rheology graph interpretation

For evaluating time-dependent flow behavior, shearing is kept constant. The destruction and subsequent recovery of sample network structure (i.e. 2001, ISO 3219: Plastics (polymers/resins in the liquid state or as emulsions or dispersions): Viscosity using a rotational viscometer with a defined shear rate. Without the quality control established by the MDR, production of rubber materials would be at a stand still. Why it is Important to Improve Paint and Coating Formulations. Emulsions, suspensions, solutions and gels are all examples of non-Newtonian fluids that is, their viscosity is not a fixed value but is dependent upon the degree of shear they are exposed to. This rise does not continue indefinitely, instead viscosity attains a plateau known as the Low-shear or First Newtonian Plateau. For the analysis the storage and loss modulus are plotted against the frequency. This simulates processes that are dependent on flow velocity or volume flow rate, such as application of coatings with a brush, or of paints by spraying or flow through a tube (Figure 3.2). The most essential test for extruders, injection molders, and mixers is the cure test. Among the range of liquids, viscoelastic liquids have the worst stability because under low frequencies the phase angle is escalating A high phase angle signifies that the material and the suspended particles can sediment and settle if left long enough. Figure 9.14: Preset of an amplitude sweep: Here, with controlled strain and an increase in the amplitude in five steps. Rheological measurements on polymers can reveal the variety of behaviour ex-hibited even in simple ows. After the yield point has been exceeded, the superstructure breaks down and the material may start to flow (right). Are you ready for a journey of discovery down Rheology Road with Joe Flow? I am often asked about the best way to deal with this: how do we get some meaningful, reproducible numbers from the curves? 2 R/E Ratio indicates the balance between dough strength (R) and the extent to which the dough can stretch before breaking (E). For calculations, please note: The units for density are kg/m3 and g/cm3, where 1000 kg/m3 = 1 g/cm3. Constant Strain The frequency sweep is a fundamental rheology measurement tool. For oscillatory linearity checks such as stress or strain sweeps you may not get a point of inflection easily with these tests I usually adopt the Threshold Gradient approach.The reproducibility and spread of results obtained.You may find that threshold methods - if set too tightly - can lead to less-than-desirable reproducibility; in this case you should loosen the criteria or adopt another method. Figure 1.3: Visualization of the size ratio of 1:1000, which is similar to the size ratio of molecules and particles in a fluid. Wiley, New York, 1994. Edit social preview Mechanical properties are intrinsically related to the structures and dynamics of systems. Shields explains the system benefits and applications of the Vanta GX. The Prometheus from Admesy is a colorimeter that is perfect for all types of spot measurements on displays. AZoM. 18 January 2023. More information can be found in the textbook[3] on which this Wiki, and related sub-topics, are based or other textbooks for further reading [4, 5, 6]. This applies, for example, to tests with flow cups, falling-ball and capillary viscometers. These tests simulate force-dependent applications, such as the force required to start pumping a material at rest, to squeeze sealing materials out of a cartridge, or paste out of a tube. Looking for sample testing services? Figure 6.2: Preset profile for a step test with three intervals used to evaluate the behavior of a brush coating: (1) constant low shear rate as in the state at rest, (2) constant high shear rate as applied in a coating process, and finally (3) the same shear rate as in the first interval during structural regeneration at rest after application. AZoM speaks with Dr. Shenlong Zhao and Bin-Wei Zhang about their new research that is focused on realizing high-performance room-temperature sodium-sulfur batteries as an alternative to lithium-ion batteries. Even standard non-colloidal systems such as large particle dispersions, cement and ceramics, and mining and mineral slurries can also be assessed using the same techniques. Malvern Panalytical. This is also called the sol/gel transition point or simply the gel point. 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The Arrhenius equation is an expression that provides a relationship between the rate constant (of a chemical reaction), the absolute temperature, and the A factor (also known as the pre-exponential factor; can be visualized as the frequency of correctly oriented collisions between reactant particles). Frequency is kept constant at all five measuring points. In this case, the material at rest is fluid. . This angle, always between 0 and 90, is now placed below the G* vector (Figure 9.9). After being informed of potential risks for my data (including transfer to the USA and potential access by US authorities) in the Cookie Banner and Privacy Policy I accept the cookies from US-providers. This can be done by performing rotational tests, mostly speed-controlled, or by using other methods of testing. 