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Advanced Seminar Rheology of Construction Materials

Rheological measuring systems

Content

Overview Finger, Ford cup Capillary viscometer Falling ball viscometer Rotational viscometer Rotational rheometer Selected accessories
Temperature control units Measuring geometries Modules

Extensional rheometer

How can you measure viscosity ?

Feed back to other physical quantities, viscosity value relative or absolute. Rheometer: additional measurements of other (elastic) material characteristics

Principle Biosensor

Device Finger Changel Ford cup (High pressure ) Capillary viscometer (Mikro) Faling ball viscometer Laray-viscometer Torsion viscometer Compression viscometer Krebs-Stormer-viscometer Rotational viscometer / - rheometer

Measured quantity Resistance (Force, Pressure) Time Time (Pressure, Displacement) Time Damping Force, Displacement Force, Displacement

Volum flow

Falling weight Torsion Compression Rotation sensor

Testing of Viscosity: Finger

... the cheapest viscometer
Advantages: + cheap + easy handling + fast + easy cleaning Disadvantages: - relative - no reproducability - risky hazardous materials

Ford-Cup
Advantages: + cheap + easy handling /robust + fast + easy cleaning Method: Measurement of time t (for a defined volume), seconds as an index for the viscosity

Disadvantages: - relative, type of cup and dye have to be stated e.g. DIN-cup Type A Dye Nr. 4 - no temperature control - wrong times for non-Newtonian fluids - not suitable for fluids with yield point

Capillary viscometer (Gravity is the driving force)

Advantage: + Relatively cheap + Very precise for low and medium viscosities + Can be calibrated + Absolute for Newtonian fluids Disadvantage: - Long measuring time - High cleaning effort - Labor intensive (manual version) - relative values - for Non-Newtonian fluids - Doesn't work for samples with a yield stress - Limited operating temperature range Method: The time is measured how long it takes for the fluid to pass two marks

Capillary viscometer (Gravity is the driving force)

Result:

= C4 * t
C4 viscosity (kinematic) Capillary constant,

Application: Low viscous fluids e.g. oils

[ mm2 / s ] =*

depends on the used capillary and has to be determined by calibration

Boundary condition:

L/D > 30

(L: length, D: diameter)

High pressure capillary viscometer

Advantage: + High shear rates + Less friction heating because alway new sample is feeded + Calibration possible + Absolute Disadvantage: - High price - For test with rod capillary three test are necessary for the Bagleycorrection - Not for low viscous materials - Cleaning Application: Polymers
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Method: The sample is pressed with a piston through the capillary. Measurement of the pressure drop p and the volume flow Q

Calculations:

p = p1 - p2 = R/(2L) * p = 4/( R3) * Q = R4/8L * p/ Q

HAAKE Falling Ball Viscometer Typ C

Hppler (DIN 53015 / ISO 12058)
Advantages: + High accuracy + Temperature easy to control + Absolute results for Newtonian liquids + Calibration + Wide viscosity range + Closed system Disadvantages: - Long measuring time - Time consuming cleaning effort - Labour-intensive - Relative results for Non-Newtonian liquids - Limited to transparent samples without yield point - Sample density required
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Method: Measuring the falling time of a ball by measuring marks in a tube with 10 inclination

HAAKE Falling Ball Viscometer Typ C

Hppler (DIN 53015 / ISO 12058)

Result:
= K*(k - Fl )* t
- Viscosity (kinematic)

Applications: - Low viscous fluids e.g. oils - Evaporating fluids / solvents e.g. toluene - Gases

K - Calibration factor for the ball,

Depends on the diameter of the ball and tube, has to be calibrated

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Rotational Viscometer / Rheometer

(relative or absolute)
Advantages: + Wide range of viscosity, temperature and shear rate + Applicable for Non-Newtonian liquids and samples with yield point + Calibration (absolute measuring systems) Method: Torque measurement at a given rotational speed (CR-Method) Deformation measurement (torque) at a given torque (CS-Method) Differentiation: Searle-, Couette-type
CR-Method
Motor Torque-, Deformationsensor Bearing of measuring shaft Joint

