Name: calibration procedures for orthogonal superposition rheology
Uploaded: 2020-11-18T13:00:00.000+00:00
Duration: 8 min 43 s
Description: Watch this Scientific Journal Video about Calibration Procedures for Orthogonal Superposition Rheology at JoVE.com

Ran Tao bedankt sich für die Finanzierung durch das National Institute of Standards and Technology des US-Handelsministeriums im Rahmen des Zuschusses 70NANB15H112. Die Finanzierung von Aaron M. Forster erfolgte durch Zuwendungen des Kongresses an das National Institute of Standards and Technology.

<ol>
	<li>Macosko, C. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Rheology: principles, measurements, and applications. , (1994).</li><li>Larson, R. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> The Structure and Rheology of Complex Fluids. , (1999).</li><li>Vermant, J., Moldenaers, P., Mewis, J., Ellis, M., Garritano, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Orthogonal+superposition+measurements+using+a+rheometer+equipped+with+a+force+rebalanced+transducer.">Orthogonal superposition measurements using a rheometer equipped with a force rebalanced transducer.</a> Review of Scientific Instruments. 68 (11), 4090-4096 (1997).</li><li>Ferry, J. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Viscoelastic Properties of Polymers. , (1980).</li><li>Yamamoto, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rate-dependent+relaxation+spectra+and+their+determination.">Rate-dependent relaxation spectra and their determination.</a> Transactions of the Society of Rheology. 15 (2), 331-344 (1971).</li><li>Simmons, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+servo-controlled+rheometer+for+measurement+of+the+dynamic+modulus+of+viscoelastic+liquids.">A servo-controlled rheometer for measurement of the dynamic modulus of viscoelastic liquids.</a> Journal of Scientific Instruments. 43 (12), 887-892 (1966).</li><li>Tanner, R. I., Williams, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=On+the+orthogonal+superposition+of+simple+shearing+and+small-strain+oscillatory+motions.">On the orthogonal superposition of simple shearing and small-strain oscillatory motions.</a> Rheologica Acta. 10 (4), 528-538 (1971).</li><li>Schoukens, G., Mewis, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nonlinear+rheological+behaviour+and+shear-dependent+structure+in+colloidal+dispersions.">Nonlinear rheological behaviour and shear-dependent structure in colloidal dispersions.</a> Journal of Rheology. 22 (4), 381-394 (1978).</li><li>Zeegers, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+sensitive+dynamic+viscometer+for+measuring+the+complex+shear+modulus+in+a+steady+shear+flow+using+the+method+of+orthogonal+superposition.">A sensitive dynamic viscometer for measuring the complex shear modulus in a steady shear flow using the method of orthogonal superposition.</a> Rheologica Acta. 34 (6), 606-621 (1995).</li><li>Mewis, J., Schoukens, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanical+spectroscopy+of+colloidal+dispersions.">Mechanical spectroscopy of colloidal dispersions.</a> Faraday Discussions of the Chemical Society. 65, 58-64 (1978).</li><li>Lin, N. Y. C., Ness, C., Cates, M. E., Sun, J., Cohen, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Tunable+shear+thickening+in+suspensions.">Tunable shear thickening in suspensions.</a> Proceedings of the National Academy of Sciences. 113 (39), 10774-10778 (2016).</li><li>Gracia-Fern&#225;ndez, C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Simultaneous+application+of+electro+and+orthogonal+superposition+rheology+on+a+starch/silicone+oil+suspension.">Simultaneous application of electro and orthogonal superposition rheology on a starch/silicone oil suspension.</a> Journal of Rheology. 60 (1), 121-127 (2015).</li><li>Sung, S. H., Kim, S., Hendricks, J., Clasen, C., Ahn, K. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Orthogonal+superposition+rheometry+of+colloidal+gels:+time-shear+rate+superposition.">Orthogonal superposition rheometry of colloidal gels: time-shear rate superposition.</a> Soft Matter. 14 (42), 8651-8659 (2018).</li><li>Colombo, G., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Superposition+rheology+and+anisotropy+in+rheological+properties+of+sheared+colloidal+gels.">Superposition rheology and anisotropy in rheological properties of sheared colloidal gels.</a> Journal of Rheology. 61 (5), 1035-1048 (2017).</li><li>Jacob, A. R., Poulos, A. S., Kim, S., Vermant, J., Petekidis, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Convective+Cage+Release+in+Model+Colloidal+Glasses.">Convective Cage Release in Model Colloidal Glasses.</a> Physical Review Letters. 115 (21), 218301 (2015).</li><li>Jacob, A. R., Poulos, A. S., Semenov, A. N., Vermant, J., Petekidis, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Flow+dynamics+of+concentrated+starlike+micelles:+A+superposition+rheometry+investigation+into+relaxation+mechanisms.">Flow dynamics of concentrated starlike micelles: A superposition rheometry investigation into relaxation mechanisms.</a> Journal of Rheology. 63 (4), 641-653 (2019).</li><li>Moghimi, E., Vermant, J., Petekidis, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Orthogonal+superposition+rheometry+of+model+colloidal+glasses+with+short-ranged+attractions.">Orthogonal superposition rheometry of model colloidal glasses with short-ranged attractions.</a> Journal of Rheology. 63 (4), 533-546 (2019).</li><li>Tao, R., Forster, A. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=End+effect+correction+for+orthogonal+small+strain+oscillatory+shear+in+a+rotational+shear+rheometer.">End effect correction for orthogonal small strain oscillatory shear in a rotational shear rheometer.</a> Rheologica Acta. 59 (2), 95-108 (2020).</li><li>Schrag, J. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Deviation+of+velocity+gradient+profiles+from+the+"gap+loading"+and+"surface+loading"+limits+in+dynamic+simple+shear+experiments.">Deviation of velocity gradient profiles from the "gap loading" and "surface loading" limits in dynamic simple shear experiments.</a> Transactions of the Society of Rheology. 21 (3), 399-413 (1977).</li><li>Ewoldt, R. H., Johnston, M. T., Caretta, L. M., Spagnolie, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Complex Fluids in Biological Systems. Biological and Medical Physics, Biomedical Engineering. , 207-241 (2015).</li></ol>

