018

Coaxial Cylinder DIN 54453

Coaxial Cylinder DIN 53019

Cone-Plate Combinations

Plate-Plate Combinations

Sensor Systems

12. Sensor Systems

Make sure that the unit has been switched off before you connect or disconnect the cables. This is to avoid electrostatic charging resulting in a defect of the electronic circuit boards.

When unscrewing the rotor from the measuring shaft it should be ensured that the rotor is removed from the cone with small rotational motions.

Not use and store the plate and cone measuring geometry with ceramic shaft in steel execution in the proximity of a magnetic field, since these can be magnetized. The results of measurement are incorrect in this case.

The measurement sensors are the core of a Rheometer and determine the quality of the measuring results.

The appropriate literature mentions a variety of sensor systems which can be classified as follows:

a. Cylinder Sensor Systems

-- Immersion Disc ISO 2555

-- Immersion Cylinder ISO 2555

-- Coaxial Cylinders according to DIN 53018

-- Coaxial Cylinders according to DIN 54453

-- Coaxial Cylinders according to DIN 53019/ISO 3219

b. Cone-Plate / Plate-Plate Sensor Systems

-- Cone-Plate with various opening angles and radii

-- Plate-Plate with various radii and gap widths

Out of these numerous possibilities, Thermo Fisher Scientific supplies the following systems:

-- Cylinder systems according to ISO 2555 (optional)

-- Cylinder systems according to DIN 53019/ISO 3219

-- Cylinder systems according DIN 54453

-- Cylinder systems according DIN 53018

-- Cone-Plate combinations

-- Plate-Plate combinations

-- Vane (star-shaped) rotors for special measurements

-- Optically transparent sensors (cylinder, cone-plate and plate-plate)

These sensors cover the majority of desired applications whereby special sensor systems are developed and made available in close cooperation with customers requiring such special sensor systems.

Page 81

Sensor Systems

Calculation Factors

In the case of a rotational rheometer the viscosity of a liquid is calculated in accordance with the Newtonian conditional equation for viscosity:

Viscosity η =

Shear Stress τ

Shear Rate γ

at defined ambient conditions regarding measuring time, temperature and pressure.

In rheometers, operating in accordance with the CR-princi- ple a speed (angular velocity) is preset which in the sensor system filled with a sample causes a shear rate. The torque required for achieving and maintaining the desired shear rate is the viscosity-proportional parameter.

CS-rheometers are designed to operate according to the reversed principle. Here a torque (shear stress) is preset and the resulting movement (deformation) i.e. the resulting angular velocity (shear rate) is measured. The measurement with rotational rheometers can be summed up to the predetermination of a force and from the measurement of the resulting movement a suitable geometry can be derived. This will also define the conditional equations:

The shear stress  is proportional to the torque ’Md’ and to a characteristic geometry factor, which at Thermo Fisher Scientific is identified as ’A’ (shear stress factor).

τ = Md ⋅ A

A high torque means also a high shear stress. Large values of ’A’ stand for small sensors.

The shear rate

is proportional to the rotational movement (angular velocity) and proportional to the geometry factor ’M’:

γ.= Ω ⋅ M

A high angular velocity  means also a high shear stress

High ’M’ values stand for very small gaps. The angular velocity  results from the following equation

where the rotor speed is n in [1/min] and  is measured in units of [1/s].

 =2n/60

Page 82

Sensor Systems

Measuring Ranges

The different specifications of the models HAAKE RotoVisco 1 and HAAKE RheoStress 1 effect the measuring ranges.

For the values of measuring ranges please see chapter “Technical Specifications”.

The measuring range can be illustrated in a diagram where  =f(

) and  =f(

 - Range

The shear stress measuring range results from the measurement geometry and the presetting range of t he torque Md. Now it is quite simple to estimate the smallest and largest shear stress value for a sensor system by using the following calculations:



min

=Md

(min)

 A



max

=Md

(max)

 A

The limit values of the diagrams differ according to the model specific torque values from the above table.

- Range

Similar to the shear stress range there is also a meaningful measuring range for the shear rate

. The following correla-

tions can be derived:

min

= 

(min)

 M

max

= 

(max)

 M

The limit values of the diagrams differ according to the model specific torque values from the above table.

Page 83

Sensor Systems

 - Range

The viscosity measuring range is derived from the  -and

range in accordance with the Newtonian conditional equation.