CS-Method

Disadvantages:

- Partially cleaning intensive (cup and rotor) Slightly limited accuracy

Measuring and temperature cell

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Rotational Viscometer (relative)

Advantages: + Easy handling + Quick measurement + Minimal cleaning effort + Reasonable in price Method: Rotational viscometer with sensor geometry (flow field can not be calculated) In most cases measuring cell without temperature control

Disadvantages: - Relative results for NonNewtonian liquids - Comparable results only using same sensor and same measuring conditions (r.p.m., sensor) - Faulty viscosity readings due to variation in temperature

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Rotational Rheometer (absolute)

Advantages: + Absolute readings, calibration + Modularity thanks different temperature control units, measuring geometries and accessories + Minimal cleaning (P/C and P/P) + Small sample volume (P/C and P/P) + Computer controlled measurement, i. e. userindependent, data documentation Disadvantages: - Price - High cleaning effort (cylinder measuring geometry) Method: Rotational rheometer with coaxial cylinders, Cone-Plate and Plate-Plate geometries with a calculable flow field

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Overview about Temperature Control Units*

* HAAKE RheoStress 600 and HAAKE MARS available.

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Overview about Measuring Geometries

Coaxial cylinder geometries:

- acc. to DIN 53018 - acc. to ISO 3219 - Mooney/Ewart-system - Double gap acc. to DIN 54453

Plate/Plate- and Cone/Plate Relative measuring geometries

- Brookfield spindles acc. to ISO 2555 - Pin- and vane rotor - Krebs rotor - geometries with serrated surface -

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How to choose the measuring geometry

Subjective impression of the sample

Low to medium viscosity easy to clean

High viscous, pastes, hard to clean

Large particles sedimentation, separation Special sensors vane or helical grooved sensor

Coaxial cylinders in various dimensions

Cone/plate (without particles) Plate/plate (with particles)

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Coaxial Cylinders
Couette Method Rotor fix, measuring cup rotates (1888, Couette) + No Taylor vortex + Drive unit and torque sensor mechanical separated + Structural disadvantages (temperature controller rotates) Searle Methode Rotor rotates, measuring cup fix (1912, Searle). Common method for commercially available rheometers . + Structural advantages - Taylor vortexes at high rotation speed and low viscosity

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Coaxial Cylinders

Shear stress (r) = Md / ( 2 * L * r2 ) Shear rate . = 2 * Ri2 * Ra2 / (Ri2 - Ra2) / r2 * (r) Related to rotor surface A i = 1 / ( 2 * L * Ri2 cL) * Md = A * Md Mk i = 2 * Ra2 / (Ri2 - Ra2) * 2 / 60
Md Torque [Nm] Angular Velocity [1/s] = ( 2 * n ) /60 v(r) = * r n Rotation speed [1/min] Ratio of radiie =Ra / Ri cL Coefficient of resistance

n = Mk * n

Information and calculations for measuring geometries acc. to Searle method.

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Coaxial Cylinders acc. to DIN 53018

Application:
Samples with medium viscosities + High accuracy - Cleaning efforts - Not suitable for temperature ramps (expansion of air bubble) - Sample volume - High inertia

L > 1,5 * Ri = Ra / Ri < 1,10

LS
LS= 3 * (Ra - Ri ) cL = 1

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Coaxiale Cylinders acc. to ISO 3219

Application:
Samples with medium up to higher viscosities Standard geometry + Easy Filling + Suitabe for temperature rampes - Cleaning efforts - Sample volume - Higher inertia

i = 1 / ( 2 * L * Ri2 * cL ) * Md L > 3 * Ri = Ra / Ri < 1,0847 L = Ri L = Ri = 120 + 1 cL = 1,1

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Coaxiale Cylinders acc. to DIN 54453

Application: Samples with low viscosities Measurements at higher shear rates + Samples volume + Temperature control - Cleaning effort - Higher inertia