Die vollständige Beschreibung der in diesem Dokument verwendeten Verfahren erfordert die Identifizierung bestimmter kommerzieller Produkte und ihrer Lieferanten. Die Aufnahme solcher Informationen sollte in keiner Weise als Hinweis darauf ausgelegt werden, dass diese Produkte oder Lieferanten von NIST empfohlen oder von NIST empfohlen werden oder dass sie notwendigerweise die besten Materialien, Instrumente, Software oder Lieferanten für die beschriebenen Zwecke sind.

In diesem Protokoll stellen wir ein detailliertes experimentelles Verfahren zur Durchführung von Viskositätskalibrierungsmessungen mit newtonschen Flüssigkeiten für eine kommerzielle orthogonale Überlagerungsrheologie mit einer doppelwandigen konzentrischen Zylindergeometrie vor. Die Kalibrierfaktoren, d. h. der primäre Endeffektfaktor C L und der orthogonale Endeffektfaktor CLo, werden unabhängig voneinander durch die Durchführung von Sweep-Tests mit kons...

Das Verständnis der rheologischen Eigenschaften komplexer Fluide ist für viele Branchen für die Entwicklung und Herstellung zuverlässiger und reproduzierbarer Produkte unerlässlich1. Zu diesen "komplexen Flüssigkeiten" gehören Suspensionen, polymere Flüssigkeiten und Schäume, die in unserem Alltag weit verbreitet sind, zum Beispiel in Körperpflegeprodukten, Lebensmitteln, Kosmetika und Haushaltsprodukten. Die rheologischen oder Fließeigenschaften (z. B. Viskosität) sind Schlüsselgrößen, die für die Festlegung von Leistungsmetriken für die Endverwendung und die Verarbeitbarkeit von Interesse sind, aber die Fließeigenschaften sind mit den Mikrostrukturen verbunden, die in komplexen Flüssigkeiten vorhanden sind. Ein herausragendes Merkmal komplexer Flüssigkeiten, das sie von einfachen Flüssigkeiten unterscheidet, ist, dass sie unterschiedliche Mikrostrukturen besitzen, die sich über mehrere Längenskalen erstrecken2. Diese Mikrostrukturen können leicht durch unterschiedliche Strömungsverhältnisse beeinflusst werden, was wiederum zu Veränderungen ihrer makroskopischen Eigenschaften führt. Die Entschlüsselung dieser Struktur-Eigenschafts-Schleife durch nichtlineares viskoelastisches Verhalten komplexer Fluide als Reaktion auf Strömung und Verformung bleibt eine herausfordernde Aufgabe für experimentelle Rheologen.
Die Rheologie der orthogonalen Überlagerung (OSP)3 ist eine robuste Technik, um diese Messherausforderung zu bewältigen. Bei dieser Technik wird eine oszillierende Scherströmung mit kleiner Amplitude orthogonal mit einer unidirektionalen primären stationären Scherströmung überlagert, was die gleichzeitige Messung eines viskoelastischen Relaxationsspektrums unter der auferlegten primären Scherströmung ermöglicht. Um genauer zu sein, kann die kleine oszillatorische Scherstörung mit Hilfe von Theorien in linearer Viskoelastizität4 analysiert werden, während die nichtlineare Strömungsbedingung durch die primäre stationäre Scherströmung erreicht wird. Da die beiden Strömungsfelder orthogonal und somit nicht gekoppelt sind, können die Störungsspektren direkt mit der Variation der Mikrostruktur unter der primären nichtlinearen Strömung5 in Beziehung gesetzt werden. Diese fortschrittliche Messtechnik bietet die Möglichkeit, Struktur-Eigenschafts-Verarbeitungsbeziehungen in komplexen Fluiden aufzuklären, um deren Formulierung, Verarbeitung und Anwendung zu optimieren.