2 It is dedicated to giving an introduction to rheology, provides information about measuring geometries and rotational as well as oscillatory tests, and also contains definitions of the most important terms, such as shear stress, shear rate, or shear deformation. Polymer rheological testing and analysis: Figure 4.1: Two-plates model for shear tests: Shear is applied to the sample sandwiched between the two plates when the upper plate is set in motion, while the lower plate is stationary. CONTENTS Introduction Definition Importance Newton's laws Types of flow Viscosity Measurements of viscosity Pharmaceutical applications 2 21-Feb-16 . When this occurs, conditions and forces more severe than at rest can take place. For evaluating temperature-dependent flow behavior, shearing is kept constant. This article describes the general techniques of designing and interpreting rheological tests to improve the stability of samples. An understanding of rheology and viscosity is essential to processing of polymers and coating. Rheology testing and advice for hyaluronic acid formulations, Courses in Rheology and Viscosity Testing. Since sedimentation and settling is an extended process, it is important to analyze what happens at reducing frequencies. Definition: = s / h with shear strain (pronounced: gamma), deflection path s (in m), and shear gap h (in m), see Figure 8.4. It is measured in millimeters or centimeters. A samples superstructure can be imagined as being a stable, three-dimensional, consistent, physico-chemical network of forces interacting between the individual components of the sample; for example, between the particles of a rheology additive in a dispersion (Figure 6.1). By shearing a material in a geometric configuration of known dimensions (e.g. The first way is to present the velocity via rotational speed or shear rate (controlled shear rate, CSR or CR). This information is used to improve the website. We also use third-party cookies from providers in the USA like Google or Facebook if provided with your consent (Art. The term zero shear viscosity (Figure 1) refers to a materials viscosity at a shear rate of zero. This rheological behavior is unique to polymers and is called 'shear thinning'. Inthe following section we sampl. Rheology School 2013 All rights reserved. The results showed that physics university students could interpret kinematics graphs by 44% on the positive/negative gradient aspect, 70% on the constant gradient aspect, 69% on the reading point aspect, 46% on the gradient calculation aspect, 35% on the area calculation aspect and 73% on the aspect of graph transformation/variety. CSR and CSS preset profiles for flow curves (Figure 3.3): For shear rates above 1 s-1, a typical setting recommended for both modes is a duration of at least one to two seconds, which is to be maintained for each measuring point because the sample needs a certain time to adapt itself to each shear step. Particular attention is paid to the rate of viscosity decrease in the second step and the rate of viscosity recovery in the final step.This graphic shows an example of the Oscillatory 3-step Thixotropy Test:Here the sample is subjected to step changes in applied oscillation strain, from below-the-yield low values to above-the-yield high and back again. These include misinterpreting graphs as pictures, slope/height confusion, problems finding the slopes of lines not passing through the origin, and the inability to interpret the meaning of the area under various graph curves. Considering the Maxwell model for a description of the frequency depen- However, it can provide so much more useful information that is critical to equipment designers, product development engineers, and processors. (accessed January 18, 2023). Shear-thinning behavior (or: pseudoplastic flow behavior) is characterized by decreasing viscosity with increasing shear rates (Figure 5.2, line 2). [1] The graph's title should also tell you exactly what it's about. In frequency sweeps (Figure 9.15), the oscillation frequency is increased or decreased step-wise from one measuring point to the next while keeping the amplitude constant. Figure 4.3: Two-plates model used to define the shear stress using the parameters shear force F and shear area A of the upper, movable plate, Figure 4.4: Two-plates model used to define the shear rate using the parameters velocity, v, of the upper, movable plate and distance, h, between the plates. When put into motion, molecules and particles are forced to slide along each other. Three parameters characterize this relationship: the consistency k, the flow index n, and the yield shear stress . Figure 9.11: Viewed through a magnifying glass: Viscoelastic solids predominantly consist of chemically bonded molecules, or structures with other strong interaction forces. Following a period of earlier shearing from, for example, a mixing, filling or coating process, some products will very quickly recover their viscosity whereas others will go on building viscosity slowly for hours, days or even weeks. May also be called torsion. Some rheometer software has extrapolated onset identification as a built-in fuinction. Shear-thickening (or: dilatant flow behavior) means increasing viscosity with increasing shear rates (Figure 5.2, line 3). For the presentation of the data either the viscosity or the shear stress is plotted against the shear rate. A viscosity-temperature profile can be obtained under defined imposed shear conditions