η = τ∕γ

The four fundamental values in the diagram can be calculated as follows:

smallest viscosity at max. shear rate

(min) =  (min) /

(max)

smallest viscosity at min. shear rate (min) =  (min) /

(min)

largest viscosity at min. shear rate

(max) =  (max) /

(min)

largest viscosity at max. shear rate

(max) =  (max) /

(max)

With these four fundamentals, the viscosity range is defined. It is easily comprehensible that the measurement fault in the extreme r anges is very large. It gets smaller as the torque increases and the angular velocity decreases.

max

min



min

max



min

max



Page 84

Sensor Systems

12.1 Cylinder Sensor Systems

From the theoretical possibilities of a measurement geometry for cylinder sensor systems Thermo Fisher Scientific selected the following concepts:

12.2 Cylinder Sensor Systems Z-DIN

Application

These sensor systems were introduced for polymer dispersions. Meanwhile they became a standard in Europe as they

 render comparable measurement results with different

rheometers too;

 are easy to clean;

 are quite suitable for temperature programs.

Sensor Systems Z DIN

The sensor system Z DIN comprises one rotor and one beaker each in accordance with the standard DIN 53019/ISO

3219. They are characterized by their rotor diameter.

Z34 DIN

Z20 DIN

222-1499

222-1458

Z10 DIN

222-0621

222-1498

222-1487

222-1497

Sealing set for Z43DIN Order no. 222--1290 Sealing set for Z20DIN Order no. 222--1291 Sealing set for Z10DIN Order no. 222--1292

Page 85



L’

= 1, 0847

= 0, 3

= 3

L′ R

= 1

 = 120 (2,094 rad)

Sensor Systems

Geometry:

Sensor systems according to the standards mentioned have the following peculiarity in that all measurements are relative to the radius of the rotor. In DIN 53019 the following values are defined which are confined and partly extended in ISO 3219.

The expressions have the following meaning:

 =Ra/Ri(radius ratio) L = Length of Cylinder R

= Radius interior cylinder (Outside  of the rotor/2) Ra= Radius outside cylinder (Interior  of the beaker/2) Rs= Radius of the rotor shaft a = Distance  = Angle of the cone L’ = Distance of the rotor

Page 86

Sensor Systems

Calculation Equations to DIN 53019/ISO 3219

Shear Stress : The shear stress  is proportional to the torque ’Md’ and the

stress factor ’A’.

 =A Md

Thefactor’A’canbecalculatedasfollows:

A =

2 ⋅ π ⋅ L ⋅ R

2 i

⋅ C

⋅

1 + δ

2δ

with Ri= Radius of ’Rotor’

L = Length of Rotor CL= Resistance Coefficient

(CL= 1.1 according DIN 53019)

It has the unit of an inverse volume.

 = Radius ratio Ra/R

(A) = L

-- 3

Shear Rate

The shear rate

is proportionally linked to the angular veloc-

ity and thus also to the speed and shear factor M.

γ.=M ⋅ Ω

The angular velocity  is calculated according to

2π 60

⋅ n

The factor M is calculated: M=

1 + δ

δ2− 1

2= Radii Relationship Ra/R

2= 1.0847 (DIN 53019)

Deformation : The deformation  is linearly linked to the angular deflection

and the geometry of a sensor system.

 =M with  = Torsion angle [rad]

 is a dimensionless number

Filling Volume: The standard lists the equation for the calculation of the filling

volume as follows: V = 8.17

 R

(cm3)

Page 87

Sensor Systems

Cylinder Sensor System according to DIN 53019/ISO 3219

Sensor Z10DIN Z20DIN Z34DIN

Rotor order No. 222--0621 222--1458 222--1499 Mass m (g) 37.4 62.0 87.3 Material: Titan DIN No. 3.7035 InertiaI(kgm2)E--6 0.4 1.60 15.39 Radius Ri(mm) 5.000 10.000 17.000  delta Ri(mm) 0.0015 0.002 0.004 Length l (mm) 15 30 51  delta l (mm) 0.015 0.03 0.06 Clearance to bottom (mm) 2.1 4.2 7.2 Cup 222--1497 222--1487 222--1498 Radius Ra(mm) 5.425 10.850 18.44  delta Ra(mm) 0.002 0.00295 0.004 Material: Steel DIN No. 1.4305 Gasket (200 C) Order No. 222--1292 222--1291 222--1290 Ratio of Radii Ra/R

