Instruction Manual Viscotester VT01 / 02 808-0701 2-1-060-1/3 10.1993 Thermo Haake (International) Thermo Haake (USA) Thermo Rheo (France) Dieselstraße 4 D-76227 Karlsruhe 5225 Verona Road Madison, WI 53711 99 Route de Versailles 91160 Champlan Tel. +49(0)721 4094-444 Fax +49(0)721 4094-418 info@thermohaake.com www.thermohaake.com Tel. 608 327 6777 Fax 608 273 6827 infousa@thermohaake.com www.thermohaake.com Tel. +33(0)1 64 54 0101 Fax +33(0)1 64 54 0187 info@thermorheo.com www.thermohaake.com Table of Contents General Notes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 1. Description . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 1.1 Measuring Principle . . . . . . . . . . . . . . . . . . . . . . 1.2 Drive . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.3 Measuring Ranges . . . . . . . . . . . . . . . . . . . . . . 3 3 3 2. Functional and Operating Elements . . . . 4 3. Measurement . . . . . . . . . . . . . . . . . . . . . . . . . 6 3.1 3.2 3.3 3.4 3.5 3.6 3.7 3.8 3.9 Measuring Method I . . . . . . . . . . . . . . . . . . . . . 7 Measuring Method II (only VT 01) . . . . . . . . . 7 Measuring Method III (only VT 01) . . . . . . . . . 7 Measuring Method IV (only VT 02) . . . . . . . . . 7 Influence of the Temperature . . . . . . . . . . . . . . 8 Non-Newtonian Behavior . . . . . . . . . . . . . . . . . 9 Reproducibility . . . . . . . . . . . . . . . . . . . . . . . . . . 9 Accuracy of Measurements . . . . . . . . . . . . . . . 9 Information concerning the CE sign . . . . . . 10 4. Technical Specifications . . . . . . . . . . . . 11 5. Optional Accessories . . . . . . . . . . . . . . . 13 6. Terms of Rheological Measurements . 14 1 General Notes ! This device may only be operated according to the following instructions! This instruction manual describes exactly how this device is to be used. The following points should especially be kept in mind: ! The device should only be used by trained personnel in conjunction with the instruction manual. ! Only personnel with the particular know how should be allowed to carry out repairs. ! Only original parts and accessories should be used, when repairs are carried out. ! 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. The symbols used in this manual and their meaning: ! Warns that damages to the device and injuries to the user are possible. Denotes an important remark. 1 ⇒ Indicates the next operating step to be carried out and . . . . . . what happens as a result thereof. Your Contacts at Thermo Haake Please get in contact with us or the authorized agent who supplied you with the unit if you have any further questions. Thermo Haake (International) Dieselstraße 4 D-76227 Karlsruhe, Germany Tel. +49(0)721 4094–0 Fax +49(0)721 4094–300 Hotline +49(0)18 05 04 22 53 E-mail info@thermohaake.com www.thermohaake.com ThermoHaake Dieselstr. 4 D–76227 KARLSRUHE Thermo Haake (USA) 5225 Verona Road Madison, WI 53711 Tel. 608–327–6777 Fax 608–273–6827 Thermo Rheo (France) 99 route de Versailles 91160 Champlan Tel. 01 64 54 01 01 Fax 01 64 54 01 87 infousa@thermohaake.com www.thermohaake.com info@thermorheo.com www.thermorheo.com The following specifications should be given when product enquiries are made: TYP V/Hz Unit name printed on the front of the unit and specified on the name plate. 2 Description 1. Description The Viscotesters VT 01 and VT 02 are simple rotational viscometers, specially suited for fast comparison tests on liquids. 1.1 Measuring Principle A rotor, driven by a speed-controlled, battery-operated motor, is immersed into the liquid to be tested. The viscosity of the liquid is measured as a resulting torque and is indicated directly on the scale. 1.2 Drive Speed controlled motor, battery: 6 V. Speed of rotor: 62.5 min–1. 1.3 Measuring Ranges Both Viscotesters have three measuring ranges each. There is a special rotor for each measuring range. The scale indicates which rotor should be used. The scale values given are calibrated with Newtonian liquids (mineral oils). VT01: Scale 4 5 3 VT02: 3 1 2 Measuring Range 1.5 ... 33 mPas (cP) 15 ... 150 mPas (cP) 50 ... 330 mPas (cP) Rotor 4 5 3 0.3 ... 13 dPas (P) 3 ... 150 dPas (P) 100 ... 4000 dPas (P) 3 1 2 Please note: 1 mPas (milli Pascalsecond) = 1 cP (centi Poise) 1 dPas (deci Pascalsecond) = 1 P (Poise) 1 dPas (deci Pascalsecond) = 100 mPas 3 Functional and Operating Elements 2. Functional and Operating Elements 1) Battery container Four 1.5 Volt leak-proof Mignon-batteries. Insert the batteries according to the drawing on the bottom of the instrument. 