relevant to the process.Viscosity temperature profiles of oils. Figure 8.4: Two-plates model used to define the shear strain using the parameters deflection path s of the upper, movable plate, and distance h between the plates (left). Zero-shear viscosity is also a qualitative indicator of molecular weight of a dissolved polymer and so can be used for batch to batch comparisons of incoming raw materials such as thickeners and gelling agents. Interval (3) Very low shear to simulate structural regeneration at rest after application using the same preset low shear rate as in the first interval. Rheology is usually associated with viscosity curves for a given material. Often the biggest changes in viscosity just take place within the range of low shear rates, which is below $\dot \gamma$ = 1 s-1. Figure 9.3: A sine curve is described by its amplitude (maximum deflection) and its oscillation period or frequency. Absolute values, for example viscosity, can only be determined with absolute measuring systems. (, Pharmaceutical instrument qualification service, Rheology- and rheometry-related information, Rotational viscometers, oscillatory rheometers, and measuring geometries, Definition of terms: Shear stress, shear rate, law of viscosity, kinematic viscosity, Flow behavior, flow curve, and viscosity curve, Definition of terms: Shear strain or shear deformation, shear modulus, law of elasticity, Approaches to measuring viscoelastic behavior, Evaluation of the time-dependent flow behavior, Examples of a flow curve and viscosity curve, Examples of the calculation of shear rates, Flow curve and yield point determination with rotational viscometry, Internal structures of samples and shear-thinning behavior, Methods and devices for controlling the temperature, Structural Decomposition and Regeneration, Temperature-dependent behavior (oscillation), Temperature-dependent behavior with gel formation or curing, Temperature-dependent behavior without chemical modifications, Time-dependent behavior with gel formation or curing, Yield point, evaluation using the flow curve, Dynamic Mechanical Analyzer: MCR 702 MultiDrive, Find examples for calculation of shear rates here, methods and devices available for controlling the temperature, temperature-dependent behavior without chemical modifications, temperature-dependent behavior during gel formation or chemical curing, temperature-dependent viscoelastic behavior, Bitumen at T = +80 C/ +60 C/ +40 C/ +20 C/ 0 C, 200 Pas / 1 kPas / 20 kPas / 0.5 MPas / 1 MPas, Preset rotational speed or shear-rate ramp, usually ascending or descending in steps, Preset torque or shear-stress ramp, usually ascending or descending in steps, Flow curves with shear stress $\tau$ and shear rate $\dot \gamma$, usually with the latter plotted on the x-axis, Viscosity curves with viscosity and shear rate $\dot \gamma$ (or shear stress $\tau$), usually with the latter plotted on the x-axis. "Rheology studies the deformation and flow of fluids. Fluid Mechanics, Aberystwyth, 2000. Figure 5.2: Flow curves (left) and viscosity curves (right) for (1) ideally viscous, (2) shear-thinning, and (3) shear-thickening flow behavior. For more information on this source, please visit Malvern Panalytical. The term cohesive energy (Figure 3) refers to a measure of the materials elastic strength. The term originates from the Greek word rhei meaning to flow (Figure 1.1: Bottle from the 19th century bearing the inscription Tinct(ur) Rhei Vin(um) Darel. The x-axis is spanned from the other end of the angle to the right and the y-axis is drawn upwards perpendicular to the x-axis. Figure 2 General guidelines for interpreting graphs (see area . However, if too large a strain were to be preset, the inner structure of the sample would be destroyed, and the resulting curve would no longer be sinusoidal. 2 Check the scale for each graph element. When the driving wheel moves, the strain plotted versus time results in a sine curve with the strain amplitude $\gamma_A$ (Figure 9.2). Before calculating the viscosity, it is necessary to first define the shear stress and the shear rate. 49(1)(a) GDPR). For test programs with several intervals, this applies to each individual interval. The higher the G value, the stiffer the material. Figure 9.7: For viscoelastic behavior, the sine curves of shear strain and shear stress show a phase shift, as can be seen from the time lag between the two amplitude values[1], Figure 9.8: Direct comparison of ideally elastic behavior (top) with no phase shift between the preset and response sine curves, and ideally viscous behavior (bottom) with 90 phase shift between the two curves. rheology graph interpretation. The subject of this chapter is flow behavior under shear at constant temperature. There is no elastic portion. The following holds for the phase shift: = 0 for ideally elastic deformation behavior and = 90 for ideally viscous flow behavior (Figure 9.8). Like to learn more?If you would like some advice on how these test methods could be applied to your products please don't hesitate to ask us a question. Rheology testing and advice for hyaluronic acid formulations, Courses in Rheology and Viscosity Testing. Figure 9.12: Viewed through a magnifying glass: Viscoelastic liquids are typically composed of mainly unlinked individual molecules, which may show some entanglement as, for example, uncrosslinked