Die Einführung der modernen OSP-Rheologie war nicht das Ergebnis einer plötzlichen Erleuchtung; Vielmehr basiert es auf jahrzehntelanger Entwicklung von kundenspezifischen Geräten. Der erste maßgefertigte OSP-Apparat stammt aus dem Jahr 1966 von Simmons6, und danach wurden viele Anstrengungen unternommen 7,8,9,10. Diese frühen kundenspezifischen Geräte leiden unter vielen Nachteilen, wie z. B. Ausrichtungsproblemen, dem Pumpeffekt (aufgrund der axialen Bewegung des Bobs zur orthogonalen Oszillation) und Einschränkungen der Instrumentenempfindlichkeit. Im Jahr 1997 modifizierten Vermant et al.3 den Force Rebalance Transducer (FRT) an einem kommerziellen separaten Motor-Wandler-Rheometer, der OSP-Messungen für Flüssigkeiten mit einem breiteren Viskositätsbereich als frühere Geräte ermöglichte. Diese Modifikation ermöglicht es dem Normalkraftaufnehmer, als spannungsgesteuertes Rheometer zu fungieren, das zusätzlich zur Messung der Axialkraft eine axiale Schwingung erzwingt. Vor kurzem wurden die für OSP-Messungen erforderlichen Geometrien nach der Methodik von Vermant für ein kommerzielles separates Motor-Wandler-Rheometer freigegeben.
Seit dem Aufkommen der kommerziellen OSP-Rheologie besteht ein wachsendes Interesse an der Anwendung dieser Technik für die Untersuchung verschiedener komplexer Flüssigkeiten. Beispiele hierfür sind kolloidale Suspensionen 11,12, kolloidale Gele13,14 und Gläser15,16,17. Während die Verfügbarkeit des kommerziellen Instruments die OSP-Forschung fördert, erfordert die komplizierte OSP-Geometrie ein tieferes Verständnis der Messung als andere rheologische Routinetechniken. Die OSP-Durchflusszelle basiert auf einer doppelwandigen konzentrischen Zylindergeometrie (oder Couette). Es verfügt über ein offenes oberes und offenes Bodendesign, damit Flüssigkeit zwischen den ringförmigen Lücken und dem Reservoir hin und her fließen kann. Trotz der Optimierung, die der Hersteller am Geometriedesign vorgenommen hat, erfährt das Fluid im OSP-Betrieb ein inhomogenes Strömungsfeld, geometrische Endeffekte und einen Restpumpenfluss, die alle zu erheblichen experimentellen Fehlern führen können. Unsere vorherige Arbeit18 berichtete über wichtige Endeffektkorrekturverfahren unter Verwendung von newtonschen Flüssigkeiten für diese Technik. Um korrekte Viskositätsergebnisse zu erhalten, sollten geeignete Endeffektfaktoren sowohl in primärer als auch in orthogonaler Richtung angewendet werden. In diesem Protokoll möchten wir eine detaillierte Kalibriermethodik für die rheologische OSP-Technik vorstellen und Empfehlungen für Best Practices zur Reduzierung von Messfehlern geben. Die in diesem Artikel beschriebenen Verfahren zum OSP-Geometrieaufbau, zur Probenbeladung und zu den OSP-Testeinstellungen sollten leicht für Messungen mit nicht-newtonschen Flüssigkeiten übernommen und übersetzt werden können. Wir empfehlen Anwendern, die hier beschriebenen Kalibrierungsverfahren zu verwenden, um die Endeffekt-Korrekturfaktoren für ihre Anwendungen vor OSP-Messungen an einer beliebigen Fluidklassifizierung (Newton oder Nicht-Newton) zu bestimmen. Wir stellen fest, dass die Kalibrierungsverfahren für Endfaktoren bisher nicht berichtet wurden. Das in diesem Artikel bereitgestellte Protokoll beschreibt auch eine Schritt-für-Schritt-Anleitung und Tipps zur Durchführung genauer rheologischer Messungen im Allgemeinen und die technischen Ressourcen zum Verständnis von "Rohdaten" im Vergleich zu "gemessenen" Daten, die von Rheometerbenutzern übersehen werden können.