2) Screw To open 1). 3) Socket for mains power Note: When using an external power supply, the batteries must be removed from the instrument. 4) Main switch Move switch in direction of the arrow to start the instrument. 5) Indicator With 3 scales. 5a) Scale number Corresponds to the number of the rotor used. 6) Battery-charge indicator (ON/OFF indicator) Ready status with light emitting diode display red. If the left LED flashes, change the battery. 7) Level During measurement, the instrument must be held horizontally. 4 Functional and Operating Elements 8) Tapped hole (1/4”) for rod to fit instrument onto a stand. 9) Clamp the measuring system is locked when this lever is pushed in the direction of the arrow. 10) Clamps for measuring cup (VT 01 only). 11) Drive shaft for rotor When mounting a rotor, lock the measuring system with the clamp 9); attach the threaded coupling of the rotor to the drive shaft and switch on the drive motor. The coupling will be screwed in automatically. To remove the rotor, turn it in a clockwise direction (the threaded coupling has a left-handed thread). 5 Measurement 3. Measurement 1 Lock measuring system with clamp 9). 2 Connect rotor and, if required, measuring cup. 3 Immerse rotor into the liquid up to the dip mark on the shaft. 4 Switch on the instrument, holding it in a horizontal position. 5 Release clamp 9). 6 Read the viscosity from the scale corresponding to the rotor. Measurements can be made in any chosen vessel, or in the measuring cups provided. The Thermo Haake measuring cups should be used for maximum reproducibility. The scale numbers given are only valid when using the cups provided and when Newtonian liquids are being measured. 6 Measurement 3.1 Measuring Method I The rotor is immersed in any available vessel. The distance between rotor and wall of the vessel should not be smaller than the diameter of the rotor. Advantage: The viscosity can be measured in the container where the sample is normally stored. After the test, only the rotor needs to be cleaned. Disadvantage: Suitable only for approximate measurements. 3.2 Measuring Method II (only VT 01) Measuring cup A is attached to the Viscotester and the liquid is measured in this cup. Advantage: Precise measuring conditions, reproducible at any time; temperature can be controlled by immersing the cup in a bath circulator (e.g. Thermo Haake -series); only approximately 400 ml of test substance required. 3.3 Measuring Method III (only VT 01) Measuring cup B – attached to the Viscotester – is immersed into the measuring substance. Advantage: Exact and easily reproducible measuring conditions; measurement can be made directly in any container. 3.4 Measuring Method IV (only VT 02) Measurements with cup 3 – temperature control possible in a bath circulator. Advantage: Exactly reproducible measuring conditions; only approximately 150 ml of test substance required; exact temperature control possible. 7 Measurement 3.5 Influence of the Temperature Viscosity is usually very dependant on temperature. This is why for all viscosity measurements the test substance should be exactly temperature-controlled, regardless of the type of viscometer used. If a specific constant temperature cannot be maintained all the time, it is necessary to record the temperature for each viscosity value, e.g. η 26.3°C = 160 mPas (i.e. viscosity at 26.3°C = 160 milli Pascal seconds). It is possible to determine the viscosity dependance on temperature by conducting viscosity measurements at two different temperatures. This enables the user to measure the viscosity at any temperature and calculate the corresponding viscosity value, going back to the reference temperature. Example: Room temperature could vary between 18°C and 24°C. The chosen reference temperature should be 20°C. 200 mPas were measured at 18°C and 170 mPas at 24°C. Simple Temperature Correction The temperature difference of 24–18=6°C. This corresponds to a viscosity difference of: 200 – 170 = 30 mPas. Viscosity Consequently, the viscosity changes by 5 mPas (cP) for every 1°C temperature change. It helps to plot the measured viscosity values on a chart (as shown in the example on the left). The viscosity of a sample measured at 20°C has a value of 190 mPas (cP). T(°C) Temperature 8 