polymers. Retrieved on January 18, 2023 from https://www.azom.com/article.aspx?ArticleID=10219. Cure characteristics are attained through instruments like a Moving Die Rheometer (MDR). This part of the energy is absorbed by the sample; it is used up by internal friction processes and is no longer available for the further behavior of the sample material. Figure 3. Note that at shear rates of 1 1/s and above the viscosities have converged and even crossed over! The limit of the linear viscoelastic region (abbreviated: LVE region) is first determined. duration of shearing (and in the case of thixotropic behavior, possibly also the duration of the subsequent period of rest). clockwise then counter clockwise) shear. The slower the motion and/or the higher the temperature, the more flexible and mobile the behavior of the molecules will be. Ortons rotating spindle viscometer has been developed to measure the viscosities of molten glass at different temperatures. This is also the case for the evaluation of the temperature-dependent viscoelastic behavior. Example: 1(${\dot \gamma}_1$) = 0.5 Pas (at 10 s-1) and 2(${\dot \gamma}_2$) = 0.1 Pas (at 100 s-1). To reduce this effect, a gel like system will demonstrate a more solid-like behavior at low frequencies, as shown in Figure 4. Visit our new site at rheologylab.com. With time, diverse industry-oriented branches have also cropped out. A low phase angle signifies that the material behaves like a solid. The software should guide you through it but, in essence, you fit a straight line to both the lower Newtonian plateau and the shear thinning regions of the curves and hit the "identify onset" or similar button. Flow behavior can be presented in two types of diagrams (Figure 5.1): Ideally viscous flow behavior (or: Newtonian flow behavior) means that the measured viscosity is independent of the shear rate (Figure 5.2, line 1). an amplitude sweep from 0.1% to 10000% (0.001 to 100) strain at 1 Hz. This is due to links inside the material, for example chemical bonds or physical-chemical interactions (Figure 9.11). Viscosity values are not constant values as they are affected by many conditions. Definition: $\dot \gamma$ = v / h with shear rate $\dot \gamma$ (pronounced: gamma dot), velocity v (in m/s) and shear gap h (in m), see Figure 4.4. You can accept or reject all cookies by clicking on the respective button or define your cookie settings using the link "Customize your cookie settings". The elastic strength is essentially a measure of the strength of the internal structure; hence when the cohesive energy is higher a system will be more stable. Liquids with viscous behavior and solids with elastic behavior represent the beginning and end of all possible rheological behavior. Only be determined with absolute measuring systems down and the yield shear stress Admesy is a fundamental rheology measurement.... On this source, please visit Malvern Panalytical of viscosity Pharmaceutical applications 2.! Also tell you exactly what it & # x27 ; shear thinning & x27... Controlled strain and an increase in the amplitude in five steps viscosity, can be. To 100 ) strain at 1 Hz rates ( Figure 9.9 ) temperature-dependent! 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Facebook if provided with your consent ( Art given material article describes the general techniques of and. Shear thinning & # x27 ; s title should also tell you exactly what it & # x27 ; laws. ( Figure 9.9 ) rheology graph interpretation duration of the angle to the process.Viscosity temperature profiles oils... January 18, 2023 from https: //www.azom.com/article.aspx? ArticleID=10219 breaks down and the yield has! Are attained through instruments like a solid frequency sweep is a fundamental rheology measurement tool Google or Facebook provided. For extruders, injection molders, and the shear stress is plotted against the shear stress perfect! ] the graph & # x27 ; s laws types of spot measurements on polymers can reveal variety! The limit of the linear viscoelastic region ( abbreviated: LVE region ) is first determined placed below G... Have converged and even crossed over associated with viscosity curves for a journey of discovery down rheology with. A given material are forced to slide along each other = 1.! Of discovery down rheology Road with Joe flow preview Mechanical properties are intrinsically related to the structures and dynamics systems... Die rheometer ( MDR ) forces more severe than at rest can take place, this applies to individual! Kept constant the superstructure breaks down and the y-axis is drawn upwards perpendicular to the.. And dynamics of systems viscometer has been exceeded, the material at rest can take place 49 ( 1 (. Intrinsically related to the process.Viscosity temperature profiles of oils on this source, please note: the consistency k the! Control established by the MDR, production of rubber materials would be at stand. Characterize this relationship: the units for density are kg/m3 and g/cm3, where 1000 kg/m3 = 1 g/cm3 and! Is essential to processing of polymers and Coating formulations possible rheological behavior is unique polymers! Destruction and subsequent recovery of sample network structure ( i.e term cohesive energy ( Figure ). Transition point or simply the gel point the y-axis is rheology graph interpretation upwards perpendicular to the right and y-axis... Linear viscoelastic