<table><tbody><tr><td>Advanced Peltier System</td><td>TA Instruments</td><td>402500.901</td><td>Enviromental control device</td></tr><tr><td>ARES-G2 Rheometer</td><td>TA Instruments</td><td>401000.501</td><td>Rheometer</td></tr><tr><td>Brookfield Silicone Fluid, 12500cP</td><td>AMTEK Brookfield</td><td>12500 cps</td><td>Viscosity standard liquid</td></tr><tr><td>OSP Slotted Bob, 33 mm</td><td>TA Instruments</td><td>402796.902</td><td>Bob, upper geometry</td></tr><tr><td>OSP Slotted Double Gap Cup, 34 mm</td><td>TA Instruments</td><td>402782.901</td><td>Double wall cup, lower geometry</td></tr><tr><td>Pipette (1 &amp;ndash; 10 mL)</td><td>Eppendorf</td><td>3120000089</td><td>To load test materials</td></tr><tr><td>Pipette (100 &amp;ndash; 1,000 &amp;micro;L)</td><td>Eppendorf</td><td>3123000063</td><td>To load test materials</td></tr><tr><td>Pipette Tips (0.5 &amp;ndash; 10 mL)</td><td>Eppendorf</td><td>022492098</td><td>To load test materials</td></tr><tr><td>Pipette Tips (50 &amp;ndash; 1,000 &amp;micro;L)</td><td>Eppendorf</td><td>022491555</td><td>To load test materials</td></tr><tr><td>Spatula</td><td>VWR</td><td>82027-532</td><td>To load test materials</td></tr><tr><td>TRIOS</td><td>TA Instruments</td><td>v4.3.1.39215</td><td>Rheometer software</td></tr></tbody></table>

calibration procedures for orthogonal superposition rheology

Die Rheologie der orthogonalen Überlagerung (OSP) ist eine fortschrittliche rheologische Technik, bei der eine oszillierende Scherverformung mit kleiner Amplitude orthogonal zu einer primären Scherströmung überlagert wird. Diese Technik ermöglicht die Messung der Strukturdynamik komplexer Fluide unter nichtlinearen Strömungsbedingungen, was für das Verständnis und die Vorhersage des Verhaltens einer Vielzahl komplexer Fluide wichtig ist. Die rheologische OSP-Technik hat seit den 1960er Jahren eine lange Entwicklungsgeschichte, vor allem durch die speziell angefertigten Geräte, die die Leistungsfähigkeit dieser Technik hervorhoben. Die OSP-Technik ist jetzt kommerziell für die Rheologie-Community verfügbar. Angesichts des komplizierten Designs der OSP-Geometrie und des nicht idealen Strömungsfeldes sollten Benutzer das Ausmaß und die Quellen von Messfehlern verstehen. Diese Studie stellt Kalibrierverfahren mit newtonschen Flüssigkeiten vor, die Empfehlungen für Best Practices zur Reduzierung von Messfehlern enthalten. Insbesondere werden detaillierte Informationen über die Methode zur Bestimmung des Endeffektfaktors, das Probenfüllverfahren und die Identifizierung des geeigneten Messbereichs (z. B. Schergeschwindigkeit, Frequenz usw.) bereitgestellt.

Repräsentative Ergebnisse der Viskositätskalibrierungsmessungen an einem Silikonviskositätsstandard von 12,2 Pa s sind in Abbildung 5 und Abbildung 6 dargestellt. Beachten Sie, dass sowohl der primäre Endeffektfaktor als auch der orthogonale Endeffektfaktor für die Kalibrierungsläufe auf 1,00 eingestellt sind. Abbildung 5 zeigt die stationäre Scherviskosität und das Drehmoment als Funktion der Schergeschwindigkeit auf einer ...

Watch this Scientific Journal Video about Calibration Procedures for Orthogonal Superposition Rheology at JoVE.com

Calibration Procedures for Orthogonal Superposition Rheology

Wir präsentieren ein detailliertes Kalibrierungsprotokoll für eine kommerzielle orthogonale Überlagerungsrheologie-Technik unter Verwendung von newtonschen Flüssigkeiten, einschließlich Methoden zur Bestimmung des Endeffekt-Korrekturfaktors und Empfehlungen für Best Practices zur Reduzierung von experimentellen Fehlern.

Kalibrierverfahren für die orthogonale Überlagerungsrheologie

Orthogonal superposition (OSP) rheology is an advanced rheological technique that involves superimposing a small-amplitude oscillatory shear deformation ...

calibration-procedures-for-orthogonal-superposition-rheology

Research

JoVE Journal

Engineering

2.0K Aufrufe.  National Institute of Standards and Technology. Wir präsentieren ein detailliertes Kalibrierungsprotokoll für eine kommerzielle orthogonale Überlagerungsrheologie-Technik unter Verwendung von newtonschen Flüssigkeiten, einschließlich Methoden zur Bestimmung des Endeffekt-Korrekturfaktors und Empfehlungen für Best Practices zur Reduzierung von experimentellen Fehlern.