Measurement 3.6 Non-Newtonian Behavior Test results of Newtonian liquids (e.g. mineral oils, sugar solutions, glycerine), obtained with the Viscotester, can be compared with the results of other viscometers. Most liquids, however, change viscosity with the shearing conditions (which depend on the size and the design of the rotors, and their rotor speed). Test results of non-Newtonian liquids obtained by two different types of viscometers are usually not comparable. Such determinations require viscometers with variable shearing conditions, suitable for plotting viscosity curves or flow curves. For such purposes we recommend our Viscotester or the Rotovisco. Flow curves can be plotted automatically with the Rotovisco. 3.7 Reproducibility Two consecutive measurements under identical measuring conditions will not differ by more than ± 2 % of total range. 3.8 Accuracy of Measurements The absolute accuracy which can be obtained with the Viscotesters VT01 and VT02 depends on the rotor used. Rotors 1, 3 and 5: accuracy ± 7 % of total range; Rotors 2 and 4: accuracy ± 10 % of total range. These accuracies will be obtained if measurements are taken in the cups provided by Thermo Haake. 9 Information concerning the CE sign 3.9 Information concerning the CE sign Thermo Haake measuring and control instruments carry the CE sign which confirms that they are compatible with the EU guideline 89/336/EEC (electromagnetic compatibility). The tests are carried out according to module H (official sheet L380 of the European Community) as our quality assurance system is certified according to DIN / ISO 9001. It was tested according to the strict EMV test requirements of the EN61326-1/A1 (EMV requirements for electrical equipment for measuring technology, conduction technology and laboratory usage). This means it was tested for interference resistance and interference emission according to public low-voltage mains (household and commercial usage). The following basic standards were applied in detail: Interference resistance: EN61000–4–2 electrostatic discharge EN61000–4–3 electromagnetic fields EN61000–4–4 fast transients EN61000–4–5 surge voltages EN61000–4–6 wire–guided HF–signals EN61000–4–8 magnetic field of mains frequency EN61000–4–11 voltage drop/short–time interruption Interference emission: CISPR16/class B wire–guided interference emission CISPR16/class B radiated interference emission EN 61000–3–2 EN 61000–3–3 Voltage variations and flickering Over-compensation voltage flows The application in industrial and commercial (public mains) environments is thus possible. A declaration of conformity is supplied with the ordered unit on request. Our strict standards regarding operating quality and the 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 units which carry the CE sign such as monitors or analytical instruments can be affected if their manufacturers accept an interference (e.g. the flimmering of a monitor) as the minimum operating quality under electromagnetic compatibility conditions. For this reason we recommend you to observe a minimum distance of approx. 1 m from such units. 10 Technical Specifications 4. Technical Specifications Data on VT01: Motor: Rated voltage of motor: . 4.5 to 6.5 Volts Rotor: Rated speed of rotors: . . 62.5 min–1 ± 5% Dimensions: No. 3 4 5 D (mm) 45.1 +0/–0.3 78.0 ± 0.5 61.2 ± 0.2 h (mm) 47.0 +0.2/–0 46.0 ± 0.1 36.0 ± 0.1 Material: Rotor 3: . . . . . . . . . . . . . . . stainless steel Rotors 4 and 5: . . . . . . . . anodized aluminium Measuring Cup: Dimensions: Type Da (mm) Di (mm) h1 (mm) h2 (mm) A 90.0 ± 0.5 – 93.5 ± 0.2 75.5 ± 0.5 B 90.0 ± 0.5 30 93.5 ± 0.2 75.5 ± 0.5 Material: . . . . . . . . . . . . . . anodized aluminium Sample volume: . . . . . . . . 400 ml A standard Viscotester VT01 consists of: Basic unit VT01; three rotors and two measuring cups, as above; four batteries. 11 Technical Specifications Data on VT02: Motor: Rated voltage of motor: . 4.5 to 6.5 Volts Rotor: Rated speed of rotors: . . 62.5 min–1 ± 5% Dimensions: No. 1 2 3 D (mm) 24.00 ± 0.1 15.00 ± 0.05 45.10 +0/–0.3 h (mm) 53.0 ± 0.1 1.00 +0.05/–0 47.0 +0.2/–0 Material: . . . . . . . . . . . . . . stainless steel Measuring Cup: Dimensions: No. 3 D (mm) 52.6 ± 0.25 h (mm) 75.0 Material: . . . . . . . . . . . . . . stainless steel Sample volume: . . . . . . . . approx. 150 ml A standard Viscotester VT02 consists of: Basic unit VT02; three rotors and one measuring cup, as above; four batteries. 