1.0847 Gap (mm) 0.425 0.85 1.44 Sample volume (cm3) 1.0 8.2 40.1 perm.temperature max. ( C) 200 Calculation factors A(Pa/Nm) 356800 44600 9080  delta A (%) 0.2 M(s

-- 1

/rad s

-- 1

) 12.29

 delta M (%) 0.8 0.5 0.5

Page 88

Sensor Systems

HAAKE Rheometer Measuring Range of Sensor

1,0E-02

1,0E-01

1,0E+00

1,0E+01

1,0E+02

1,0E+03

1,0E+04

1,0E+05

1,E-05 1,E-04 1,E-03 1,E-02 1,E-01 1,E+00 1,E+01 1,E+02 1,E+03 1,E+04

Shear rate (1/s)

Shear stress (Pa)

1,E-04

1,E-02

1,E+00

1,E+02

1,E+04

1,E+06

1,E+08

1,E+10

1,E+12

1,E+14

Viscosity (mPas)

RS1-Z10DIN

RS1-Z20DIN

1,0E-02

1,0E-01

1,0E+00

1,0E+01

1,0E+02

1,0E+03

1,0E+04

1,E-06 1,E-05 1,E-04 1,E-03 1,E-02 1,E-01 1,E+00 1,E+01 1,E+02 1,E+03 1,E+04

Shear rate (1/s)

Shear stress (Pa)

1,E-04

1,E-02

1,E+00

1,E+02

1,E+04

1,E+06

1,E+08

1,E+10

1,E+12

1,E+14

Viscosity (mPas)

HAAKE Rheometer Measuring Range of Sensor

RS1-Z40DIN

Page 89

Sensor Systems

1,0E+00

1,0E+01

1,0E+02

1,0E+03

1,0E+04

1,0E+05

1,E-01 1,E+00 1,E+01 1,E+02 1,E+03 1,E+04

Shear rate (1/s)

Shear stress (Pa)

1,E-04

1,E-02

1,E+00

1,E+02

1,E+04

1,E+06

1,E+08

1,E+10

1,E+12

1,E+14

Viscosity (mPas)

HAAKE Rheometer Measuring Range of Sensor

RV1-Z10DIN

RV1-Z20DIN

1,0E-02

1,0E-01

1,0E+00

1,0E+01

1,0E+02

1,0E+03

1,0E+04

1,E-06 1,E-05 1,E-04 1,E-03 1,E-02 1,E-01 1,E+00 1,E+01 1,E+02 1,E+03 1,E+04

Shear rate (1/s)

Shear stress (Pa)

1,E-04

1,E-02

1,E+00

1,E+02

1,E+04

1,E+06

1,E+08

1,E+10

1,E+12

1,E+14

Viscosity (mPas)

HAAKE Rheometer Measuring Range of Sensor

RV1-Z40DIN

Page 90

Sensor Systems

12.3 Cylinder Sensor System Z

Application

This sensor system is preferred for medium viscous liquids when a comparability of the measurements in accordance with DIN 53018 is requested. These sensors have an extremely small front surface influence and are therefore intended for exact measurements. Temperature programs are not recommended as the volume of the trapped air bubble will change its volume with the temperature. This also has an effect on the front surface influence.

Sensor System Z

The sensor system Z comprises a collapsible beaker Z43 and 3 rotors with different radii.

222-1461 222-1460 222-1459222-1488

Z43 Z31 Z38 Z41

Sealing set for Z40 Order no. 222--1290

Page 91

Sensor Systems

Geometry

The geometry of this sensor system corresponds to DIN

53018.

Calculation Equations:

Shear Stress : The shear stress  is proportional to the torque ’Md’ and to

a geometric factor i.e. stress factor ’A’.

 =A Md

(Stress Factor*Torque)

The factor ’A’ can be calculated as described by the following equation:

A =

2 ⋅ π ⋅ Ri2⋅ L

[A] =

It has the unit of an inverse volume.

Shear Rate

The shear rate

is proportionally linked to the angular veloc-

ity or speed and the shear factor ’M’.