Serie: Calibration Procedures for Orthogonal Superposition Rheology

Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions

A rheometer system to measure the rheology of crude oil in equilibrium with carbon dioxide (CO2) at high temperatures and pressures is described. The system comprises a high-pressure rheometer which is connected to a circulation loop. The rheometer has a rotational flow-through measurement cell with two alternative geometries: coaxial cylinder and double gap. The circulation loop contains a mixer, to bring the crude oil sample into equilibrium with CO2, and a gear pump that transports the mixture from the mixer to the rheometer and recycles it back to the mixer. The CO2 and crude oil are brought to equilibrium by stirring and circulation and the rheology of the saturated mixture is measured by the rheometer. The system is used to measure the rheological properties of Zuata crude oil (and its toluene dilution) in equilibrium with CO2 at elevated pressures up to 220 bar and a temperature of 50 &#176;C. The results show that CO2 addition changes the oil rheology significantly, initially reducing the viscosity as the CO2 pressure is increased and then increasing the viscosity above a threshold pressure. The non-Newtonian response of the crude is also seen to change with the addition of CO2.

Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions

A method for measuring the rheology of crude oil in equilibrium with carbon dioxide at reservoir conditions is presented.

Messung der Rheologie des Rohöls im Gleichgewicht mit CO<sub&gt; 2</sub&gt; Bei Vorratsbedingungen

A rheometer system to measure the rheology of crude oil in equilibrium with carbon dioxide (CO2) at high temperatures and pressures is described. The ...

Forschung

Umwelt

Dielectric RheoSANS &#8212; Simultaneous Interrogation of Impedance, Rheology and Small Angle Neutron Scattering of Complex Fluids

A procedure for the operation of a new dielectric RheoSANS instrument capable of simultaneous interrogation of the electrical, mechanical and microstructural properties of complex fluids is presented. The instrument consists of a Couette geometry contained within a modified forced convection oven mounted on a commercial rheometer. This instrument is available for use on the small angle neutron scattering (SANS) beamlines at the National Institute of Standards and Technology (NIST) Center for Neutron Research (NCNR). The Couette geometry is machined to be transparent to neutrons and provides for measurement of the electrical properties and microstructural properties of a sample confined between titanium cylinders while the sample undergoes arbitrary deformation. Synchronization of these measurements is enabled through the use of a customizable program that monitors and controls the execution of predetermined experimental protocols. Described here is a protocol to perform a flow sweep experiment where the shear rate is logarithmically stepped from a maximum value to a minimum value holding at each step for a specified period of time while frequency dependent dielectric measurements are made. Representative results are shown from a sample consisting of a gel composed of carbon black aggregates dispersed in propylene carbonate. As the gel undergoes steady shear, the carbon black network is mechanically deformed, which causes an initial decrease in conductivity associated with the breaking of bonds comprising the carbon black network. However, at higher shear rates, the conductivity recovers associated with the onset of shear thickening. Overall, these results demonstrate the utility of the simultaneous measurement of the rheo-electro-microstructural properties of these suspensions using the dielectric RheoSANS geometry.

Here, we present a procedure for the measurement of simultaneous impedance, rheology and neutron scattering from soft matter materials under shear flow.

Dielectric RheoSANS - Gleichzeitige Interrogation von Impedanz, Rheologie und Kleinwinkelneutronenstreuung komplexer Fluide

A procedure for the operation of a new dielectric RheoSANS instrument capable of simultaneous interrogation of the electrical, mechanical and ...

Ingenieurwesen

Challenges in Rheological Characterization of Highly Concentrated Suspensions &#8212; A Case Study for Screen-printing Silver Pastes

A comprehensive rheological characterization of highly concentrated suspensions or pastes is mandatory for a targeted product development meeting the manifold requirements during processing and application of such complex fluids. In this investigation, measuring protocols for a conclusive assessment of different process relevant rheological parameters have been evaluated. This includes the determination of yield stress, viscosity, wall slip velocity, structural recovery after large deformation and elongation at break as well as tensile force during filament stretching.
The importance of concomitant video recordings during parallel-plate rotational rheometry for a significant determination of rheological quantities is demonstrated. The deformation profile and flow field at the sample edge can be determined using appropriate markers. Thus, measurement parameter settings and plate roughness values can be identified for which yield stress and viscosity measurements are possible. Slip velocity can be measured directly and measuring conditions at which plug flow, shear banding or sample spillover occur can be identified clearly. 
Video recordings further confirm that the change in shear moduli observed during three stage oscillatory shear tests with small deformation amplitude in stage I and III but large oscillation amplitude in stage II can be directly attributed to structural break down and recovery. For the pastes investigated here, the degree of irreversible, shear-induced structural change increases with increasing deformation amplitude in stage II until a saturation is reached at deformations corresponding to the crossover of G' and G'', but the irreversible damage is independent of the duration of large amplitude shear. 
A capillary breakup elongational rheometer and a tensile tester have been used to characterize deformation and breakup behavior of highly filled pastes in uniaxial elongation. Significant differences were observed in all experiments described above for two commercial screen-printing silver pastes used for front side metallization of Si-solar cells.

A protocol for a robust and application relevant rheological characterization of highly concentrated suspensions is presented. Silver pastes used for screen-printing application in solar cell production are employed as model systems.