12 Optional Accessories 5. Optional Accessories Order No. 808–0703 808–0754 808–0719 808–0720 808–0716 808–0714 808–0715 808–0717 808–0718 808–0721 222–0036 808–0722 Subject to alterations Parts Support stand Mains power supply 220 V; 115 V Rotor 1 Rotor 2 Rotor 3 Rotor 4 Rotor 5 Cup A Cup B Cup 3 Battery charger, incl. 4 cells Ni-Cd. Extension shaft for VT02 (90 cm) Printed in Germany (FRG) 13 2.1.060.123–10.03 Terms of Rheological Measurements 6. Terms of Rheological Measurements Rheometrical measuring modes: Categorized into preset values: CD: Controlled Deformation Measuring mode for the determination of relaxation modulus. (Thermo Haake RotoVisco / RheoStress) CR: Controlled Rate Measuring mode, e.g. for the recording of flow curves and the analysis of thixotropy; here the shear stress reaction of the substance on a preset shear rate ramp is evaluated. (Thermo Haake ViscoTester / RotoVisco / RheoStress) CS: Controlled Stress Measuring mode e.g. for the examination of a sample’s structure or for the recording of flow curves in the very low shear rate range; here the deformation reaction of the substance on a preset shear stress ramp is evaluated. (Thermo Haake RheoStress) Categorized into signal forms: Steady Rotation: Creep/Recovery CS measuring mode to determine the viscous and elastic properties of a material, e.g. for the determination of the zero-viscosity or as a criterion of shelf life. (Thermo Haake RheoStress / RheoWave) Stress Growth/Decay CR measuring mode to determine the time behavior and steady state flow curves. (Thermo Haake ViscoTester / RotoVisco / RheoStress) Steady Rotation with ramps: Measuring mode where the stress changes over the time e.g. to determine a yield point or a dynamic flow curve (thixotropy loop). (Thermo Haake ViscoTester / RotoVisco / RheoStress) 14 Terms of Rheological Measurements Oscillating movement: OSC: Oscillation Measuring mode for the non-destructive determination of elastic and viscous material properties. Here e.g. the influence of the frequency by forced oscillating stress on the storage and loss modules (G’ and G”) can be investigated. The measuring data gained in the linear visco-elastic range allow conclusions on other physical quantities (e.g. molecular quantities for polymers) (Thermo Haake RheoStress / RheoWave) Flow properties regarding viscosity behavior: Newtonian: Property of substances where the viscosity will not change under shear rate and shear stress. (Thermo Haake Falling Ball Viscometer, System Höppler) Pseudoplastic: Property of substances where the viscosity will decrease under shear rate and shear stress. (Most common material behavior) Dilatant: Property of substances where the viscosity will increase under shear rate and shear stress. Thixotropic: Non-Newtonian substances where the viscosity decreases under shear (structure break-down). The substances will eventually regain their viscosity after the shearing has stopped. Rheopectic: Non-Newtonian substances where the viscosity increases under shear (structure build-up). The substances will eventually regain their viscosity after the shearing has stopped. (Rare phenomenon) Plastic: Property of non-Newtonian substances which only start flowing after being subject to a certain force (shear stress), i.e. after a certain yield point. The yield point strongly depends on external parameters like temperature and change rate of the acting force. Therefore, a ”practical” yield point is determined taking in account the environmental conditions specific for the application. (Measuring modes: CD, CS) (Thermo Haake ViscoTester 550 / RotoVisco1 / RheoStress) 15 Terms of Rheological Measurements Typical quantities of rheometry and rheology: Instrument quantities: Md Ω φ ω FN R, h, ... Measuring parameter: T p t – torque – angular velocity – rotation angle – angular velocity ( 2⋅π⋅f ) – normal force – dimensions of sensor – etc. – temperature – pressure – time – etc. Rheometrical quantities: τ – shear stress g – shear rate – deformation g N1, N2 – normal stress differences – etc. Rheological quantities: Material functions: η, η∗, η+, η– – viscosities Ψ1, Ψ2 – normal stress functions G – shearing modulus G*, G’ G” – dynamic shear moduli J – compliance J*, J’, J” – dynamic compliances – etc. Material parameters: η0 – zero viscosity τy – yield point Ψ10 – 1st normal stress coefficient – etc. 16