γ.=M ⋅ Ω

The angular velocity  is calculated according to

2π 60

⋅ n

from the speed n. The factor M is calculated: The factor ’M’ is calculated as follows:

M =

2 ⋅ R

2 a

-R

2 i

Deformation : The deformation  is linearly linked to the angular deflection

and the geometry of a sensor system.

 =M with  = Torsion angle rad

 is a dimensionless number

Page 92

Sensor Systems

Cylinder Sensor System Z

Sensor Z31 Z38 Z41

Rotor order No. 222--1461 222--1460 222--1459 InertiaI(kgm2)E--6 11 21.00 28.0 Material: Titan DIN No. 3.7035 Radius Ri(mm) 15.720 19.010 20.710  delta Ri(mm) 0.0020 0.004 0.004 Length l (mm) 55  delta l (mm) 0.03 Clearance to bottom (mm) 8.1 8.1 3 Cup 222--1488 222--1488 222--1488 Radius Ra(mm) 21.700 21.700 21.700  delta Ra(mm) 0.004 0.004 0.004 Material: Steel DIN No. 1.4305 Gasket (200 C) Order No. 222--1290 222--1290 222--1290 Rato of Radii Ra/R

1.3804 1.1415 1.0478 Gap (mm) 5.98 2.69 0.99 Sample volume (cm3) 52.0 33.0 14.0 perm.temperature max. ( C) 200 Calculation factors A(Pa/Nm) 11710 8010 6750  delta A (%) 0.5 M(s

-- 1

/rad s

-- 1

) 4.21 8.60 22.40

 delta M (%) 0.5

Page 93

Sensor Systems

1,0E-02

1,0E-01

1,0E+00

1,0E+01

1,0E+02

1,0E+03

1,0E+04

1,E-06 1,E-05 1,E-04 1,E-03 1,E-02 1,E-01 1,E+00 1,E+01 1,E+02 1,E+03 1,E+04

Shear rate (1/s)

Shear stress (Pa)

1,E-04

1,E-02

1,E+00

1,E+02

1,E+04

1,E+06

1,E+08

1,E+10

1,E+12

1,E+14

Viscosity (mPas)

HAAKE Rheometer Measuring Range of Sensor

RS1-Z31

RS1-Z38

1,0E-02

1,0E-01

1,0E+00

1,0E+01

1,0E+02

1,0E+03

1,E-05 1,E-04 1,E-03 1,E-02 1,E-01 1,E+00 1,E+01 1,E+02 1,E+03 1,E+04

Shear rate (1/s)

Shear stress (Pa)

1,E-04

1,E-02

1,E+00

1,E+02

1,E+04

1,E+06

1,E+08

1,E+10

1,E+12

1,E+14

Viscosity (mPas)

HAAKE Rheometer Measuring Range of Sensor

RS1-Z41

Page 94

Sensor Systems

1,0E-01

1,0E+00

1,0E+01

1,0E+02

1,0E+03

1,E-02 1,E-01 1,E+00 1,E+01 1,E+02 1,E+03

Shear rate (1/s)

Shear stress (Pa)

1,E-04

1,E-02

1,E+00

1,E+02

1,E+04

1,E+06

1,E+08

1,E+10

1,E+12

1,E+14

Viscosity (mPas)

HAAKE Rheometer Measuring Range of Sensor

RV1-Z31

RV1-Z38

1,0E-01

1,0E+00

1,0E+01

1,0E+02

1,0E+03

1,E-01 1,E+00 1,E+01 1,E+02 1,E+03 1,E+04

Shear rate (1/s)

Shear stress (Pa)

1,E-04

1,E-02

1,E+00

1,E+02

1,E+04

1,E+06

1,E+08

1,E+10

1,E+12

1,E+14

Viscosity (mPas)

HAAKE Rheometer Measuring Range of Sensor

RV1-Z41

Page 95

Sensor Systems

12.4 Double Gap Cylinder Sensor DG43 according to DIN 53544

Application

This sensor system is preferred for low viscous liquids (<1000 mPa  s) or for small sample volumes. The double shearing surfaces of this particular system result in a higher shear stress than what is customary for comparable DIN sensors. It is standardized as DIN 53544 for measurements with low viscous glues.

Sensor System DG43

The sensor system DG43 is made up of a dismountable beaker and either the bell-shaped rotor.