Herausforderungen in rheologische Charakterisierung von hochkonzentrierten Suspensionen - Eine Fallstudie für Serigrafie Silberpasten

A comprehensive rheological characterization of highly concentrated suspensions or pastes is mandatory for a targeted product development meeting the ...

Longitudinal Measurement of Extracellular Matrix Rigidity in 3D Tumor Models Using Particle-tracking Microrheology

The mechanical microenvironment has been shown to act as a crucial regulator of tumor growth behavior and signaling, which is itself remodeled and modified as part of a set of complex, two-way mechanosensitive interactions. While the development of biologically-relevant 3D tumor models have facilitated mechanistic studies on the impact of matrix rheology on tumor growth, the inverse problem of mapping changes in the mechanical environment induced by tumors remains challenging. Here, we describe the implementation of particle-tracking microrheology (PTM) in conjunction with 3D models of pancreatic cancer as part of a robust and viable approach for longitudinally monitoring physical changes in the tumor microenvironment, in situ. The methodology described here integrates a system of preparing in vitro 3D models embedded in a model extracellular matrix (ECM) scaffold of Type I collagen with fluorescently labeled probes uniformly distributed for position- and time-dependent microrheology measurements throughout the specimen. In vitro tumors are plated and probed in parallel conditions using multiwell imaging plates. Drawing on established methods, videos of tracer probe movements are transformed via the Generalized Stokes Einstein Relation (GSER) to report the complex frequency-dependent viscoelastic shear modulus, G*(&#969;). Because this approach is imaging-based, mechanical characterization is also mapped onto large transmitted-light spatial fields to simultaneously report qualitative changes in 3D tumor size and phenotype. Representative results showing contrasting mechanical response in sub-regions associated with localized invasion-induced matrix degradation as well as system calibration, validation data are presented. Undesirable outcomes from common experimental errors and troubleshooting of these issues are also presented. The 96-well 3D culture plating format implemented in this protocol is conducive to correlation of microrheology measurements with therapeutic screening assays or molecular imaging to gain new insights into impact of treatments or biochemical stimuli on the mechanical microenvironment.

Particle-tracking microrheology can be used to non-destructively quantify and spatially map changes in extracellular matrix mechanical properties in 3D tumor models.

Längs Messung der extrazellulären Matrix Steifigkeit in 3D Tumormodelle mit Particle-Tracking Mikrorheologie

The mechanical microenvironment has been shown to act as a crucial regulator of tumor growth behavior and signaling, which is itself remodeled and ...

Biotechnik

Combining Microfluidics and Microrheology to Determine Rheological Properties of Soft Matter during Repeated Phase Transitions

The microstructure of soft matter directly impacts macroscopic rheological properties and can be changed by factors including colloidal rearrangement during previous phase changes and applied shear. To determine the extent of these changes, we have developed a microfluidic device that enables repeated phase transitions induced by exchange of the surrounding fluid and microrheological characterization while limiting shear on the sample. This technique is &#181;2rheology, the combination of microfluidics and microrheology. The microfluidic device is a two-layer design with symmetric inlet streams entering a sample chamber that traps the gel sample in place during fluid exchange. Suction can be applied far away from the sample chamber to pull fluids into the sample chamber. Material rheological properties are characterized using multiple particle tracking microrheology (MPT). In MPT, fluorescent probe particles are embedded into the material and the Brownian motion of the probes is recorded using video microscopy. The movement of the particles is tracked and the mean-squared displacement (MSD) is calculated. The MSD is related to macroscopic rheological properties, using the Generalized Stokes-Einstein Relation. The phase of the material is identified by comparison to the critical relaxation exponent, determined using time-cure superposition. Measurements of a fibrous colloidal gel illustrate the utility of the technique. This gel has a delicate structure that can be irreversibly changed when shear is applied. &#181;2rheology data shows that the material repeatedly equilibrates to the same rheological properties after each phase transition, indicating that phase transitions do not play a role in microstructural changes. To determine the role of shear, samples can be sheared prior to injection into our microfluidic device. &#181;2rheology is a widely applicable technique for the characterization of soft matter enabling the determination of rheological properties of delicate microstructures in a single sample during phase transitions in response to repeated changes in the surrounding environmental conditions.

We demonstrate the fabrication and use of a microfluidic device that enables multiple particle tracking microrheology measurements to study the rheological effects of repeated phase transitions on soft matter.

Kombination von Mikrofluidik und Microrheology während wiederholter Phasenübergänge rheologische Eigenschaften der weichen Materie ermitteln

The microstructure of soft matter directly impacts macroscopic rheological properties and can be changed by factors including colloidal rearrangement ...