L > 3 * R3 = R2 / R1 = R4 / R3 < 1,15 i = 1 / ( 2 * L * (R22 + R32)) * Md i = 2 * 2 / (2 - 1) * 2 / 60 * n

As special with helical growings against sedimentation

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Cone/Plate measuring geometry acc. to ISO 3219

Application:
Samples with medium up to high viscosities + Shear rate within measuring gap is constant + Easy cleaning + Small sample volume + Fast and accurate temperature control + Low inertia - Correct gap setting necessary
R

"Truncation"

= 3 / ( 2 *

R3

) * Md = A * Md

= 1 / tan * 2 /( * 60) * n = Mk*n < 4 Recommendation: = 1

Truncation >3 x bigger particle size

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Plate/Plate measuring geometry acc. to DIN 53018

Application:
Samples with medium up to high viscosities With particles + Easy cleaning + Variation of shear rate range due to variable setting + Small sample volume + Low inertia + As disposable geometries available + Temperature ramps H - Shear rate within gap not constant

(R) = 2 / ( * R3 ) * Md = A*Md

Mk

(R) = v / H = * R / H = 2 * R /(H * 60) * n H << R

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Recommended measuring range

1,0E+10

1,E+10

1,0E+08

1,E+08

Cone 20 mm/1
1,0E+06 Shear stress (Pa) 1,E+06 Viscosity (mPas)

= 10 Pas
1,0E+04 1,E+04 1,0E+02 1,E+02

1,0E+00

1,E+00

Cone 60 mm/1
1,0E-02 1,E-02 1,0E-04 1,E-03 1,E-04 1,E+05

1,E-02

1,E-01

1,E+00

1,E+01 Shear rate (1/s)

1,E+02

1,E+03

1,E+04

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Double cone geometry

Double cone geometry as a quasi closed measuring cell.

Application:
Samples with low up to medium viscosities + Evaporation blocked + High accuracy + Low sample volume + Easy Cleaning - Sample temperature - Gap setting - Inertia higher than standard cone /plate geometry

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Disposable measuring geometries

Application:
For measurements on samples with curring behaviour with high cleaning efforts

+ + -

No cleaning necessary Higher measurement rate Set-up measuring device Lower Parallelism than standard geometry

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Measuring geometries with serrated surface

Application:
For samples with Slippage effect Hard surface

+ -

Improvement of contact between sample and measuring geometry Quasi absolut geometry (reduced accuracy) Higher cleaning effort

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Relative measuring geometries

Application:
Samples, which can not be measured with a standard geometry due to: big particles sedimentation

+ Easy handling + Flexibiliy of design - Relative - Temperature control

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Measuring Cell for Construction Materials

Application: Rheological properties of fresh building materials + Easy and quick adaptation of the measurement geometry to new materials + Easily adaptable serration profile + Vane sensors with various diameters + Prevention of slippage layer formation + Measurement in both rotational and oscillatory mode + Large specimens possible + Robust detailing of equipment + Optional temperature control Shear rate within gap not constant Temperatur control
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Measuring Cell for Bitumen

Application: Determination of properties acc. to SHRP Aging behaviour Deformation behaviour (Measurement of application behaviour at 135C in rotational mode) + Easy sample trimming in plate / plate measuring geometrie (8, 25mm) + Water temperature controlled + Measurement in both rotational and oscillatory mode - Temperature range 5 up to 95C

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RheoScope Module

Combination of two analytical test methods: Correlation between rheological properties und structur

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HAAKE MARS + RheoScope Module

Rheological Data

Images

Example: Polyethylene

Click: Video

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HAAKE CaBER 1 (Capillary Breakup Extensional Rheometer)

Sample

Lasermicrometer

[Click Image to repeat animation.

Extensional flows occur in many industrial processes and applications and influence these processes often to a great extent. As a consequence the knowledge of extensional properties is important. Extensional properties can not be measured with rotational rheometers.

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Questions?

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