The temperature vessel should not be employed for temperatures above 200C. There must be a sufficiently long heating period so that the inner part of the beaker, which is not temperature controlled, can adopt the desired temperature. Heating times of 5 to 20 minutes, depending on the viscosity and liquid, are quite common.

002-6748

Rotor DG43 222-1559

003-4727

Beaker DG43 222-1489

Sealling set for DG41/43 222--1293

Page 96

R1 R R R

2 3 4

Sensor Systems

Geometry

The geometry of the sensor system is designed so that radii relationship of the shear surfaces is almost equal so that identical shearing conditions in both gaps can be expected.

R1= Radius Beaker (Inside) R

= Radius Beaker (Outside) R3= Radius Rotor (Outside) R2= Radius Rotor (Inside) L = Length of Shear Surface a = Distance

Calculation Equations:

Shear Stress : The shear stress  is proportional to the torque ’Md’ and to

a stress factor i.e. stress factor ’A’.

 =A Md

The factor ’A’ can be calculated as described by the following equation:

A =

2 ⋅ π ⋅ L ⋅ (R

2 2

+ R

2 3

)

[A] =

Shear Rate

The shear rate

is proportionally linked to the angular veloc-

ity and thus speed and the shear factor ’M’.

γ.=M ⋅ Ω

The angular velocity  is calculated according to

2π 60

⋅ n

from the speed n. The factor M is calculated: The factor ’M’ is calculated as follows:

M =

2 ⋅ R

2 a

-R

2 i

Ra= R4, R2

Ri = R3, R1

Deformation : The deformation  is linearly linked to the angular deflection

and the geometry of a sensor system.

 =M with  = Torsion angle rad

 is a dimensionless number

Page 97

Sensor Systems

Double Gap Cylinder Sensor System DG43 according to DIN 53544

Sensor DG43

Rotor order No. 222--1559 Radius R1(mm) 17.75  delta R1(mm) 0.004 Radius R2(mm) 18.35  delta R2(mm) 0.004 Radius R3(mm) 20.99  delta R3(mm) 0.004 Length l (mm) 55  delta l (mm) 0.06 Clearance to bottom (mm) 5.1 InertiaI(kgm2)E--6 35.1 Mass m (g) 117.0 Cup 222--1489 Radius Ra (mm) 21.7  delta Ra (mm) 0.00434 Material: Steel DIN No. 1.4305 Gasket (200 C) Order No. 222--1293 Ratio of Radii Ra/Ri 1.0338 Gap R4-- R3(mm) 0.71 Gap R2-- R1(mm) 0.6 Sample volume (cm3) 11.5 perm.temperature max. (C) 200 Calculation factors A(Pa/Nm) 3701  delta A (%) 0.1 M(s

-- 1

/rad s

-- 1

) 31.08

 delta M (%) 6

Page 98

Sensor Systems

1,0E-03

1,0E-02

1,0E-01

1,0E+00

1,0E+01

1,0E+02

1,0E+03

1,E-05 1,E-04 1,E-03 1,E-02 1,E-01 1,E+00 1,E+01 1,E+02 1,E+03 1,E+04 1,E+05

Shear rate (1/s)

Shear stress (Pa)

1,E-04

1,E-02

1,E+00

1,E+02

1,E+04

1,E+06

1,E+08

1,E+10

1,E+12

1,E+14

Viscosity (mPas)

HAAKE Rheometer Measuring Range of Sensor

RS1-DG43

1,0E-01

1,0E+00

1,0E+01

1,0E+02

1,0E+03

1,E+00 1,E+01 1,E+02 1,E+03 1,E+04 1,E+05

Shear rate (1/s)

Shear stress (Pa)

1,E-04

1,E-02

1,E+00

1,E+02

1,E+04

1,E+06

1,E+08

1,E+10

1,E+12

1,E+14

Viscosity (mPas)

HAAKE Rheometer Measuring Range of Sensor

RV1-DG43

Page 99

Sensor Systems

12.5 Solvent trap for Z10, Z20, Z31, Z34, Z38, Z41 und DG43 (222--1509)

Page 100

Sensor Systems

12.6 Solvent trap for Z43 (222--1593)

Thermo Scientific HAAKE RotoVisco 1, HAAKE RheoStress 1 Instruction Manual

Specifications and Main Features

Frequently Asked Questions

User Manual