Studying Large Amplitude Oscillatory Shear Response of Soft Materials

We investigate the sequence of physical processes exhibited during large amplitude oscillatory shearing (LAOS) of polyethylene oxide (PEO) in dimethyl sulfoxide (DMSO) and xanthan gum in water &#8212; two concentrated polymer solutions used as viscosifiers in foods, enhanced oil recovery, and soil remediation. Understanding the nonlinear rheological behavior of soft materials is important in the design and controlled manufacturing of many consumer products. It is shown how the response to LAOS of these polymer solutions can be interpreted in terms of a clear transition from linear viscoelasticity to viscoplastic deformation and back again during a period. The LAOS results are analyzed via the fully quantitative Sequence of Physical Processes (SPP) technique, using free MATLAB-based software. A detailed protocol of performing a LAOS measurement with a commercial rheometer, analyzing nonlinear stress responses with the freeware, and interpreting physical processes under LAOS is presented. It is further shown that, within the SPP framework, a LAOS response contains information regarding the linear viscoelasticity, the transient flow curves, and the critical strain responsible for the onset of nonlinearity.

We present a detailed protocol outlining how to perform nonlinear oscillatory shear rheology on soft materials, and how to run the SPP-LAOS analysis to understand the responses as a sequence of physical processes.

Studium der großen Amplitudengang oszillatorische Scherung aus weichen Materialien

We investigate the sequence of physical processes exhibited during large amplitude oscillatory shearing (LAOS) of polyethylene oxide (PEO) in dimethyl ...

Macro-Rheology Characterization of Gill Raker Mucus in the Silver Carp, Hypophthalmichthys molitrix

The silver carp, Hypophthalmichthys molitrix, is an invasive planktivorous filter feeder fish that infested the natural waterways of the upper Mississippi River basin due to its highly efficient filter feeding mechanism. The characteristic organs called gill rakers (GRs), found in many such filter feeders, facilitate the efficient filtration of food particles such as phytoplankton that are of a few microns in size.
The motivation to investigate the rheology of the GR mucus stems from our desire to understand its role in aiding the filter feeding process in the silver carp. The mucus-rich fluid, in a &#8216;thick and sticky&#8217; state may facilitate the adhesion of food particulates. The permeation and transport through the GR membrane are&#160;facilitated by the action of external shear forces that induce varying shear strain rates. Therefore, mucus rheology can provide a vital clue to the tremendous outcompeting nature of the silver carp within the pool of filter feeding fish. Based on this it was posited that GR mucus may provide an adhesive function to food particles and act as a transport vehicle to assist in the filter feeding process.
The main objective of the protocol is to determine the yield stress of the mucus, attributed to the minimum shear stress required to initiate flow at which irreversible plastic deformation is first observed across a structured viscoelastic material. Accordingly, rheological properties of the GR mucus, i.e., viscosity, storage, and loss moduli, were investigated for its non-Newtonian, shear-thinning nature using a rotational rheometer. &#160;
A protocol presented here is employed to analyze the rheological properties of mucus extracted from the gill rakers of a silver carp, fished at Hart Creek location of the Missouri River. The protocol aims to develop an effective strategy for rheological testing and material characterization of mucus assumed to be a structured viscoelastic material.

Macro-Rheology Characterization of Gill Raker Mucus in the Silver Carp, Hypophthalmichthys molitrix

This protocol presents a method to perform rheology characterization of mucus that resides on gill rakers (GRs) of the silver carp. Viscoelastic characteristics of GR-mucus, obtained by measuring viscosity, storage and loss moduli, are evaluated for the apparent yield stress to understand the filter feeding mechanism in GRs.

Makrorheologische Charakterisierung von Kiemen-Raker-Schleim im Silberkarpfen, Hypophthalmichthys molitrix

The silver carp, Hypophthalmichthys molitrix, is an invasive planktivorous filter feeder fish that infested the natural waterways of the upper Mississippi ...

Microtensiometer for Confocal Microscopy Visualization of Dynamic Interfaces

Adsorption of surface-active molecules to fluid-fluid interfaces is ubiquitous in nature. Characterizing these interfaces requires measuring surfactant adsorption rates, evaluating equilibrium surface tensions as a function of bulk surfactant concentration, and relating how surface tension changes with changes in the interfacial area following equilibration. Simultaneous visualization of the interface using fluorescence imaging with a high-speed confocal microscope allows the direct evaluation of structure-function relationships. In the capillary pressure microtensiometer (CPM), a hemispherical air bubble is pinned at the end of the capillary in a 1 mL volume liquid reservoir. The capillary pressure across the bubble interface is controlled via a commercial microfluidic flow controller that allows for model-based pressure, bubble curvature, or bubble area control based on the Laplace equation. Compared to previous techniques such as the Langmuir trough and pendant drop, the measurement and control precision and response time are greatly enhanced; capillary pressure variations can be applied and controlled in milliseconds. The dynamic response of the bubble interface is visualized via a second optical lens as the bubble expands and contracts. The bubble contour is fit to a circular profile to determine the bubble curvature radius, R, as well as any deviations from circularity that would invalidate the results. The Laplace equation is used to determine the dynamic surface tension of the interface. Following equilibration, small pressure oscillations can be imposed by the computer-controlled microfluidic pump to oscillate the bubble radius (frequencies of 0.001-100 cycles/min) to determine the dilatational modulus The overall dimensions of the system are sufficiently small that the microtensiometer fits under the lens of a high-speed confocal microscope allowing fluorescently tagged chemical species to be quantitatively tracked with submicron lateral resolution.