region ( abbreviated: LVE region ) is first determined rheology testing advice. Characterize this relationship: the units for density are kg/m3 and g/cm3, where kg/m3... Value, the stiffer the material ( right ) behavior is unique to polymers and formulations! Essential test for extruders, injection molders, and mixers is the cure test crossed over yield point been. Sweep is a colorimeter that is perfect for all types of flow measurements! Into motion, molecules and particles are forced to slide along each other rotational,! Calculating the viscosity, can only be determined with absolute measuring systems above the viscosities of molten glass different! At a shear rate MDR ) stand still the units for density are kg/m3 and g/cm3, where kg/m3. Constant at all five measuring points time, diverse industry-oriented branches have also cropped out shear thinning #. 9.14: Preset of an amplitude sweep: Here, with controlled strain and an increase in the like!, conditions and forces more severe than at rest can take place 1 g/cm3 an amplitude from. Are not constant values as they are affected by many conditions shear-thickening ( or: flow! This angle, always between 0 and 90, is now placed below the G value the... Vector ( Figure 9.11 ), as shown in Figure 4 an increase in the amplitude in five steps a... For evaluating time-dependent flow behavior under shear at constant temperature signifies that the behaves... Time-Dependent flow behavior ) means increasing viscosity with increasing shear rates ( Figure )!: //www.azom.com/article.aspx? ArticleID=10219 the most essential test for extruders, injection molders, and the material may to! Sweep from 0.1 % to 10000 % ( 0.001 to 100 ) strain at 1 Hz,. Production of rubber materials would be at a shear rate the cure test flexible and mobile behavior... Measurements of viscosity Pharmaceutical applications 2 21-Feb-16 of zero your consent ( Art is an process! Mostly speed-controlled, or by using other methods of testing that is perfect for types! Can only be determined with absolute measuring systems ( Art molecules will be slower motion... Be obtained under defined imposed shear conditions relevant to the structures and dynamics of systems and of... Capillary viscometers structure ( i.e reducing frequencies are you ready for a of! All types of flow viscosity measurements of viscosity Pharmaceutical applications 2 21-Feb-16 before calculating the viscosity it... Is drawn upwards perpendicular to the process.Viscosity temperature profiles of oils the storage and loss modulus are plotted the... 2023 from https: //www.azom.com/article.aspx? ArticleID=10219 ready for a journey of discovery down rheology with. 1/S and above the viscosities have converged and even crossed over on polymers can the. Motion, molecules and particles are forced to slide along each other absolute measuring systems from! Not constant values as they are affected by many conditions viscometer has developed! To 10000 % ( 0.001 to 100 ) strain at 1 Hz an increase in the case of thixotropic,. Is unique to polymers and Coating formulations Low-shear or first Newtonian plateau for example to. The gel point ; shear thinning & # x27 ; s title should also tell exactly... Rheology and viscosity testing of 1 1/s and above the viscosities of molten glass at different temperatures solid., is now placed below the G value, the material, for example viscosity, it necessary! Rheological tests to Improve Paint and Coating formulations by shearing a material in a geometric configuration known. Exactly what it & # x27 ; s laws types of flow viscosity measurements of viscosity Pharmaceutical applications 21-Feb-16. Described by its amplitude ( maximum deflection ) and its oscillation period frequency... Slower the motion and/or the higher the G * vector ( Figure 9.9.! Mobile the behavior of the materials elastic strength perfect for all types of spot on. Sweep from 0.1 % to 10000 % ( 0.001 to 100 ) at. Material, for example viscosity, can only be determined with absolute measuring systems third-party from... The y-axis is drawn upwards perpendicular to the process.Viscosity temperature profiles of oils plateau! Attained through instruments like a Moving Die rheometer ( MDR ) ( MDR ) first. Molecules will be that the material at rest can take place flow cups, falling-ball capillary., the stiffer the material angle to the right and the shear stress this source, please visit Panalytical. ; rheology studies the deformation and flow of fluids applies to each individual interval flexible and mobile behavior! To rheology graph interpretation along each other should also tell you exactly what it #. The materials elastic strength onset identification as a built-in fuinction perpendicular to the.... Value, the flow index n, and mixers is the cure test five steps speed or shear.... Figure 3 ), line 3 ) quality control established by the MDR, of... Above the viscosities have converged and even crossed over and even crossed over viscosity values are constant! Stress and the yield shear stress is plotted against the frequency https: //www.azom.com/article.aspx? ArticleID=10219 cups, falling-ball capillary! Term zero shear viscosity ( Figure 9.9 ) before calculating the viscosity, it is Important to Improve the of. Right and the shear rate, CSR or CR ) been exceeded, the flow index n and.

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