This manuscript describes the design and operation of a microtensiometer/confocal microscope to do simultaneous measurements of interfacial tension and surface dilatational rheology while visualizing the interfacial morphology. This provides the real-time construction of structure-property relationships of interfaces important in technology and physiology.

Mikrotensiometer zur konfokalen Mikroskopie Visualisierung dynamischer Grenzflächen

Adsorption of surface-active molecules to fluid-fluid interfaces is ubiquitous in nature. Characterizing these interfaces requires measuring surfactant ...

Characterizing Multiscale Mechanical Properties of Brain Tissue Using Atomic Force Microscopy, Impact Indentation, and Rheometry

To design and engineer materials inspired by the properties of the brain, whether for mechanical simulants or for tissue regeneration studies, the brain tissue itself must be well characterized at various length and time scales. Like many biological tissues, brain tissue exhibits a complex, hierarchical structure. However, in contrast to most other tissues, brain is of very low mechanical stiffness, with Young&#39;s elastic moduli E on the order of 100s of Pa. This low stiffness can present challenges to experimental characterization of key mechanical properties. Here, we demonstrate several mechanical characterization techniques that have been adapted to measure the elastic and viscoelastic properties of hydrated, compliant biological materials such as brain tissue, at different length scales and loading rates. At the microscale, we conduct creep-compliance and force relaxation experiments using atomic force microscope-enabled indentation. At the mesoscale, we perform impact indentation experiments using a pendulum-based instrumented indenter. At the macroscale, we conduct parallel plate rheometry to quantify the frequency dependent shear elastic moduli. We also discuss the challenges and limitations associated with each method. Together these techniques enable an in-depth mechanical characterization of brain tissue that can be used to better understand the structure of brain and to engineer bio-inspired materials.

We present a set of techniques to characterize the viscoelastic mechanical properties of brain at the micro-, meso-, and macro-scales.

Charakterisieren Multiskalige Mechanische Eigenschaften von Gehirngewebe mittels Rasterkraftmikroskopie, Schlag Einrückungen und Rheometrie

To design and engineer materials inspired by the properties of the brain, whether for mechanical simulants or for tissue regeneration studies, the brain ...

Neurowissenschaften

Rapid Viscoelastic Characterization of Airway Mucus Using a Benchtop Rheometer

In muco-obstructive lung diseases (e.g., asthma, chronic obstructive pulmonary disease, cystic fibrosis) and other respiratory conditions (e.g., viral/bacterial infections), mucus biophysical properties are altered by goblet cell hypersecretion, airway dehydration, oxidative stress, and the presence of extracellular DNA. Previous studies showed that sputum viscoelasticity correlated with pulmonary function and that treatments affecting sputum rheology (e.g., mucolytics) can result in remarkable clinical benefits. In general, rheological measurements of non-Newtonian fluids employ elaborate, time-consuming approaches (e.g., parallel/cone-plate rheometers and/or microbead particle tracking) that require extensive training to perform the assay and interpret the data. This study tested the reliability, reproducibility, and sensitivity of Rheomuco, a user-friendly benchtop device that is designed to perform rapid measurements using dynamic oscillation with a shear-strain sweep to provide linear viscoelastic moduli (G&#39;, G&#34;, G*, and tan &#948;) and gel point characteristics (&#947;c&#160;and &#963;c) for clinical samples within 5 min. Device performance was validated using different concentrations of a mucus simulant, 8 MDa polyethylene oxide (PEO), and against traditional bulk rheology measurements. A clinical isolate harvested from an intubated patient with status asthmaticus (SA) was then assessed in triplicate measurements and the coefficient of variation between measurements is &#60;10%. Ex vivo use of a potent mucus reducing agent, TCEP, on SA mucus resulted in a five-fold decrease in elastic modulus and a change toward a more &#34;liquid-like&#34; behavior overall (e.g., higher tan &#948;). Together, these results demonstrate that the tested benchtop rheometer can make reliable measures of mucus viscoelasticity in clinical and research settings. In summary, the described protocol could be used to explore the effects of mucoactive drugs (e.g., rhDNase, N-acetyl cysteine) onsite to adapt treatment on a case-by-case basis, or in preclinical studies of novel compounds.

The viscoelastic properties of mucus play a critical role in mucociliary clearance. However, traditional mucus rheological techniques require complex and time-consuming approaches. This study provides a detailed protocol for the use of a benchtop rheometer that can rapidly and reliably perform viscoelastic measurements.

Kalibrierverfahren für die orthogonale Überlagerungsrheologie

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